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NPRA97
NPRA97
50th Anniversary
NPRA Question and Answer Session on
Refining and Petrochemical Technology
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STERNFELS:
Good morning, ladies and gentlemen. It is really a
pleasure and an honor to be here to help celebrate a
momentous event for NPRA, for the refining industry,
the petrochemical industry which is now becoming part
of this process session, and with you as the participants,
the essential ingredient, in this historic day for the Q&A.
The NPRA, as you know, has had this session going
on nominally for 50 years. And I am here this morning
to first of all say that I am very proud to be invited to
celebrate with you what I think is one of the cornerstone’s
of the refining industry’s technology development, and
also a cornerstone of something else I would like to talk
about this morning. And that is it is a cornerstone for
the development of you and all of your peers.
One thing I have observed in my tenure at NPRA is
the fact that the people who sit in this room or rooms
like it, and have sat for years at these sessions, end up
being the folks that I ultimately deal with as presidents
of their companies, as vice presidents of refining compa-
nies in this country as well as those overseas. You are seen
as the up and comers in the industry. Otherwise, you
would not be here. I think it is important to note that
what makes this industry so great is the participation, the
quality and the dedication that this type of conference
illustrates best.
I am here this morning really to give you a history
INTRODUCTIONS lesson to some extent. I will be followed by Roger Hem-
minghaus who is the Chairman of the organization this
year and last, and he will talk more about some of the
FRITZ: fine people who have contributed to the success of this
Good morning, and welcome to the 1997 NPRA Ques- meeting and to the association’s endeavors. But this morn-
tion & Answer Session on Refining and Petrochemical ing I would like to mention to you the fact that the
Technology. NPRA is an organization that goes back even beyond the
I am Paul Fritz, Vice President of Engineering for 50 years we celebrate today. Very soon in the beginning
Pennzoil Products Company and the current Chairman of this next century we will be celebrating our 100th
of the NPRA Manufacturing Committee. On behalf of anniversary as an organization.
the Committee, I welcome you to the celebration of our I would like to go back and visit history for a moment
50th Q&A. because even though this kind of endeavor is 50 years
old, it has its underpinnings and its beginnings going
Our industry has come a long way over the past 50 back even farther.
years, surviving through some rough ups and downs. The The NPA, the National Petroleum Association, which
technology we have developed along the way has been was the first organization founded out of the companies
the backbone of our success, and the NPRA Q&A has in the Pennsylvania oil fields in 1902, was developed
played a key role in this process. As a former panelist not by staff, but by its members, by company people,
myself, I can appreciate all that goes into these sessions. executives and some of the independent refining compa-
I was proud then to be a part of it, and I am proud to nies who saw a need to have an opportunity to get together
participate today. and talk about the industry’s problems, to get to know
Before we begin, I am privileged to introduced Urvan their competitors and to basically become more
Sternfels, President of NPRA, who is here today in recog- acquainted with business as it was being done by other
nition of our 50th anniversary. Urvan has been with people, and to find out how they could learn how to do
NPRA since 1971, after receiving his law degree from it better themselves.
the Georgetown University Law Center. In March of I would like to read to you from a history book written
1982, he was appointed President of the association and by Fayette B. Dow, who was the second executive of the
has held that position ever since. Association.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 5
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The history reads that, ‘‘a meeting of representatives to me that he does not have a forked hoof anymore. He
of independent oil refiners was held in the private dining is an all right guy.’’
room of the Hotel Lincoln in the City of Pittsburgh on I then thought that if there were four refiners that had
June 17th, 1902 at 10:00 a.m.’’ The minutes read; ‘‘W.E. come to the realization that they had a lot in common,
Wall who had called the meeting was elected Chairman, and that they needed to get together and come to know
and Herbert Eaton, Secretary. The Chairman stated the one another better, that this was an all right organization.
objectives of the meeting. He requested that all those I went up to the desk and put down our money and
present give their views on the situation and suggest any joined; and that is why I joined, sir.’’
plan that would result in securing good to the independent I think this illustrates the point that this Association
oil refiners of Pennsylvania and Ohio.’’ has, as many others do, as its basis, the concept that
Well, that was the genesis, and you can already see camaraderie, getting to know one another better, has
that this was something that was moving towards how developed not only a strong relationship situation that
refiners could better themselves. Later in the history, there lasts for years, but it also has commercial value to the
is an interesting story about the Department of Manufac- companies. Because once you know someone, you are
ture of the association of the NPA which was very active willing to ask him questions, and willing to respond to
and taking quite an interest in technological activities. questions a lot more forthrightly and helpfully rather than
During the last two years the Department of Manufacture considering him the enemy.
had undertaken a program of cooperative engineering, Don O’Hara, my predecessor, the third guy in the
participated in by 15 to 20 member companies. A very chain, wrote part of the history of this Association and I
competent combustion engineer was employed to bring would like to read to you something about trade associa-
about boiler room economics; analysis of existing perfor- tions that he wrote in his history of the second 25 years
mance were made, changes in practice instituted. The of the Association.
history goes on to record how the beginnings of this type He wrote, ‘‘a trade association is organized to serve
of conference played a part in the development of the the commercial needs of the members and its activities
association. Over the years, the NPA and the WPRA are necessarily directed towards commercial affairs, but it
developed activities involving the sharing of technological is more than that. When men of goodwill meet together
interests or technical interests. There was also a camarade- for any common purpose, they will form friendships and
rie and a learning about each other as well as fierce compe- retain memories that are founded on more than commer-
tition, not only within the independent sector, but cial interests. Such a history deals with the formal actions
of the association and it is difficult to find the proper
between the independents and the majors if you will, the
chapter to recall the actions and personal relationships
‘‘House,’’ Standard Oil companies.
which grew out of these meetings.’’ I think that is
There was one very interesting rendition in this history
entirely true.
book that I will paraphrase for you. It was about an These memories are part of this organization’s history.
independent oil man who was an employee. He told his It is part of the fiber of this Association. It is part of this
employer, the President of his company, that he was going industry, and it is a part that I think will bear you fruit.
to go to a meeting of the Association to see what it was Your interests in learning about the technological aspects
like and his employer said, ‘‘well, that is fine, just do probably come first, but not followed far behind are those
not join.’’ that you develop with the people and the personnel that
The employee went to the meeting and he joined. you deal with, both in your plants and certainly with
When he returned, he reported this fact to his boss and your competitors.
his boss said, ‘‘well, that is interesting, but certainly you The other point I would like to leave you with is while
recall the fact that I told you not to join. Surely, you must the Association is honoring the 50th anniversary of this
have had a good reason for joining this organization.’’ activity, it is not only a demarkation line of where we
The fellow said, ‘‘well, I am not sure I have a good have come, it is also an indication of where we are going.
reason, but here is what happened.’’ I think the promise of the advances we see in this industry
I was at the meeting and I was standing near two will probably be enhanced by the relationships and the
refiners that happened to come upon one another. They exchange of information that comes about here in this
knew each other and they were talking about how they room.
saw old Bill the other day and discovered that he really There was one other aphorism in this book that I
does not have horns. thought you should know. It is simply that if each of the
I listened to this conversation and very soon thereafter refiners has one dollar and they exchange them, they still
I came upon another conversation between two others have one dollar. If two refiners each have one idea and
fellows in the business who said, ‘‘I remember old John. they exchange them, they each have two ideas. That is
I was talking to him the other day and it really occurred the equation that this conference is built upon.
6 Introduction
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I commend you for being here. I hope that you will city to hold this 50th anniversary. There is a lot of Q&A
take the time to look to your left and look to your right on the streets of New Orleans.
and look to the man or woman in front of you and the Over the past day, I have observed how proud the
one in back of you because I think when you do that NPRA staff is to be hosting this 50th celebration. I hope
you will find that in the future you will have looked at you too are proud of your individual and your company’s
somebody that is going to be one of the leaders of this contribution to the success of Q&A and the role it has
industry. I hope it is you. I am confident that you will played in the advancement of refining and petrochemical
see one of them in the leadership of this organization in technology.
the future. I thank you for being here. Please celebrate What is unique about Q&A is that it is truly a team
with us and enjoy the rest of this conference. Thank effort with input from diverse disciplines across the indus-
you again. try. Its success is dependent on contributions from com-
petitors, suppliers and customers and if successful, which
Q&A certainly is, we all walk away winners.
FRITZ:
Contributions to the Q&A start at the top. The senior
Thank you, Urvan. The history was very informative,
executives of your company have made a commitment to
and it occurred to me that there is a living history of
fund and manage NPRA and support its technical activi-
refining today, here within the audience. I would ask at
ties. They have also made a commitment to provide
this time all former panelists of the Q&A to stand and
resources to staff the committees responsible for the meet-
be recognized. Thank you. Would all former panel moder-
ings and provide participants and sign your expense
ators in the audience stand and be recognized? Thank you.
accounts. And we thank you, Paul, for your and the
Also with us today is Roger Hemminghaus, Chairman
manufacturing committee’s contributions and all those
and Chief Executive Officer of Ultramar Diamond Sham-
who serve on the screening committee.
rock and current Chairman of the NPRA. Roger started
Next there are the panelists. A good looking group.
his career in the refining and marketing industry as an
They not only spend 2 1⁄2 days on this stage, but countless
engineer for Exxon USA.
hours, much on their own time, preparing and editing.
In December of 1996, Roger assumed his current posi-
And we all know that during this preparation that their
tion following the merger of Diamond Shamrock and
normal jobs continue and pile up.
Ultramar Corporation. Prior to the merger, Roger was
The suppliers and vendors who serve our industry also
Chairman, Chief Executive Officer and President of Dia-
play a very major role as regular or associate members of
mond Shamrock.
the Association, they, too, fund and contribute to the
management of NPRA. Vendors offer panelists, literature
HEMMINGHAUS: and their expertise. Thank goodness they also sponsor
I am very proud of this opportunity to serve as Chair- events, including receptions and riverboat rides that make
man of the organization that lends its name to this session. a day of technical discussion much more palatable.
NPRA is the premier trade association for the hydrocarbon Members of the trade press have been instrumental in
processing industry. This is an exciting time to be in this advertising our meetings and they also report on key
industry and it is an exciting day to be here among the happenings and expand on the communications of the
leaders in this industry. proceedings. Based on the pile of paper out in front
The economy is good. Technology is changing rapidly. of my room this morning, they also provide jobs for
Our customers and shareholders are becoming much more paper workers.
demanding and we do not lack for regulatory challenges. Last but not least, there is, you, the participants. There
I spent all day Monday in a White House conference are those who have been around a long time and have
on climate change. It seems all of Washington is focused not been bashful to comment from the floor or engage
on global warming and the preparation for the interna- in vibrant conversation. Folks like Pete Andrews, Bob
tional negotiations on this subject in December in Kyoto, Davis, Chuck McCoy, Anders Nielsen and the late Bob
Japan. Just when we have spent tens of billions of dollars Flanders to name just a few. Others have provided occa-
and solved most of the Clean Air Act challenges, bet your sional but vital comments and questions. Then there are
money we will be handed some CO2 global warning those who may just have listened and learned and most
challenges in the future. Please keep your eye on this importantly brought back new concepts to their plants.
issue. It will impact our businesses and all of society. Throughout the history of this industry there have
The 50th anniversary of any organization or any event been monumental challenges at each crossroad. The future
is truly a momentous occasion. But the 50th anniversary promises even more. Perhaps the most important tool we
of a technical meeting like Q&A which has played such can use to reach our goals and remain viable is technical
an important role in the industry and to society as a whole teamwork. The best answers are found when people sat
is a truly remarkable event. And New Orleans is an exciting down and shared information and ideas. With innovative
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 7
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thinking, quality principles and teamwork we will make As Mr. Hemminghaus said, NPRA is proud to be
the quantum leap into the 21st century. recognizing the 50th Anniversary of Q&A. We thank all
I thank each and every one of you for your contribu- who have contributed so much over the years.
tions to NPRA and the Q&A. I am sure that this meeting I had an interesting conversation last night which
will serve as a major catalyst for technology development reflects the comaraderie which has developed within the
and sound operation of petroleum refineries and petro- industry over the years, which was also alluded to earlier.
chemical processing plants. But even if the outcome of The children of two of our long term screening committee
this meeting were to lead to only one idea, and that idea members, Art Suchanek and Marty Grosboll, were mar-
avoids an accident or tragedy, well, then I think it is well ried a few years ago. Last night they learned that they
worth the investment. were grandparents to be.
I must tell you that last night after conducting serious Throughout the next two and a half days, the panel
Association business over a scotch and dinner, Urvan will respond to questions submitted by industry and
Sternfels insisted that he and I patrol Bourbon Street to screened by a panel of experts. I will first call upon the
ensure your safety. Now, we must have been very early panelists to respond to each question and then open the
or you must have been very smart, because I did not see discussion to the floor. I encourage your active participa-
many of these name tags on the street. tion. When commenting, please state your name and com-
I hope you have a great conference and enjoy this 50th pany.
celebration. Please be careful, Urvan and I will not be Approximately two weeks after the meeting, a copy
out there tonight checking on your safety. Have a great of the comments will be mailed to each participant for
conference and enjoy the celebration. Thank you. corrections, additions, or deletions as deemed necessary.
After the return of the participants’ comments, they will
be printed and published in a hardback book by NPRA.
FRITZ: Each registrant at the 1997 NPRA Question and Answer
Thank you, Roger. I can report I had breakfast with Session on Refining and Petrochemical Technology will
Roger and Urvan this morning and they were much more receive the bound transcript of the meeting. The bound
chipper than I was. So, my conclusion is they are tougher transcription includes a subject index which identifies
than I am. pages where specific topics are covered. Some of the tran-
Before I introduce our moderator for the session, I scripts (i.e., 1990-94) are also available in electronic for-
would like to give recognition to your hardworking NPRA mat with search capabilities. Additional post 1994 years’
staff who really pull this meeting together and do the transcripts will be available electronically at some time in
countless small tasks that make the Q&A session a success. the future.
I would like to introduce the Technical Director of Again, NPRA encourages your participation. We also
the NPRA, Terry Higgins. Terry has held that position encourage you to take advantage of the hospitality pro-
since 1992, and will forever remain one up on me for vided throughout the week by the various suppliers.
the picture of me that he posted outside the Q&A session Experts are available to discuss their products and answer
last year when I was a panelist in 1975 with my mutton questions not adequately covered during the sessions. The
chop sideburns and long hair. I have yet to achieve any hospitality rooms offer an excellent opportunity to become
payback for Terry—but his time is coming! I would like better acquainted with those who serve our industry.
to introduce Terry Higgins. Background information on the panel can be found
in your program book and will be available in the back
section of the transcript.
HIGGINS: NPRA welcomes suggestions or criticisms for improve-
Thank you, and I welcome you all. I would like to ment of our program. Evaluation sheets are available for
thank Roger and Urvan for their time and also Baker this purpose or attendees can contact NPRA’s Washing-
Petrolite for the fine entertainment last night. ton office.
IMPORTANT NOTICE
The information and statements herein are believed to be reliable but are not to be construed as a warranty of
representation for which the participants assume legal responsibility. Users should undertake sufficient verification
and testing to determine the suitability for their own particular purpose of any information or products referred to
herein. NO WARRANTY OF FITNESS FOR A PARTICULAR PURPOSE IS MADE.
Nothing herein is to be taken as permission, inducement, or recommendation to practice any patented invention
without a license.
8 Introduction
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I. GENERAL PROCESSING
A. Treating and Desalting WILLIAM HEIMBAUGH (Howe-Baker Engineers, Inc.):
For those refiners who are considering specific gravity
Question 1. and viscosity reduction with naphtha, kerosene or similar
What new techniques have been successfully used to diluents, please keep in mind there may be a significant
enhance breaking tight emulsions in desalting heavy impact on electrical transformer requirements due to the
crudes? increased conductance of the diluted feedstock.
Question 2.
FOSTER: Has anyone encountered fouling of downstream preheat
At Lyondell-Citgo Refinery we process 17°API gravity trains when emulsion polymers were used in desalter
Venezuelan crude. We see very tight emulsions. Typical applications?
incoming salt ranges about 30-40 lb/mbs. Our desalted
crude content is about 1 lb/mb, so we run about 96-98 BINFORD:
percent salt removal efficiency. At both Lyondell-Citgo and Citgo Corpus Christi, we
We have two main crude stills that process 17°API fed our NOVUS technology for over three years in desalter
gravity crude. We have upgraded our older crude still and washwater with no detrimental impact on downstream
from a Petreco Low Velocity to a standard Howe-Baker fouling. When properly fed, emulsion polymers will not
design. We operate it with two single stage desalters opera- enter the bulk hydrocarbon phase for several reasons. First,
ting in parallel. The oil/water mixture enters from a hori- because of their very high molecular weight (⬎1 million),
zontal feed pipe below the third grid, but above the oil/ they are totally insoluble in hydrocarbon. Second, their
water interface. The new crude still, No. 537, has a Petreco charge densities make them totally insoluble in the crude
Bioelectric design with two stages in series. The oil/water oil. The only way that emulsion polymers can enter the
mixture is injected between the first and second grids and preheat train is with water carried over in the desalted
between the second and third grids. crude. Consistent desalter operation, especially in terms
We usually demulsify our injection into both the oil of dehydration, is key. Third, with normal water carry-
and desalter wash water utilizing Betz’s EMBREAK over, the amount of emulsion polymer leaving with the
(2W157) demulsifier. We actually see lower chemical desalted crude is negligible compared to both inorganic
usage and more consistent water separation from the paral- and organic foulants in the desalted crude.
lel design than we do from the series design and that is As an example, our NOVUS technology is typically
fed at 0.5ppm or less based upon crude charge. If 5%
due to the longer residence time which is about 40 minutes
desalter water is used in the desalter, this equates to 10ppm
versus the 20 to 25. It is also due to the greater disengag- NOVUS in the wash water. At 0.5% water carryover,
ing height. there will be 0.05ppm of NOVUS exiting the desalter.
There is nothing wrong with the Petreco desalter itself. Inorganic sediment content of even a relatively clean crude
It is just that operating it in series is more forgiving for would be 10 ptb. At a typical 60% desalter sediment
water slugs because of a longer residence time. In fact we removal efficiency rate this would equate to 4 ptb in the
intend to go to series operation on the other crude still desalted crude, or about 100 ppm. Thus the contribution
at the next opportunity. Our washwater rates run about
six to eight percent of crude rate, mixed valve settings
around 6 to 12 psi and we do a mud wash about once
a week for about 30 minutes at a time. Operating tempera-
ture runs about 285 to 300°F.
CAIN:
At the Delaware City plant, we have success using the
split feed technology to desalt heavy crudes. Betz patented
the split feed approach to desalting. It means injecting part
of the primary emulsion breaker into desalter washwater as
well as the crude charge. In addition to the crude, the
washwater contains emulsion stabilizers. Injecting the pri-
mary breaker into the washwater allows intimate contact
between these stabilizers and the chemical. As a result,
better dehydration is achieved.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 9
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to fouling from an well run desalter emulsion polymer is manufactured in Australia. However, their steel inlet
program would typically be 2000 times less than that of nozzles would eat out in about a week with that high
the inorganic particulate in the desalted crude. Insoluble pressure drop and the solids in the water. We got Coors
asphaltenes, another common foulant in crude preheat to make some ceramic nozzles for them. They had a life
trains, can exceed several weight percent, making these a of about six weeks. Fortunately the Vortoils could be
greater source of fouling as well. taken apart and refurbished in just a few hours.
Additionally, our NOVUS technology decomposes at There was a good paper written on the subject of
around 350°F. So in the hottest exchangers of the preheat desalting heavy crudes by Nalco, and presented at the
train, small oligamers are formed composed of primarily 1990 NPRA Annual Meeting. It is AM-90-18. Inciden-
carbon, nitrogen and hydrogen. This coupled with the tally, I find that these papers are a good source of informa-
negligible content in the desalted crude to begin with tion, and some of them turn out to be classics. I always
eliminates any contribution to preheat fouling. insist that my Technical Library gets a complete set of
the papers that are presented every year.
JAMES D. WEITH (Fluor Daniel):
To borrow a line from the panel member that suggested PAUL FEARNSIDE (Nalco/Exxon Energy Chemicals, L.P.):
that the best way to reduce NOx emission from an FCC We have had some very good successes lately using our
Regenerator was to shut down the Main Air Blower, I ultimar polymer technology. It is a new style polymer. It
would say that the best way to break a tight emulsion is does not require any inversion equipment. This has
not to make it so tight in the first place. Although that allowed people to run the very heavy crudes, typically
sounds a little glib, there is a point to it. heavy Venezuelan, without the need to reduce your
One of my fond memories that I will always treasure throughput by using diluent like that gentleman just pre-
as an Engineer was when I was given the opportunity by vious to me mentioned.
Unocal to supervise their Oil Shale Retort in Parachute,
Colorado. The Shale Oil (Kerogen) that was produced JIM ZEIBIN (Husky BPU Operations):
had a specific gravity of about .93, and contained a lot We have had fouling of the brine line due to polymer
of grit from the decrepatated mineral matrix of the Oil overfeed. The polymer was fed at over 3 ppm and as high
Shale (rock). In order to avoid plugging up the catalyst as 5 ppm. We have also seen polymer deposits in the
beds of the downstream hydrotreater, we needed to wash desalter during turnaround. The polymer addition also
that grit out of the Shale Oil. We used the same principle allowed a fine abrasive clay to be carried over to the
to accomplish this as is used for desalting Crude Oil. crude overhead and ended up in our overhead washwater
That is, wash the Shale Oil with water, and hope that resulting in seal damage of the washwater pumps.
the wetted solids will remain with the aqueous phase. As
you can imagine, a very tight emulsion can be made with ED ALVERSON (Baker Petrolite):
these ingredients. New chemistry has been developed to enhance the
We learned that it was easier not to make a tight treatment of heavy predominately solids laden, crudes,
emulsion than it was to break a tight emulsion. The lesson such as Cold Lake, Lloydminster and San Joaquin Valley.
here is to not run with the delta P across the mix valve Completed field trials have shown increases in salt removal
too high. Run with it just as low as you possible can to and decreases in BS&W, oil and brine.
still get the net effect. The best way to get good contact Also, secondary water clarification costs from the
between the water and the solids with a minimum pressure desalters and through the wastewater treatment plants
drop is to reduce the viscosity of the oil. This can be have been reduced. It has been our experience lately that
done by increasing the temperature of the oil, but it can many of the new techniques that we have employed in
only be increased to the point that you run out of amper- dealing with heavy crudes really are a return to closer
age across the grid. So if you are starting from scratch, adherence to the fundamentals of the desalting process.
you want to design in lots of horsepower for the grid. In the past, the lighter crudes which were run had a
Another method is to recycle a light oil stream such as little more margin for error in treating. What we find
naphtha to reduce the viscosity (and the specific gravity). with the heavier crudes is that we have lost that margin
However, this reduces the residence time of the oil, so for error. So we must pay closer attention to the desalter
you now have to make the vessel larger. process fundamentals in processing heavy crudes. This
In order to get clean Kerogen out the top of the Desalt- would include maintaining proper washwater mixing and
ers (we called them Deashers) we had to let some of the proper electrostatic field strength.
oil go out the bottom with the water and the emulsion In conclusion, we would say that the strategy for treat-
layer. We put in some Vortoils to further process the ing heavy oils must include three points. One is a proven
water stream, and to recover some of that Kerogen. The desalter design. The second is a properly and carefully
Vortoil is a high pressure drop hydroclone that I believe chosen chemical treatment that would consider the effects
10 General Processing
TOC/INDEX
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 11
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color body formation. Most downstream product tankage plant for at least one location, but there is limited interest
contains oxygen since nitrogen blanketing of these tanks from the cement plant’s application.
is uncommon. This introduced another source of oxygen
that can initiate color body formation. Some antioxidants JAMES MANN (Merichem Company):
can be added upstream of the Merox without adversely Clay life is very dependent on the amount of water
affecting the Merox unit itself. Choosing the proper type used, and soaps and surfactants carried over from the
of antioxidant is critical, however. If the Merox is not caustic washwater systems to the clay treater. We have
working and additives are not either, the only options are historical information that the life will range from 30,000
to either get the cracked stock out of the finished product barrels per ton of clay to 120,000 barrels per ton. A typical
or to make some processing changes upstream as Mr. life for a FIBER FILM娃 system is about 100,000 barrels
Joseck has already described. per ton. Functionally, the purpose of the clay is to remove
metal chelates that cause JFTOT failure, and surfactants
CYNDIE M. FREDRICK (Merichem Company): that cause WISM failure. Clay treaters have also been
Nitrogen compounds, sulfur compounds, diolefins, used for solids removal, color body removal, and residual
naphthenic acids, and phenolic compounds are possible water removal. Free water can significantly shorten the
color precursors in kerosene streams. In the presence of clay life. For this reason, the unit design usually places
air, the precursors would oxidize to color bodies such as the clay treater downstream of the salt dryer. The salt
coupled phenolics, polymers and color bearing nitrogen dryer reduces the freewater haze point by an average of
compounds. The problem could be minimized by apply- about 25°F below the salt tower inlet temperature. The
ing either a pre-treatment or a post-treatment. A caustic change of the bed is dictated by test failure, generally
pre-wash could be a good pre-treatment for naphthenic WISM or pressure drop across the clay treater. We are
acids, thiophenols and phenolic compounds, and an acid only aware of two methods of clay disposal. In some
wash process could be a good treatment for the removal of instances, the clay can be incinerated. The most common
nitrogen compounds. A more expensive hydroprocessing disposal option is land filling.
option may be considered. Question 5.
How do refiners handle outside feedstocks that are high
Question 4.
in sodium prior to an HDS and/or FCCU, i.e., an outside
What is the typical clay life experienced in jet fuel caustic
gas oil with high sodium levels?
treating systems? What clay disposal methods are used?
BARLOEWEN:
MALEK: The question asks how to deal with high sodium con-
The normal design criteria that we use for clay life is taining feedstocks to an FCCU or an HDS unit. A number
approximately 20,000 barrels per ton of clay. The life can of refiners have installed dedicated separate electrical
be extended significantly beyond this by proper clean up desalters to handle that situation. The people that are
of the feed before it goes to the clay treater. Generally, most inclined to do that are the ones that import a lot
clay treaters are preceded by a waterwash column, a salt of external feeds purchased on the open market. The main
dryer, or perhaps some electrostatic separation device. source of contamination is typically ballast water in the
The operation of these devices will affect your clay life. tankers or barges. There is a good reference in the August,
Frequent changeout of the washwater will improve clay 1996 issue of Hydrocarbon Processing entitled ‘‘Using
life. Desalting for FCC Feedstocks.’’
Concerning the type of feedstocks that are going
through the system, there are a certain amount of olefinic BINFORD:
materials which can be found in some jet fuel. These I agree with Mr. Barloewen’s comments that purchased
olefin compounds get caught up in the clay and cause feeds need to be desalted prior to downstream processing.
deterioration. If the purchased feed is going to be caustic washed or has
The typical disposal of spent clay is to industrial land- been caustic washed to remove H2S, this should be done
fills. prior to desalting the feed. Acid injection into the desalter
washwater can sometimes be beneficial to emulsion resolu-
JOSECK: tion. The acid will neutralize the caustic, break the emul-
We use clays for various treating processes including sion and transfer any organically bound sodium back into
jet fuel. We are able to dispose of spent clay as non- the desalter brine as an inorganic salt. If coker gas oil is
hazardous waste after steam stripping. We are able to used, the coke fines can be a problem. Coke fines have
dispose of clay due to low flash, low toxicity, low reactivity already been covered relative to fouling, but in a gas oil
and acceptable pH. We have approval for uses in a cement desalter, they can accumulate at the interface and wreak
12 General Processing
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havoc in terms of separating that emulsion. We know of attack, unlike some of the other stainless steels. But, of
one refiner that has installed a filter upstream of their gas course, if it is an existing unit, then what you have to do
oil desalter to remove the coke fines and help the desalter is employ a proactive program to ensure that you are
operate more effectively. controlling any acids that are forming or any results of
the acids which are formed.
FLETCHER:
A common way of handling high sodium feedstocks BINFORD:
is to segregate high sodium feedstocks in separate tankage Still the most common method being employed to
if available and then slip them into the unit into the deal with naphthenic acid in crudes processed on an
FCCU in a controlled manner. The second most common opportunity basis is dilution. Most refiners tend to start
method as the sodium is hitting the unit is to increase at a relatively low blend ratio of the naphthenic acid crude
fresh additions or fresh plus equilibrium catalyst additions to the other crudes in the blend. They blend to a total
until the sodium reaches acceptable levels in circulating acid number value and then increase the blend if corrosion
inventory. is not observed.
Utilizing high temperature corrosion inhibitors to treat
PAUL FEARNSIDE (Nalco/Exxon Energy Chemicals, L.P.): naphthenic acid corrosion in specific areas of the tower
One way we have been able to help people out on can allow the refiner to increase the percentage of naph-
purchased gas oils is to suggest injecting some condensate thenic acid crude beyond the ‘‘untreated maximum’’ while
or boiler feedwater with that cargo as it is offloaded into controlling corrosion. Since the type and the amount of
tankage along with a demulsifier. We have been able to naphthenic acid is crude specific, the refiner should also
achieve upwards of 50 percent removal of the sodium. be concerned with the interaction between the blends.
It is important to note that even with the same naph-
Question 6. thenic acid crude, corrosivity of the crude blend can be
What steps are refiners taking to handle increased quite different if the other crudes that are being blended
amounts of naphthenic acid crudes? Please comment on change such that the sulfur content changed. This is due
a) dilution, b) metallurgy, c) monitoring, and d) analyti- to the fact that some sulfur species act as a passivators
cal testing as they relate to the crude and vacuum units. against the naphthenic acid in the system. Steels have
Please comment, as well, on downstream units such as already been covered, but one important note is that
hydrotreaters, hydrocrackers, FCCUs, etc. 316L stainless steel needs to be specified, rather than 316.
Depending on the manufacturer, 316SS can drop below
ROMAN: the 2.5 percent minimum molybdenum content that you
Naphthenic acids are commonly found in crude oils need in order to protect against naphthenic acid.
from California, Romania, Russia, Texas and the Arabian Mr. Peterson already covered the boiling ranges of the
Peninsula. They are corrosive to carbon steel, 5 to 9 acids and where they end up. We have conducted detailed
chrome and type 304 stainless steel when the neutraliza- characterization of high naphthenic acid crudes and have
tion number is above .5 milligrams per gram and when been able to correlate naphthenic acid structure and
the temperature is above 430°F. Absence of scale and molecular weight to boiling range. This is evidenced in
grooving are characteristics of this type of corrosion. the processing unit by the distillation cuts that the acids
Crude assays should be utilized to determine the distribu- concentrate in.
tion of the naphthenic acids as they are often found to Monitoring of the product draws which are subject to
concentrate in particular cuts. naphthenic acid corrosion is the most common way to
An additional concern is their decomposition to form identify corrosion activity. A combination of high temper-
low molecular weight acids such as propionic and butyric ature electrical resistance probes and measurement of iron/
acids which will end up in the upper side cuts. Formic nickel ratios in the gas oils and the bottom streams is
acid has also been found in overhead liquids. Type 316 used, since corrosion can be very localized, thus evading
stainless steel with 2 1⁄2 percent molybdimun should be detection by the probes alone in many cases.
employed to obtain acceptable corrosion rates. It is also Spot checks of iron in the side draw streams can be
desirable to keep the fluid velocities as low as possible used to ‘‘flag’’ corrosion activity. We use a value of one
when this type of attack is present. ppm or higher in a product side draw a point of concern.
This serves as a red flag to do more extensive analysis.
TASKER: Finally, it is more common to see the acids concentrated
I agree with what has already been said. Obviously, if in the vacuum gas oil streams as opposed to the atmo-
you have a new unit, you can design accordingly. The spheric gas oils, although some of the very light naphthenic
use of 316 stainless is very good to employ because the acid crudes can contain acids that distill in the atmo-
molybdimun content does resist the naphthenic acid spheric tower.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 13
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CAIN: BINFORD:
Our primary solution to the problem has been dilution I would look at a couple of things. Number one, make
in a couple of our plants. However, in one plant we sure the metal wastage you are experiencing it is not
have upgraded the metallurgy of the hottest piping, above simply a velocity related effect. Also not knowing what
550°F in atmospheric heater, to 316L stainless steel. We the metallurgy is, you should determine if it is erosion,
closely monitor corrosion probes in the vacuum heater corrosion, naphthenic acid corrosion or possibly even sul-
outlet and vacuum gas oil draw. The HVGO draw is fidic acid attack depending on the metallurgy. Metallurgy
checked for total acid number and metals pickup rou- review, flow calculations and stream characterization
tinely. should provide enough information to properly diagnose
the problem. We have treated transfer lines chemically
FOSTER: with success and so that is certainly another option as well.
As has been said before, we make extensive use also of
316L and 317L stainless steels, both at our new crude R. RAJAMANI (Mangalore Refinery and Petrochemicals Ltd.):
still and our existing crude still, and 347 stainless in the I have two questions. We have some typical problems
heater tubes in our new vacuum meter. When we were of erosion on the crude heater outlet. There are six passes
considering the upgrade of one of our existing crude stills and six thermowells at the outlet, and also two thermowells
that had traditionally run a relatively sweet crude, the on the transfer line. Almost all of them, however, have
upgrade of metallurgy was so extensive to handle the been severely eroded during the last year of operation.
naphthenic acids that we chose instead to build a new We took it out and found that a large hole had been
crude still. It was cheaper to actually build a new crude made on each. The material was Monel. What is the best
still than it was to go through the revamp of the existing material to be used for this service? What is the experience
sweet crude still. of other refineries on such phenomenon?
We really keep an eye on any equipment in the 450 The second question is, we sometimes get crudes which
to or 750°F range rather, and especially the equipment are very acidic, pH of 3.5, possibly due to acid injection
in the 550 to 650°F range where naphthenic acid attack in the wells. We have also been advised by the Demulsifier
is most rigorous. supplier to maintain a pH of 5.5 to 6.5. Is there any
As far as monitoring is concerned, we perform periodic specific inspection procedure to be done on the desalters?
wall thickness monitoring in locations of high velocity,
turbulence, impingement and our laboratory routinely BINFORD:
measures total acid number on the crude and vacuum We have known several refiners that had thermo wells
unit product streams. Heavy vacuum gas oil is our heaviest in the heater outlet and suffered from erosion around
naphthenic acid bearing stream with TANs up to the thermo wells, especially if they were running highly
about three. naphthenic acid crudes. This is due to high velocities
created at the edges of the eddies behind the thermowells.
MICHAEL J. ZETLMEISL (Baker Petrolite): In most cases, they just elected to take the thermowells out.
Just indexing the problem by TAN has its difficulties. Also monel would not typically be selected for this service.
We have had experience with cuts that have identical
TANs and did not have anywhere near the same corrosi- FOSTER:
vity. One improvement on this is to look at weight percent I might talk a little bit about crude compatibility. The
naphthenic acids which looks at the carboxylic acid group gentleman said a minute ago the TAN of crude certainly
in particular. But even there, two crudes with the identical does not tell the whole story. There is also the issue of
carboxylic acid content will not necessary have the same crude compatibility.
corrosivity. People now postulate that this has something We were very concerned about crude compatibility
to do with the structure of the acids. Other than that, early on because we were in a mode of operating with
our experience closely follows what the panel and others some Venezuelan crudes and also running some of our
have said. We have been successful also in using high traditional crudes at the same time. So we did extensive
temperature inhibitors. corrosivity testing with mixtures of Venezuelan crudes
and various sour crudes and found that the mixtures
ELKIN CARMONA CUADROS (EcoPetrol): themselves are much more corrosive sometimes than either
According to this, we have a lot of corrosion/erosion crude by itself, no matter what the TAN number was.
problems in our topping units in the transfer line to the There may be some value in doing that in your case
atmospheric tower. Have you any experience with this? as well, in looking at the specific crude mixtures that you
Could you recommend any operation practice for minim- are running and trying those crude mixtures and some
izing this? In any case, could you recommend a special of the cuts from those crude mixtures in combinations
metallurgy? of various metallurgies. It is not a well understood science
14 General Processing
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yet. It is getting more well understood all the time. But crudes. This question is a bit confusing. I suspect that
until that time, we have a lot of testing to do for specific the person submitting this question is equating high naph-
crude combinations that we are going to be running. thenic acid containing crudes to a high naphthene concen-
tration in the distillates. We do not see this relationship
BINFORD: in the crudes that we run.
Regarding the question on acid and the pH in the
effluent water for the desalters, we have had experience ROMAN:
where we have had effluent water from desalters running Insofar as the relationship does hold, we have run
down in pH’s of 2 or 3, and not seen significant corrosion naphthenic crudes that have naphthenic acids in them.
in the desalter shell. That was in California, however, and The only problem we have had is that occasionally the
our determination there was that the acids were weak cetane number of the diesel cut is low. We have had to
organic acids that were depressing the pH. Therefore, we add cetane improver when we run those crudes.
did not see any major corrosion. If it is truly a strong
mineral acid, I would suspect that you would see corro- TASKER:
sion. The first thing I would do is go upstream to the In the Canadian upgrading complex where the feed
crude supplier, and put a stop to the use of strong mineral typically has higher naphthenic acid content, there does
acids in the upstream production. not appear to be any issues relative to the kerosene and
diesel quality. They appear to be relatively unaffected.
PAUL FEARNSIDE (Nalco/Exxon Energy Chemicals, L.P.): These products are hydrotreated also.
You cannot go with any one specific analyses or process
AMANDA HOWERTON (Merichem Company):
parameter change, be it dilution or whatever. You have
to look at all of them. One of the things that we do is Merichem has considerable experience using the fiber
we not only look at the TAN number, we look at the film contactor technology to treat kerosene and diesel
sulfur content and the sulfur species involved. We also streams derived from high naphthenic acid crudes. Kero-
do something we call the NAT, naphthenic acid titration. sene treatment typically includes caustic washing, water
We are able to look at the crude, do our testing on it washing, salt and clay to produce jet fuels. Properties
and are able to tell the customer which specific problem that are affected are acid number, copper strip corrosion,
they are going to see before they even run the opportu- WISM, TOT, sodium, calcium and haze. For stove oil,
nity crudes. diesel and heating oils, a caustic wash and salt dryer
are typically sufficient when fiber film contactor systems
are employed.
DAVID SLOAN (The M.W. Kellogg Technology Company):
One non-traditional application that a number of refin- Question 8.
ers are studying is to send the ATBs to a deasphalter for What are the critical parameters measured to assess the
gasoil separation and recovery at temperatures that are naphthenic acid corrosiveness of crude oils, such as
below the threshold for naphthenic acid corrosion. The TAN, sulfur, etc.?
acids are then decomposed in the downstream conver-
sion processes. BINFORD:
This was fairly well covered I think when we discussed
Question 7. Question 5, both from the panel and several good com-
Please poll the panel as to whether or not they are having ments from the floor. But just to quickly summarize the
problems maintaining kerosene and diesel quality when critical parameters that we feel need to be measured: total
processing high naphthenic acid crudes. If so, how are acid number, some form of a naphthenic acid number
they solving these problems? to look at naphthenic acid specifically, the amount and
different types of sulfur in the crude and the relationship
CAIN: between those sulfur compounds and the naphthenic acid.
Our main experience with high naphthenic acid crudes Finally, characterizing the naphthenic acids relative to
has been Main Pass crude. We notice that when charging their distillation profile. This is a critical element because
more than 6 percent of main pass, the kerosene developed it can give you an idea of where the naphthenic acids will
a tea colored tint and the diesel develop a yellow tint. end up thus allowing you can make a judgment as to
This problem cleared up once hydrotreated and presented whether or not the metallurgy in a given area is going to
no problem with the finished product quality. withstand the napthenic acids.
HENKE: FOSTER:
We do not experience problems maintaining kerosene I spoke just a moment ago of the crude compatibility
and diesel quality when processing high naphthenic acid issues with high sulfur crudes. We are interested in getting
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 15
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at this answer and other answers regarding naphthenic had put a new supply line into service for the MDEA
acid attack more thoroughly. We are participating in an and apparently had some pipescale or other dirt get into
industry sponsored effort with CLI International, centered the system. We setup some pretty tight emulsions in the
in Houston. If you are interested, you can give them a two-phased separation. The continuous phase was the
call and see if you want to participate. This group is MDEA in this contactor. We used some silicone antifoam
investigating the corrosivity of different crudes, with a which gave us temporary relief. The one thing that helped
special emphasis on naphthenic acid bearing crudes. us out a little longer term was to move the level to where
One of its goals is to discern which species of the there was a level tap in the tower and we drew off the
naphthenic acid family is most corrosive. So there is a lot emulsion offending layer and dirt through that tap and
more learning currently going on in this area. that gave us a little more permanent solution.
Question 9. S.N. PURI (Indian Institute of Petroleum, Dehradun, India):
In our LPG Merox unit, we are experiencing frequent When an LPG stream is treated with aqueous NaOH
carryover of caustic with LPG in the RSH extractor even solution, some entrainment of caustic is possible unless
at lower than design LPG flow rates. What could be additional facilities are provided. The treated LPG from
the reason for this carryover? Please suggest methods the over head of the extractor usually contains on an
to minimize. average less than 5 ppmw sodium. However in case of
upset, such as fall of column pressure, much more caustic
FOSTER: can be entrained. Therefore, installation of a knock out
We have had some problems dealing with caustic carry- drum at the overhead of the extractor should be considered
over, and I can relate some of the problems we have had as a safety option. From this vessel, the treated product
and why we have had them. The main reason we have may be passed through a sand filter coalescer to reduce
had problems is because of extractor tray fouling due to the amount of entrained caustic to less than 1 ppmw.
thiosulfate salts. This compound is formed when you have
a feed that is high in H2S that contacts the circulating CYNDIE M. FREDRICK (Merichem Company):
caustic and produces sodium bisulfide. It is then subse- The treating unit licensor should provide a low carry-
quently oxidized in the caustic regenerator. over design by utilizing the proper technology. Some of
Once the level of this salt reaches saturation in your the design features of a FIBER FILM娃 Contactor system
extractor, it tends to precipitate out in your extractor. that help minimize carryover are concurrent flow with
The symptom of this is a dark black appearance of caustic. the hydrocarbon, minimal mixing, and low pressure drop.
Another symptom is your extractor stops extracting and A proper system design should guarantee caustic carryover
you begin to carry over caustic. That is what happens to us. specifications of less than one ppm as sodium.
Taking the equipment out of service and subjecting it The experience Merichem has had with caustic treating
to a mild citric acid wash usually clears the equipment, over the years has shown us several operating factors that
but the best prevention, best solution is to keep H2S out can affect caustic carryover. High recycle rates have a
of the feed to begin with. You need to go further upstream, tendency to cause carryover problems. High caustic
probably to your fluid units or cokers to really address strength also increases the chance that carryover will occur.
the H2S issue. But properly designed units come with a Another factor that may lead to carryover is fluctuations
prewash that has a weak caustic stream that knocks out in pressure and/or flow. Caustic temperature and caustic
most of the H2S or virtually all of your H2S before it level are also variables that should be monitored.
enters your extractor area.
We are working to correct the problem this year. We EDWARD SMITH (UOP):
did not design our system with the proper prewash. We The panelists and participants have addressed many of
are correcting that problem this year on one of our extrac- the key points. UOP agrees that caustic carry-over from
tors and the next year on the other. an LPG Merox extractor can be due to salt deposition
on the active area of the trays, the presence of a foaming
CAIN: system, possibly caused by carryover from the upstream
The only thing I have to add is that temperature in amine system, or fluctuating operating pressures. The
the LPG Merox should be about 100°F and entrainment corresponding solutions to these problems are: circulating
increases with decreased temperature. The lowest practical caustic maintenance (strength, % spent, etc.), prevention
operating temperature is 70°F, according to UOP. of amine carryover, and proper pressure control of the
unit. As with any type of unit, excessively high throughput
PETERSON: relative to design capacity can also be a problem source.
We had seen something in our LPG MDEA contactor One additional and very important item is that the
which might relate to possible problems here as well. We extractor trays are specified to be seal welded so that they
16 General Processing
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are leak tight. Before commissioning, the trays are leak S.N. PURI (Indian Institute of Petroleum, Dehradun, India):
tested and repaired if necessary. There have also been Caustic carryover problem from the hydrocarbon prod-
cases where after many years of service, leaks developed uct in the Merox treater can be solved by any of the
in the trays that impacted extractor hydraulics. Once following methods:
repaired, extractor performance was restored. ● Using sand coalescer, caustic carryover can be
UOP has designed over 400 units for LPG type feed. brought down to about 1 ppmw. Properly sized sand
Please contact us directly to discuss a specific problem. filter can eliminate caustic carryover appreciably.
● New Merfining FIBER-FILM娃 technology—Mer-
Question 10. ichem Co. has developed a sweetening process using
What is the best way to separate the carried over sodium/ a proprietary FIBER-FILM娃 bundle to achieve inti-
caustic from the hydrocarbon product in a Merox treater? mate contact between hydrocarbon feed and caustic
solution. FIBER-FILM娃 bundle comprises long
continuous small diameter fibers placed in a pipe.
SAMUELS: The caustic solution wets the fibers creating a large
In looking at this question, the panel was not sure interfacial area. The hydrocarbon stream flows as a
whether we were talking about LPG treaters here or fixed continuous phase through the fibre bundles. The
bed. So we will answer both. For LPG Merox treaters, treated hydrocarbon stream contains minimal caus-
to separate caustic from the LPG, UOP recommends a tic carryover.
downflow sand filter. It has been our experience with
olefin treaters, for example that this is very effective. We AMANDA HOWERTON (Merichem Company):
drain caustic water on a regular basis and we do not have There are two approaches to resolve a problem involv-
problems in the coalescers upstream of the alky feed dryers. ing caustic carryover. The first approach is to minimize
For kerosene Merox treaters, we do see some problems the amount of caustic that is carried over in the hydrocar-
with caustic hydrocarbon separation in the waterwash bon by identifying process parameters or improperly
vessels. We believe the root cause here is due to a high designed or applied equipment which may be causing the
pH in the water wash. If you get up around a 12 pH, problem. Possible causes of high caustic carryover are
this will cause a separation problem and some emul- vigorous mixing producing emulsions, high caustic to
sion problems. hydrocarbon ratios, high hydrocarbon rate, insufficient
We tried two solutions. One was a more frequent hydrocarbon caustic separation tankage, high viscosity of
change out of the water, but that was not very effective caustic due to an increase in concentration.
due to the water wash alkalinity. So we have actually Another approach would be to add equipment to sepa-
injected a salt, MKP, monopotassium phosphate as a rate the caustic and hydrocarbon or to coalesce entrained
buffer to reduce the pH and that seems to be effective. caustic. A water wash system can also be added. Another
option to consider is a nonmixing mechanism such as
FUSSELL: that produced in a FIBER FILM娃 Contactor.
We also use sand filters on our LPG Merox units. Question 11.
Another thing that you need to consider is your disulfide What problems are associated with using ammonia
oil off of your Merox. You will have caustic carryover instead of caustic to oxidize mercaptans in gasoline and
into that stream as well, and you need to be careful about kerosene? What have been the results, and how have
where you put it. these problems been solved? What is the impact of H2S
in concentrations less than 5 ppmw?
CHARLES T. ORLANDO (Pall Corporation):
Caustic carryover can be readily reduced down to less MALEK:
than 0.5 parts per million sodium by the use of a new UOP has successfully applied its caustic free Merox
technology, high efficiency coalescer, especially when the process on a number of applications, both in gasoline and
IFT values go very low, down in the 1.5 dynes per centime- kerosene. The process is basically similar to the Merox
ter range. process using caustic, but ammonia is used instead of
caustic as the alkali source. The reactor beds are pre-
impregnated with specialized Merox catalysts to accom-
JIM STONE (Louisiana Dept. of Environmental Quality): modate both applications.
If this is a jetdeck unit, there is a weephole that is A problem that has been of concern to this technology
sometimes under the downcomer. If it goes to the tray is the disposition of the aqueous ammonia waste. There
below, you can be jetting material into the downcomer is free ammonia in the aqueous waste water stream that
and flood the tower. is drawn from the unit. Also some ammonia organic
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 17
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18 General Processing
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Question 14.
Is any refinery co-processing crude and condensates? Is
this causing any crude heat exchanger fouling problems?
If yes, how is it tackled?
BINFORD:
We have seen and still are seeing several refiners co-
process crude and condensates. Depending on the conden-
sate and crude composition, either minimal or severe
fouling has been observed. Severe fouling has been most
common when condensates were blended with highly
asphaltenic crudes. The most effective solution is proper
feed stream characterization which usually includes blend
studies to ensure that the asphaltenes in the base crude
blend will not precipitate with the amount of condensate
that is being blended. It is important to note that as the
temperature of the crude is increased through the preheat
What apparently is happening is the ammonia is neutraliz- train, the asphaltenes will become less soluble in the blend.
ing the organic acid based NACE inhibitor. So if you do a blend study at room temperature, we would
We have since used a different H2S agent, a BetzDearb- suggest that the maximum condensate be set 15 or 20
orn product. It is far more expensive than ammonia but percent below what the blend study predicts as the ‘‘theo-
it allows us to cut back dramatically the amount of NACE retical maximum.’’ This will prevent you from getting
inhibitor in the pool. into a problem in the hot train of the exchangers. If
We may have also seen some tank particulate and tank economics dictate that higher percentages of condensates
corrosion problems dealing probably back to the H2S and should be run, chemical antifoulant programs can help
ammonia and we’re working with BetzDearborn at this to disperse the asphaltenes through the preheat train.
point to try to resolve those issues. Once you get past the crude furnace and the condensate
is distilled overhead, the asphaltenes will usually stay in
Question 13. solution through the rest of the system.
Has any refinery tried injecting a stream of H2 into the
MALEK:
crude feed prior to the first crude preheat exchanger to
Condensates are routinely run commingled with crude
mitigate fouling problems that are mainly associated
oil. However, it is very infrequent that a significant
with auto-oxidation reactions?
amount of condensate can be added to an existing crude
operation because condensates tend to have much higher
BINFORD: yields of distillate and naphtha. They tend to overwhelm
We have not heard of any refinery injecting hydrogen the overhead condensing system, tower diameter, and
into the crude feed in an attempt to mitigate polymeriza- heater capacity if you are trying to maintain throughput
tion of unsaturated components. There are several reasons in the unit at anywhere near original design capacity.
why this probably would not be practical. As far as fouling, in addition to the asphaltene precipita-
Number one, most crude units are not designed to tion phenomenon that was previously discussed, we have
recover the hydrogen. In most U.S. refineries today the seen some of the sour condensates that are produced from
value of hydrogen would be such that you certainly would the Canadian gas production which have extremely high
not want to lose it into your fuel gas. levels of sulfur. Some of it even appears in a free form.
Number two, crude units are not operated at sufficient This material can cause fouling in the heat exchanger
temperatures and pressures to saturate the double bonds train and aggravate fouling and corrosion. This may be
without the presence of a catalyst surface. So, even if what this question is alluding to. But on the whole, con-
hydrogen was injected it is unlikely that it would really densates are handled with a minimal amount of fouling
have an effect. Somebody did suggest putting some cata- in most operations.
lyst into the front of the crude unit and letting it run down
the line, but we did not think that was very practical either. B. Lube Oil Manufacturing
Number three, it is unlikely that the crude preheat
exchangers would be optimized for two-phase flow if you Question 15.
did inject hydrogen, and that may very well throw you What type of catalysts are refiners using when hydrotreat-
into a pressure drop limit somewhere along the preheat ing waxes (slack and hard waxes) for color improvement?
exchanger train. Are there any new developments?
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 19
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20 General Processing
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performance both affect light neutral oil volatility. Modifi- It is not economical to produce Group II base stocks
cations to improve the wash and stripping section perfor- with solvent extraction due to the very high yield losses
mance are usually less costly than modifications to the experienced in extraction in order to reduce aromatic
vacuum column. content as opposed to extraction to increase viscosity
index.
Question 17. Our current base oils contain 15-25 percent aromatics.
What saturate levels are refiners targeting in their fin- Most of these are monoaromatics and this makes it diffi-
ished base oils? From what type of refinery feedstocks cult to reduce aromatics via solvent extraction. A C25
are these produced? monoaromatic has a distribution coefficient with furfural
that is very similar to that of a C25 naphthene or even a
JOSECK: C 25 paraffin. Increasing treat rates to remove these
For light viscosity neutrals, depending on the applica- monoaromatics also removes an unacceptable amount of
tion, we are targeting a minimum of 90 percent saturates naphthenes and paraffins.
for passenger motor oil applications for the Group II Hydrocracking processes are able to minimize this yield
base oil specification. We are currently processing Myan, loss by saturating the aromatic rings and also by cracking
Appalachian, East Texas and North Louisiana crudes higher boiling range material down into the base stock
using either all hydroprocessing or extraction and hydro- cut to replace some of the components that have been
processing technology. The API recognizes two groupings, cracked to diesel and lighter material. As ILSAC GF3
(Group I and Group II) of conventional base oils in the volatility standards are adopted, we would expect that
API 1509 publication, Engine Oil Licensing and Certifi- only GF2 stocks will be used in the lighter multigrade
cation Systems, Fourteenth Edition, December 1996. engine oils such as 5W30 and 10W30.
The specifications are for the two groups, group one, Solvent refined Group I stocks will be used for heavy
less than 90 percent saturates, group two, greater than 90 duty engine oils and other higher viscosity single grade
percent saturates. Group I base oils are typically produced passenger car motor oils.
utilizing the solvent extraction technology. Group II base
oils are typically produced using hydrocracker technology. FOSTER:
Both processes produce base oils satisfactory for lubricant I will just add that some refineries are looking at the
compounding, blending. inclusion of very high volatility index oils, over 1120, to
Our refineries utilize a variety of paraffinic crudes to boost overall saturate levels as the result of performance
produce both groupings of base oils. The specific crude of their base oils. Mr. Roman covered the hydroxy vapor-
oil feed stocks dictate the process technology necessary ization, dewaxing and so forth.
to produce base oils. The saturate level a particular refiner Conventional solvent extraction will only be satisfac-
chooses is based on what they can produce utilizing their tory for a few select crudes. Otherwise, severe hydrorefin-
refinery hardware as well as what markets they intend to ing must be used.
supply. All oil formulations do not require Group II
base oils. Question 18.
What is the normal, average consumption (losses) of
NMP in a lube extraction process? How are the products
MALEK: of decomposition of NMP dealt with? Do these products
I agree with those comments. The group two specifica- play a role in corrosion within the unit? Are there any
tions that are proposed primarily relate to oxygen stability. recommended chemical treatments that reduce/elimi-
One of the areas of controversy is that the very low nate the corrosion? Does anyone have a program that
aromatics content or the high saturates content may actu- cleans or renews the solvent either internal or external
ally impede the effectiveness and solubility of additives. to the extraction unit?
ROMAN: JOSECK:
Group I lube stocks are defined as having more than The average loss of NMP in the lube extraction unit
10% aromatics, and Group II lube stocks are defined as is less than 0.1 lb per mbbls. The NMP solvent is recovered
having 10% or less aromatics. Group II stocks have higher by distillation from the extract and raffinate. We have
boiling points at a given kinematic viscosity than Group not identified any products of decomposition from the sol-
I stocks and as a result are able to meet the new lower vent.
volatility requirements which the engine manufacturers In the NMP unit, the corrosion rates are extremely
are demanding. They also have better oxidative and ther- high in the extract recovery section, particularly in high
mal stability characteristics. Their only downside is their velocity areas. The corrosion rates are low in the raffinate
poor solvency for soot which is a problem in diesel engines. recovery section indicating a corrosion relationship
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 21
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between the solvent, extract, and the extract recovery like we may be able to effectively deal with both through
section. We have been using a chemical corrosion treat- a different chemical treatment.
ment program for years with favorable results.
The filming and neutralizing chemical treatment is CAIN:
targeted at specific hot corrosion areas, typically areas We lose about one gallon of solvent per 10,000 barrels
with high velocities in the extract section. We have also of charge oil. Corrosion is controlled with soda ash injec-
upgraded metallurgy using hastelloy C威 in the high corro- tion to maintain the desired pH. Soda ash is injected in
sion areas, although this is extremely expensive. the extract mix surge vessel.
We recently increased the number of chemical addition
points and the total chemical injection rate for the protec- CHARLES HARRISON (Bechtel):
tion of additional high corrosion areas. Upon increasing I agree in general with the comments, including the
the chemical feed, fouling occurred in several towers. The mechanical losses as well as the process losses. If you have
fouling was identified as thermal decomposition of the a well maintained and well operated plant, we are aware
filming and the neutralizing amines. We are in the process that you can achieve losses of 10 ppm by volume based
of switching to Betz chemicals based on improved bench on charge rate. The decomposition products of NMP are
thermal decomposition testing. organic acids. Bechtel recommends neutralization of these
acids with soda ash solution. If left unneutralized, these
acids definitely play a role in the unit corrosion. This
BINFORD: corrosion usually occurs in the hot areas such as heater
I’ll add some comments to Mr. Joseck’s answer on tubes and heater outlet transfer lines and in areas of high
some of the things that we did to choose the chemical turbulence such as trays and in pumps.
that he has just switched to. We assume that by cleaning and renewing the solvent,
The goal of Pennzoil’s research program was to increase which is the third part of that question, that you mean
the run length of the unit by a factor of two. As Mr. removing the organic acids and/or products of neutraliza-
Joseck said, the real problem with the neutralizer program tion from the NMP. We do not know of any program,
was that the previous program was reacting with the degra- nor do we know of any refiner who attempts to clean or
dation acids. The salts of those acids were corrosive as renew the NMP. We do recommend neutralization. The
well as being insoluble in the NMP, thereby causing a neutralization products are removed in the extract and
fouling problem as well. do not build to unacceptable levels in the unit.
A product that we developed provided equal corrosion
protection to the program that was used previously and V.K. KAPOOR (Indian Institute of Petroleum):
significantly lowered fouling potential on the bench. At Although my concern is not related to this particular
this point, we have been applying the new product in the Question 18, I believe the refractory index is the reason-
unit for about six weeks. We are feeding the corrosion able method for the final lube quality control rather than
inhibitor into the extract column bottoms and into the BI. Is there any experience available for using online
flasher overhead. Coupons installed in the dryer side draw instrument?
vapors have just been pulled at the end of week five. This
area has historically seen the most aggressive corrosion in JOSECK:
the system. The first set of readings on these coupons We are using online refractive index in the hydro-
indicate that corrosion rates have been cut in half, from cracker, but not in the NMP unit.
15-20 mils per year down to about 9 mils per year. Corro-
sion probes installed in the flasher overhead have held
at historic rates of less than one mil per year on the C. Solvent Deasphalting
new program.
Fouling in the flasher bottoms loop, the area that has Question 19.
historically limited unit run length due to fouling, is Are new technologies being developed for the processing
being monitored with a deposition coupon installed in of heavy solvent deasphalter bottoms? Has anyone been
the flasher bottoms piping feeding the extract stripper. able to produce a stable asphaltene/water emulsion or
This coupon was also pulled at the end of week five and dispersion?
showed no indication of fouling. We are also installing
a split stream filter, which was designed for this area to JOSECK:
monitor buildup of foulants in the system. We will have We have developed an emulsion formulation for a
additional data from that slip stream filter shortly. resinous asphalt with as much as 40 percent oil as a multi-
Based on these initial results, we do see a correlation component blend. The product is marketed as a road
between corrosion and fouling in the unit and it looks dust suppressant called Pennz Supress 威 D. A significant
22 General Processing
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amount of information is available on the Internet for new technologies are being developed and implemented
asphalting emulsions. There is a manufacturing associa- in tray systems?
tion for asphaltic emulsions called the Asphalt Emulsion
Manufacturing Association. HENKE:
There have been significant developments in fraction-
TASKER:
ation tray technology in the past several years. Two key
A number of years ago we performed plant tests, and
developments are active area enhancements and inlet area
with the data from those tests we produced some case
enhancements. Each of these technologies can be applied
study estimates of routing the solvent deasphalter bottoms
without major welding modifications to the fractionator.
to an H-Oil unit. The tests actually showed that a quality
Active area enhancement technologies, incorporating
fuel oil could be produced from the high conversion
small fixed or movable valves can typically increase the
bottoms from the H-Oil unit. To date, however, we
vapor handling capacity of conventional trays by up to
have not had a customer sufficiently interested and with
30 percent.
sufficient capital to invest in this unique scheme. How-
Inlet area enhancement technologies utilizing the area
ever, we did issue a paper on this a few years ago.
underneath the downcomer to increase the vapor handling
To answer the other part of the question about the
capacity, can increase the vapor handling capacity of con-
emulsion, our parent company IFP has studied the emul-
ventional trays by up to 25 percent.
sion approach for disposal of deasphalter bottoms and
Overall fractionation efficiency and turndown capabil-
this approach has shown that there are some interesting
ity are not affected by the change to these trays.
data for good burning.
TOM HALFORD (Petro-Canada): ANDREW W. SLOLEY (Process Consulting Services Inc.):
Petro-Canada operates a slurry hydrocracker reactor in There are numerous new high capacity trays available
the Canmet unit at its Montreal Refinery. This technology in the marketplace. These high capacity trays all use basi-
is supported by pilot plant work in the National Center cally one or both of two different methods to increase
for Upgrading Technology in Devon, Alberta. the effective vapor handling capability of the trays. Several
Recently, the M.W. Kellogg Technology Company of the trays use a smaller valve design or a smaller valve
had a pilot plant test done at NCUT on the Canmet design in conjunction with a directional valve. While the
pilot plant using a ROSE de-asphalter bottoms as feeds- inherent capacity increase from the smaller valve designs
tock. They got as high as 73% conversion of the nC5 is approximately 6-8%, the improved capacity claims run
asphaltenes. The only reason they stopped at 73% was as high as 30%. This simply is not true. The other method
that they ran out of feed. to increase the vapor handling capacity of a tray is to
This data is published in a paper entitled ‘‘The Role utilize a portion of area under the downcomer for vapor
of Polar Aromatics in Residual Hydrocracking’’ presented flow. On a conventional tray, the area at the bottom of
at the NCUT Conference ‘‘Directions in Refining and the downcomer is a solid plate.
Marketing of Synthetic Crude Oil and Heavy Oil’’ held The various vendors use different patented and proprie-
in Edmonton, Alberta, September 1997. tary techniques to utilize the bottom area of the down-
comer. Several high capacity trays ‘‘hang’’ the downcomer,
ELKIN CARONA CUADROS (EcoPetrol): which allows active area under the suspended downcomer.
Do you have any experience for reaching high yields Many of these high capacity trays perform well. However,
in DMO up to 56 percent in volume for heavy residue the design of these trays is inherently more complex. More
with 40-50 of penetration in a demet deasphalting with complete design information is required. High capacity
unit with LPG solvent for bottoms obtaining five percent tray failure rate is high relative to conventional trays.
weight of concarbon in DMO? Do those new technologies While the capacity of these trays is higher, the tray turn-
include high yields with high quality like this? down range is lower. Prior to implementing a high capac-
ity tray design, the various operation modes should be
HIGGINS: studied thoroughly. Installation tolerances and inspection
No response. requirements of high capacity trays are very important.
D. Crude Distillation BRIAN D. ALBERT (Koch-Glitsch):
1. Mechanical Significant developments in tray technology have been
introduced in the past five years. Two tray advancements,
Question 20. active area enhancements and inlet area enhancements,
There has been significant discussion on advances in are particularly well-suited for increasing capacity without
random and structured packing in recent years. What major modifications to the column.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 23
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Active area enhancement technologies about treating some of these high mercury crudes. Work
Tray active area performance has been enhanced by is being done by IFP and UOP on this particular problem.
new tray technologies that employ small fixed or movable
valves. The Bi-FRAC娂 tray, developed by Koch Engi- BINFORD:
neering Co., Inc. is an example of a fixed mini-valve and Elemental mercury has been found in the top of atmo-
the Glitsch VG0 is a example of a moveable mini-valve. spheric towers, for example, in the manways when the
The mini-valve designs can increase the vapor handling columns open for maintenance. One instance occurred
capacity of conventional trays by up to 30%. in the Pacific Northwest refinery that had been processing
the Southeast Asia condensate. The condensate contained
Inlet area enhancement technologies trace amounts of mercury.
MAX-FRAC娂 and Nye威 trays by Koch-Glitsch are As a result of extended processing of the condensate,
examples of high performance trays which utilize the area small amounts of mercury condensed and collected into
under the downcomer to increase the vapor handling visible quantities in the tower. During routine inspection,
capacity. These trays can increase capacity by as much as the inspector found tablespoonful quantities of liquid
25% in comparison to conventional trays, while maintain- mercury in the upper manway nozzle. The presence of
ing the same efficiency and turndown capability. mercury in this fashion represents a personnel hazard from
Inlet area enhancements are particularly appropriate both breathing and skin contact.
for trays that have relatively large downcomers, but are Mercury spill kits are available to remove mercury and
jet flood limited with conventional valve or sieve trays. thereby minimize danger to personnel entering vessels,
Retrofitting conventional trays with Nye威 or MAX- and should be used whenever mercury is detected. There
FRAC娂 trays provides a capacity increase approximately are also instruments that can be used to detect mercury
proportional to the increase in tray active area. The result- vapor in small concentrations. The capability of these
ing lower vapor velocity through the enlarged active areas instruments has increased by several orders of magnitude
results in a reduced tray pressure drop and lower levels over the last several years. These better analytical capabili-
of entrainment. ties alone may be accounting for some of the increase in
Superfrac威 tray by Koch-Glitsch is a high performance mercury being cited in crude units.
tray which utilizes both inlet area and active area enhance- Mercury does not attack carbon steel or steel alloys. It
ments to achieve higher capacity and efficiency. is not corrosive to most other metals, except for aluminum
Most revamps with high performance trays do not and aluminum alloys where it causes stress corrosion
require extensive modifications to the existing tower weld- cracking. The gas processing industry has avoided the use
in attachments and can easily be accomplished during a of aluminum because of this. It also does not react readily
short turnaround. with sulfur or other trace crude contaminants to form salts.
And as a result, rarely plays a role in equipment fouling.
Question 21. There is good information in NACE literature (1998
To what extent is the industry experiencing the presence annual meeting, 1996 fall meeting minutes) and through
of mercury in crude overhead systems, and what have the GPA (Gas Processing Association) concerning mer-
been the associated problems? cury found in equipment during turnaround inspections
in both the refining industry and the gas processing
MALEK: industry.
The appearance of mercury is relatively uncommon in Finally, it is common for heavy foreign crudes to be
crude oil, although it has shown up on certain specific blended back with condensates to achieve a gravity spec
crudes. If concentrations of mercury appear in the total or to bring the viscosity down to a manageable level. We
crude in excess of one to two parts per million, you can have seen some of this with South American crudes. The
expect that some of it will show up in the overhead of mercury found in these crudes may not be from the base
the crude tower system. You can also expect it to show crude at all, but from the condensate that is being used
up in practically all of the product side streams. The to blend the crudes back.
solubility of elemental mercury is about one to three parts
per million in hydrocarbon. Mercury also appears in crude HAHN:
oil and other hydrocarbons in two other forms. It appears I would just add that there is some concern that mer-
as cinnabar (mercuric sulfide) and also as organic mercury cury can attack monel and you get rapid metal embrittle-
compounds which have a broad boiling range. ment or cracking. It takes a combination of precisely the
The organomercury compounds are relatively unstable correct temperature and usually in the presence of caustic
and will breakdown under the temperature conditions of to make that happen. So if you are going to experience
the crude heater. There is considerable work going on at that, it is usually a rather rapid event and you will either
the research level to try and determine what can be done have it or not. We have had mercury in our overheads,
24 General Processing
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as evidenced by small droplets when we have opened up pretty high levels. It may be time to relook at justification
overhead exchangers and not found any detrimental effects for crude preheat antifoulants in your particular system.
from the mercury other than just the hazard of disposing
of it. CAIN:
We have success with crude unit antifoulants in two
CARLOS CANZIANI (Refineria San Lorenzo S.A.): plants. In one plant we are using Nalco/Exxon and the
In the case of crude oils with mercury content between other plant we are using Betz.
400 and 1100 ppb, what are the impact on environment,
considering gaseous and liquid effluents and final products R. RAJAMANI (Mangalore Refinery and Petrochemicals Ltd.):
quality, when those crude oils are processed in a low There is a school of thought that antifoulants should
complexity refinery? not be dictated midway through operations. Once the
preheat exchangers are clean antifoulant injection can
MALEK: be done.
We believe that probably the most effective way to
capture this mercury will be in the form of mercuric Question 23.
sulfide. So I think most of the work is directed toward What atmospheric and vacuum heater outlet conditions
removing any of mercuric sulfides solids in the crude, (temperature and pressure) are practiced by refiners pro-
and to try and convert the other forms of mercury to a cessing heavy crude oils, in particular heavy Canadian
sulfide so that it can be removed. crudes? What impact does the heater design have on
selecting these conditions?
2. Process
CAIN:
Question 22. At our Louisiana plant, we charge mostly Arab Medium
What is the panel’s recent practice and experience with and we achieve a cutpoint around 1050 to 1060°F. In our
regard to the effectiveness of crude preheat antifoulants? atomospheric heater, preheat runs around 600°F, heater
outlet, 730-750°F. The flash zone pressure is 27-32 psig.
JOSECK: In the vacuum heater, the outlet is 760-765°F and flash
Our experiences are mixed. We have historically used zone pressure is 48 mmHg.
antifoulant for years at one refinery when energy prices
were high. As energy prices decrease, the antifoulant pro- TASKER:
gram was determined to be uneconomical. We redesigned For the Canadian crudes, the heater outlet temperatures
the crude pretrain, specifically the desalted crude preheat generally run in the order of 370-380°C or 700-710°F.
exchangers for offline cleaning. The offline cleaning design We have not seen many problems in this range. Obviously,
was more for turnaround extension. With the offline the heater design comes into play when trying to push
cleaning, we are currently able to extend the crude unit the unit to its absolute ultimate capacity. The designs
turnaround cycle to over five years. Turnaround duration with which I am familiar have not had any major design
is not currently limited by preheat train fouling. differences compared to other heaters.
At a second refinery, we had two crude units processing
the same crude. The two units were shutdown and ANDREW W. SLOLEY (Process Consulting Services Inc.):
replaced with a third. We experienced fouling in both Atmospheric and vacuum heater outlet operating tem-
the older two crude units, while the fouling is greatly perature and heater design are integrally linked. Operating
reduced using antifoulant in the replaced crude unit. The atmospheric and vacuum heater outlet temperatures of
antifoulant program by Betz began in 1981 and is still 760 and 790°F are achievable on heavy Canadian or heavy
active. Venezuelan crudes. However, the heater design is very
important. Oil mass flux rates, heater coil size transitions,
BINFORD: and oil residence times (number of heater passes) deter-
There is a tremendous amount of literature in past mine the maximum operating temperature prior to ther-
NPRA meeting transcripts on preheat antifoulants. I mal cracking. Heater outlet temperatures and heater coil
would just say that the limited use of crude preheat anti- design determine the maximum peak oil film temperature.
foulants, especially in the late ’80s up through a couple In one case, the atmospheric heater operating on a blend
of years ago is really the result of poor payback due to of Canadian crude operated at a 760°F outlet. The atmo-
low energy prices and relatively low capacity utilization spheric heater was initiating cracking that loaded the vac-
in the U.S. In the last few years, however, as we have all uum jets. Reducing vacuum heater outlet temperature
noticed, capacity utilization has steadily increased to now had very little impact on ejector load. Instead, a 20°F
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 25
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26 General Processing
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poorly designed stripping trays on start-up, the total atmo- however, you typically do not get to high enough tempera-
spheric distillate yield loss from damage will be approxi- tures to actually decompose the silicone. As a result, the
mately 10% of the atomospheric tower bottoms (ATB) silicone product is going to end up going with bottoms
when operating at 8 lb/bbl of ATB stripping steam rate. in both the crude tower and the vacuum tower. This
Simply keeping the trays intact through improved typically does not cause a problem unless, of course, you
mechanical design will increase diesel and atmospheric are hydroprocessing or cracking resid. Then you would
gas oil product yields. Installing standard design trays have to look at silicone uptake on that catalyst.
practically assures they will be damaged if there is any Also, you do need to check for silicone level in the gas
unit upset such as high liquid level. oil draw and the bottom side cuts. Even though you are
not going to get any decomposition you could get some
Question 26. entrainment up into that section and so you would want
What operational measurements are being used to moni- to check to make sure this is not occurring in your system.
tor/detect flooding or foaming in a crude tower? What
actions can be taken to address the problem? With the MALEK:
need to run ever higher crude rates, this is becoming a I would make a similar comment as I made yesterday
more common problem. on heat exchangers in a crude unit. The process simulation
tools that are now available to your process engineers
are capable of predicting flooding in crude towers very
FOSTER:
precisely. They all have fairly good rating calculations for
This question has to do with operational measurements
specific types of internals. So get to know your crude unit
for monitoring and detecting foaming or flooding. The
by a process simulation before you make major operational
traditional, but reactive approach is to determine where
changes. As you change crude oils and change operating
your flood prone conditions are and then monitor the
conditions, you can anticipate flooding conditions well
differential pressure in that section.
before they occur.
Short term actions to address a flooding problem or
ranging from a modest increase in tower operating pres-
ROMAN:
sure to shifting pumparound heat removal to limit the
Jet flooding and system capacity flooding should be
traffic in the restricted sections. Since this is a bit reactive,
distinguished from foaming. It is generally the preflash
it is a better idea if you have an online capacity factor
tower which is most prone to foaming. Foaming takes
demonstrated at the operator’s DCS console.
places in preflash towers due to the entrainment of vapor
For our vacuum column, the C factor is continuously
into the liquid as it enters into the flash zone.
calculated for the column loadings between the wash zone
These bubbles have a characteristic rise velocity which
and the heavy vacuum gas oil draw, since this is the section
can be rather low due to the viscous nature of the crude
in our particular tower with the highest loading. This
liquid. When the downward velocity of the crude liquid
enables some proactive operation to remain below
exceeds the upward velocity of the vapor bubbles, a stable
flood conditions.
foam results. The presence of sodium naphthenates creates
The best idea and the one that we intend to implement
smaller bubbles and makes the situation more likely. Avail-
is to encode these calculations and the tactical responses
able solutions are to design the tower with a large enough
into our advance control logic along with many other
diameter below the feed tray to allow these bubbles to
crude capacity constraint calculations like heater firing
disengage, minimize the amount of naphthenic crudes
and so forth. Therefore, we are always running the crude
in the mix, and inject an antifoam to improve bubble
rate too, but not exceeding those constraints.
disengagement. At one of our installations, we successfully
Longer term but a more expensive option is to look
used Petrotech 1964 at 5 ppm to control this foaming.
at the high capacity packing of your tower. I think that
We have also utilized standard laboratory foaming tests
Mr. Henke has already covered that.
to identify which crudes are most likely to foam.
BINFORD: SAMUELS:
Some of the other panelists are going to talk about We have historically seen foaming in our 165,000 bpd
mechanical modifications, so I will concentrate on opera- preflash column in Robinson refinery. This spring we
tional issues. Several refineries in the United States and expanded the unit to 185,000 barrels per day. To address
overseas have used high temperature defoamers as either the foaming, we installed a drum upstream of the preflash
a shortterm solution to solving the problem or when a column as part of the retrofit. The drum has a seven
mechanical or operating option could not be justified. minute residence time and we have been able to run up
The products are silicone-based defoamers similar to to 200,000 barrels a day with no foaming problems on
what is used in a coker. As opposed to the coker operation, a variety of crudes.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 27
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28 General Processing
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 29
TOC/INDEX
Just because the fuel color degrades due to the presence JAMES MANN (Merichem Company):
of UV light, it does not mean it will necessary turn color Middle distillate color instability results from reactions
in dark storage. Most refiners either hydrotreat and/or started by or involving one or more compounds including
use clay filters to overcome color problems. nitrogen, diolefins, sulfur and naphthenic acids. The most
In some cases, an approved antioxidant or metal deacti- reliable method to eliminate color in stability is to hydro-
vator will lessen color degradation in kerosene. Color treat the distillate at pressures sufficiently high to render
problems in kerosene may be crude related, but are most these impurities nonreactive.
often caused by compounds produced in conversion pro- Another process which has been successfully applied
cesses in the refinery. Color degradation in the presence for color stabilization is sulfuric acid treating to remove
of sunlight means that very reactive alpha olefins, acids, unsaturates and nitrogen compounds. This process can
or bases are present. These are typically formed in severe be economical for refiners who operate sulfuric acid alky
conversion operations such as delayed coking, visbreaking, units and already manage spent acid streams. FIBER
or catalytic cracking. FILM娃 technology is an excellent option for acid treating.
Coker streams are highly reactive and seldom can be
stabilized with additives alone. The reason is that the E. Instrumentation
concentration of reactive molecules are so high and the
thermodynamics are so strong that the dosages of inhibitor
Question 29.
are prohibitive or cause problems at those high dosages.
What are the status of and requirements for the approval
The only practical way to stabilize these highly reactive
of NIR for gasoline blend (ASTM) certification?
streams is to hydrotreat them immediately or blend them
down to a low concentration in a larger stream so that ROMAN:
chemical treatment can be effective. NIR spectrophotometry provides a fast, reliable, very
Another initiator of color degradation is metal contami- accurate means to measure motor and research octanes
nation. Transition metals, noticeably nickel and copper online. Statistical methods are used to correlate the octanes
will catalyze degradation reactions. Metal deactivator, with the higher vibrational harmonics of benzyl, methyl,
which essentially coats the metals with an organically methylene and methyne carbon- hydrogen bonds. Ash-
protected film making them unable to catalyze the color land holds 75 percent of the patents on this technology
reactions, can be used to prevent color degradation. and has proposed a standard to D.02.04 Section F on
Other mildly reactive kerosene streams that show absorption spectroscopy.
longer term stability problems as measured by an induc- There has been some opposition to recommending this
tion period or 300°F 90 minute test can be effectively standard due to disagreements over the statistical methods
treated by antioxidants. Many chemistries are approved and the accuracy and precision standards. There also is
by the military and ASTM for use in jet fuel. These and a desire on the part of some of the subcommittee members
others can be used in the refinery for nonjet streams as to have Ashland and British Petroleum, who holds the
well. Some crudes or crude derived streams will be more remaining NIR patents, to release these methods into the
affected by thermal or catalytic cracking than others. The public domain. The subcommittee membership would
effect of crude charge changes on finished product specifi- also like to see more than one vendor participate and
cations has not been compiled to our knowledge, probably British Petroleum is working with Ashland to help get
because it would require so many caveats that the process this standard approved.
might not be worthwhile.
Question 30.
Many refiners are trying to optimize and more closely
JOSECK:
control chemical additives (corrosion inhibitors, emul-
Our virgin kerosenes tend to discolor over time. We
sion breakers, dyes, etc.). Are there more accurate meth-
hydrotreat and bauxite treat for special applications with
ods of controlling the usage than with metering pumps?
strict color specifications. The hydrotreated and bauxite
treated kerosenes tend to be more stable than the vir-
BINFORD:
gin kerosenes.
Regarding optimizing or closely controlling chemical
additives, two things that are becoming pretty common
R. RAJAMANI (Mangalore Refinery and Petrochemicals Ltd.): are automatic stroke control or variable speed control on
One of UOP’s guarantees is that the color deterioration pumps, driven by a 4-20 miliamp signal that is directly
in the kerosene Merox does not exceed 10 (Saybolt). So, tied to the refiner’s DCS system. The real key here is
practically with all types of crude we get color deteriora- tying these into the right control scheme and the rest of
tion of about 6 to 8 between upstream and downstream the process, whether it is directly tied in or through the
of the Merox reactor. use of an appropriate model.
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 31
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data which we use in unit monitoring tools and unit yet being directly passed to the business accounting sys-
optimization. We have not integrated the reconciled plant tems.
data directly with business accounting systems at this time.
As an aside, we derived many unanticipated benefits from BRIAN HART (Aspen Technology, Inc.):
implementing this program. The discipline required dur- Aspen Technology has been working with data recon-
ing implementation uncovered several errors that had ciliation and balance resolution for the past six years in
crept into our internal material balances during the years. refining and petrochemical plants. Our experience is that
reconciled data has value in optimization applications,
JOSECK:
but resolved values are much more valuable to the business
Pennzoil currently uses a SAP accounting system and systems. This is because reconciliation forces closure by
Signafine software data gathering system at the refinery distributing error across all measurements in proportion
level for throughput and yields. Signafine recovers data to their likely contribution to that error. Resolution on
from the upper level Setpoint and PI systems. Setpoint the other hand uses available measurements and other
and PI are used as an upper level data gathering system, information to pinpoint likely sources of error and recom-
trending, data historian, and optimization system for the mend corrections which generally can be validated. It is
DCS. We are aware that Foxboro has an SAP interface. the latter case which has value to the business account-
The SAP interface requires a Foxboro 50 series or higher ing function.
hardware platform to run the software and provide the
ethernet connections. H.C. KLIESCH (Treiber Controls):
All of our data reconciliations is at the Signafine level. Data reconciliation and parameter update is an integral
We have integrated Signafine to SAP using in-house soft- part of our online optimization of a unit. Because an
ware. Currently, the facilities do not reconcile data back open equation format is used for the model of the unit,
to the historians for supporting data for optimization. the same simultaneous equations are solved for data recon-
Reconciled data is used to validate the plant LP, schedul- ciliation, only the objective functions are changed.
ing activities, and monthly or weekly tracking of key unit
data from the PI and Setpoint systems. BEN WALKER (Coastal Eagle Point Oil Co.):
At our plant, we find that the reconciled data very
often provides a less accurate unit material balance on
ROMAN: many of our units. Most times we depend on metered
The refinery’s yield accounting system uses a statistical unit information to provide better closure on our unit
based reconciliation approach whereby balance errors are material balances and test runs.
distributed to flow meters which have the highest standard
deviation. More rigorous model development activities in Question 32.
both inferential control and online optimization rely upon LP Planning Systems continue to be the main vehicle to
either first principle model based reconciliation systems determine overall refinery optimum operations. How do
or neural network based pattern reconciliation systems. refiners measure how well their LP in fact matches refin-
The first principle, fundamental based data reconcilia- ery process capability? What data are collected and how
tion systems, as their name implies, use redundancies and often? How is it compared to LP predictions? How closely
flows, temperatures and pressures, along with chemical do they compare?
engineering based relationships such as material and
energy balances, flash calculations and heat exchange HAHN:
equations to validate data and make alternative recom- We do several different things to check our LP model.
mendations on those points felt to be in error. Periodically, we conduct unit test runs to verify the indi-
The neural network based approach establishes pattern vidual unit submodels, particularly whenever we make a
models across a set of related data points to establish process or hardware change on the unit or when we have
whether a data point deviates from the pattern the neural a significant feedstock change.
network identifies for it. We also conduct back cast or audits that we do after
If there is disagreement, the neural network recom- the fact, taking a whole month’s run and back casting
mends an alternative value to cause the suspected data that with actual crude input and rerunning the model
point to better fit the pattern established for it. Neural and see what the answer is, applying spot prices to those
network based approaches have been found to accurately volumetrics and seeing how close we came to what we
perform steady state as well as dynamic data reconciliation. actually did as far as volumetrics go. We have been very
The disadvantage of this approach is that a large set of successful at this. Typically, our plant model is within a
sample data of relatively good quality must be available cent a gallon profit on a gross basis based on those spot
in order to train the models. Reconciled plant data is not prices for a typical month. We also check such critical
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parameters as exhaust benzene, i.e., what the model said To aid the unit engineers in this effort, we have devel-
by calculation and what we actually experienced. Once oped spreadsheets and have been able to track actual yields
again, our model generally predicts that fairly accurately, accurately against the LP for most of the major units. We
within about .1 milligrams per mile on exhaust benzene. have a mass balance day every week, so that data are
So we are satisfied with our model, but it does take generated automatically.
constant attention to keep up with the ever changing Additionally, we use KBC, UOP, Profimatics and other
process units and crudes. kinetic models to enhance the measured data by establish-
ing better yield partials over a larger operating range.
CAIN: We try to explain the differences between predicted
We do a complete refinery backcast each month. Indi- yields versus actuals in monthly or quarterly tech service
vidual units are backcast weekly by using a spreadsheet reports. The LP is updated on a semiannual basis.
submodel to compare actual vs. model yields for the actual In many cases, the predictions consistently match very
quality and volume of input. The individual submodels well, plus or minus five percent for individual product
are reviewed every three months for potential model revi- yields. If the yields are generally over or under the pre-
sions. The complete refinery backcast is a supporting dicted amount, but directional shifts are properly repre-
tool for individual unit changes and may also point out sented, the base yields can be adjusted. Consistently poor
additional model revision requirements (i.e., blending, correlations and response generally indicates that a reeval-
volume gain, hydrogen balance, etc.). uation of the yield partials should be considered. Addi-
tional yield partials are also considered in some cases. But
FLETCHER: having the unit engineers involved is the key.
I think the only thing I would add is that one of our
customers compares their LP yields to observed yields on
a monthly basis and then changes to the LP model are ANDREW W. SLOLEY (Process Consulting Services Inc.):
made when a significant deviation reoccurs over a three The accuracy of a refinery LP is measured by perform-
month period. ing a ‘‘reconciliation.’’ A reconciliation compares actual
plant data to LP predictions for a given time period. A
FUSSELL: reconciliation is a necessary step in maintaining a reason-
Earlier this year we purchased a new LP model which able LP representation of a refinery.
was a lot more flexible than the model we had been using A reconciliation is conducted during a period that is
previously. We set ourselves a very aggressive goal of consistent with yield accounting and financial reporting.
getting our new model up to speed as quickly as possible. These activities typically occur monthly. The close of the
This year we have probably run more test runs than we accounting books will often produce a ‘‘charge and yield’’
have ever done in the 15 years I have been at Fina and report. This information is more accurate than the sum-
our lab has felt that. We have integrated the information mation of many refinery flow meters. This report is pro-
from these test runs into our LP model. Once a month duced with receipts from all custody transfer meters and
we compare what we actually did to what the LP model changes in tank inventories. It is a good practice to verify
predicts. We find the areas where we are off the most tank levels at the beginning and end of the period. The
and we do more test runs and continue to try to fine presence and amount of water is noted for each tank.
tune it. Right now our LP model is within plus or minus The LP model is constrained to match crude slate,
five cents per barrel on our margin. pricing data, and process unit charge rates for the period
of reconciliation. The crude slate is obtained from the
HENKE: charge and yield report. The pricing data is obtained from
Our experience is similar to that described. Since it is the financial reporting. The average process unit charge
so labor intensive, we only perform detailed comparisons rates are obtained from the plant data information sys-
of LP output with plant data when significant changes tems.
occur. The time period is between monthly or quarterly. The output from the constrained LP run is compared
to the actual yields to measure the accuracy of the LP
SAMUELS: model. The gasoline, distillate, LPG, specialty chemical,
As far as global analysis of the model, we have covered and residual volumes from the LP run are compared to
that pretty well. I would like to say that getting the the actual yields for the period. The actual yields are
individual units accurately represented ensures that incre- obtained from the charge and yield report.
mental processing decisions will be made correctly. The This procedure is used to monitor the accuracy of the
key to improving LP accuracy is to get the unit engineers LP. A large difference between the actual yield and the
to take responsibility for reviewing the individual unit predicted yields for any of the products is an indication of
representations. a problem. Typical problems encountered are inaccurate
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 33
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crude oil outpoints, incorrect crude oil assays and process LEE TURPIN (Honeywell Hi-Spec Solutions):
unit representations in need of calibration in the LP. Profimatics, (the company name prior to acquisition
The problems can be corrected with close work with by Honeywell) put on the first closed loop alkylation
the unit process engineer. The solution often requires optimization and control with a kinetic model into service
unit test run data. in the late 1960’s. We have installed several real-time
A well maintained LP with accurate crude oil assays optimization packages since then.
can match actual plant yields within 97%. For example, One post installation audit report showed benefits of
gasoline and distillate predictions for a 100 mbpsd refinery about $125/day on a 20,000 bpd HF alkylation unit. See
with total gasoline and distillate production of 50 mbpsd NPRA paper CC-93-139, ‘‘On-Line Optimization at El
and 45 mbpsd, respectively, can be Ⳮ/- 1500 bpd. Palito Refinery’’ for details.
Question 33. H.C. KLIESCH (Treiber Controls):
With the increased importance of alkylation units due to Our real time optimization software CRO (Closed-
gasoline regulation concerns, what is the experience loop Reconciliation and Optimization), uses a first-princi-
using both kinetic (rigorous) and statistical computer ples, non-linear chemical engineering model of the entire
models? What kind of unit performance improvements alkylation unit. We are calculating a new values for up
have been realized with each model type? to 25 setpoints, which are sent to the controllers every
45 to 60 minutes. Among these setpoints are the isobutane
BINFORD: target for an OPC (Optimal Predictive Control) multi-
We know of several refiners that do have kinetic models variable predictive constraint controller and unit olefin
built for their alkylation units that are used as optimizers. rate. This results in an economically optimal retention of
To our knowledge, there is no one that has a kinetic isobutane in the plant and use of olefin feed to exploit
model that would be what we would consider real time, all available isobutane. The optimizer generally holds the
and certainly none that are being used for closed loop operation against 15 to 20 mechanical and quality con-
control of the process, although we certainly think that straints. Among other performance improvements, the
people are moving in that direction. unit has run at 140 percent of design alkylate production
We use an in-house statistical model called PEAKS, of sustained periods. The application has been running
which stands for Process Emulation and Artificial Knowl- continuously and profitably for over five years. The fol-
edge Synthesis, that is based on the neural network tech- lowing is a reference on the application:
nology. The model is developed from actual plant data Treiber, S., R.S. McLeod, T. J. Boyle, G. Powley, &
that we trained to be very accurate within the constraints S. Lee, ‘‘Closed-loop Plant Wide Optimization,’’ CPPA
of the model that is built. Then we verify the model on Control Systems ‘92 Conference, Whistler, British
independent data sets to ensure that the model is valid. Columbia, September 29-October 1, 1992.
In most cases we have gotten very good match between
Question 34.
our neural network base technology and refiners’ kinetic
Taking an overall view, crude unit product properties
models. There have been cases where we have seen the
can be obtained from lab samples, on-line analyzers, or
two models diverge from each other. We have been able
inferential calculations. What percentage of your crude
to get to the root cause of that and correct it, but it
side streams are controlled by each method?
certainly involves a lot of work in doing so.
FOSTER:
BRIAN HART (Aspen Technology, Inc.): Right now we use 100 percent lab samples for control
Aspen Technology has done successful online optimiza- of product properties on both of our large crude units.
tion calculations using correlation based alkylation mod- With advanced control projects in progress, we plan to
els. We are also currently working jointly with two clients have one crude unit on 100 percent inferred properties
to develop more rigorous kinetic based models for their by end of year and the other crude unit on 100 percent
alkylation processes. These will be used to do online opti- inferred properties by this time next year. These inferential
mization applications. calculations are intended to be bias updated by lab sam-
Online constrained multivariable control, however, can ples. The only area we see a need for an analyzer applica-
also provide significant benefits through empirical models. tion is for the heavy vacuum gas/oil in deep cut operation.
Unit profitability is maximized by achieving the following We expect to use a UV analyzer for color control in that
objectives: maximizing isobutane to olefin ratio, maximiz- application.
ing feed rate, maximizing propane removal, minimizing
isobutane losses to butane and propane streams, maintain- FUSSELL:
ing alkylate RVP target, minimizing acid consumption We have two atmospheric columns in Port Arthur.
and losses and maintaining all systems inventories. One is a 140,000 barrels a day unit. The other is 40,000
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barrels a day. We have 100 percent inferential controls are controlled by laboratory feedback through inferential
on the product draws on both of these units. These are calculations. This ranges from towers with no analyzers,
reset with lab data as the lab data is received into the to towers with some analyzers, to towers with all analyzers.
system. We will be presenting a paper on our crude unit
control system next week at Aspen World in Boston. R. RAJAMANI (Mangalore Refinery and Petrochemicals Ltd.):
I observed from the comments of the panel that most
HAHN: of them are using 100 percent inferential controls in the
On our crude unit, we are generally volumetrically crude unit. I would like to know what has been the
constrained or pushing that unit quite hard. So although payback in cents per bbl.
we have developed inferential qualities, we do not actually
use them in our closed loop control generally. However, CAIN:
we do have 20 percent online analyzers on crude unit The use of a calculated or inferred property in crude
side cuts and the rest of the 80 percent is with lab samples unit control systems, particularly MVC, has yielded sub-
at this time. On our vacuum tower, we are using 100 stantial benefits. These benefits are in the form of:
percent lab samples at this time. —improved volumetric yields.
—reduced off-spec production.
CAIN: These control benefits have been measured directly in
We have 100 percent inferential and DMC controls the form of improved yields beyond previous record rates
on crude stills in two plants. (max naptha or max avjet) on the order of $0.02/ bbl
We also have 100 percent inferential controls on our charge. Additionally there are less tangible benefits
crude units. The inferential estimators do a good job at believed to be of the same magnitude for times when we
measuring distillation and flashpoints. However, particu- are in a downstream limited mode of operation. During
larly in a changing crude environment, the inferential these times correctly matching the downstream limitation
calculations do not do a particularly good job on other consistently yields optimum results. Total benefits are
properties such as kerosene freeze point or diesel cloud $0.03-0.05/crude bbl charge. (Solomon Industry standard
point. benefits are $0.050-07/crude bbl charge.).
These benefits are because of the consistency the infer-
SAMUELS: ential prediction provides. As unit constraints are pushed
We use both lab samples and inferential calculations inferred properties are important to assure the important
at our Robinson crude unit. Inferential controllers are property quality specifications are not violated. Inferred
used to pull all light products, lighter than gasoils. Daily properties can be constructed to account for multiple
lab samples are used mainly for checks and to make minor effects to a specific property beyond the primary influence.
adjustments to the inferential controllers. This enhances the ability of the control scheme to adjust
for disturbances which might not have been corrected for
BRIAN HART (Aspen Technology, Inc.): by an operator.
I agree with the panel generally on the way inferentials In conjunction with an automated update to the infer-
are used. I would also like to say from our experience we ential bias against a lab result a systematic response to
would estimate that about 95 percent of the applications deviations in lab results can be accomplished. This system-
we have done use product inferentials in some form. atic response imparts consistency beyond individual oper-
Approximately 30 percent may have some analyzers that ator estimates of appropriate responses to lab data
are used for actually updating inferential calculations. The fluctuations which may be the result of a change in the
remainder of them just use laboratory results for doing process or a result of natural variation in lab accuracy.
those updates.
Question 35.
H.C. KLIESCH (Treiber Controls): Significant savings are possible through the use of refin-
We always use inferential calculations for all our refin- ery scheduling programs. Please poll the panel as to
ery advanced control applications, including crude units. their experience in using these software tools and indi-
We use inferential calculations with feedback from either cate what the benefits have been.
laboratory measurements or analyzers. Inferential calcula-
tions increase the on-line time of our control applications, JOSECK:
because they keep running even when analyzers fail or One of our refineries is currently using an in-house
are taken out of service for calibration, or when operators scheduling model. The other uses Trios to schedule the
forget to update laboratory feedback to the controls. lube plants and WKBLEND娃 to schedule pipeline ship-
About 50% of our controlled crude unit product streams ments and gasoline blending. We have estimated that the
have analyzers with inferential calculations while the rest WKBLEND娃 software has reduced octane giveaway by
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 35
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0.2 to 0.3 and RVP by 0.2 to 0.3 numbers. We also see b) regulatory control, c) advance control, d) closed-loop
an added benefit of simplifying a complex scheduling unit optimization, and e) overall plant optimization.
problem including pipeline shipments with
WKBLEND娃. FOSTER:
This relates to implementing computer process control.
ROMAN: We have about 80 percent of the refinery on DCS for
We utilize Wright Killen’s Trios scheduler at all of our unit control, including all crude and conversion units.
refineries. We find it to be a valuable tool to allow control We are upgrading the refinery to standard TDC3000
of both finished and intermediate product inventories, and standard with scheduled completion in the year 2000.
to accommodate changes in crude deliveries and product We have just commissioned a few months ago our multi-
pipeline and barge shipments. variable controller on the fluid unit. We are starting up
The refinery LP determines the optimum mode of the closed loop optimizer this month. We too will be
operation and the scheduling spreadsheet is utilized to presenting a paper at Aspen World.
try to translate these targets into a daily and weekly plan By year end, we will have one coker and one crude
of operations. We recently tried to implement an exten- still on multivariable control with plans to complete the
sion of this basic scheduling tool whereby we assign prices other coker and crude still by third quarter ’98. Those
to the various products and intermediates. This was sup- projects have been approved. Closed looped optimization
posed to allow the scheduler to modify the spreadsheets will then be done subsequent to multivariable control on
to take advantage of economic opportunities. both crude stills. We also have projects in the works for
This proved to be of little or no value due to the our FCC feed hydrotreaters and low sulfur diesel units
complexity of the refinery and the multitude of options on multivariable control, third quarter ’98.
available.
FUSSELL:
HENKE: In Port Arthur, all of our process units are on Honey-
We also use Trios for overall refinery scheduling and well distributive control systems. We are in the process
we are very pleased with this product. In general, it has of converting all of those over to the 3000 system from
helped us to significantly smooth out crude transfers, the 2000. We have quite a few supervisory controls from
stabilize the crude unit operation, and reduce inter-tank our computer system on various units where we feel they
transfers. It has helped us have the right ships and people are justified. We have a lot of these on distillation towers
at the right place, at the right time. It has also helped us as well as charge ramps and things like that. We have
balance other transfers at our loading docks and reduce recently installed multivariable optimizer on our crude
that amount of time spent waiting around. In general, units. Last year we installed the same type of system on
there are a lot fewer surprises. our FCCU.
CAIN: HAHN:
We also use Trios. The major benefits realized are We also are 100 percent DCS controls. We also have
inventory control, feedstock optimization, unit charge some form of advanced control on all of our processes.
consistency and extended batch runs. These can include things all the way from simple ratio
controls to multivariable controllers to unit wide multi-
BRIAN HART (Aspen Technology, Inc.): variable controllers and unit wide multi-constraint con-
Aspen Tech has extensive experience in scheduling trollers.
applications in refining. Recent developments in opti- At some of our facilities we have done advance closed
mized schedules which drive toward meeting overall eco- loop optimization across whole units such as crude units
nomic objectives are a new technology that has come and vacuum units. These are based on very rigorous multi-
about. A key technology which has also recently been variable controllers. But we do not yet know exactly
developed is a link between scheduling and rigorous online whether or not these are economically justifiable in all
unit optimization to drive a plant appropriately as operat- cases. But they are definitely technically feasible and are
ing conditions change throughout the course of a produc- in operation at one of our facilities.
tion day.
CAIN:
Question 36. Basically, in all three of our plants, we have some form
Most refiners have made significant strides in imple- of advance controls on all major units. We have a closed
menting computer process control. Please poll the panel loop unit optimizer on the vacuum pipe still at Louisiana
with respect to a) installation of DCS instrumentation, plant and also at Port Arthur Plant. We also have a
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project in place to put an optimizer on the FCCU at the system using average conditions, capabilities, and con-
Louisiana Plant. straints. However, a short term opportunities on a daily
or weekly basis, can be exploited to an advantage by
HENKE: using a refinery operational scheduling and optimization
Our refineries are almost 100 percent DCS. Approxi- program. Use of such a tool can take advantage of spot sit-
mately 20 percent of the control loops are on some type uations.
of advance control. At the present time, our FCCUs are Some of the unplanned situations brought up are unit
the only units utilizing closed loop optimization. We are upsets, unit emergency shutdowns, ships are late, surprise
not using any overall plant optimization control systems shipments, customer goes down at peak inventory, equip-
at this time. ment repairs, etc.
The study also says that in general about four or five
JOSECK: options to take care of each of the above mentioned
The lube refineries have all the process units on DCS situations. In the past, decisions were based on experience,
control, with some advanced process control on various history, gut feel, etc., but with a refinery scheduling and
units. The units were either converted from pneumatic or optimization program, the operator/scheduler can reach
built with DCS controls. We are continuously converting the optimal solution and do it quicker.
from pneumatic to DCS based on lower installation costs, Some of the benefits cited are smoother operations, no
improved accuracy, lower maintenance, and improved jerking of the units, less off spec products, less demurrage
information flow. Some of the units have simple closed charges or shipping delays and identified holes in planning
loop optimization, no upper plant optimization is strategies. The study claims that at least one poor decision
employed. a month is saved and incentives are calculated at about
$5-$10 million a year. So that is a significant amount
ROMAN: of money.
DCS instrumentation and regulatory controls were The other study that I found relates to crude blending
installed at nearly 100 percent of the installations across scheduling and optimization. In that particular case the
all of Ashland sites with Honeywell’s TDC 3000 being benefits calculated from use of the same type of program
the predominant system. We have 100 percent installation were about $3-$4 million a year.
of advanced controls at our Canton and St. Paul refineries,
with a current installed base of nearly 75 percent at our G. Safety and Reliability
Catlettsburg refinery. Projects are underway for the
remainder of the installations at Catlettsburg.
Advanced controls range from lower level, feed forward Question 37.
and ratio controls all the way to the multivariable control- What safety precautions are taken to prevent a sour water
lers in more difficult applications. Utilizations are good, tank rupture? What secondary containment is used? Are
particularly in those areas where operations has embraced there any vapor suppressing systems in place?
the concept. With the exception of online preheat
exchanger optimization which are closed loop, the concept JOSECK:
of unit online optimization at Ashland is fairly new. On one sour water tank, we scrubbed the vent with
Online optimization development began just over one fresh water to reduce vapors. We also held a hydrocarbon
year ago. FCC unit optimizers and isomerization unit layer in the top of the tank. A later Hazop review brought
optimizers have been developed and released into the field. to light significant areas for future review, both from
Currently, unit support engineers run these optimizers employee exposure and fire hazards and recommended
on a daily basis and relay the results to operations for review of the tank’s location. During the tank’s citing
consideration. These optimizers are just beginning to review and part of the Hazop study, the tank was consid-
impact the way we operate our plants. The initial results ered as a tank in flammable, combustible liquid service.
have been good. We considered adding a floating roof, caustic scrubbing
the vent, and an impregnated carbon filters as enhance-
DANIEL HARTLEY (Haverly Systems, Inc.): ments to the vapor and safety hazards.
This is a topic of high interest to refiners. In this regard,
I would like to share a couple of study reports on this ROMAN:
subject that I found in my files. In the first one, the study Ashland protects sour water tanks against rupture from
showed that historically at this particular location, there over pressure with the pressure relief valve that vents to
were on average about five major and ten minor the atmosphere. Protection against damage from vacuum
unplanned events each month that caused deviations from is accomplished with a gas blanketing system that makes
the optimal plan. The refinery LP is a long term planning up gas, either refiner fuel gas or nitrogen, to the tank on
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 37
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low pressure and vents excess gas on pressure control when only leads to the proper corrective action to ensure that
the tank pressure begins to build. The excess gas is routed the particular failure does not occur again, but the lesson
either to the SRU incinerator or to flare. One sour water often applies plant-wide and company-wide.
tank also protects against vacuum damage with a combina- Management of change ensures that we do not ‘‘build
tion of pressure relief vacuum breaker valve. The tanks in’’ unreliability. The fewer times that you have to crash
are enclosed in the dike for secondary containment, but a unit, the longer it is going to operate between turn-
there is no vapor suppression system. arounds.
Fixed bed catalyst technology improvements along with
STEVEN M. FISCHER (CITGO Petroleum Corporation): better feedstock quality and operating controls have led
In March of 1997, API revised their Recommended to longer run lengths without some of the steeper end-
Practice 521 which relates to the design of relief systems. of-run yield decline penalties we have seen in the past.
In this revision, they inserted a new section which appears As a simple example at Robinson on our hydrocracker,
to have changed their past philosophy of not allowing two years used to be a long run. Today we are able to
the taking of credits for instrumentation to reduce relief achieve four to five years with this hydrocracker. Looking
loads for individual pieces of equipment, not just common at total catalyst life cycle cost has changed a lot of the
flare headers under two significant conditions. One of traditional decisions we have made relative to feedstock
those conditions is that you have to show that your control balancing between units and operating severities.
system is at least as reliable as the relief valve installation.
The second is where the application of the relief devices HENKE:
alone would be impractical. The increase in turnaround intervals is clearly being
I have two questions for the panel. Who is changing driven by the marketplace. Margins have been very slim
their design practices to allow this new practice of relying the last couple of years which has driven refiners to take
on instrumentation to reduce a relief load, and therefore, a hard look at their businesses to find ways to improve
allow smaller relief valves to protect equipment and what their profitability. If the units are not running, they are
has been your interpretation of when relief valves alone not making money.
are impractical to provide the relief protection? Recent advances in reliability centered maintenance,
catalyst systems, process control, and training have played
JOSECK: a role in the trend to longer turnaround intervals. How-
We have not applied that anywhere in our plant. ever, I look at these as more facilitating the change rather
than driving it.
H. Miscellaneous JOSECK:
We are using inspection software programs to predict
Question 38. equipment life, identify future turnaround dates and iden-
There seems to be a trend toward longer turnaround tify equipment requirement inspection and replacement
intervals on most units. Is this due to a) new maintenance to meet the next turnaround target date. We are continu-
technology, b) catalyst improvements, c) changing eco- ously improving regeneration procedures to extend cata-
nomic environments, or d) other? lyst life and catalyst systems to reduce pressure drop.
As an added note, we view the turnaround planning
SAMUELS: as a quality process which can be improved for reducing
Turnarounds are immensely expensive. Just calculate turnaround costs, improving execution, and extending
the present worth of removing one plant turnaround out turnaround intervals.
of five in a 20 year period by going from four year to
five year cycles. It is not hard to do the math. CAIN:
Yes, maintenance technology has changed, with better There is not much else to add except that there is
inspection tools available and more emphasis on equip- increasing pressure to do as much maintenance on-line
ment inspection. There is a greater understanding of fail- and to minimize the scope during the turnarounds.
ure mechanisms. Understanding failure mechanisms
allows you to set turnaround times based on maximum HAHN:
safe run lengths for equipment versus simply using histori- In addition to what has been said already, the lost
cal intervals such as three, four or five years. opportunity cost that you experience whenever you are
Additionally, root cause analysis and management of down has had an increasing impact lately. People are
change procedures along with better process monitoring finally starting to actually quantify that. That cost is so
and troubleshooting are improving onstream reliability much more than any maintenance cost during a shutdown
for process units. The root cause analysis of a failure not that it is one of the big new drivers that we are finally
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able to realize. We use this opportunity to do a lot of But because of all the safety and environmental responsi-
more sophisticated predictive type maintenance and pre- bilities and requirements, eliminating operating supervi-
ventative maintenance, because the payout really is there. sion is not something that Marathon is considering. We
certainly are doing as much as possible like everyone else
Question 39. to empower our operators. In fact, at the 1995 NPRA
With reorganization of refinery work processes, has any- Q&A, I described our five shift schedule which is similar
one: a) converted operations to totally self-directed work to what Mr. Joscek just mentioned. We rotate operators
teams; or b) scheduled operator time to do specific tasks, through maintenance every fifth shift where they gain
similar to scheduling a craftsman’s time? maintenance skills and then apply these skills on shift.
They actually maintain an ‘‘operator’’ backlog and this
HAHN: has contributed to bringing the maintenance backlogs
We do not have totally self-directed work teams, but down. We have eliminated routine maintenance contrac-
we have been successful at gaining union buy in to what tors completely.
we refer to as MMO or Minor Maintenance by Operators. With the business unit/area team concept, each area
We train our operators in some of the basic craft skills such team is responsible for maintenance costs. One way to
as steam trap repairs, threaded pipe work and insulation. bring their costs down is to assign operators out of their
The operators are provided the materials for the jobs area into another area or into a construction group.
and a list of the work that is suitable to be interrupted Also as was described, I think a key factor in having
if it needs to be. That is the only type of work they can your operators do work around the clock is making sure
do because they may have an upset and have to drop that they do have the proper training, and that you do
that maintenance work and get back to their primary provide them with the necessary tools and supplies.
operating job. Another key focus has been to train operators in the
The operators are encouraged to work on the items basic economics of the refinery. They are not just thinking
on the work list as time permits during their regular in terms of barrels, but understand the economic drivers
operating shifts. We have had fairly good success with for their units.
this without actually having to schedule the work.
Question 40.
We track our backlog and we have seen the backlog
How are refiners training their operators to take advan-
come down significantly after implementation of this pro-
tage of new process control systems that provide access
gram. We are considering further training of operators
to process and business information?
in routine vibration monitoring and other predictive type
analysis on rotating equipment so that we can free up
our machinists and technicians for more advanced work FOSTER:
while the operators gather the data. This relates to the training of operators. We do have
standard training for DCS. The key for us has been to
have top notch process control engineers on the unit.
JOSECK: These people have been our key knowledge transfer agents
At one refinery, we use a five crew work schedule. One throughout all stages of the process control development.
week out of five, the operators are either filling in for These are not system types. These are process engineers
vacations or working on specific projects including trained to be process control minded.
Hazops, training, procedure development, procedure They need to be able to think about the dynamics of
updating, maintenance or specifically assigned projects. the unit operation and not all process engineers can make
Operators routinely work in teams under the direction that leap from a static mind to a dynamic mind type of
of the unit leader, such as turnaround planning. I am not thinking. They also need extensive and expensive training
sure that we would classify this as a self-directed work themselves. Further, they must be willing to log a lot of
team, but we were able to eliminate the shift supervision time on the unit and be willing to and able to communi-
with the five crew schedule. cate with the operators about the problems that the opera-
We also see benefits and improvements in operator tors were having and so forth.
selection hiring, improvements in training and education, Let us go over the typical stages of a typical project
wide distribution of information and heightened expecta- and how we do training. It is really primarily on the unit
tions and accountability. The operators actually aid in training. We do have some classroom training, but a lot
the hiring process. of our training is on the unit training with the process
control engineer as the key learning transfer agent.
SAMUELS: They talk about base regulatory problems during the
Empowering employees to reduce supervisory decision DCS implementation stage. They implement a log book
making is a good goal for today’s business environment. to help collect concerns. The operators have the engineer’s
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 39
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home phone number and they call them with questions training is necessary, nothing can replace real time opera-
and suggestions on the system. We also help the operators tor response to the process. Operation of these systems
establish alarm management. We just put on several brand must be well documented so that operators will have a
new units. These brand new units have numerous alarms resource available to them on shifts when the support
and they all go off at once sometimes. They are not priori- engineer is not readily available.
tized.
When we get finished with the initial project, we had
R. RAJAMANI (Mangalore Refinery and Petrochemicals Ltd.):
a lot of alarm management to do in order to bring the We installed a training simulator before the start up
operators to where they could maintain sanity on the unit of the refinery. We have trained the operators and engi-
during even a normal operating data. Operators appreci- neers on it with very good results.
ated this and they gained respect for the process control
engineer in the process. Question 41.
The second stage of multivariable control building is What are typical problems associated with processing
during the step tests on the unit which is where we gather natural gasoline, natural gas condensates? What is being
data about the responses that a unit will make. We held done to alleviate the problems?
non-stop discussion with them about the unit’s dynamic
responses to change. After model development and build-
ing, we had discussions on how the multivariable control- SAMUELS:
ler is different than single loop systems. We also held This answer addresses problems associated with pro-
some classroom instruction in this area. cessing natural gasoline at our Robinson refinery. One
Finally, during implementation and cutover of the major problem encountered is the highly corrosive, erosive
multivariable controller, engineers continued to monitor nature of natural gasoline. Dissolved salts coupled with
the operation daily, review it and fine tune it. They are entrained water cause highly accelerated rates of corrosion
putting together constraint reports for both hourly and in the overhead systems in the feed fractionation section.
supervision to look at and learn from. In other words, We take the natural gasoline and split out the C5s and
you want to know what constraints are constraining your C6s for isomerization. To combat this corrosion, a filming
unit at rate and conversion all the time and why. They corrosion inhibitor is added to the overhead system to
are interested in not only which constraints they are but reduce the corrosion potential in these towers.
how much they are costing you. Another problem which we have encountered is high
This is a learning process for the engineer, the operators, fouling rates in the Penex hydrotreater feed effluent
supervision and management too. Some of the old exchangers which has been linked to the contaminants
assumptions that we had about rate versus conversion such as cyclic and dicyclic diolefins in the incoming natu-
have gone out the window when you really have the built- ral gasoline shipments. Ethers such as MTBE and associ-
in knowledge of the advanced controller. ated peroxides along with dissolved oxygen have also been
Finally, as we put these systems in, we are displaying detected in the incoming natural gasoline. The diolefins
more and more economic information to the console begin a Diels-Alder type polymerization which is some-
operators about things such as constraint costs. The engi- times accompanied by a free radical polymerization initi-
neer on the application typically spends a fair amount of ated by the ethers and peroxide species. These reactions
time working with the operators not only to understand form a high molecular weight polymer which lays down
the constraints, but also what it is going to take to remove on the exchanger tubes in the vaporization zone, basically
the constraint and what is the value of removing the con- the hottest, or last two exchangers in the train.
straint. To alleviate this problem, more rigorous controls have
been placed on the natural gasoline shipments. We are
doing quite a bit of sampling throughout the system.
ROMAN: That in itself has helped the problem. I think people
Ashland has just begun deploying Windows NT sta- that may be dumping material are backing off of that to
tions with an interface to the control room board opera- some degree.
tors. It is planned that these systems will include higher The best solution to the problem obviously is to elimi-
level programs for assessing plant operations such as opti- nate the source of the contaminates. But even though
mization, expert based troubleshooting guides and statisti- this appears to be happening, I do not think that we can
cal process control. Several plans for operator training are count on this on a regular basis.
also being evaluated. We evaluated an oxygen stripper, adsorption beds and
Both navigational issues and interpretation of results chemical treatments. There is no chemical treatment that
are important. Ashland has found that as with all automa- we found for the Diels-Alder reaction. The oxygen stripper
tion systems, while some degree of generalized classroom is expensive and only addresses part of the problem. The
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adsorption beds and their associated regeneration equip- of natural gasolines, especially as related to feed to hydro-
ment would be costly and we question their effectiveness. treaters. We have been able to use those analytical tech-
The solution that is being implemented is the installa- niques to solve some other problems.
tion of a second set of the hottest feed/effluent exchangers
that can be switched ‘‘online’’ to clean the exchangers. ANDREW W. SLOLEY (Process Consulting Services Inc.):
At its worst point, we were only able to operate the Processing significant amounts of natural gas conden-
unit for three months at a time. The installation of the sate through a refinery typically loads the atmospheric
new exchangers will keep the unit online as we continue crude column condensers and the saturate gas plant.
to try to eliminate the source of the contaminants to Depending on the quantity and composition of the con-
extend the run length between cleanings. densate the effects can be significant. When processing
condensate the atmospheric column flash zone pressure
will rise. In some cases the pressure change can be as high
PETERSON: as 15-20 psi. This lowers atmospheric column cutpoint
We ran into a problem with elemental sulfur formation and loads the vacuum unit heater and column. If the
in our saturated gas unit running natural gasoline. The condensers are designed for the condensate the impact
apparent cause of this was oxygen that got into the trans- is negligible.
portation trucks that were bringing the natural gasoline
to our refinery. The natural gasoline was charged to a DONALD BIGGS (Silver Eagle Refining, Inc.):
saturated gas debutanizer. In the overhead system, the Mr. Samuels, was this corrosion on the deisopentanizer
H2S and the oxygen reacted and made the sulfur. This overhead system?
resulted in 4 A copper strip corrosive normal butane,
which after fractionation, is where the sulfur ended up. SAMUELS:
This was a problem discovered on a Friday afternoon, so That is correct. The natural gasoline is first debutanized
we had to solve it pretty quickly. We tried everything we and then deisopentanized. Both columns exhibit overhead
could that afternoon. We were just starting to sell butane corrosion problems, not reboiler problems.
seasonally instead of blend it all into the gasoline pool. Question 42.
We switched it over to the naphtha hydrotreater and What are the experiences and/or new developments with
we have not had any of the problems that Mr. Samuels the use of cloud point depressants?
has alluded to with natural gasoline going through the
hydrotreater. We must have a cleaner source of natural PETERSON:
gasoline than he has. The Alma refinery has a big market for low cloud
point materials since they market in an area where the
temperature gets down to 40 below zero in the wintertime.
BINFORD:
They also do not want to use a lot of their No. 1 fuel
We worked with Marathon Research on the problem oil in No. 2 as blendstock. They have put in an MDDW
that Mr. Samuels was referring to. A couple of interesting (Mobile Distillate Dewaxing) process several years ago
things really came out of that. One of them was that the and they have just in the last year been working with
standard analytical characterization of the natural gasoline BetzDearborn on cloud point depressants. The depression
streams did not show a propensity to foul significantly that we have seen has ranged from 3 to 6°F depending
since the natural gas condensates were low in unsaturates. on what streams are going into the pool at the time.
Therefore, bromine number did not tell us anything. The Experimentation is still continuing at this time.
streams also had low existence gums content and they did
not form gums by oxidation in a potential gum test either. BINFORD:
As a result, many of the reaction mechanisms and Yesterday there was a question asked about economics
reaction precursors that Mr. Samuels talked about were in the diesel pool and I deferred that to this question. I
discovered through more sophisticated analytical tech- will try to answer it here today as well as talk a little bit
niques. I wish that I could report that it was a BetzDearb- about some of the fungibility issues with using cloud
orn chemical that solved the problem. Obviously, he did point depressants. I know this has been a real key issue
not refer to one. We did try chemistry there and found in the refining sector this year in downstream marketing
that the polymerization was just too aggressive and the as well.
contaminants in that particular stream were too high to We have used cloud point depressants at dosages
be solved by a chemical antifoulant program. between 25 and 100 ppm and therefore have had less
However, I think it was a very worthwhile project impact on other cold flow additives as opposed to tradi-
because it did lead us to some new analytical techniques tional cloud point depressants that are used at much
and some new logic trees to be able to evaluate the impact higher dosages.
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Traditional cloud point depressants are nucleators that use of cloud point depressant in these cases is justified
cause many sites to initiate crystal formation, making each on the diesel uplift value. The downgrade of diesel range
site smaller than additized at the cloud point. That is product also has consequences on downstream conversion
what gives you the depression. When the wax is crystallized units as was discussed previously.
in great numbers at the pour point, the amount of nucle- If you can pull the tail end of the AGO out, usually
ation sites cause an increase in the crystal formation and a compelling reason to do so is the fact that you can
propagation. Thus the traditional cloud point additive purchase AGO to back fill the FCCU and still maximize
can effectively raise the pour point. To offset this problem, your charge rate to the FCCU. Obviously, some people
traditionally much more pour point depressant has been have the capability or the means to do that by purchasing
needed versus the normal or base case without cloud gas oil, while for others the economics may not drive it
point depression. that way.
As a result, the use of cloud point depressants in the Regarding fungibility, the last issue that I will cover,
past have not been economical in most cases. New, more one question that continually arises is the fungibility of
effective cloud additives have been developed in the last cloud point additives with other refinery additives and
two years that are effective at much lower treatment rates. downstream terminal additives. As a result of the concerns
The lower treatment rates solve many of the incompatibil- raised by several refiners and pipeline companies last win-
ity problems between cloud and pour. ter, we tested the compatibility of our additive in many
Regarding economics, the main economic driver that environments. We performed testing using dosages of
we see justifying cloud point depressant programs is the cloud additives that represent ten times the normal refin-
reduction of jet kerosene blend into the diesel to meet the ery treatment. This is to show the worst case overdose situ-
cloud point specification. Many refiners use jet blending at ation.
the tank farm as a trim input to manage the cloud point The overdose fuel we tested were subjected to NACE
spec or to make different batches of distillate products corrosion tests and 300°F 90 minute stability tests with
with different cold flow specifications using the same no impacts on either of those tests and no degradation
diesel base stock. from the level of base fuel. The overdosed fuels were then
We have noticed that there are not systems or people dosed with acidic based corrosion inhibitors and distillate
in place in many refineries to economically capture jet inhibitor additives. In these cases, the overdosed additive
diesel margins that appear in the winter season. In most did not affect the responses of the other two additives.
cases, the complete amount of kerosene blended into the We have also seen that the cloud point additive is
diesel cannot be eliminated, so an optimal amount of viable in a fungible cloud/pour environment. Early this
kerosene relative to chemical is needed. The optimum winter we collected fuels from three different regions of
will change depending on the overall reduction needed the country: northwest, Gulf Coast and East Coast. In
in the economic margin between kerosene and diesel. each region, at least one untreated fuel was obtained as
For many refiners, the jet or kerosene market is not well as two others that were treated with pour point
compelling enough or available enough to pursue. These depressant at the refinery. The untreated fuel was treated
refiners blend all of their kerosene range product into with cloud depressant until the fungible pipeline spec was
distillate fuels because there is no other disposition or met and then it was blended into each of the other regional
they do not produce any kerosene range cut to start fuels to mimic transportation in the pipeline.
with from their crude fractionation towers. In most cases, In each case, the untreated fuel caused no product
however, these same refiners limit the endpoint of their harm. The fuel started on spec and after mixing they
distillate fuels due to cloud point. ended on spec. This data not only showed that the cloud
ASTM sets the 90 percent distillation point of No. 2 additive was responsive to a broad range of fuels, but also
diesel at 640°F and some pipelines set the endpoint spec that it posed no risk to cloud/pour fungibility.
at about 690°F. Very few refiners actually meet these
specifications. Most will limit their 90° or endpoint HAHN:
because they cannot meet their cloud point specifications We independently verified that the newer cloud depres-
at the same time. As a result, the tail end of the diesel sants can be economically attractive and are planning a
range product gets downgraded into gas oil. I use that term full scale field trial this fall when the economics change
down grade loosely because there was a lot of discussion in favor of jet fuel. There are farther pipeline and terminal
previously about whether or not diesel is a good thing or issues to resolve before these additives can be used at
a bad thing to put in your FCC. Obviously that is very our facility.
situation and refinery specific.
If there is a benefit to pulling the tail end of the AGO THOMAS SOPKO (Lubrizol Corporation):
up into the diesel pool, the economic spread between The experience of our customers using Lubrizol’s cloud
those two cuts can be typically very large. Therefore, the point depressants has been very positive as stated by the
42 General Processing
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previous speaker. By depressing cloud point with an addi- flame pattern which sometimes blows out the pilot. That
tive, refiners were able to increase their operational effi- problem is an easy one to solve, you just do a better job
ciency and profitability in three ways: of inspecting your flares.
1. pulling kerosene out for jet; For inappropriately remanufactured or reconditioned
2. upgrading heavier stocks to diesel; and pilots, one of the things that we are doing right now is
3. running at higher end points. revamping our engineering standards for flares to ensure
These refiners are achieving 4 to 8°F cloud point that only the appropriate placement parts or equipment
depression along with getting pour point depression with are purchased for the pilots.
the same additive and at modest treat rates. Simple returns Finally, for thermocouple failures, we are testing Stack-
on investment in excess of 100 percent are very common. match igniters, retractable thermocouples to see if these
To further answer this question, we have a two minute offer a better solution.
video introducing and documenting the performance of
Lubrizol’s cloud point depressant and it has been recently JOSECK:
sent to each oil movement manager at each refinery in At one refinery, all the pilots have been targeted, includ-
North America. Additional videos and case histories in ing flare, boilers and process heaters for conversion to
literature are available from the Lubrizol Corporation. natural gas due to fouling. A significant number of the
pilots have been converted.
LINAS JOKUBAITIS (The Lubrizol Corporation): Although the expense is large to use natural gas versus
In Lubrizol’s development of new cloud point depres- refinery gas, the reduction of lost production time due
sants, we found it important to match wax characteristics to a total process heater shutdown versus a single burner
to additive selection. shutdown is not insignificant.
To address a broad range of fuel qualities, we developed The reliability of the burners in process heaters have
products around four distinctively different chemistries. beeing improved, resulting in an opinion of safer opera-
This allows the refiner to achieve cloud point by matching tions. A second refinery has switched the flares and the
the right additive to their fuel. Our customers are using sulfur incinerator pilots to natural gas to eliminate fouling.
these additives in continuous as well as batch operations. Question 44.
They experience treat rates of 50 to 250 ppm giving a Has anyone had success in improving refinery loss
nominal 4 to 8°F cloud depression, which exceeds the accounting by measuring mass directly with mass flow
two degree of test reproducibility. They also see pour meters on key input and output streams?
point reduction from the same additive.
In the video that was recently sent to each refinery, we ROMAN:
document that our cloud point additives are not masking Ashland installed coriolis based mass flow meters on
agents, but truly modify the thermodynamics of wax crys- two crude units with the goal of improving the weight
tal formation. balance at one of its refineries. They proved to be of very
little use and are not used by the yield department. The
Question 43. overall refinery balance is still based on pipeline deliveries
Are you experiencing pilot problems on your flares, incin- and changes in crude oil inventory. The density meters
erators, air heaters, boilers, etc.? Explain the problems, which came with them, however, have been very reliable
and, if you have solved them, please explain how. and have become very valuable in determining and
responding to crude oil switches.
FUSSELL:
We have a lot of problems with our pilots at our Port Question 45.
Arthur refinery. Most of these problems are caused by a Do you employ any non-destructive testing techniques
variety of contaminants in our refinery fuel gas system. to check blockage of lines at high temperature, when
We are slowly converting all of our pilots over to natural radiography can not be done?
gas. We started out with the most critical ones which CAIN:
would include the flares, the incinerator on our sulfur We use infrared imaging equipment which has been
units as well as our thermal reactors on our sulfur units. successful to check for blockages of lines that have high
temperature.
FOSTER:
Our main problems with flare pilots come down to HENKE:
four basic causes. One is plugged pilot gas filters. To We have successfully employed gamma ray techniques
correct this, we have replaced carbon steel. A lot of our to check for blockage in lines operating at high tempera-
carbon steel gas lines on our older flares have stainless ture in our refineries. Tru-Tec tells us that they are fre-
damaged flare tips. The damaged flare tips cause an erratic quently asked to use neutron back scanner and gamma
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 43
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44 General Processing
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 45
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 47
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thermal expansion of the coke and the refractory which material to be properly squeezed back behind the hexmesh
causes the spalling during the temperature cycles. anchor to provide maximum holding power. As far as
We assess remaining useful life by taking core samples vibracasting is concerned, most refractory manufacturers
during shutdowns and by online thermography to observe do not recommend installing vibration cast materials if
thinning or failure. the requirement is less than three inches thick. For
cyclones, the overall weight of the cyclones, complexity
TASKER: of the forms, and the cost of the installation would be
I agree with what Mr. Roman has said. In regard to prohibitive.
the second section of this question, we have had good
experience in Japan with double layered refractory. How- SAMUELS:
ever, when cracks do occur, you can get coke migration. In Marathon’s experience refractory wear in cyclones
The coke between the layers of refractory is what leads is due to a number of factors: improper refractory prepara-
you into spalling tendency. Some operators have had very tion or installation, improper refractory anchoring systems
bad experiences in that regard. and exceeding design conditions on cyclones.
We have used hexmesh for the upper layer abrasion We are probably going to be the odd man out here,
protection, but the experience has not been very good. but AA-22 remains our current choice of refractory lin-
It is best to limit the use of hexmesh to the internals. ings. We would agree though that regenerator cyclones
With single layered refractors, there are less problems; use are good candidates for ceramics and plastics, due to
of the Resco RS9 has been good. ease of dry out and some of the things that Mr. Roman
In relation to the next question coming up, use of mentioned. But we have little experience with this. I think
Resco AA-22 or its equivalent has also been good. This iron content can be very important in your refractory
is a very hard abrasive resistant refractory. Typically, we selection in the regenerator due to the presence of CO.
see that patching is performed every second turnaround Refractory anchoring and workmanship is critical to
and complete replacement is very infrequent. the long life of refractory linings. For repair work, S bars
are good anchors for small areas. Original construction
PETERSON: is hexmesh. Flexmetal is also starting to be used, but
Our original reactor refractory lasted about 15 years Marathon does not have a lot of experience with this.
in the Ardmore refinery. There was some cracking and Weld patterns of hexmesh are critical in getting long
some spalling problems over the last few years. It was a anchor life as well as working with the proper metallurgy
two component system comprising AR400 and LW80. in your welding rods.
The Arkansas City refinery installed new reactor refractory
in 1992 which held up well until the refinery was shut REZA SADEGHBEIGI (RMS Engineering, Inc.):
down last year. We put the same system, which is a If the cyclones are properly designed, a typical one
six inch single layer of thermex ES, in the reactor. The inch thick refractory lining using AA-22S or a plastic
anchoring system uses steerhorn and stainless steel wire should be adequate for long cyclone life.
screen. Details can be included in the transcript. Premature failure of this refractory is often related to
We used periodic thermographic surveys to look for the following three factors. The first is, excessive catalyst
the hot spots and we have not been inside this reactor loading into the first stage cyclone and the ability of the
yet. We hope to not get into it until late 1999. first stage cone and diplegs to get rid of the catalyst.
We normally recommend that the design of the primary
Question 6. diplegs should be so that the mass flux through the primary
Due to unit expansions, we have experienced wear of diplegs would not exceed 125 pounds per second per
the AA-22 refractory cyclone lining. What new types of square foot.
refractory, ceramics, or installation technology (e.g., If the loading gets too high in the primary dipleg, the
vibracasting) are refineries using to extend cyclone life? secondary cyclone are not normally designed to handle
that additional catalyst loading. Therefore, you may see
ROMAN: extensive erosion in the primary cyclone inlet and primary
Ashland has not used AA-22 in our cyclones for several cyclone outlet.
years. We are currently using a fine grain 85 percent The second parameter is, as the panelists stated, high
aluminum phosphate bonded plastic ramming refractory cyclone inlet and outlet velocities. We would recommend
which provides excellent service with abrasion loss per that these velocities be maintained less than 60 feet per
ASTM-704 of around four ccs. The added benefit with second for the inlet and definitely less than 100 feet per
the use of plastic is the ease with which the material can second for the second stage outlet.
be placed. The material is moldable up to the initial Many FCCUs, especially in regenerators, are running
phosphate reaction temperature of 450°F. This allows the cyclone outlet velocities as high as 250 feet per second.
PETERSON:
We have seen a qualitative association between how
much air or oxygen is brought in with the aerated catalyst
back to the reactor. I do not have an exact correlation,
but it is the kind of an association that we have seen. If
we are running higher phenols, we will take a good look
at how we are aerating the catalyst coming back in.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 49
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Also, if you are recycling water back through the strip- The result is that per gram of platinum the In Situ
per to the desalter, you need to be careful that your not Pro has been demonstrated commercially to be two to four
losing amine from the gas treating system into the refinery times as effective as the separate combustion promoter
sour water system. Amines coming back through the additives. So with the more effective platinum, you would
desalter with the stripped sour water can not only cause expect that the NOx would go up and that is true. How-
problems in the desalter itself, but some of those amines ever, this technology allows you to use a much lower level
can form salts in the crude tower depending on the type of platinum and also allows you in many instances to
of amine and tower operating conditions reduce the excess O2 significantly without after burn.
I have one commercial example to illustrate this. This
customer had a UOP high efficiency regenerator design
3. Regeneration running in total combustion prior to the use of In Situ
Pro catalyst. They were using bag promoter. The platinum
Question 8.
averaged 0.5-1.0 ppm on the Ecat, and they had occasional
What can be done to reduce NOx emissions?
problems with after burn.
Using the In Situ Pro they were able to stepwise lower
FLETCHER: the level of platinum to 0.3 ppm with no trace of after
Reduction of NOx can be achieved by (1) minimizing burn. The steady addition of promoter with the fresh
flue gas excess oxygen levels or operation in partial burn catalyst led to noticeably smoother temperatures in the
mode, (2) minimizing promoter usage, (3) using additives regenerator which allowed them to operate at significantly
such as NOx, SOx or De-SOx, and (4) hydrotreating lower flue gas oxygen levels, less than 1.0%. Besides reduc-
the feed. ing the promoter cost by about $30,000 a year, they
Regarding minimizing oxygen in the flue gas, NOx measured significantly lower NOx emissions.
reductions can be achieved by operating at partial burn One very excellent reference that I would recommend
or with as close to zero excess oxygen as is feasible. One is a paper written by Alan Peters entitled ‘‘Origin of NOx
pilot riser study undertaken to demonstrate the advantage in the FCCU Regenerator’’. This paper was published in
of switching from a full combustion to a partial combus- the May/June, 1995 issue of Fuel Reformulation.
tion operation observed a drop in NOx from 85 to 20
ppm. MALEK:
For the full burn operation, operating at or below 0.5% Currently, there is not a lot of control of NOx down-
excess O2 reduced NOx about 20 percent when compared stream of FCC regenerators. However, there are available
to the same operation at one to two percent excess O2. technologies, and refiners are preparing to implement
One of our customers which operates in full combustion these as the need arises. As one example of this on partial
mode measured 370 ppm NOx with nearly zero excess burn units, the Cohen Corporation has demonstrated
O2; 430 ppm NOx with 0.5% excess O2, and 540 ppm commercially the ability to control NOx significantly by
NOx with 2.0% excess O2. staged combustion in the CO incinerator. They do this
This data indicates a 25 percent and 45 percent increase by controlling the addition of air to the combustion zone
in NOx for increasing the excess oxygen from zero to a in a secondary location. This allows two temperature zones
half a percent and then from a half a percent to two inside the combuster.
percent, respectively. So there are some advantages in Another approach is to use ammonia based compounds
minimizing O2. in CO boiler on a partial burn type of unit. Urea solutions
Regarding the NOx-SOx type additives, these have or other forms of ammonia can be used. Generally, this
been shown to reduce NOx in both pilot plant risers and requires operation in the 1,500 degree range for the use
commercial units. One pilot riser test demonstrated that of additives to be effective.
adding 0.5 wt% DeSOx produced a 20% reduction in Another technology that is offered by Belco Technolog-
NOx, while additions at 1.0 wt% reduced NOx by 30- ies, and this operates at a much lower temperature. They
35%. provide in their design of wet gas scrubbers for the addi-
Regarding the use of combustion promoters, it has tion of a proprietary catalyst which is added into the
been demonstrated that they increase NOx formation. system ahead of the wet scrubber. While operating in the
Pilot riser work has shown that the addition of 0.5 wt% range of about 600°F, they get very effective control of
loose promoter increases NOx four-fold. One alternative NOx using this technique.
promoter technology for those refiners that are forced to
use the combustion promoter is Akzo Nobel’s In Situ Pro ROMAN:
technology. This approach impregnates the platinum on NOx can be reduced by operating the regenerator in
the catalyst itself rather than having a loose additive which partial burn, using selective reduction with ammonia or
results in better dispersion of the platinum crystals. area and by hydrotreating the feed. Our work has shown
that approximately seven percent of the nitrogen in the One of the ways we have cooperatively gotten people
coke leaves the regenerator as NOx. Even though hydro- to reduce NOx is to simply reduce throughput for four
treating of FCC feeds is performed primarily to lower to six hours which will shave the ozone peak off ozone
sulfur in cracked products, it will also lower contaminant high for the day and hopefully keep us out of exceedences.
nitrogen. Feed nitrogen and consequently coke nitrogen I do not know if it would work in other parts of the
can be decreased by up to 90 percent. country or not, but reducing emissions four to six hours,
Temperatures in the regenerator are too low to form two or three days a year is sure a lot cheaper than some
thermal NOx from nitrogen, but this can take place if of the other NOx control systems.
you have a CO boiler downstream in the regenerator. We
have looked at additives to reduce NOx. Blending FCC REZA SADEGHBEIGI (RMS Engineering, Inc.):
catalyst with copper ZSM-5 at levels above one weight I would like to clarify what was said by the panel about
percent reduced NOx by 50 percent, but unfortunately the partial combustion. Although partial combustion has
resulted in substantial losses in gasoline selectivity and many benefits, the total NOx leaving the CO boiler is
increased coke and hydrogen production. going to be higher in partial combustion than in full
The loss in gasoline selectivity was mainly a result of combustion. Oxygen enrichment and urea injection are
the ZSM-5 component. two of the methods used to reduce NOx emissions from
Taking a regenerator from partial burn to complete a partial combustion operation.
burn results in an increase in NOx of between 35 and
135 percent. We usually see the NOx increased by at LAWRENCE J. LACIJAN (UOP):
least 100 percent across the CO boiler due to the thermal In addition to the comments already made about oxy-
fixation of nitrogen from the combustion air. gen, we believe that minimizing platinum is really one
Use of combustion promoters or de-SOx additives can of the keys for reducing NOx. In the combustor style
also increase NOx. In one test, the presence of one ppm regenerator that we use where we mix the spent and the
platinum on the catalyst doubled the NOx. We have also regenerator catalyst before combustion, we operate in full
seen NOx increases as high as 50 percent caused by the combustion without any platinum. We believe that we
presence of de-SOx additives. can get down in most cases with reasonable feed nitrogens
to less than 50 ppm NOx.
TASKER:
In addition to all of that, we think part of the problem G. ANDREW SMITH (INTERCAT, Inc.):
associated with NOx is that ammonia is used in the Using INTERCAT’s low platinum promoters with our
catalyst manufacturing for leaching the catalyst and this patented injection system, we have been able to reduce
remains with the catalyst or some of it does. This is released NOx emissions in full burn units by as much as 50%.
during the regeneration leading to NOx production. It We believe this is an excellent way to address this problem
can be avoided by double stripping of the catalyst, but with minimum cost.
this tends to be somewhat expensive.
Also, as mentioned, if the feed is deeply hydrotreated, SAMIR HALAWANI (Saudi Aramco):
then the nitrogen is reduced and therefore NOx emissions What is the NOx and SOx testing frequency and the
are also reduced. We feel that NOx emissions from a method to measure them?
cracker should be in the range of 50 to 150 ppm depending
on the nitrogen in the feed. If values are much higher ROMAN:
than this, the unit is probably using a CO promoter It depends on our facilities. Most of our operating
and there will be excess oxygen. One of the newer non- permits require annual testing. Heaters which have trig-
platinum promoters can be used or the excess oxygen can gered NSPS usually have continuous emission monitors.
be reduced.
Catalytic reduction of the NOx emissions produced DAVID SAMS (Grace Davison):
can be used as an extreme case though the normal amount As many of the panelists have mentioned, it is well
of NOx leaving the FCC does not warrant implementa- known that platinum based promoters contribute to the
tion of such technology unless regulations require that. formation of NOx. To address this, Grace Davison has
developed a new promoter called Ex-NOx which has a
JIM STONE (Louisiana Department of Environmental Quality): unique chemistry.
One of the reasons that we control NOx is to control Earlier this year, a West Coast refiner conducted a trial
ozone. In Louisiana, we are kind of lucky because we where they replaced their platinum based promoter with
have a model which shows us when we are likely to have Ex-NOx. Following the transition period, the NOx level
an ozone problem; it comes over from Texas and then lined out at about 50 percent of the base level with compa-
over Beaumont towards our area. rable CO after burn control. They considered it a success
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 51
TOC/INDEX
and also a clear demonstration of the contribution that UMA SHANKER (Indian Institute of Petroleum, Dehradun, India):
platinum makes to the formation of NOx. NOx emission from FCC regenerator flue gas can be
controlled within acceptable limits by the controlled use
of oxidation promoters and air. DeSOx additives are also
R.C. SKOCPOL (Akzo Nobel Catalysts, FCC):
known to catalyze the union of CO/coke and NOx to
I believe it was Mr. Tasker who mentioned the ammo-
form molecular nitrogen and CO2 thereby diminishing
nia in the fresh catalyst might possibly lead to NOx. I
NOx emissions. Refineries having electrostatic precipita-
disagree. Look at the other ammonia that is around in
tors and CO boilers using both CO-oxidation promoter
the system, all the nitrogen in the coke, which is like
and DeSOx additive are using selective reduction of NOx
almost half of the nitrogen in the feed. According to the
by injecting NH3 into cooled regenerator flue gas. Devel-
literature, all the nitrogen is in coke gas through a cyanide
opment of DeNOx additive is still in research stages.
or an ammonia intermediate before it winds up being
either NOx or N2. Luckily most of it winds up as N2. Question 9.
Any traces of ammonia added with the catalyst might Please discuss the advantages and disadvantages of
even react with NOx to get rid of it and turn it into N2. operating in partial burn versus operating in complete
All in all, if you look at all the sources of nitrogen and burn with heat removal devices, such as catalyst coolers,
ammonia that are present, any good or bad effects of a when processing resid.
little bit of ammonia coming in from another source such
as fresh catalyst would be pretty negligible. ROMAN:
As you increase the concarbon, you will have to go to
RAGHU MENON (BOC Gases): partial burn, add a catalyst cooler or both in order to
In general terms, FCC-related NOx can be reduced heat balance the unit. It is certainly cheaper to install a
by four types of approaches: catalyst cooler than a CO boiler and that would be our
1. feed nitrogen reduction by hydrotreating; first choice.
2. choice of suitable FCC operations modes; As the vanadium increases, catalyst activity will decline
3. hardware/unit-design based approaches; and and consideration should be given of going to partial burn
4. flue gas treatment. with a CO boiler. Operation in partial burn keeps the
Because it has now been established that FCC-related vanadium in a plus four valence state and renders it rela-
NOx originates from feedstock nitrogen, the first tively immobile. This reduces the loss in catalyst activity
approach can be very effective. Removal of the types of at high loadings.
feed nitrogen, which principally go to FCC coke, require This benefit is somewhat offset by the higher carbon
medium to high severity hydrotreating, which is very on catalyst levels that most partial burn units experience.
expensive. A number of process variable manipulations Most resid catalysts have an active matrix which distributes
are known to effect NOx. For example, for complete the carbon over the whole catalyst particle and the effect
combustion operation, NOx can be reduced by lowering of increasing carbon on regenerated catalyst is not as
the level of excess oxygen in regenerator flue gas and pronounced as it used to be.
decreasing the level of Pt promoter addition. Operation Ashland also operates a two stage regeneration system
using oxygen-enriched air can also be expected to lower which requires both a catalyst cooler and a CO boiler. This
NOx due to higher coke and carbon monoxide levels for allows most of the carbon to be burned off in reducing
certain types of operations. Other approaches reported in atmosphere while still attaining complete removal of car-
literature include injection of NOx reducing gases into bon from the catalyst.
the regenerator vessel or downstream sections, and the The second stage section is maintained in a completely
addition of Pt promoter for NOx reduction in partial oxidizing atmosphere, but the residence time is quite low
combustion operation. The use of catalyst additives for to minimize the redistribution of vanadium.
NOx reduction is not yet widespread. A number of the
hardware approaches are based on the contact characteris- TASKER:
tics between the coke-laden catalyst and flue gas. Examples The two philosophies that we have are the complete
of flue gas treatment include selective noncatalytic reduc- regeneration and the partial burn. We typically use the
tion approaches involving the addition of compounds two stages to burn most of the hydrogen off the soft coke
such as ammonia and urea, standard and novel types of in the first regenerator. Most of the water is removed
flue gas scrubbing approaches, and SCR (selective catalytic at that stage. This represents about 60 percent of the
reduction). The scrubbing and SCR approaches may be combustion.
used for reduction of NOx to very low levels, but are Now, the catalyst deactivates as you know mostly due
both expensive and involve waste disposition require- to vanadium contamination. The vanadium attacks the
ments. zeolite by first forming V2O2 which then forms a vanadic
acid in the presence of water. So if the water is removed advantages. Partial burn regenerators have lower gas vol-
early, there is less chance that the catalyst will be attacked. ume in the regenerator vessel allowing smaller vessels and
In addition with the partial burn, oxygen will be less and, cyclones and lower cyclone velocities.
of course, oxygen is required to form V2O2. Another design consideration is that the balance of the
In the first burn stage, CO is formed since there is a combustion air can be put into the CO boiler at lower
lack of oxygen, therefore, vanadium oxidation will be pressure, so that the blower operates against lower head.
minimized. In the second stage since most of the water Operating advantages include lower catalyst additions as
has already been removed, there is less tendency to make a result of the lower oxidation state of vanadium and also
vanadic acid. This gives more protection of the catalyst lower afterburning. High pressure super heated steam can
and results in better operation. But, of course, there are be produced in the CO boiler.
differing opinions on this mechanism. Finally, there is lower hydrogen yield achieved in partial
burn as a result of lower nickel activity and this frees up
JOSECK: some compressor capacity.
For the RCC in Shreveport, the new unit, by running
a 4.4 mole percent CO in the off gas, the regenerator RAGHU MENON (BOC Gases):
heat load is reduced by 30.5mm Btu/hr. The catalyst Partial combustion mode operation enables better tem-
cooler is designed to remove an additional by design perature control, but requires a flue gas boiler for CO
52mm Btu/hr. Both are independent ways to adjust the post-combustion, and can result in high CRC (carbon-
heat balance. Since going from full burn into partial burn on- regenerated catalyst) levels. The use of catalyst coolers
involves an unstable region, we maintain the regenerator for complete combustion operation enables temperature
in partial burn and use the catalyst cooler to adjust regener- mitigation from a regenerator/flue gas hardware perspec-
ator temperatures. The unit has a capacity of 10,600 tive, and allows for the catalyst-to-oil (C/O) ratio to be
barrels a day running at 80 percent conversion and pro- maintained at reasonable levels. Complementing a catalyst
cesses feedstocks with gravity of 19° API. The feed con- cooler with increased coke burn capability and efficiency
tains lube extracts and vacuum resids with a Conradson using oxygen enrichment or other means can enable
carbons between 6 and 7%. exploitation of higher C/O (higher conversion) and a
wider operating range, while simultaneously maintaining
FLETCHER: CRC levels. Ability to control CRC enables better reactor
For the complete burn operation, catalyst coolers allow product selectivity.
the reduction of carbon on regenerated catalysts but pay
a penalty in coke yield and blower capacity. Producing UMA SHANKER (Indian Institute of Petroleum):
steam in a catalyst cooler requires heat and thereby In partial combustion mode some of the carbon on
increases coke yield. The complete combustion mode is the spent catalyst is incompletely burned to carbon mon-
easier to operate and provides a distinct operating benefit oxide but regenerator temperature is limited and con-
for a refiner whose regenerator is subject to maldistribu- trolled by regulating flow of air. The full combustion
tion of catalyst and air. mode of regenerator utilizes excess oxygen for complete
A risk observed with a complete combustion operation CO combustion and reduction of carbon on the regener-
is that of the catalyst cooler or bed coil failure which ated catalyst to less than 0.1% wt increasing the catalyst
will damage the catalyst inventory and potentially limit activity and selectivity.
throughput. Advantages and disadvantages of full combustion are:
For the partial burn operation, there are also several Advantages:
benefits. The metals benefit has been covered. The partial ● higher catalyst selectivity because of lower carbon
burn operation allows control of the regenerator tempera- on the regenerated catalyst;
ture without the additional coke make and thereby reduces ● lower CO content of flue gas, allowing it to be
blower capacity. The key to good partial combustion released to the atmosphere; and
operation is air distribution which allows the carbon on ● higher heat release in the regenerator beneficial for
the catalyst (CRC) to be kept within reasonable limits. processing hydrotreated stocks not producing suffi-
With the partial burn operation, you also have the benefit cient coke for heat balance.
of operating with a lower regenerator superficial velocity. Disadvantages:
● lower catalyst/oil ratio because of higher regenerator
DAVID MCCAFFREY (Exxon Research & Engineering Company): temperature;
We have experience running feeds in the three to four ● harder impact on catalyst activity due to thermal/
concarbon range with partial burn regenerators and feel hydrothermal deactivation;
that this approach offers design, operating and yield ● greater requirement of air; and
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 53
TOC/INDEX
process which has been proven to upgrade the FCC cata- G. ANDREW SMITH (INTERCAT, Inc.):
lyst inventory through magnetic separation and removal Monitoring the hydrogen-to-methane ratio works well
of the oldest most metal laden, least active and least with antimony, an EPA listed hazardous chemical, and
selective FCC catalyst particles. bismuth, a chemical that is not listed by the EPA as
Removal of these particles leads to improved gasoline hazardous. However, with bismuth less methane is pro-
selectivity as well as lower coke and gas selectivity. Test duced resulting in higher ratios with the same hydrogen
runs at our first commercial unit at our Canton Refinery production.
showed significant profitability improvements, primarily Unless these additives are over used, the impact on
due to increased alkylation charge and gasoline yields at CO Oxidation promoter is minimum.
lowered fresh catalyst addition rates. The FCC unit Solid vanadium traps offer additional benefits over
showed conversion increases from 75 to 82 percent and liquid programs with no impact on the CO Oxidation.
gasoline yields increased from 62 to 65 percent. Hydrogen INTERCAT has not observed negative impacts with
yields decreased as did coke by material balance, regenera- the use of liquid vanadium or nickel passivators on our
tor temperature and air blower demand. The clearest SOx reduction additives.
example of this effect was shown in the MAT analysis of
the FCC catalyst inventory, even though the fresh catalyst RAY MOTT (Grace Davison):
addition rate had been reduced by one-third to maintain It is important to recognize that most modern catalyst
inventory and unit activity in the proper range. The key designs use multiple methods of passivating and trapping
parameter changes at constant MAT were: the metals, things like RAM and OCM matrix, SAM
matrix, RV technologies, etc. They are all complementary.
Base Case 100% Magnacat They are all built into your catalyst systems already. That
Mat Conversion (vol%) 71.0 70.3 is why the industry has made a lot of progress in the
H2 Yield (wt%) 0.22 0.16 amount of metal levels they can process and the reductions
H2/C1 Ratio 0.56 0.38 in the amount of hydrogen produced.
Gasoline Yield (vol%) 59.4 63.3 I also wanted to comment on the effect of the reduced
Gasoline Selectivity (v/v) 85 91
retention of antimony in modern catalysts. What we think
Coke Yield (wt%) 3.9 2.7
is going on there is when the catalyst matrix has already
reacted with nickel or taken it out of service, what you
For further details, please refer to our 1997 NPRA see is that the antimony does not have anything remaining
paper, AM-97-32. to adhere to because it adheres primarily to the nickel.
When you see very low antimony retentions on modern
catalysts, that is indicating that the catalyst has already
R.C. SKOCPOL (Akzo Nobel Catalysts): passivated the existing nickel level in the inventory.
I thought I would offer a quick and easy check that
we found for catalyst based nickel trapping effects. If you DAVID B. BARTHOLIC (BARCO):
are also using antimony, and you begin using a catalyst One of the process technologies available for passivating
which traps nickel such as Akzo Nobel’s ‘‘i’’-technology, metals is the design feature incorporated into the Milli-
you will see that the retention of the antimony goes down. Second Catalytic Cracking (MSCC) Process available
For example, it might be 15 to 20 percent of the nickel from UOP. The ultra short contact time reactor design
by weight as opposed to the usual 30 or 40. You can see feature incorporated into the MSCC process results in
clearly that something is going on. passivating the metals so that one can greatly reduce the
Something is encapsulating or reacting with the nickel catalyst consumption as compared to conventional resid-
making it unavailable to react with the antimony. This ual oil FCC technology. As regards to SOx additives, the
suggests that the nickel is also unavailable to make coke dual reaction system design feature that can be incorpo-
and hydrogen, which is, of course, what we measure both rated into the MSCC reactor can result in a significant
in the lab and in commercial FCCU’s. reduction in SOx additive usage. These MSCC design
features will significantly reduce the catalyst costs and
SOx additive costs as compared to conventional residual
LANA CULLON (Wynnewood Refining Company): oil FCC technology.
We use antimony to passivate nickel and have had
good success. We have also tried a trial run with Nalco’s FRANK ELVIN (Coastal Catalyst Technology):
product for vanadium passivation. We saw passivation of Coastal’s new Demet process removes contaminant
the vanadium with no drastic effects on our CO promoter. metals from the FCC catalyst. What it does is increase
We chose not to continue the passivation of vanadium, catalyst activity and reduce the catalyst deactivation rate.
because the results were less than what we expected. But the most important thing it does is it reduces the
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 55
TOC/INDEX
catalytic coke at a fixed conversion, by at least 50 percent. to operate a single stage regenerator at high temperatures
If you use Demet, your regenerator CO2 emissions will with such high sodium levels.
go down and you will probably get a plaque from Green- Two stage regeneration is very effective for metals pas-
peace for encouraging ‘‘global cooling.’’ sivation. We have data from a number of our resid crackers
around the world, and many are typically running 10,000
MIKE ZETLMEISL (Baker Petrolite): to 12,000 ppm metals. Vanadium levels of 7,000 to 8,000
In addition to the traditional passivators, we have one ppm are being run on several of the units with no serious
developmental product which has shown some real prom- catalyst deactivation. Regenerator temperatures are run-
ise against vanadium. After several series of MAT type ning from 1,300 to 1,400°F in the second stage so this
tests working with one of the oil companies, this company is certainly an alternative. Two stage, independent regen-
also tested the product in their FCC pilot unit and based erators give the partial burn benefits without the problems
on the observed increases in gasoline yield and decreases of trying to control the carbon on catalyst.
in hydrogen and dry gas as well as coke, they are about All of the catalysts that we have used have had the
to trial the product in an actual operating unit. various metal traps that the catalyst suppliers are making.
Their products are continually improving and make resid
DAVID STONECIPHER (Nalco/Exxon): cracking the preferred cracking mode for the future.
Nalco/Exxon has been involved with the injection of
liquid feed additives to combat contaminant metals in Question 11.
the FCC since 1980. Our most recent experience is with What is industry experience with external reactor
a vanadium passivation technology marketed under the cyclones? Have there been any problems with leaks or
trade name MVP. It is described in the 1997 NPRA paper coking?
AM-97-29.
CAIN:
Over a dozen field applications and half dozen indepen-
dent laboratory studies have proven the viability of the Our Delaware City refinery tried one of these external
technology. We have generally seen up to a 50 percent reactor cyclones on the fluid coker and it coked up rapidly
reduction in the vanadium effect on the FCC catalyst. and developed leaks.
The benefits have included improved catalyst activity and
GEORGE QUINN (Amoco):
surface area, and this translates into higher gasoline and
With regard to external rough cut cyclones, we have
light olefin yields, more resid processing capabilities and/
installed rough cut cyclones on three units. Two of them
or an ability to cut back on fresh catalyst addition rates.
have been in place for 11 and 9 years. We have experienced
Proving vanadium passivation commercially can be a
no coking whatsoever in those rough cut cyclones, very
difficult subject due to the time required to flush out the
minimal refractory repair over that ten year period time,
deactivated catalyst from the unit, which can take two or
and no leaks on the bodies of the cyclones. I am aware
three months in some cases. We have gone with several
of a small leak on one unit which was rapidly repaired
different techniques to prove the viability of the technol-
on the rectangular crossover duct into the rough cut
ogy in a commercial unit.
cyclone. So our experience with external rough cut
The first technique is simple trending of unit operating
cyclones has been excellent.
data. Secondly, we will do point-to-point comparisons of
mass balanced operations. Third, we will perform some DAVID B. BARTHOLIC (BARCO):
off-line catalyst analysis, coupled with kinetic modeling to The Milli-Second Catalytic Cracking (MSCC) standard
smooth any feedstock differences. Reaction Mix Sampling reactor design contains external cyclones to clean up the
(RMS) may be employed here as well. Fourth and finally, reactor vapors upstream of the main fractionator. These
a new technique we are employing is to use more sophisti- systems have been in operation for more than three years
cated statistical modeling techniques. MVP has not been and there have been no problems.
shown to have any negative impact on NOx, SOx or CO
promoter additives. Question 12.
Refiners may increase FCC unit pressure to expand
WARREN S. LETZSCH, (Stone & Webster Engineering capacity. Increased reactor pressure is known to increase
Corporation): delta coke in gas oil FCCUs. Is the effect of pressure
Regarding sodium passivation, some past catalysts that different when processing residual feeds? What yield
contain special aluminas would form a sodium aluminate and product shifts might be expected?
that was very stable. I have seen a number of units that
could run with sodium levels about .8 up to 1.2 weight ROMAN:
percent and not suffer any real activity loss. Refiners might Ashland’s RCC technology utilizes both low reactor
want to consider such a catalyst. It may not be prudent pressure and lift gas to reduce hydrocarbon partial pressure
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 57
TOC/INDEX
Recently, we lowered the rare earth on the Robinson condensers; and (3) installing new high capacity tray tech-
FCC catalyst from 2.3 to 1.5 weight percent. C3 and C4 nology in the fractionators and the absorbers.
olefin yields both increased by a relative seven vol% at
constant reactor temperature. For this rare earth decrease, CAIN:
40 percent of the butylene shift was to isobutylene. One thing I would like to add is the use of advance
Just some general comments under operating changes controls. We have that in our Louisiana plant using DMC
to maximize recoveries, you can improve propylene recov- technology and we achieve above 94 percent propylene
ery by not over stripping in your de-ethanizer, increasing recovery.
your absorber pressure, and increasing the cooling of the
lean oil and the lean oil circulation rates. Also, hydrogen FLETCHER:
impairs recoveries and can be minimized through a metals It is often best to maximize light olefins production
passivation program. In all cases you have to keep the by making operational adjustments to lower light ends
ethane out of the debutanizer. yield and then adding ZSM-5. Lowering reactor tempera-
We think that the easiest way to dramatically increase ture or increasing rare earth on catalyst will lower light
propylene yield relative to butylene yield is choosing the ends yield. The propylene and butylene yield can then
correct ZSM-5 additive. Varying the silica to alumina be increased by the addition of ZSM-5. In this way the
ratio in the ZSM will substantially vary the ratios of dry gas and LPG saturates yields will be limited while
butylene produced per volume of propylene. We recom- maximizing C3 and C4 olefins.
mend that you work with your vendor to optimize your A high reactor temperature should be used if there is
propylene production. no limitation on dry gas yield. A proper riser termination
device is essential if very high reactor temperatures are to
TASKER: be run to minimize the degree of thermal cracking in the
The deep catalytic cracking process is designed to max- reactor vessel.
imize propylene for either petrochemicals or RFG produc- It is also important to optimize rare earth levels on the
tion. We have four units operating and four more in catalyst when maximizing light olefins yields. The ZSM-
engineering. This technology uses reactor temperatures, 5 response or effectiveness is improved with low rare earth
hydrocarbon partial pressures and contact time to maxim- levels with zero rare earth levels providing the greatest
ize propylene along with high levels of pentocil type zeo- response.
lites. Cryogenics or chillers can be used to maximize The following rules of thumb are offered for maximiz-
propylene recovery. Propylene yields approaching 25 ing light olefins.
weight percent have been obtained commercially with the
Z/M Rare
DCC process, though this is feedstock dependent. More
Ratio Earth Activity ZSM5 Riser T
typical yields are in the range of 17 to 21 weight percent.
Recycling naphtha is another option that can be used Propylene High High High Yes High
to maximize propylene. If it is used upstream of the feed Normal
Butylenes Low Low High No Moderate
nozzles, it will also increase dry gas yield. The effectiveness
Isobutylene Low Low Moderate No Moderate
of this variable diminishes as the naphtha becomes
more aromatic. In order to maximize propylene yield while minimizing
Another procedure is to boost the riser outlet tempera- butane yields, it is best to run a high rare earth level on
ture to around 530 to 535°C and add ZSM-5 to the a low zeolite-to-matrix ratio catalyst and then operate at
extent of about three to five percent. This results in a high temperatures using ZSM-5. The high rare earth,
propylene yield increase. low z/m catalyst will minimize overall LPG production.
Increased riser temperature reduces the butylene produced
HENKE: through catalytic cracking and increases the propylene
Several things can be done to maximize light ends production. And finally, the ZSM-5 will produce propyl-
recovery and unit capacity. These include maximizing ene at a ratio of approximately 2:1 over butylene. The
the operating pressure, removing hydraulic constraints, end result is maximum propylene production with limited
improving heat transfer capability, and improving separa- C4 handling capacity.
tion efficiency.
Mechanical modifications that we plan to incorporate HAHN:
into our light ends recovery units include: (1) installing In regard to the previous mention about injecting naph-
UNIFIN motor coolers on the wet gas compressor electric tha, we have demonstrated that to be a very effective
drivers. This will allow us to fully utilize the motor service technique at our El Dorado facility. Texaco now has a
factor with confidence; (2) improving the design of the patent on this and there are some tricks to this process.
exchanger bundles in absorber intercoolers, reboilers and Properly done, it can be very successful.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 59
TOC/INDEX
ROMAN:
Ashland operates several different spent catalyst stripper
high as 75%, and this product should be readily available designs including a three tray side-to-side baffle external
during the first quarter of 1998. stripper with the steam chest distributor, a seven disk and
doughnut tray external stripper with dual level ring steam
JIM STONE (Louisiana Department of Environmental Quality): distributors, a four chevron tray internal stripper with a
When you make mechanical changes in your plant, pipe steam distributor, and a seven disk and doughnut
change the injection point where you actually have to go tray internal annual stripper with a pipe steam distributor.
out and do something or you change catalysts, you may The critical operating parameters are considered to be
have an event that triggers a change in your permit. When the catalyst flux rates and the stripping steam flow ratio
you do these things, review it and make sure that you do to catalyst flow. Ashland’s catalyst flux design criteria for
not trip into something that could get you into trouble. new strippers is 50,000 lb/hr-ft2, and 75,000 lb/hr-ft2 for
existing strippers being reused in a revamp. Ashland’s
Question 15. design criteria for stripping steam rates is 2.0 lb of steam/
Stripping of hydrocarbon from spent FCC catalyst is criti- 1,000 lb of catalyst circulation, but actual operation has
cal for optimized operation of an FCC unit. Could the covered a range of 0.8-2.0 lb/1,000 lb of catalyst. Spent
panel describe their stripper design, critical operating catalyst stripping effectiveness is measured by the calcu-
parameters and actual performance achieved? What per- lated hydrogen content of coke derived from a material
formance improvements have been seen following strip- balance of the regenerator. The strippers generally achieve
per revamps? How is performance being evaluated? a hydrogen content in the coke of 8.4% to 9.5%, with
lower coke hydrogen contents indicating more effective
JOSECK: stripping. A revamp that was installed primarily to reduce
As a benchmark the new Shreveport RCC unit is of catalyst fluxes did not yield a notable change in stripping
the new UOP design with annular flow baffles. The design performance. A revamp that was installed to increase the
stripping steam rate is 1.9 lbs of steam per 1,000 lbs of number of contacting trays apparently did improve strip-
catalyst with a hydrogen content in the coke of 6.5 per- ping effectiveness, but work has not yet been conducted
cent. After performing stripping steam tests and optimiza- to define and document the change in performance. That
tion, we are using 1.5 lbs of steam and getting to the same revamp eliminated a steam chest distributor in favor
design hydrogen content in the coke. of dual level ring steam distributors, which did result in
a significant improvement in the retention of catalyst
PETERSON: static head pressure across the stripper and spent catalyst
We had an annular stripper in our original design with standpipe. The improved retention of static head pressure
no internals other than just two steam rings. The bottom from that revamp resulted in increased spent catalyst slide
one worked and the top one was not effective, so we did valve differential pressure and hence better operating flexi-
not use it. In our 1996 turnaround, we went to a struc- bility.
tured packing in our FCC stripper which seemed to do
some good on hydrogen in coke. We have seen a calculated SAMUELS:
hydrogen coke drop from 9.3 to 6.8 weight percent. But Getting down to a 5.5 to 6 weight percent hydrogen in
our delta coke has not dropped very much at all. One coke is possible. The cost to reach this is heavily dependent
factor in that may be that the residence time of the stripper upon the current stripper configuration. Revamps are
has gone from one minute to 2.6 minutes. costly on units with annual strippers where incremental
diameter is desired. If only stripper internal modifications was increased by 25,000 b/d, and maintain a low level
are required, these types of revamps show tremendous of hydrogen in the coke due to effective hydrocarbon strip-
rates of return in the order of 1.5 year simple payouts. ping.
The critical operating parameters are somewhat design
specific, but include stripping steam to catalyst ratios, TASKER:
typically 2 to 2.5 pounds of steam per thousand pounds Stripper design is effective if it is multi-stage and has
of catalyst, a one minute residence time, and a catalyst good contacting capability. The key parameters are strip-
flux rate typically of 900 to 1,000 pounds per foot squared per temperature, total pressure, catalyst mass flux rate and
per minute. catalyst residence time. It helps if dilute phase stripping
Improvements in stripper operation can readily be seen precedes the dense phase. Hydrogen in coke should be
in regenerator dense bed temperature as was seen in our about six percent or less with a steam consumption of
Robinson refinery FCCU. With an older single stage shed between 2 to 3 pounds of steam per thousand pounds of
tray design, a one minute catalyst residence time and a catalyst circulation. What we have seen is that after
catalyst flux rate of 790, increasing the stripping steam revamps lower hydrogen coke contents have been observed
rate from 2.6 to 3.5 pounds per 1,000 pounds of catalyst as well as a reduction in regenerated temperature.
circulation cooled the regenerator dense bed temperature
by 20°F. On this unit the hydrogen content in the coke HENKE:
typically runs in the 6 to 7 percent range. We have seen a 2 weight percent improvement in
I have an excellent revamp case study from our Gary- hydrogen on coke after revamp of one of our strippers.
ville FCCU. The Garyville refinery provides a case study I would like to point out that riser terminators have a
on the effects of revamping a stripper as FCCU design big impact on stripper performance and design. A properly
capacity is increased. The Garyville FCCU is an Exxon designed riser terminator can significantly unload the
Flexicracker II commissioned in 1979. It was originally stripper.
designed for 75,000 bpd charge, 42 tons/minute catalyst We evaluate performance of our strippers by first mea-
circulation rate (CCR), and 3.5 lb reactor stripping steam/ suring hydrogen on coke. This is easiest to watch; however,
mlb catalyst. Steam entered the reactor stripper at a single the results can be somewhat misleading in a partial burn
elevation below the lowest row of sheds. unit. Unburned hydrocarbons leaving with the flue gas
In 1992, coincident with installation of M.W. Kellogg’s do not get counted. This error can be corrected by using
Close Coupled Cyclone technology, the reactor stripper a chromatograph to measure the hydrocarbon content of
was modified to include M.W. Kellogg’s two stage strip- the flue gas. Second, we evaluate by direct measurement
ping. Approximately half of the existing shed rows were of the stripped catalyst hydrocarbon content; third, by
removed and two new stripping steam distributors were direct measurement of the interstitial vapor hydrocarbon
installed—one below and one above the remaining shed content; fourth, comparing the actual performance of the
rows. The 1992 revamp design basis was 95,000 bpd stripper to the performance predicted by the technology
charge, 45 tons/minute CCR, and 2.5 lb steam/mlb cata- licensor; and last using Tru-Tec gamma scans and tracer
lyst. The reactor stripper was designed to operate with techniques. Tracers are used to measure the steam distribu-
total stripping steam divided 40/60% between the upper tion, catalyst residence time, backmixing, and hydrocar-
and lower distributors, respectively. The upper stream is bon behavior in the stripper. Gamma ray scans are used
intended to eliminate most of the hydrocarbon vapors to measure density at selected cords through the stripper.
entrained with the catalyst flow. The lower steam is
intended to recover hydrocarbon vapors from within the CAIN:
catalyst pores. Our Louisiana plant reactor stripper contains alternat-
The Marathon Garyville FCCU currently operates at ing hat and doughnut baffles and it has two steam rings.
100,000 bpd charge, 65 tons/minute CCR, and 3.0 lb We generally average about 6 weight percent hydrogen
steam/mlb catalyst. By flue gas analysis, the calculated on coke and our current steam rate is a little high. It is
hydrogen in coke at current rates varies from 6.0-7.0 4.9 pounds steam per 1,000 pounds of catalyst circulation,
wt%. Operating data have confirmed the 40/60% distri- but we are working to get that down some.
bution of stripping steam to be effective. Stripping effi-
ciency and hydrogen in coke are especially sensitive to FLETCHER:
changes in the lower steam rate. Stripping efficiency begins From a catalytic standpoint, we believe the two most
to decline above 65 tons/minute CCR as indicated by significant variables related to stripping hydrocarbon from
increased hydrogen in coke (8.0-9.0 wt%) despite the catalyst particle in the stripper are the surface charac-
increases in stripping steam ratio. teristics and porosity. With respect to surface characteris-
This revamp has allowed the Garyville FCCU to tics, the proper balance of strong acid sites is critical. This
increase catalyst circulation by 55%, while the charge rate becomes important as the quality of the feed deteriorates
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 61
TOC/INDEX
becoming increasingly polar. Chemisorption of polar mol- added to the bottom of the stripper actually flows upward
ecules occur on the strongest acid sites. Subsequent crack- to the reactor.
ing leads to production of dry gas leaving behind hydrogen Mobil and Kellogg have developed and commercialized
deficient hydrocarbons. Chemisorption leads to coke for- flux tube stripper technology which can significantly
mation and pore blockage. An additional characteristic improve stripper performance and extend the range of
required for optimal stripping is good catalyst porosity. acceptable stripper operation. This stripper technology
We recommend high catalyst pore volumes with a large which to date has been commercialized at four Mobil
percentage of meso porosity. refineries and in one non-Mobil unit can allow a refiner
In addition, Akzo Nobel has developed two state of to increase conversion by as much as two vol% and profits
the art test methods designed to aid proper catalyst selec- by more than $1 million per year for a 50,000 barrel a
tion for units that are running highly polar feeds with day capacity unit.
H2-on-coke values. These include a thermal extraction
unit followed by a gas chromatograph and a mass spec- JAMES D. WEITH (Fluor Daniel):
trometer. This allows identification of the types of mole- The FCCU in Los Angeles that I am familiar with had
cules undergoing chemisorption on the stripped catalyst a Kellogg revamp five years ago. The annular stripper was
and gives characterization of soft and hard coke. A second converted to two-stage stripping. We did see immediate
method is used, a fixed fluidized bed reactor with the benefits from that. I do not know whether that was just
capability of burning coke in situ. This allows time, tem- because we could get more steam in, because we also had
perature and nitrogen rate trials with various formulations changed from 60 psi steam to 150 psi steam for stripping
for tough polar feeds. This unit is especially useful in the steam, or whether it was the two-stage stripping. I suspect
study of stripper hot soak reactions. it was a combination of the two.
The type of molecules undergoing chemisorption and Recently we ran an eight run, seven factor design opera-
differences in chemisorption between different formula- ting experiment that was advocated by our statistical pro-
tions is readily possible. The combination of these two cess control consultant, QualPro. That experiment
methods presents the refiner an option for optimizing indicated that although the lower steam ring was very
catalyst formulations for a given unit design and feed important, the upper steam ring also had a significant
quality. impact on the stripping operation. The experiment also
showed that one of the most significant items affecting
stripper performance is temperature. The higher the tem-
FUSSELL:
perature, the better the stripping. Unfortunately, if you
At our Port Arthur refinery, we have a UOP FCCU
have an FCCU that is limited by other things, you cannot
that we started up in 1991. The reactor riser is internal
always increase the reactor temperature to improve the
to the stripper. We have 11 shed decks. We have a steam
efficiency of the stripper.
ring at the base of these decks and another steam ring at
the base of the stripper. Our flux rate is 850 pounds per
SIDNEY ANDERSON (Saudi Aramco):
minute per square foot. We have discovered that we really
For stripper designs that contain two stripping rings
have to stay above the 2 pound per thousand pounds of
at different elevations, I would like to poll the panelists
catalyst circulation on our steam. When our catalyst aver-
to what proportion of the total stripping steam is allocated
age particle size gets above 80, we start having some
to each ring.
pretty major circulation problems if we are not above
that number.
PETERSON:
When we tried to run with two steam rings, the uppr
PATRICIA SPARRELL (Mobil Technology Company): ring received less than 25% of the steam. It was not very
Mobil currently has a variety of commercial stripper effective on the top.
designs in operation which include both UOP annual
strippers and Kellogg internal strippers. Key performance CAIN:
indicators, as a number of you have indicated, include 25-30% of the stripper steam is routed to the upper
the percentage of steam upflow and upstream hydrocarbon ring.
as a percent of total coke.
In good strippers, about 70 to 80 percent of the steam SAMUELS:
added to the bottom of the stripper flows upward to the In the Garyville stripper, 40 percent of the steam is
reactor and unstripped hydrocarbon accounts for less than injected in the top, 60 percent in the bottom and I think
6 percent of the total coke. In poor strippers, unstripped that is where we are currently running. That is the most
hydrocarbon can account for more than 15 percent of effective operation. The upper steam is intended to elimi-
the total coke load and less than 20 percent of the steam nate most of the hydrocarbon vapors entrained in the
catalyst flow. The lower steam is intended to recover not familiar with the test methods and good published
hydrocarbon vapors from within the catalyst pores. results on acidity. Could you respond to that, please?
LAWRENCE A. LACIJAN (UOP): PAUL MINTON (Stone & Webster Engineering Corporation):
We would agree with a lot of the comments made In some ways I think this question on stripping also
about the prime parameters in the design of a stripper, relates to the question on feed injection. If we look at
i.e., residence time, flux rate, steam distribution are very stripping design, it is often very easy to displace the emul-
critical. Our experience is that most units do not stay at sion phase gas from around the catalyst particles. But we
the design condition very long. The Fina unit started out do have a distinct problem in terms of trying to displace
at about 45,000 bpd and they are not at 100,000 yet, the non-volatile heavy components.
but they are on their way. In many cases, the non-volatile heavy components are
It is very difficult to evaluate a stripper performance there at the stripper because they have not been properly
on unit that is been in operation for a long time and is vaporized at the feed injection stage. I would just warn
running a higher flux because the heat balance is so inti- people to avoid looking at the stripper as being their first
mately involved. When you reduce the hydrocarbon and port of call when they think they have too much coke.
the coke on the spent catalyst going to the regenerator, It may come back to the fact that the feed is improperly
the regenerator cools off, which is the desired benefit. vaporized and injected in the first place.
The catalyst-to-oil ratio increases and the conversion goes
up, and you have replaced that unwanted entrained cata- LANA CULLON (Wynnewood Refining Company):
lyst to oil coke with catalytic coke. You wind up with Two years ago we put in a Kellogg stripper and saw
the same coke yield because the unit is heat balanced, immediate results. We are now able to feed at least two
but hopefully you have more conversion as a result. to three percent more DAO to our unit and have seen
Some people focus on the weight percent hydrogen in dramatic decreases in our regenerator temperatures. We
the coke as the key variable in that whole picture, but I run about 5,000 to 5,400 pounds of steam per hour to
do not think that is complete enough to use as a guideline the stripper and we have a catalyst to oil ratio of 6 to
because there is a lot more involved. You really have to 6.5. Our feed rate is 16,000 to 18,000 bpd.
look at the whole unit. You have to look at the conversion
increase as a result of the improved stripper performance
PETERSON:
to really see what the true economic benefit is. Remember
In response to the Stone & Webster comment, we
that as the H2 in coke decreases, the heat of combustion
changed feed nozzle design at the same time we did the
decreases also. This means more pounds per hour of coke
structured packing stripper. So that is another factor that
must be produced and burned to provide the same amount
clouds how we evaluate how our stripper worked.
of heat to the reactor.
Question 16.
JAMES D. WEITH (Fluor Daniel): How have people used cold flow modeling or computa-
Responding to Sidney Anderson’s question on distribu- tional fluid dynamics to improve FCCU performance?
tion, I think we were first set up to run with 55% of the What types of problems have been modeled? How well
total steam in the lower steam ring and 45% in the upper did the model relate to the commercial unit?
steam ring. The total steam rate was at the normally
accepted industry standard of two pounds of steam per SAMUELS:
thousand pounds of catalyst. As a result of the statistical One unit in the Marathon system had cold flow model-
analysis experiment that we ran, I think the proper distri- ing performed on its riser termination system to determine
bution was determined to be about two-thirds of the if a distribution problem existed with direct connected
steam to the lower steam ring and one-third to the upper riser cyclones. Excessive catalyst loss was being experienced
steam ring. However, at this point I need to caution you while design data did not indicate a problem should have
when altering the distribution of the steam not to let the been present.
steam velocity through the holes in the lower steam ring The model clearly showed that a problem did exist
exceed 250 ft/sec. Around this velocity, the steam will with a catalyst and vapor maldistribution. Essentially,
erode the holes and you will lose the advantage of using most of the catalyst went through one-half of the termina-
more steam in the lower steam distributor. tion system while most of the vapor was going up through
the other half. A prominent EPC company was involved
STEVE PAVEL (Coastal Catalyst Technology): with assisting the refinery and solving this problem along
As far as the catalyst, it is well-published and easy to with a consultant. I believe it was Zenz who actually built
determine pore sizes by nitrogen and mercury. But I am the model.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 63
TOC/INDEX
reactive distillation technology. C3’s need to be fraction- ethyl mercaptan, 50 to 110 ppm dimethyl sulfide, and
ated out due to arsenic which will poison the catalyst. If 140 to 190 dimethyl disulfide and 10 to 20 methyl
H2S carries over into the mercaptan oxidation system, it ethyl disulfide.
will form sodium thiosulfate which is not regenerable and
causes a high caustic consumption. TASKER:
Total amount of mercaptans is very much a function
MALEK: of the feed sulfur. Based on some test results from various
The fractionation of the propylene stream in U.S. refin- samples taken from different refineries, we found the
eries is becoming almost the norm, because such a large following distribution is typical. In the FCC LPG, the
percentage is going into chemical sales. It is more practical mercaptans would be 85 to 95 percent methyl mercaptans
from a hydraulic and cost standpoint to fractionate before and 5 to 15 percent ethyl mercaptans. The C3 stream
the treating. This also will tend to debottleneck the amine contains mainly CoS and the methyl mercaptans and the
contactor. H2S removal from the C3 stream is generally ethyl mercaptans are predominately in the C4 stream.
sufficient in to allow the sale of that propane/ propylene Depending upon the downstream processing units, it is
stream directly to your customer. The treating of the C4 difficult to comment on whether or not there is an advan-
residue stream from the C3 splitter column will hydraulicly tage fractionating the C3’s from the C4’s before sulfur
unload the Merox treater ahead of the alkylation unit. is removed.
PETERSON: CAIN:
In one of our refineries, we do the fractionation before We do treat our C3’s and C4’s before we fractionate
we do the treating and the mercaptans would stay with them due to our current configuration. In our combined
the C4’s and only H2S would go with the C3’s. This has C3/C4 stream after DGA treating, we have 30 ppm by
kind of been born out in another one of our refineries weight H2S, 256 ppm methyl mercaptans and 23 ppm
where we severely hydrotreat the FCC feed to the point ethyl mercaptans.
where we no longer run the Merox on the LPGs. When
we have an upset in the FCC feed treater, we do not see HENKE:
mercaptan sulfur in the propylene. All I wish to add is that we find it economical in our
The advantages to doing fractionation first would be Corpus Christi refinery to fractionate before we treat. At
that you can really reduce the liquid rate to the contactors, our Minnesota refinery it is just the reverse, we treat
both the Merox and the amine contactor that were before we fractionate.
designed for the full rate. You can withstand capacity
creep, expansion of the unit, using ZSM-5 catalysts or Question 18.
changes in feed quality from hydrotreating the feed. What impact on yields have refiners observed when
Disadvantages are potentially wet propylene stream, including diesel range material in the FCC feed? Is this
which used to be dry if fractionated after you did all the impact different than would be expected based on crack-
treating, going to the alkylation unit. That would only ing diesel range material alone in a pilot plant? If so,
occur if you had to do Merox treating. Again, if your why?
feed sulfur is clean enough to the FCC you may not even
have to do that. FLETCHER:
One other thing you would want to look at is you In general, conversion increases when the 650 minus
now introduce a lot of H2S to your splitter tower that material is supplied to the FCC due to increased cat-to-
did not use to be there, you may want to check the oil ratios resulting from lower delta coke. The effect of
metallurgy of your design. decreased delta coke overwhelms the effect of the lower
crackability of the diesel range molecules to smaller gaso-
ROMAN: line and LPG molecules. The increased catalyst to oil ratio
The H2S content is so large that it masks the mercaptans results in deeper conversion of the 650°F plus fraction of
if analyzed before the MDEA scrubber. We have obtained the feedstock.
samples after the amine treating and analyzed the sulfur The commercial unit being a dynamic system, is diffi-
species by flame photometric gas chromatography. For cult to isolate heat balance effects cat-to-oil, from molecu-
the FCC unit, the sulfur compounds measured were 69 lar yield shifts (conversion). Therefore, a pilot plant
ppm methyl mercaptan, 25 ppm ethyl mercaptan, 35 investigation is usually initiated to define the effects.
ppm dimethyl disulfide and 49 ppm ethyl propyl disulfide. Before and after yields are generally compared at specific
As would be expected, the sulfur levels are much higher conditions such as constant conversion or catalyst-to-oil.
in our RCC unit. After amine treating, the values ranged Unfortunately, pilot plants are not heat balanced opera-
from 160 to 300 ppm methyl mercaptan, 160 to 240 tions, nor are they as dynamic as a commercial unit.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 65
TOC/INDEX
Therefore, very different yield slates may be observed on cracked pure in a pilot plant? I think I have a simple
a pilot plant when compared to a commercial unit. explanation for this.
Conversion improvements on the commercial unit may Studies have shown that heavy material cracks a lot
be attributed to any or all of the following effects: (1) faster than light . Also, the heavy material makes a lot of
lower nozzle viscosity-oil droplet size may be reduced coke which deactivates the catalyst. If you put a mix of
improving catalyst and oil mixing. This is particularly heavy and light feeds together into an FCCU, the heavy
true on some heavy oil crackers. (2) The lower boiling stuff is going to crack fast, coke everything up, and you
range feedstocks (⬍500°F), being nearly inert in the FCC, are left with few active sites to crack the light material.
increases the catalyst-to-oil ratio which reduces the degree I think that explains the things that people see, i.e.,
of thermal cracking in the mix zone of the base of the that the diesel cracks worse in a real world FCCU feed
riser. This will result in lower regenerator temperatures mixture compared to what it might pure in a pilot riser.
with corresponding increases in catalyst-to-oil. (3) Diesel That might be especially important if you are mixing
in the feed typically increases total charge to the unit. diesel it with resid as Mr. Tasker mentioned because the
Overall riser resident time drops which results in lower resid is going to crack very fast and make a lot of coke
coke yield and in increased cat-to-oil ratios. quickly and not leave much activity left over for the
Diesel boiling range paraffins, do not generally crack slower-cracking diesel.
except under high severity operations. Therefore, these
waxy molecules typically result in high cloud point LCO. JAMES D. WEITH (Fluor Daniel):
Heavy naptha and light diesel in the feed generally display From the panel it would sound like the best thing in
low crackability. This tends to reduce heavy gasoline aro- the world is to run all the diesel back up the riser in order
matics due to a dilution effect which typically results in to increase the catalyst-to-oil ratio and conversion. The
a lower octanes. The bottom line is that much of the FCC I referenced in Los Angeles tended to show the
unrealized clean diesel ends up as low quality middle contrary, but maybe for several reasons.
distillate in the FCCU. One was that with higher catalyst-to-oil ratio we made
more gas. This particular FCCU is often limited by the
CAIN: refinery fuel gas balance. At times whenever we made
We found the diesel swing cut which is in the 600 to more gas, we would have to back off on the reactor
650°F range appeared to crack in the range of 70 to 74 temperature. That had two negative effects on the opera-
percent conversion which is lower than virgin gas oil tion of the FCCU. First, the performance of the catalyst
which cracks in the 78 to 80 percent conversion range. stripper would decrease, as I mentioned in my response
to question 15. As the stripping efficiency decreased, the
SAMUELS: regenerator cyclones would get hotter. Second, taken to
I would agree with the comments made. extremes, this sometimes meant backing off on the charge
rate to the FCCU to keep the cyclones from overheating.
TASKER: All things considered, our conclusion was that including
In a gas oil operation, the lighter feed is harder to diesel in the feed to the FCCU was not a very good thing
crack, but this also lowers the delta coke and increases to do.
the catalyst-to-oil ratio. Higher reactor severity can be Having said all that, I can now respond to the gentle-
effective in cracking this material as well as high concentra- man that inquired: ‘‘If increasing diesel in the feed
tion as forward site in the catalyst. Yield increases of increases the octane of the FCC gasoline?’’ Not if it results
gasoline and propylene usually result. Presumably this in having to lower the reactor temperature to do so.
mode of operation would only be practical in a maximum
gasoline scenario since the straight run middle distillate SAMIR HALAWANI (Saudi Aramco):
would have a high value as diesel. When residue is pro- Going back to Fletcher’s comment, could I understand
cessed, the middle distillate has a bigger effect on feed that running the diesel would not be a good idea, even
properties. It lowers the Conradson carbon and metals if we have a CN over CP high enough to encourage
by dilution and it is also a hydrogen donor. The increased running it through the riser?
catalyst-to-oil ratio can have a significant impact on yields,
particularly when the starting catalyst to oil ratio is less FLETCHER:
than six. High gasoline yields would be expected along If I have understood the question properly, if you have
with higher overall C3 plus liquid yields. limited capacity in your unit for catalyst circulation, then
putting diesel in the unit would probably not be as eco-
R.C. SKOCPOL (Akzo Nobel Catalysts): nomical or profitable as putting in fresh feed. We would
The question also asked why diesel might behave differ- always recommend to put in fresh feed first. If you are
ently in a real world FCCU feed mixture, compared to operating a unit in which you are running all the feed
that is being produced and you still have catalyst circula- Upgrade values seen on the slurry product can be signifi-
tion room, then it is worth doing a trial to see where the cant.
economics come out for your particular unit. Ash levels in our untreated slurry are typically around
0.1 weight percent. During occasional high conversion
LEE E. TURPIN (Honeywell Hi-Spec Solutions): operation on this FCCU, deashing becomes difficult due
The following table was prepared using the FCC-SIM to the low gravity and viscosity; we are talking about a
kinetic model, and shows the yield pattern as diesel is minus 6° API gravity slurry and high viscosity. Product
added to FCC feed. The base feed was a mixed gas oil run down temperatures are raised to about 300°F. Steam
with the following inspection: coils are utilized in the tanks, and the chemical dosage
23.1 API, 10/50/90 D1160 of 723/831/953°F. The rates are increased from about 150 ppm to 250 ppm.
diesel used had the following inspection: 32.4 API, 10/ In Marathon’s experience, the most economical
50/90 D2887 of 441/551/649°F. The feed was increased method of disposal for the clarified slurry oil sediments
in three steps to show the shift in yield pattern as the when you are cleaning your tanks is to process the material
diesel in the feed was increased. through thermal desorption units or TDUs. The TDU
Case 1 2 3 4
removes hydrocarbons from the sediment for recycling.
Base Feed-bpd 58987 58987 58987 58987
The remaining sediments are then land filled.
Diesel Feed-bpd 0 5000 10000 15000
The U.S. EPA issued a proposed rule to list clarified
Total Feed-bpd 58989 63988 68988 73988
slurry oil sediments as hazardous waste. This means that
Riser Temp-°F 450 450 450 450
in the future clarified slurry oil sediments will have to be
FCCU Circulation Ton/Min 47 51 56 61
stored, treated and disposed of as a hazardous waste.
Riser Outlet Temp-°F 1011 1011 1011 1011
Processing the slurry sediments through a TDU provides
Wet Gas Rate-MSCFH 2538 2712 2884 3054
an opportunity to allow the remaining sediments to be
Conversion-wt% 70.49 69.68 68.92 68.19
delisted as a non-hazardous waste which would dramati-
H2ⳭC1ⳭC2ⳭC2e-Vol%Feed 4.90 4.87 4.84 4.81
cally reduce the disposal cost once the agencies proposed
Total C3-Vol%Feed 11.26 10.98 10.74 10.53
listing becomes effective.
Total C4-Vol%Feed 13.70 13.46 13.26 13.08
I would like to recommend an outstanding information
Total C5-Vol%Feed 12.98 12.79 12.62 12.48
source on this entitled ‘‘Listing Background Document
C5Ⳮ Naphtha-Vol%Feed 54.79 54.05 53.34 52.65
for the 1992 to 1996 Petroleum Refining Listing Determi-
C6Ⳮ Naphtha-Vol%Feed 41.81 41.26 40.72 40.17
nation.’’ It was prepared for the U.S. EPA Office of
Total C4e-Vol%Feed 7.98 7.85 7.73 7.63
Solid Waste Characterization and Assessment Division by
Total C5e-Vol%Feed 4.15 4.08 4.03 3.98
Science Applications International Corporation, October,
C3eⳭC4e-Vol%Feed 14.94 14.63 14.36 14.13
1995. The paper discusses in detail how clarified slurry oil
C3eⳭC4eⳭC5e-Vol%Feed 19.08 18.71 18.39 18.11
is handled by a large segment of the U.S. refining industry.
C3 ⳭLiquid-Vol%Feed 107.6 107.3 107.0 106.8
BINFORD:
Standard Naphtha-Vol%Feed 57.69 56.92 56.17 55.45
Well, again I agree with most of Mr. Samuels’ com-
Question 19. ments. I want to provide a little information about
What techniques are used to improve catalyst settling upstream effects and then go to downstream. There are
from slurry oils in tankage? How are catalyst fines techniques upstream of tankage to reduce solids in the
removed from slurry oil tankage, and what methods are clarified slurry oil. Those include filtration, centrifugation,
currently employed for disposal? hydrocyclones, and electrostatic precipitators for separa-
tion. These have all been used successfully.
SAMUELS: In our experience, however, our customers have been
Catalyst settling storage is a strong function of slurry plagued with mechanical unreliability with these systems
oil viscosity and settling time. Marathon data indicate and have expressed a lot of frustration. This has really
that minimum settling temperatures should be 125°F, been the ‘‘catalyst’’ (pun intended) for chemical settling
but higher temperatures are often of benefit as oil viscos- aids in the clarified slurry oil tanks themselves.
ity increases. Mr. Samuels mentioned that the outlet for their clari-
Settling time is typically five to eight days. So you are fied slurry is carbon black feedstock rather than blending
probably going to need a couple of tanks in this service. it into the No. 6 fuel oil pool. Some refineries also get
Chemical deashing or settling aids can dramatically an upgrade for selling low ash content, premium fuel oil
improve solid separation. At the Robinson refinery, FCC as a higher grade of essentially a No. 6 fuel oil product, and
settling agent, Nalco/Exxon, EC 3040A, is used to reduce a few sell their slurry as feedstock for anode grade cokers.
slurry ash levels in tankage below .05 weight percent which There are slurry oils containing between 0.1 and 0.4
is typical of carbon black feedstock quality specifications. weight percent ash which might not settle further in a
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 67
TOC/INDEX
storage tank operating even at elevated temperatures, (even HEROS DERGREGORIAN (Valero Refining & Marketing
above 200°F). Many of these slurries can be successfully Company):
chemically treated to reduce ash to as little as .01 weight Has anybody been able to justify installing a system
percent. The rate and type of settling aid will vary directly to remove catalyst from the slurry product by recycling
with the initial ash concentration and the physical charac- it back to the unit?
teristics of both the slurry oil and the catalyst fines them-
selves. HIGGINS:
The variability in the slurry oil characteristics can be No response.
attributed to variations in the gas oil charge the unit, the
catalyst type, the degree and type of metals loadings on BINFORD:
the catalyst and the operating conditions such as reactor I would like to make one other real quick comment
temperature and catalyst-to-oil ratio. The effect of these on slurry settling aids. One of the key questions we always
variables on the physical characteristics of the slurry deter- get is ‘‘am I going to fill up my slurry tanks faster and
mines the selection of the most effective chemical set- am I going to have more solids to dispose of?’’ Obviously,
tling aid. you are going to have more solids to dispose of. There
We have six commercially proven settling aids, five of is no doubt about that. A couple of methods have been
which are covered under individual U.S. and international used for disposal. One is to install a sparging system in
patents for each of those products. We typically see a the bottom of the tank where so you can periodically stir
greater than 90 percent success rate in providing a payout up the catalyst fines in the bottom of the tank and then
for the refiner. That is pretty substantial as Mr. Samuels sell (on a periodic basis) a tank of low quality fuel oil.
had indicated previously. Obviously you would think you would fill up your
tank a lot faster using a chemical additive with settling
rates being higher. Surprisingly, we really do not see a
CAIN:
drastic increase in the catalyst fine fill rate in the tank.
We have good luck with settling aids as well. We have We believe this is the effect of better agglomeration of
a different situation at our Louisiana plant. Our heavy the solids and better compaction in the tank. We have a
cycle gas oil is routed to our H-Oil unit and any sediment higher solids level of sludge in the tank with less oil
or catalyst fines that remain go out with the fuel oil. trapped in the pores. These conclusions are a result of
our experience in several sytems. I certainly would not
FLETCHER: say we have the hard data to support this statement.
One of our customers reports that they recycle the
bottoms from their slurry storage tank back to the FCCU 7. Catalysts
on an annual basis. They point out that this procedure
is only possible for those units with some kind of capturing Question 20.
technology such as an ESP or which are not faced with What is the maximum ZSM-5 additive level in the circu-
opacity limitations since in their operation a fair percent- lating inventory being used commercially? At what opera-
age of the fines may be passed through the regenerator ting conditions? What are the effects on yields,
into the stack. specifically light olefins, coke and BTX? Is there any
practical limit on the level of ZSM-5 used?
generally operate with riser outlet temperatures in excess However, if the refiner is willing to use a very high zeolite
of 1000°F while gasoline operations generally operate with containing fresh catalyst the dilution effect from high
riser outlet temperatures less than 1000°F. levels of additives can be easily offset.
Light olefin yields benefit primarily from increased The highest commercial application of ZSM-5 additive
propylene yield. Propylene olefinicities approach 80%. we have had to date is a unit using 16% PENTACAT.
Maximum light olefin yield occurs at approximately 45- We have several units running above the 10% additive
50 wt% ZSM-5 concentration in the inventory. Gasoline level. None of these units have reduced catalyst make-up
yield is reduced as the light olefin yield increases. BTX rate or suffered dilution effects.
yields increase slightly due to the concentration effect.
Coke yields are unaffected by ZSM-5 since this is a Question 21.
medium pore zeolite. A large pore zeolite is needed to MAT, fixed fluid bed and riser pilot plant tests are widely
produce coke precursors. Yields may vary substantially used to predict catalyst performance in an FCC unit.
between suppliers due to the concentration of zeolite in According to commercial experience, how reliable are
the additives supplied. these predictions, particularly when a new catalyst or a
ZSM-5 response is a strong function the rare earth very high ZSM-5 addition rate are being tested? How
level in the circulating inventory. Light olefin yield and can catalyst deactivation be properly simulated?
octane response drops as the rare earth concentration
increases. The greatest ZSM-5 response occurs on a zero ROMAN:
rare earth catalyst. The response can be correlated against We do not recommend MAT comparisons of signifi-
the hydrogen transfer index (iC4/Total C4). cantly different catalysts, particularly when matrix effects
are present. MATs are excellent screening tools for similar
PETERSON: catalysts or when zeolytic effects only are being considered.
I agree with what Mr. Fletcher has just said. I would They can be useful for ZSM relative comparisons, but
like to add specific numbers from one of our refineries. the results should not be used for predicting commercial
We added ZSM-5 at 6 percent in the past. We increased performance. Fixed fluid beds are better, but still have
to 10 percent when propylene prices were a little bit the same concerns as the MAT units.
higher. We saw a yield of about one to two liquid vol% Pilot plants give the best reactor simulation results and
higher propylene yield and it is about 75 to 78 percent can readily handle differentiation of zeolite versus matrix
olefin in the C3 stream. There are some extraneous pro- performance. However, all three suffer from a major limi-
pane streams that we recover in the FCCU. So the actual tation often ignored in laboratory studies. The catalyst
olefinicity is probably a little over 80 percent. We do not being tested must accurately portray the history it will
measure BTX components in our gasoline. The effect on see in the proposed use. Most MAT fixed fluid bed and
coke make is not noticeable and the economic tradeoff even many pilot tests use artificial aging techniques which
that each refinery has to look at is lower gasoline yield, do not accurately reflect the proposed end use.
less real catalyst in the FCCU to go after the other crack- In one example, high temperature steaming was used
ing, and gasoline octane. followed by MAT testing to prove the superiority of a
TASKER: particular catalyst. When this was disproven commer-
Well, my response is very much the same. The highest cially, post audit studies pointed very clearly to (1) differ-
levels of octane as generally reported for commercial oper- ential response to high temperature steaming versus
ations are about 12 to 15 percent. This translates to a 2 normal regenerator conditions, (2) zeolite versus matrix
to 3 percent pentasol zeolite. Gasoline yield is reduced aging was different in test versus commercial, and (3)
and LPG is increased along with gasoline octane. There the catalyst with the highest matrix content was severely
is a paper by Buchanan and a gentleman whose name I penalized in the MAT test.
cannot attempt to pronounce reporting data containing We have developed sophisticated protocols to address
about 25 percent of ZSM-5. these phenomenon and in particular recommend that any
At a high severity operation with a USY FCC catalyst, testing program contain the following:
we have the following yield changes. Gasoline went from 1) preparation of a valid pseudoequilibrium catalyst
41.4 down to 33.35 percent. The C3 olefins went from which has a proper age distribution and at the
4.59 to 10.02 weight percent. The C4 olefins went from metals level at which the catalyst is anticipated to
5.14 to 8.05 percent, and the RON went from 93.3 to operate under;
95.1. Again, the coke make was essentially unchanged. 2) use of real feeds;
3) correlation to commercial operations;
G. ANDREW SMITH (INTERCAT, Inc.): 4) definition of performance measurement windows;
We believe there is some practical limit to how high 5) blind post audit of actual results;
a concentration level of ZSM additive you may go to. 6) periodic and frequent baselines.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 69
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FLETCHER:
Pilot plants give the best predictions of FCC catalyst
performance, closely followed by fixed fluid beds (FST
and FACT), with conventional MAT’s a distant third.
Reliability of the data is directly proportional to the care
taken to simulate the current operation. Pilot plants will
provide the best simulation of the unit while the MAT
while generally provide the poorest simulation.
Careful attention must be paid to how the coke yield
from the pilot plant is used to predict FCC response to
catalyst changes. Differences in residence time in both
the stripper and reaction zone between pilot units and
commercial units make delta coke prediction on the com-
mercial unit from pilot plant results difficult. Many refin-
ers incorrectly observe yields from pilot plants at constant
coke and do not take into account the problem of proper
coke prediction from laboratory testing. A better method ZSM-5. If the ZSM-5 is placed on top of the bed, little
is to use a comparison at constant conversion to determine or no reactions will have occurred providing reactant for
selectivity adjustments. This data is then used in a process the ZSM-5. If the ZSM-5 is placed in a layer in the center
model tuned to the unit in question to determine the of the bed the conversion will be very high. If the layer
yield shifts expected. If the process model has stripper is placed at the bottom of the bed only moderate reaction
modeling capabilities, catalyst stripping characteristics tes- will occur since the reaction rate is relatively low.
ting can be used to improve the delta coke prediction A key factor to remember is that all test work involves
from laboratory testing. compromises and that the results gathered are simulations
The best deactivation procedure is the one that most of a commercial operation. Highly sophisticated test pro-
closely simulates commercial equilibrium catalyst from cedures are available but are both time consuming and
the particular unit. This is best achieved using a large costly. A balance must be struck between time, cost, data
number of cycles in a cyclic deactivation unit at low reliability, and the economic opportunities that are avail-
temperatures. Deactivated catalyst should be withdrawn able.
at predetermined cycles and cracked in a fixed fluidized
bed using the unit feed. Each cracking run should be HAHN:
compared to data produced from cracking the unit feed I think Mr. Roman and Mr. Fletcher have given a
over ecat withdrawn from the unit. Special attention to thorough review of all the issues involved in catalyst per-
the oxidation state of the deactivated catalyst must be formance testing. Generally testing costs become a key
made to match the equilibrium catalyst in lab scale testing driver. We use MAT with a great deal of scrutiny, judg-
(but not in the pilot plant testing where regeneration ment and attention to catalyst conditioning and test feeds-
exists). This process is both time consuming and costly. tock used.
Low metals operation (⬍1000 ppm total metals) are
better simulated using steam deactivation. Very high Con- STEPHEN K. PAVEL (Coastal Catalyst Technology, Inc.):
radson carbon feeds (⬎3.0 wt%) should be cracked in a Thank you for the excellent responses on methods of
fixed fluidized bed capable of in situ coke burning for testing and their problems. We agree with the comments.
adequate mass balance. Usually we all have to come to some sort of decision
When using ZSM-5, one must be careful to avoid aside from going straight into a commercial operation.
the dilution effect of the additive. In addition, proper Generally we use any of the above test methods and some
deactivation of additives is important. One ZSM-5 sup- modeling to interpret it to the commercial state.
plier recommends mixing fresh additive into the deacti-
vated catalyst sample while most deactivate the ZSM-5 Question 22.
along with the catalyst. Directionally, a fresh ZSM-5 Has anyone used gasoline sulfur removal catalyst addi-
additive will show higher light olefin yields than will a tives as a means to control total pool gasoline sulfur
deactivated sample. levels? If so, what reduction levels were obtained?
Proper mixing of ZSM-5 is important when using fixed
bed reactors (MAT). If ZSM-5 is placed on top of the FLETCHER:
bed almost no reaction will occur. This is due to the fact Gasoline sulfur reduction additives have only demon-
that the ‘‘Y’’ zeolite cracks the gas oil molecules into C7- strated sulfur reductions of about five weight percent
C10 olefins that are the primary reactants cracked by the commercially. Although 25 to 30 percent reductions can
be measured under controlled metals free laboratory con- G. ANDREW SMITH (INTERCAT, Inc.):
ditions. Our particular additive is also used to upgrade more
As a rule of thumb, for nonhydrotreated feeds, about of the bottoms to gasoline. So we tend to see two effects
ten percent of the feed sulfur will end up in the FCC here. One is reduction in sulfur in the gasoline, but also
gasoline. Whereas for hydrotreated feeds this number an increased gasoline yield. So there are certain traps that
drops to about five percent. When compared to an FCC are available that would actually reduce the volume of
catalyst with little matrix concentration, a catalyst with the gasoline, but we have not felt those were what the
a high concentration of an active selective matrix can refiner wanted to accomplish.
show a reduction in sulfur of up to 25 percent for a
nonhydrotreated feed. This sulfur is converted to H2S. 8. Fractionation
This can be further enhanced by a high rare earth level.
Aromatic sulfur containing molecules such as benzothia- Question 23.
phene are too large to enter the zeolite cage in order to How are the current methods of corrosion monitoring in
gain access to the strong acid sites necessary for their easy the FCCU performing? What is the industry’s experience
destruction, but some reduction occurs. In the FCC, with reliability of various hydrogen probes? What non-
the easier sulfur compounds to convert are the sulfides, intrusive hydrogen permeation devices are available?
disulfides and mercaptans found primarily in the light
FUSSELL:
and mid-cut fractions. Reduction of benzothiaphenes is
affected most by matrix type. In Port Arthur on our gas concentration unit, we use
We believe the primary reason for the disappointing ultrasonics and corrosion probes for inspection. We have
results observed to date with sulfur reducing additives is some hydrogen patch type probes that are permanently
that the refiners with the greatest sulfur problems are installed on our unit, but we no longer use those due
cracking heavy feeds and are already using the high matrix to maintenance problems and difficulty in interpreting
bearing catalyst. the data.
FOSTER:
G. ANDREW SMITH (INTERCAT, Inc.):
We currently use a combination of traditional corrosion
In response to the sulfur reduction, we have people
probes and water sampling. We also use non-intrusive
using the bottoms cracking additive that we manufactured
Beta foils which have served us well.
specifically with the goal of reducing the gasoline sulfur.
The problems are that the Beta foils do have to be
We have seen 25 and 35 percent reduction in total gasoline
perfectly sealed to work properly, and are very expensive.
coming off the FCCU. We also have a new additive
The diffusion through the metal can change from applica-
that should be available hopefully the first quarter that
tion to application, so unless you stay on top of the
promises even higher gasoline sulfur reductions.
correlations, they do not give a very highly accurate quan-
titative answer.
JOHN HALEY (Grace Davison):
On the other hand, the Beta’s do offer transportability
Further to Mr. Fletcher’s comments, several refineries
and reusability. We are able to get a wider range of data
have realized up to a 25 percent reduction in gasoline
around the plant, which enables us to a tailor the level
sulfur with Grace Davison’s first generation gasoline sulfur
of inspection more appropriately to those areas that show
reduction additive, GSR, and further research is continu-
the most activity. It helps us marshal our resources to the
ing in this area towards a goal of more than 50 percent
right areas.
reduction in full range gasoline sulfur.
SAMUELS:
ZIYAD AZZOUZ (Saudi Aramco): As Mr. Foster just mentioned, part of the problem
Will the use of those special additives to reduce sulfur in with hydrogen probes is that they are effective, but they
the gasoline affect the yield of gasoline, sulfur, and octane? are limited in the monitoring area. You are monitoring
a small area in a large system. Several types of non-intrusive
FLETCHER: hydrogen permeation devices have proven to be reliable
Generally our observation is that the catalyst properties and I will list those: Baker Petrolite’s, HPC11, hydrogen
that most affect the sulfur reduction, are the matrix and permeation monitoring system, the Beta Corporation beta
rare earth. As you increase the matrix component in the foil system and the CCT hydrogen patch probe. These
catalyst, you would expect that the cracking to light diesel can be reliable if used properly.
and heavy gasoline will increase. And as you increase the
rare earth, the amount of cracking into LPG will be Question 24.
reduced and will be observed as an increase in gasoline We are currently injecting ammonium polysulfide into
yield. the FCC wet gas downstream of the compressor. We
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 71
TOC/INDEX
have seen some fouling problems downstream that we 1992. They never did register any pressure build up, and
believe are related. Have other refiners experienced this I was always suspicious of them. They consisted of a
problem, and what action was taken to solve the bottom part that was welded onto the vessel or line, and
problem? then a top part that snapped on through an O Ring of
neoprene or rubber. I always thought that if the hydrogen
BINFORD: was tenacious enough to get through an inch of steel, it
The NACE Group formed a task group to study this could get past the O Ring in nothing flat. However, at
and other FCCU corrosion issues several years ago. The the 1995 turnaround we found no indications of any
results reported in NACE meeting minutes in 1991, con- hydrogen blistering in the neighborhoods that these were
firmed a high incidence of downstream fouling with located. So there was no reason to see a pressure build up.
ammonium polysulfide applications. I will note that sev- I have become familiar with the Beta Foil that was
eral people are successfully using ammonium polysulfide. mentioned earlier, and I think that is a much more practi-
So I do not mean to infer that it is ineffective. cal arrangement. It does not depend on a pressure build
The users reported that as a group 42 percent had up. Instead it has a vacuum pulled on it and you check
observed some fouling with the use of ammonium polysul- to see if the vacuum ever get broken.
fide. Use of corrosion inhibitors was also studied and
surveyed. The use of corrosion inhibitors had a better SAMIR HALAWANI (Saudi Aramco):
track record in terms of fouling with only a ten percent We had severe corrosion problems in interstage and
incidence of fouling reported by NACE. high pressure coolers several years back. We resolved the
The control in feeding of APS was a key area that the problem by increasing the water wash to these coolers.
study indicated need improving. Overfeed was a major We were very low in water and then we increased it to
problem in downstream deposition and fouling, especially the normal practice of 2 ppm per 1,000 barrels of fresh
sulfur deposition. Also, carryover of water into the dry feed. The problem was resolved.
sections (or supposedly dry sections) of the FCC gas
conservation section was noted as a serious problem, caus-
ing downstream corrosion and fouling in distillation B. Coking
equipment when the water flashed off and left the inor-
ganic foulants behind. In some instances water separation 1. Mechanical Reliability
equipment may be operating above design throughput
causing this problem, (especially the FCC main column Question 25.
overhead receiver). The use of filming amines with good What is the life expectancy of coke drums? What cycle
dispersant properties have been successful in addressing length goes with this life expectancy? For those who
some of these fouling issues if the operation of seperators have recently replaced drums or are planning to do so
could not be improved to alleviate the problem. in the near future, what criteria are being used to deter-
mine that replacement is necessary?
SAMUELS:
I think my answer looks like APS 101. Ammonium FOSTER:
polysulfide, APS, is used to control hydrogen blistering For Lyondell-Citgo Refining, replacement will become
and cracking in FCCs and cokers. Cyanide present in the necessary when the cost of repair (and the associated
gas concentration section reacts with iron sulfide to form downtime) outweighs the cost of replacement. This crite-
ferocyanides. Without the iron sulfide protective layer, ria might be complicated somewhat if we consider replace-
hydrogen is available to penetrate to clean the steel. APS ment of the existing drums to increase capacity.
reacts with the cyanide to keep it from reacting with the Foster-Wheeler cites 20 years. Ours are 29 years and
iron sulfide. If excess APS is added, the elemental sulfur still going. Others have seen close to 10 years. The actual
can drop out of solution and cause pluggage and can also life expectancy can be a lot more or it can be a lot less,
be a corrosive species. depending on how the drums are operated. Although the
To avoid this, we would recommend that you add just overall cycle length is important, what is more important
enough APS in a stoichiometric amount to react. The is the quality of the cycle.
way to test for this would be to measure the cyanides in Since the quench is where the drums sustain the major-
your water boot. You want to just eliminate the avail- ity of the damage, we watch this very closely and try to
able cyanides. have a very soft quench. We monitor the cycles with
temperature and strain gauge measurement to see where
JAMES D. WEITH (Fluor Daniel): the opportunities lie in our coking cycle. For example,
The FCCU that I referred to in Southern California we found some fat in our warm-up cycle and were able
had Hydrogen Patch Probes on it. We put those on in to reduce that time and get to a shorter cycle without
drastically reducing our quench and incurring undue ves- internal cracking. Fatigue cracks are monitored and
sel strain. tracked from year to year.
We operate on a 16 hour cycle on our older coker and
have been on this cycle for about 20 plus years. We
SAMUELS:
contracted a company (ERA) to look into the remaining
Marathon does not use laser inspection of coke drums.
life of our drums. They did a lot of work on the drum
We believe this is an extremely accurate and expensive
base material and found that the shell material was in
technique for measuring bulges and other drum distor-
good condition for being 29 years old. Their report stated
tions.
that if we continued to watch our quench cycle and
In addition to taking physical measurements, we have
continued to repair the drums in the same manner as we
employed strain gages, thermocouples, finite element anal-
had in the past, they feel we have a number of good
ysis to determine when drum damage occurs. In addition
years remaining.
to predicting drum life, these techniques allow you to
optimize your cycle times.
HENKE:
Typically for coke drums that have seen 24 hour cycles Question 27.
throughout the major portion of their service life, the life What run lengths between decoking are typically being
expectancy has been 20 to 30 years. I have been told that achieved on coker heaters and transfer lines? What meth-
there are approximately six sets of drums in North America ods are being utilized to maximize coker heater run
that have been in service for longer than 30 years. The length?
drums at our Corpus Christi Refinery have been in service
for 38 years. Recent information suggests that the drum
replacement time will drop into the range of 15 to 25 SAMUELS:
years, due primarily to the reduction in cycle times. The Robinson’s two 13,000 barrels per day cokers produce
size of the drums is a significant variable. The large drums anode grade coke on identical feed to both units. Vacuum
will directionally require replacement before the smaller resid charge is typically 10° API gravity. Each unit operates
drums. at 20 to 25 percent recycle and the furnace outlet tempera-
We evaluate the amount of bulging, cracks, cost of tures are set to achieve a 9.5 VCM specification for the
repairs, and exposure to leaks and fires, with the primary coke. The number two coker achieves 1.5 to 2 year runs
replacement criteria centering around safety and the cost or has achieved that in the recent past. Currently, we
of drum repair. are on ten month runs due to a significantly heavier
crude resid.
Question 26. The run length is typically limited by a maximum
What is industry experience with regard to the use of furnace tube wall temperature of 1,300°F. An antifoulant
laser beam inspection of coke drums, coupled with finite is used in the coker furnace and transfer lines and will
element analysis, in forecasting repairs? What other be discussed more in Question 37. The number one coker
tools are being employed to predict required repairs or furnace operates at a higher severity and typically achieves
remaining life of coke drums? six month run lengths between decoking. We are able to
spall and steam-air decoke this furnace on the run. It is
a two pass furnace and we can take one pass off at a time
CAIN: and decoke keeping the unit on line at a reduced rate.
At our Port Arthur plant, laser beam inspection is used Variables that impact run length include the asphaltene
before each turnaround to map the inside of the shell. A content of the charge, and furnace firing severity. You
video camera is attached to the drill stem during the should minimize the maximum flux rate for a given outlet
mapping. Before this delayed coker’s first turnaround this temperature to minimize film cracking. Here, burner
year, the drums were mapped and no bulges were found. modifications can reduce the maximum flux rate com-
Other methods employed in drum inspection include wet pared to the average flux for the furnace. Also, double
mag particle testing on welds and expansion joints. fired furnace designs will lower the maximum flux rate.
For coke drum pressure, obviously lower is better. The
FOSTER: recycled rate can be a tradeoff between yields and run
We use laser scan techniques to map the bulges in our length. Adjusting velocity steam injection can help opti-
old coke drums to measure changes over time. This is mize your run length. We have found the use of antifoul-
expensive, but it is only way we have found that we can ants to be unit specific. Minimizing transfer line heat loss
truly measure the size, severity and dynamics of bulges. between the furnace and coke drum is important. You
We also do ultrasonic inspection of all of the horizontal should have minimum pressure drop, short length and
weld seams on these drums every year, looking for any proper insulation.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 73
TOC/INDEX
Normal bulk cracking gives skin temperature increases 1. Minimize light material in the unit feed. For
of about 1°F per day, while film cracking can be as high instance, when we process slop we are careful to
as 5°F per day. Some details comparing the two cokers profile the tank in question. We also look at cold
is below: feed tanks to make sure the cutter is not stratified
in the tank.
#2 Coker: #1 Coker:
2. Even more important is the procedure used to
Furnace outlet 930°F Furnace outlet 945°F
warm-up a pump in preparation for a pump switch.
70-100 psig furnace outlet 90-150 psig furnace outlet
The warm-up procedure must not allow too much
pressure pressure
flush, especially cutter, to enter the pump that is
900#/hr velocity steam to each 1500#/hr velocity steam to
running during the warm-up step.
of 4 passes each of two passes
Maximum allowable flux rate, Maximum allowable flux rate,
HAHN:
23m Btu/sq ft/°F 16m Btu/sq ft/°F
T u b e w a l l t e m p i n c r e as e, T u b e w a l l t e m p i n c r e as e,
I agree with the previous comments. Our coker runs
0.7°F/day 0.9°F/day
about 14 months on a typical cycle and one time we were
even able to get 18 months on our delayed coker. We
found steam velocities in the heater to be very important,
MALEK: and, of course, proper instrumentation. One other item
Good design practice on high severity coker operations that you might want to pay attention to is the paraffinicity
would strive to achieve somewhere between eight months of your crudes. Highly paraffinic crudes mixed with non-
to one year of online service on the heater. The secret to paraffinic crudes present a challenge. We have adapted
doing this is the maintaining superficial tube velocities at certain guidelines that we follow so that we do not run
sufficiently high levels. Seven to ten feet per second are over a certain maximum amount of paraffinic crude. We
good bulk tube velocities that need to be sustained. If have established that guideline so that we do not coke
flow rates fall below the normal design rates, these bulk our heater prematurely.
velocities must be maintained by the addition of sweeping
steam along with the feed in order to keep the velocity PAUL STEEL (Conoco):
at a sufficiently high level. I just wanted to add that through our alliance with
The heat flux issue on the design is very important. Bechtel, Conoco licenses its patented distillate recycled
Generally, new heaters are designed with an average heat technology as a proven method of improving coker eco-
flux of no more than 9,000 Btus per hour per square foot. nomics by increasing liquid yields and reducing coke yield.
Every attempt is made to keep the peak flux temperatures However, this technology also delivers the additional ben-
down to as low as possible by spacing of the tubes and efit of measurably increasing furnace run length between
arrangement of the burners. decokes. This year one of our own refineries demonstrated
One of the biggest contributors to loss of run length this technology to extend its coker heater run length by
is feed interruptions. Just a very slight feed interruption 30 percent. We believe this technology can enable a well
will cause coking to occur. It is very important in the designed furnace to obtain run lengths of over one year
design to be able to sustain smooth feed at a steady flow between decokes for most resid feeds.
rate and at a relatively steady inlet temperature because
of the heat response on the heater. Provision for sweeping
ASHUTOSH GARG (Furnace Improvements):
the heater should be automatically provided. In the event
of inadvertent feed loss, steam should be rapidly added I would like to add the importance of uniform firing
to the coil to sweep the feed forward into the coke drums. of coker heaters. Most coker heaters have lots of burners
and if you put equal amount of fuel and equal amount
of air to all the burners and have good flame that could
CAIN: improve the run length.
Again, at Port Arthur our coker heaters run four to
six months between spallings and approximately four years Question 28.
between turnarounds when pigging is used to decoke. Have delayed coker operators been successful in decok-
Skin temperatures are monitored constantly and high fluid ing heater tubes with pigging methods? Has the fouling
velocity is maintained in the tubes. rate been the same/better/worse after pigging as com-
pared to steam/air decoking methods? Is it necessary to
FOSTER: follow pigging with steam/air decoking?
We can get nine months between on-line spalls. The
main thing that puts us into a premature spall are feed TASKER:
interruptions due to heater charge pump cavitation. We One of our licensees has a coker downstream of an H-
have addressed this problem in two ways: Oil unit and that heater design allows online decoking
one pass at a time, running the coker at reduced rate. It life. They have also installed special pigging breakout
is a pigging method that is used and we believe that this connections on the coker which facilitate the rapid hookup
has been very successful. Since steam-air decoking has not of the pigging apparatus.
been practiced in this location, it is not easy to make
direct comparisons between the two techniques. But based PETERSON:
on unit performance, it would appear that the pigging We do not have a coker, but we do have some experi-
method is better than the traditional method. ence with pig decoking of a vacuum heater. We found it
Typically, a special studded pig is used for the main to be faster and more effective than steam-air decoking
part of the decoking operations and this is followed by with no need to follow with steam-air decoking. We had
a polishing pig which has less studs and is less abrasive. an occasion where we were going to do some mechanical
Both ends of the heater can be worked similar to the work to the shock tubes of our convection section. We
steam-air decoking method. cut these tubes open. They were extremely clean inside.
Usually, a service company is used for this operation That raised the possibility that we were removing metal
and this has led to cleaner startups. There are also no from the tubes Inspection showed that we were okay on
disposal problems associated with this because it is all that aspect, too.
taken care of by the service. A typical improvement would
be approximately 160°F, back on the skin temperatures.
SAMUELS:
The tubes are not exposed to excessively high temperatures
A recent tube pigging attempted in our Robinson
during decoking if you use a thermal technique. We found
Number 2 coker failed. The cause of the failed attempt
that it is somewhat superior to the steam-air decoking.
was pig damage due to the heater plug design of the
In regard to the timing, we believe that one cell has
furnace built in 1968. The diameter of the header is just
been done in about eight hours and typically around
slightly smaller than the diameter of the tubes. It caused
about 14 hours would be a usual time. This method has
enough pig damage to render the pigs ineffective. That
also been used in crude and vacuum tower heaters. As an
is something to watch out for if you still have that design.
alternative, there is the steel shot and nitrogen technique.
It is a proprietary technique and that is also a very good
method. It does not expose your tubes to high tempera- HAHN:
tures. I think that procedure has been discussed in previous We have also found pigging to be a very effective
NPRA sessions. method. We used to steam-air decoke. The first time we
did our pigging, we noticed on startup that there was a
CAIN: significant difference in startup delta P. We attributed
We use spalling to decoke our heater tubes on a regular that to the removal of inorganics that we had not pre-
basis. We did use pigging during our unit’s first turn- viously been able to remove with steam-air decoking. We
around this year and it was not followed by steam-air took advantage of the reduced pressure drop to increase
decoking. charge rate rather than extending run length. We continue
to have 14 month run lengths.
HENKE: We have also done quality checks with a boroscope to
Our Minnesota refinery successfully pigged two verify the cleanliness after pigging and found that to be
delayed coker heaters during a turnaround in 1996. We quite effective. There was no tube damage that we noticed,
measured heater inlet pressures slightly lower at start-of- so we consider it a very successful method and we do not
run than after a normal steam/air decoke. This seems to steam-air decoke afterwards.
suggest that pigging will remove material from the heater
tubes that the steam/air decoke procedure can not, possi- JIM ZEIBIN, (Husky BPU Operations):
bly noncoke deposits such as salts. If the pigging is done I work at the plant that Mr. Tasker mentioned concern-
properly, you should not have to decoke the heaters ing pigging. We tried three methods of cleaning the heater
after pigging. tubes. We have tried pigging, mechanical turbining and
steam-air decoking. We used pigging the first time to
MALEK: determine where the most coke was found in the heater.
One of our clients in Texas has adopted the pigging This allowed us to locate our tube skin thermocouples
procedure as routine. They have traditionally steam-air to the point of the highest coke laydown. We tried
decoked in the post. They report that the tube surfaces mechanical turbining, but it did not clean the tubes suffi-
are completely freed of nonorganic obstructions that oth- ciently and we also had slight tube damage. We tried
erwise would not be removed by the steam-air decoking. steam-air decoking. We are a relatively new plant and we
Because of this, they believe that the cleaner internal had some difficulty with the system. So we have elected
surfaces will slow the build up of coke and extend run to continue with pigging and have excellent success. We
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 75
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 77
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CAIN: HENKE:
In Port Arthur, the silicone antifoam has a viscosity As I mentioned in Question #30, we have had very
of 60,000 centistoke. The carrier oil is light coker gas oil. good success with structured packing in our main coker
A study done there on three different viscosity grades of fractionators. Structured packing and other devices are
silicone antifoam showed no overall benefit to using the used to reduce pressure drop, improve fractionation and
high viscosity variety. provide the capability to increase overall coker
throughput.
Operation at lower recycle ratios will lead to fouling
JACK HARRELL (Baker Petrolite): of internals in the wash sections if they are not designed
I would agree with the panel and all of the comments and operated correctly. The design and operation of the
they have made so far except for one thing. We have internals is dependent on the heavy coker gas oil quality
found that in cokers that are using the lower viscosity requirements.
antifoams and are having significant carryover of the sili- With stringent quality requirements, the best choice
cone into the distillates off of the fractionator, going to is grid. Grid packing withstands process upsets better than
the higher viscosity materials usually cuts the carryover conventional internals and can also operate with high
about half. levels of coke fouling.
With flexibility in the heavy coker gas oil quality and
Question 32. an objective of ‘‘zero’’ recycle operation, we would tend
Has anyone used a non-silicone antifoam? How did it per- to lean toward a hybrid open spray chamber design. Grid
form? packing will foul and require periodic replacement if it
is not adequately wetted.
BINFORD:
Silicones have traditionally been the only effective MALEK:
product in high temperature hydrocarbon environments My comments pretty much support that. The use of
that we have seen. We have five patents on non-silicone the grid or the structured packing are very effective in
and reduced silicone programs for high temperature delayed coker fractionators. However, application of these
hydrocarbon environments. So this has been active devices in the lower sections of the coker fractionator can
research topic for us. The goal of our non-silicone be pretty troublesome when coking occurs. It is very
defoamer development was to reduce downstream HDS difficult, if not impossible, to clean these surfaces without
catalyst poisoning which is the problem most people are damaging or destroying them. So count on replacing them
going after. when you have severe coking that occurs in the bottom
Several years ago as a result of our work in this area, of your tower. You might want to consider some simpler
we tried some of these technologies in two Gulf Coast devices that are more amenable to cleaning.
refiners’ cokers. The non-silicone products were effective,
but only at very, very high feed rates. The cost for a non- HAHN:
silicone program at that time was about ten times the We also had very good success with a structured grid
cost for an existing silicone program, and we did not see in our fractionator. We did this mostly because we were
the justification for that increased expense in terms of having coke carryover up into the coker heavy gas oil
increasing of catalyst life at the HDS unit. section which we could not tolerate. The grid was very
So at this point, we would say that non-silicone pro- effective in resolving that problem.
grams in most coker systems are not justified. We know
of a few companies that claim to have low silicone coker ANDREW W. SLOLEY (Process Consulting Services Inc.):
antifoams. We have not seen any convincing side-by-side Packing use in the coker fractionator is relatively com-
comparisons against silicone that would convince us that mon. It is used to increase fractionation, lower pressure
a low silicone program actually reduced downstream drop, and lower recycle ratio. At least one coker main
hydrotreater catalyst poisoning or was cost effective. fractionator had all the trays replaced with structured and
grid packing. The coker main fractionator is really no
Question 33. different than other refinery heavy oil main fractionators
What has been the experience with grid/structured pack- as it regards packing use, with the exception of the wash
ing in coker fractionators? Are these packings being used section below the HCGO draw. The wash section is
to reduce pressure drop or improve fractionation? Has 760-780°F and the oil is thermally unstable. High liquid
operation at lower recycle ratios necessitated design residence time in the wash zone causes coking.
changes due to increased fouling in the fractionator bot- Trays, packing and spray chambers are used in the
tom section? wash zone. The specific column internal depends on the
targeted recycle ratio, HCGO quality, and column super- normally reduces the column pressure drop by 1 to 1.5
ficial gas velocity. Coker main fractionator wash section psia.
trays require 15% or higher recycle ratio to keep the trays The wash/ cleanup section of the coker fractionator is
from coking. Grid packing can be operated at recycle the most severe service that can be found in a refinery
ratios in the 7% range. Wash zone spray chambers or distillation unit. The type of distillation device used in
empty vessels operate at recycle rates of 5% or less. How- the wash zone should be carefully chosen based on the
ever, the spray chamber and empty vessel work best at refinery’s quality requirements for their HCGO.
low column superficial vapor velocity. A new coker main Designing the wash zone with grid packing is usually
fractionator is sized for a 0.15-0.18 C-factor (velocity the best choice when the quality requirements for the
term) while a revamped coker may operate at a C-factor HCGO are more stringent (Hydrotreater or hydrocracker
of 0.36-0.4. constraints) than can be achieved with a spray chamber
A revamped coker main fractionator wash section vapor design. Grid is mechanically robust and can withstand
velocity is typically 1.5-2 times the new column design. process upsets better than conventional trays or sheds.
Gravity settling of the asphaltene containing material For a given recycle or wash rate the grid packing will
occurs at C-factors of 0.15. At a C-factor of 0.36, gravity produce a cleaner and higher quality gas oil than will shed
settling does not occur. A spray chamber is not very trays or sprays. As the vapor velocity in the fractionator is
effective at removing asphaltenes. If high metals and pushed higher, grid become increasingly more effective
asphaltene HCGO product is acceptable, then spray than sheds, or weighted sprays in removing the coke fines.
chambers are adequate. The other variable is coke drum Grid packing can also operate with high levels of foul-
superficial velocity. At high coke drum velocity a consider- ing. For some ‘‘zero’’ or ultra-low recycle operations grid
able quantity of non-volatile material is entrained in the packings will foul over time and will require periodic
coke drum vapors. This material ends up in the HCGO replacement.
product if it is not removed. The specific design of the
wash section in a coker main fractionator depends on the Question 34.
What is the lower limit in coker cycle times? Please
specifics of each applications.
include a time breakdown for each of the activities. Is
this lower limit different for drums containing shot coke
BRIAN D. ALBERT (Koch-Glitsch): versus those containing sponge coke? Are blow back
Structured packing and grids have been utilized in problems increased as quench time is reduced?
coker fractionators with excellent success. For most
revamps, the primary project driver is to increase the CAIN:
capacity of the fractionator. A very common debottleneck- At Port Arthur, we use 16 hour cycles for decoking.
ing project is to replace trays in the HCGO pumparound Purge and steam, test drum takes 30 minutes and warmup
with grid or a large sized structured packing. The HCGO drum takes four hours. Switch drum time is seconds and
pumparound is the typically the most heavily loaded sec- fill empty drums takes 16 hours. Steam out full drum
tion of the column and debottlenecking here allows the takes 30 minutes, water quench takes three hours, drain
refiner to maximize the utilization of the existing col- full drum takes two hours, unhead drum takes minutes,
umn internals. drill coke takes two hours and rehead drum takes minutes.
Sheet metal structured packing (FLEXIPAC威 & GEM-
PAK威) have been successfully applied in several coker SAMUELS:
fractionators. Structured packing can often be used to Robinson’s two 13,000 barrels a day cokers produce
replace fractionating trays that are flooded or experiencing 1,400 long tons per day of anode coke. The drums are
low efficiency. When packing is used in the naphtha drilled directly into rail cars and the unit’s share a common
sections of a fractionator it is important to consider the drill water system and blow down system. Shot coke
column’s history of salting or corrosion. Because packings production is avoided as we have no means of handling
are relatively thin (0.008’’ typical) they have very little the flow from the coke drums.
corrosion allowance. Higher metallurgy materials such as When shot coke has been produced, we have seen a
Monel, AL6XN, or Hastelloy C may be required for time increase from 25 to 50 percent in the cool down
fractionators column where the overhead temperature is and drilling steps due to the hardness and structure of
expected to be below 250°F or that have a history of the coke compared to sponge coke. Blow back has not
salting or chloride corrosion. been a problem or limited quench time.
Pressure drop reductions are a natural result of utilizing We operate the two cokers on 18 hour switch times
packings in a fractionator. For every tray replaced with that are offset by nine hours. This requires decoking four
packing, the tower pressure drop will be reduced by 0.1 drums every 45 hours or the equivalent of 11 hour cycle
to 0.15 psia. Replacing 10 trays in coker fractionator times. Each coke drum’s actual cycle time is 18 hours,
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 79
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but two drums are being decoked simultaneously, nine entrainment do you want or can put up with. At this
hours apart. That is done to compensate for the common time a drum velocity maximum must be established.
drill equipment and to meet the switch times of the
two units. TARIQ MALIK (CITGO):
Automatic unheading devices and coke crushers are Vapor velocity through the drums is a function of the
not used. Rather than get into the detailed steps of the pressure that you run your drums at and the vapor density.
drilling. I have included a bar chart of the switching Normally, at a typical vapor density, you can afford a C
sequence and timing. factor equivalent to half feet per second, with a maximum
of 0.70. At higher than 0.7 C factor, you will start entrain-
PAUL STEELE (Conoco): ing coke fines to the fractionator. This is an equivalent
I just wanted to add that Conoco currently operates factor that is used in designing of fractionators.
at 11 hour drum cycles on two of our cokers at two
different facilities. We have been operating at 11 hours HIGGINS:
on one coker making shot coke for a few years now, and The 1996 Q&A transcript includes additional detail
this year we attained 11 hours on another facility’s coker on coker cycle times.
that makes a sponge anode coke. We also feel that ten
hour cycles are attainable, and we are currently studying
implementation at one of our facilities. 3. Residual Feeds
ED CHOY (Husky Oil): Question 35.
We want to increase our coker capacity by lowering What is the highest Conradson carbon material now rou-
our coke drum cycle from the current of 20 hours down tinely being fed to a delayed coker or fluid coker as a
to about 14 hours. What I want to know is what is the component of fresh feed? What is the highest Conradson
maximum coke drum vapor velocity that is allowable carbon on total fresh feed to a delayed coker or fluid
beyond which we can run into serious problems of carry- coker? What are the delayed coker heater run lengths
over and foamovers? when processing these feeds?
HENKE: FOSTER:
There is no magic number; the determining factor is Our coker feed typically runs 29-32% Conradson car-
when you start coking the overhead line from carryover. bon as a percent of total feed. The crudes we process at
In some cases ‘‘ fines carryover ‘‘ is present but the over- Lyondell-Citgo Refining are all 17°API gravity Venezue-
head line is not coking. The question then is, how much lan crude oils, with cutpoints of 1050-1100°F on the
Question 36.
TASKER:
What is the minimum furnace tube mass velocity required
In one of our H-Oil unit operations, the H-Oil bottoms to prevent coking? Do low mass velocities have any other
products does go to a delayed coker. In other ebulated effects (positive or negative) on furnace operation?
bed operations, the bottom products are also fed to carbon
rejection processes. The range of CCR contents in the
bottom products going to the cokers typically varies MALEK:
between about 20 to 25 wt% CCR and typically about Visbreaker velocity should be maintained at a superfi-
23 to 24 for Canadian crudes. cial velocity of about 8 to 10 feet per second in order to
With these levels of CCR, the run length may be prevent coking. Lower mass velocities, or those approach-
around about six months, but this may well depend on ing the minimum, usually will be beneficial because this
the timing and planning requirements for decoking. will increase the conversion achievable in the furnace
When you consider the harsh winter months in Canada, tubes themselves. Visbreakers may be designed for all coil
this is a fairly critical part of the operation. cracking or they may have soaker drums downstream of
Of course, the H-Oil is intended to reduce the amount the tubes. Some of the same comments that applied to the
of CCR which would then reduce the amount of coke. coking operation apply here, of course. Feed interruptions
But around about 25% is the maximum we generally see. promote coke lay down and need to be avoided. The
same instrumentation needs to be provided to provide
for a sweep with steam in case of loss of feed flow through
JAMES D. WEITH (Fluor Daniel): the heater.
On these heavy resid streams you are feeding, I would You will find a number of the visbreaker operations
like to poll the panel to see if anyone has a feel for what around the world are incorporated into relatively simple
the pour point of the heavy coker gas oil is? refineries. In some instances there is not as much attention
paid to the desalter as in a more complex refinery. The
presence of sodium in visbreaker feedstocks will accelerate
HENKE: a coke lay down and severely limit operation of a vis-
The heaviest HCGO that we make has a pour of 60°F. breaker. So attention needs to be paid to the desalter
operation in order to increase run lengths.
BINFORD:
BetzDearborn has not done an extensive survey on the TASKER:
relationship beteen Conradson carbon and coke fouling, I agree with a lot of what Mr. Malek said. For design
however we have been involved in several fouling control purposes, IFP designs the inlet velocity to the visbreaker
projects and have Conradson carbon data on feedstocks heater at about 2 to 2.5 meters per second or let us say
related to cokers that have a history of fouling. From the 7 to 8 feet per second.
period of 1991 to 1995, four studies were done on delayed We also use steam condensate injection to ensure that
coking operations that experienced severe fouling prob- the coking potential is minimized, and this rate is normally
lems in their cokers. Conradson carbon ranged from 14.6 about .5 wt% of the feed. We minimize the tube diameter
to 25.9. Of the four cokers studied, three out of the four to about five inch tubes and the space between the tubes
coker feeds had Conradson carbons in the 14.5 to 16.5 to about two diameters. Average heat flux is generally
range. The cokers processed resids from a variety of crude about 20 to 22 kilocalories per square meter per hour.
feedstocks, including heavy California crude (cut with Lower velocities, of course, will tend to lead to over-
ANS), Canadian crude, and heavy Venezuelan crude. The cracking and to coking conditions. For those visbreakers
coker that had the highest Conradson carbon (25.9), with soakers, the soaker temperature is kept about 20 to
processed vacuum reside derived from the heavy Venezue- 25°C lower than the visbreakers without soakers. Typical
lan feedstock. furnace run lengths are between nine and 12 months and
most of the problems which contribute to furnace coking
are in the feed preheat system. Of course, feed interrup-
EUGENE ROUNDTREE (Exxon): tions do not help as well. As part of the design, we provide
The highest carbon content feed fed to our flexi and double shell exchanger systems or spare exchangers. For
fluid coking units has been about 35 wt% concarbon. coil type furnaces without soaker sections, run lengths are
We believe that these units can process any material which typically in the order of three to four months between
is pumpable up to about 500°F. decokes.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 81
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 83
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used, erosion caused by particulates in the amine solution, The distinguishing features of the SSF娃 technology
flashing CO2, and high velocity, and localized lack of is that this membrane, versus a polymer type membrane,
metal passivation. Dow’s experience with GAS/SPEC* keeps the lighter components on the high pressure side,
CD-Plus has resulted in the following. in this case hydrogen, and also the pressure drop required
Reduction of corrosion begins with design criteria that through the membrane is much lower. A recent article
minimize these effects. Amine velocities should be limited in the June issue of Today’s Refining discusses the merits
to 3 fps in carbon steel and 7 fps in stainless steel piping. of the SSF娃 technology.
Rich loading should be limited to 0.45 moles CO2 per I would also like to refer you for the more traditional
mole amine to minimize CO2 flashing. The approach hydrogen purification technologies, to a white paper of
temperature of the lean—rich cross exchanger should UOP that discusses the selection criteria for pressure swing
be limited to 45°F to minimize CO2 flashing. Piping absorption, selective permeation and cryogenic separation
metallurgy should be 304SS for the rich amine circuit processes. The paper is entitled ‘‘UOP Process Solutions
between absorber and stripper. Exchanger tubing for all for Reformulated Gasoline.’’ I spoke with the gas separa-
four exchangers should be 304SS. tion folks at UOP. Although the paper has not been
Operating guidelines include assuring adequate amine updated since 1991, they feel that the basic principles
concentration and circulation to maintain the limit to the still hold for selection criteria. You may contact John
rich loading and adequate stripping to achieve the speci- Geeseman at UOP at (847) 391-2937 if you would like
fied lean loading. a copy of this paper.
Question 2. TASKER:
To make RFG and low sulfur diesel, refiners need more Well, in addition to addressing the first part of the
hydrogen, yet traditional sources like catalytic reformer question, we can alleviate the reformer hydrogen produc-
hydrogen are being reduced. How are refiners meeting tion by changing the reforming catalyst. As a small plug
this challenge: purchased hydrogen, new or revamped for Acreon Catalysts, they have developed a reforming
hydrogen plants, recovery systems, etc.? Are any new catalyst RG582 that produces a high level of hydrogen
feed sources or technologies being used to produce yield with a wide range of octane values. This catalyst is
hydrogen? currently being used in about 17 different units around
the world and more details can be obtained directly
SAMUELS: from Acreon.
In the area of new hydrogen production technologies, As to the second part of the question, there are a
Marathon researchers have developed the HYSULF pro- number of possible sources of purchased hydrogen, mer-
cess for the manufacture of hydrogen from hydrogen chant hydrogen, and this may depend very much on the
sulfide. The process uses redox chemistry under mild location and industrial area where the plant is located.
operating conditions to convert H2S into hydrogen and These sources include purchased hydrogen from chlorine
sulfur. The process employs two basic steps, the hydrogen manufacturing and other processes. So they may well be
sulfur production and recovery step and the hydrogen limited geographically.
purification step. A major engineering firm has estimated There are also a number of companies licensing skid
that the capital costs of the HYSULF process is 30 to 50 mounted hydrogen generation units and other companies
percent less than a claus tail-gas plant combination due that would setup with producing plants in association
to fewer major pieces of equipment that are required. with the hydrogen producers.
The process produces about 22,000 cubic feet of hydro-
gen per ton of sulfur produced. In addition to evaluating HENKE:
internal applications for this process, Marathon is cur- In our refineries, we are maximizing hydrogen produc-
rently seeking external support for the construction of a tion by focusing on getting the most out of our existing
demonstration unit in 1999. assets. We have made significant progress in four areas:
Details of the process can be found in an NPRA paper 1) we are debottlenecking our steam methane reformers
that was presented by Dr. Mark Plummer entitled ‘‘The through enhancements to the PSA systems, Benfield oper-
HYSULF Process: A Valuable Hydrogen Resource from ation, and heat removal systems; 2) we are recovering as
Hydrogen Sulfide,’’ and was presented in the Spring 1995 much hydrogen as we can from the fuel gas system; 3)
NPRA Annual Meeting. we are reducing the requirement to purge hydrogen from
In the area of separation technologies, Air Products hydroprocessing units by focusing on make-up hydrogen
has a new gas separation membrane known as selective purity control; and 4) we are improving the reliability
surface flow or SSF娃 membranes. A 0.5 to 1.5 million and mechanical availability of our hydrogen producing
standard cubic foot per day demonstration unit is in units. We have found that this last area is a significant
service and operates with full scale membrane separators. source of additional hydrogen.
84 Hydrogen Processing
TOC/INDEX
JOSECK:
At one refinery, we recently completed a study to sup-
plement the hydrogen source. One new technology we
considered in membrane purification from Air Products
was SSF . The SSF technology was considered due to the
lower hydrogen compression requirements and traditional
membrane technology. The new technology is capable of
producing hydrogen at a higher pressure than the vent gas
or heavy hydrocarbons. SSF membranes are gas separating
membranes that comprise a microporous adsorptive mate-
rial supported on macroporous substrate. The SSF mecha-
nism preferentially permeates larger or more polar gas
components to the low pressure side of the membrane.
The unit design considered increased hydrogen impurity
of a low pressure separator or off gas stream from 68
percent to 90 percent hydrogen. Product hydrogen recov-
ery was estimated at 80 percent with an inlet feed pressure ROMAN:
of 225 psig and a product hydrogen pressure of 200 psig. Ashland has developed a gasification process called
The vent permeated was at 5 to 10 psig. Hymeltt and is working with a EnviRes LLC to commer-
cialize this process. Feed is introduced below the surface
of a molten metal bath, ranging in temperature from
MALEK: 2,500 to 3,000°F. All organic material in the feed is
We have found that the hydrogen recovery techniques rapidly dissociated into its elements. Hydrogen and nitro-
and conservation in the refinery can only go so far in gen primarily evolve as gases. The carbon and sulfur dis-
meeting the RFG requirements. Usually, the next step solve in the metal. Oxygen in the feed evolves as car-
that a refiner has to take in meeting these requirements bon monoxide.
is a large increment of hydrogen. One approach that The carbon content in the bath increases with time
refiners are increasingly following is a usage of merchant and the overall reaction is endothermic. When the carbon
hydrogen. Good examples of such systems are those oper- content reaches a preset level, the feed is interrupted and
ated by Air Products in the New Orleans and Houston oxygen is then injected into the bath. The oxygen reacts
area, and the new system that is being installed by Air almost exclusively to produce carbon monoxide in an
Liquide in the Corpus Christi area. exothermic reaction, with methane or steam sometimes
These systems take advantage of the fact that there are added to provide an overall heat balance for the system.
The gas evolved in the first vessel contains more than
quite a few sources of excess hydrogen being produced
90 percent hydrogen and the gas evolved in the second
in various industries that we are not perhaps familiar with,
vessel in excess of 90 percent carbon monoxide which
i.e., ethylene plants, chlorine cells and a number of others.
can be shifted to hydrogen, converted to products such
These merchant suppliers will, as a business opportunity, as methanol or burned in a heater. We believe the process
to go out and seek these sources, put in the collection can also be operated at a pressure in excess of 400 pounds
systems, the pipelines, the compression and the purifica- and the process tolerates a wide range of feeds from meth-
tion systems. They will usually supplement these systems ane to SDA pitch.
with their own steam reforming processes to balance out Ashland built and operated a pilot plant from 1992
the hydrogen requirements. until 1996 with a nominal molten metal capacity of 300
The sources from new ethylene plants are quite signifi- pounds. When the SDA pitch was fed, the gas from the
cant. We are all aware of how much activity there is in first zone contained 92 percent hydrogen. We plan a
ethylene plant construction. For example, a one billion larger scale testing in a pressure capable vessel containing
pound per year ethylene plant can generate easily a surplus six tons of molten metal. The larger scale testing should
of 40 to 60 million cubic feet a day of hydrogen. It might provide all of the critical design information for a commer-
not be practical for a refiner on an individual basis to go cial plant with a molten metal capacity of 100 to 200
out and seek this supply. But these merchant suppliers tons, and capable of producing between 10 and 35 million
are aggressively trying to develop these pipeline networks standard cubic feet a day of hydrogen.
to accumulate these excess sources of hydrogen and to This plant is expected to have a high turn down ratio
supply a reasonable and reliable source of hydrogen. We of 4 to 1 or better and be capable of rapid responses to
believe that this type of approach will continue to acceler- change in feed rate making it ideal for process or load
ate in the industry. following. When the heating value of CO produced by
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 85
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86 Hydrogen Processing
TOC/INDEX
streams or by revamping a steam-hydrocarbon reforming way we can be prepared for the next anticipated down
type hydrogen plant. time with the appropriate number of tubes on hand and
If the refinery chooses to revamp a hydrogen plant, a have a turnaround well planned.
variety of options can be considered, applied individually
or in combination, to increase the capacity of the plant. ROMAN:
These options are: Most of our recent problems have involved poor firing
—Add a Pre-Reformer in series with the reformer. patterns in the fire box. At high turn down ratios, we
Expected increase in capacity is 10-12%. have experienced excessive air leakage into the fire box
—Add a Low Temperature Shift reactor in a PSA where the tubes enter through the floor. In an effort to
based hydrogen plant. Expected increase in capacity reduce excess air to the stack, the operators would cut
is 4-5%. the air to the burners and the oxygen starved flame would
—Increase reformer inlet temperature by adding a be pulled over against the tubes where additional air was
reformer feed preheater in the convection section. entering into the firebox.
Expected increase in capacity is 3-4 %. The resulting flame impingement caused creep damage
—Increase capacity by increasing the inside diameter and eventual failure. The tube entry holes have subse-
of the radiant tubes by upgrading metallurgy. While quently been sealed with ceramic fiber to avoid this leakage
expected increase in capacity varies from reformer and prevent a recurrence of this problem.
to reformer, up to 20% increase has been possible
in a case study. BARLOEWEN:
—Add a post reformer or a secondary reformer into I am going to focus on the potential of tube failure
the flow scheme. This has the potential to increase during start up. Startup is basically an unusual operation
capacity by more than 20% provided the down- where you have very low mass flow through the tubes
stream heat recovery train and shift reactors are able and no heat of reaction. So, right away the normal rela-
to handle the increased gas flow rate. tionships between process temperatures and furnace tem-
The technology for new hydrogen plants is continu- peratures do not apply. In addition, there are some vendors
ously being upgraded as new developments in metallurgy that recommend relatively high furnace outlet tempera-
and catalysts take place. The development of high activity tures before you cut in the hydrocarbon feed, in excess
pre-reforming catalyst has enabled the pre-reforming tech- of 1,300 to 1,400°F. At Topsoe we like to see the furnace
nology to be well established both for new and revamped outlet temperature below 1,200°F.
plant designs. Post reforming in convective, heat The final thing to emphasize on startup, and it really
exchanger type reformers, currently in use in ammonia applies to reforming furnace firing in general, is that in
plants can be applied to hydrogen plants. today’s refinery with a concentration of instrumentation
KTI has done many debottlenecking studies. We will in the control room, it is sort of like the home office.
study all the options and propose the most cost effective The home office feels like they know everything that is
scheme for debottlenecking your hydrogen plant. going on. In the control room, they feel like they know
everything that is going on. A reforming furnace is a
Question 3. classic piece of equipment that you have to monitor in
What is the panel’s advice on how to avoid overheating the field and there is no substitute for it not only during
of steam reforming furnaces? startup, but also as the run progresses.
PETERSON: CAIN:
We did have one tube fail in our hydrogen heater and Two causes that we have seen were unexpected loss of
one of the contributing factors was poor flame patterns feed to the reforming furnace and also changes in the fuel
from dirt in the fuel gas to the burners. We have gone gas btus. We have implemented advance controls that
to cleaner gas to help prevent that. We also have the detect changes in the fuel gas gravity and make adjust-
operators performing surveillance, both optically and with ments for that. We also installed an SOV (solenoid oper-
an infrared device to help find the hot spots in the heaters ated valve) to close the main fuel gas valve on heater loss
and adjust the burners accordingly. The tuning of the of steam flow, loss of the draft fans, and low level in the
PSA and other instruments as well as preventing upsets boiler. We also monitor the loading procedure of catalysts
all help to prevent the problems in heaters. to make sure that there is a good, even Delta P across all
We have also recently gone to a predictive maintenance the tubes to prevent hot spots.
system where we had a device called H-Scan. It was pro-
vided by a company called IESCO. It is a proprietary SHOOU-I WANG (Air Products):
ultrasonic method that crawls up the tubes and gets a I think the panel and KTI have suggested a number
very complete inspection of the metal condition. This of very good recommendations. I want to add one area
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 87
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on preventing a reformer furnace from a catastrophic in the reformer is much higher. KTI has experienced drift
failure, such as a melt down of reform tubes. The practice at the process outlet temperature of as much as 200°F.
we have is to use two out of three voting systems to shut In order to avoid overheating of the reformer the fol-
down the high temperature reforming process effluent lowing steps are recommended:
and also as a back up to use two out of three voting 1. Tube wall temperatures should be measured at least
system to shut down on high temperature. This is at the once per shift using an optical pyrometer that auto-
flue gas temperature at the outlet of reform radiant section. matically compensates for white wall reflection.
Optical pyrometers that do not have this capability
ANDERS NIELSEN (Haldor Topsoe A/S): will always indicate a higher tube wall temperature.
I would like to point out that some very hot tubes and Under normal operating conditions tube wall tem-
some tube failures are associated with sulphur poisoning peratures should indicate 80°F to 100°F higher
of the catalyst. This particularly occurs in the top part of than the process outlet temperature.
the tubes where the feed enters and where the temperature 2. Develop a curve based on CH4 slip in the process
and ph are low. effluent versus theoretical temperature of the pro-
The sulphur poisoned catalyst loses activity for steam cess effluent. Check the methane slip and theoreti-
reforming and the feed proceeds unconverted to the hotter cal temperature versus the indicated temperature
part of the tubes leading to coking of the catalyst. This and the tube wall temperature.
is worst in the hottest area by the tube wall. The tubes 3. Periodically (once a month) a calculation to deter-
are overheated since little heat is absorbed, and deposited mine the approach to equilibrium should be made.
coke can lead to channeling. The overheating of the This will require a full analysis of the reformer
tubes—often worse in local areas—leads to mishaps. The effluent gas.
situation becomes more critical the higher the content of 4. Although items 1 and 2 also apply to start-up of
higher hydrocarbons in the feed. the reformer, care should be taken to ensure that
there is an adequate flow of circulating nitrogen
JIM ABBOTT (ICI Katalco): through the reformer tubes to prevent overheating.
First off, I would just like to agree that it is very KTI uses a flow of 1850 scfh/per reformer tube as
important to monitor the reformer tubes out in the field a minimum and 2500 scfh/per reformer tube as
during startup. Visual monitoring is extremely important. a maximum.
The second thing I would like to draw operators’ atten- It is also recommended that a constant visual inspection
tion to is an emerging phenomenon which we have of reformer tubes be carried out during start-up. When
observed on top fired reformers. This is around the use reformers suffer damage during heat-up, investigations
of new shaped reforming catalysts which have indeed normally reveal that constant surveillance of the reformer
enhanced heat transfer and reduced tube-wall tempera- tubes would have alerted the operator in time to prevent
tures. Often the position of the peak metal temperature major damage to the reformer tubes.
has moved from a point on the top half of the tubes
down towards the very bottom. BRUCE SCOTT (Bruce Scott, Inc.):
The point I would like to make is that it is necessary One of the problems with shooting the tubes with a
to watch out when the reformer is loaded up again within pyrometer is guessing what the emissivity and the reflecti-
increased firing as indeed is possible with the shaped vity of the tube is. I would kind of like to poll the panel
reforming catalyst. When monitoring your tube wall tem-
and see if there is any experience with E2T’s little black
peratures, be sure to check where the peak temperature
hole device which is supposed to eliminate those concerns.
actually is. Measuring the tube wall temperature in the
same position as before could well give too low an answer.
You need to check all the way down and check where the HIGGINS:
highest temperature is to avoid any potential for premature No response.
tube failures.
Question 4.
ERIC FEARON (KTI Corporation): Our methanator trips on high temperature monitored at
During normal operation of the reformer we have to a thermocouple 25% down in the bed. This ensures that
take the process outlet thermocouple into consideration. the trip occurs before the bulk of the catalyst and reactor
This thermocouple is subjected to high severity service are overheated. As the catalyst ages and deactivates, is
due to the high process effluent temperatures and as such, the ‘‘25% point’’ still sensitive to a surge of CO2? Is there
is liable to drift. This means that process outlet tempera- a safer strategy to follow for the protection of methanators
tures can actually read low when in fact the temperature as catalyst ages?
88 Hydrogen Processing
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BARLOEWEN: HENKE:
In order to be of real value, an instrument in this We do not recommend a separate guard bed immedi-
services has to be able to detect sulfur concentrations ately upstream of the low temperature shift catalyst. If
down to 10 parts per billion. A modern desulfurization chlorides are suspected in the feedstock or import recycle
system followed by a hot zinc oxide system will reduce hydrogen, it is advisable to remove them in the front by
your sulfur level to well below those levels. This is the providing chloride absorbent catalyst beds upstream of
protection system most people use unless they have a the zinc oxide reactor. This is done because the chloride
known problem. There are some instruments available species have to be hydrogenated before they can be
and being used that can measure in the 10 part per billion absorbed by the catalyst. Also most catalyst manufacturers
range level. recommend installing this catalyst in a dry stream since
The second part of the question discusses the question chlorides are easily washed from the catalyst by water and
of sizing of the cobalt moly catalyst or desulfurization can be transported downstream.
system and why there is such a variation between licensors. Chlorides can also be introduced into the system
I believe the answer is that it reflects the fact that these through process steam or the use of chlorinated solvents
units are not sized for normal operation. The normal during maintenance. Steam can be easily eliminated as a
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 89
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source of poison by ensuring that the boiler design pre- both the reformer and high shift and a permanent poison
vents carryover of boiler solids into the process steam to the low shift. Even after the low shift is changed and
system. the chloride intrusion has been fixed, we have seen rapid
Having said all this, I would like to point out that deactivation from the chloride poisoning continue on low
ammonia plant operators have installed guard beds, temperature shift. What happens is that the chlorides
upstream of the low temperature shift reactor, consisting come off the upstream catalyst. Unless you change those,
of the low temperature shift catalyst itself. They do this the accelerated deactivation of the low temperature shift
because it is extremely difficult and expensive to remove will continue. It continues to come off even after the
chlorides from their process air. performance of the reformer and high temperature shift
returns to normal. So those should be considered for
JOSECK: changing, including the zinc oxide and cobalt molyb-
The concern is chlorides in the feed or chlorides from denum.
a leak in a waste heat boiler or process steam generator.
We currently use chloride guard catalysts in three units. KEN CHLAPIK (ICI Katalco):
The guard catalysts are loaded as a layer of catalyst on We believe the most effective low temperature shift
top of the main low temperature shift catalyst beds. At catalyst solution is a self guarding low temperature shift
one refinery using naphtha reformer hydrogen as a feed, catalyst. What this allows the hydrogen operator to do is
we have a chloride guard bed on the inlet to the desulfur- to maximize the effectiveness of the entire bed for the
izer reactors and the low temperature shift reactor. CO shift activity. Depending on the poison that you are
We have had one incident where we had a leak in a looking at, the kind of catalysts that we offer can provide
waste heat boiler and the chloride bed aided in the protec- up to 5 to 20 times the amount of poison retention that
tion of the low temperature shift catalyst. The low temper- is needed to fully deactivate the catalyst. So even though
ature shift catalyst was protected. The amount of guard the catalyst is fully deactivated, it is still receiving poisons
catalyst is dependent upon the severity of the chloride and absorbing poisons beyond that point.
contamination. If chloride contamination is suspected due
to short low temperature shift catalyst life, approximately Question 7.
five percent of the catalyst should be loaded as guard Are any refineries currently monitoring for methanol
catalyst. Samples of the spent low temperature shift cata- emissions from their hydrogen manufacturing facilities?
lyst can help determine the amount of guard catalyst If so, what levels of methanol are being found? What
required. analytical methods are being used?
BARLOEWEN: HAHN:
I mentioned earlier that Topsoe would provide a chlo- One of our West Coast refineries with an SMR recently
ride guard between the cobalt moly and the zinc oxide measured methanol in their emissions from that unit and
system. However, for the first charge of the low tempera- found them to be extremely low, much less than any of
ture shift, we would also provide a chloride guard on top the anticipated requirements.
of the low shift and then let the data from that first That unit had both a low temperature shift and a high
cycle determine whether it is necessary by measuring what temperature shift. We have learned that the amount of
chloride pickup occurred during that cycle, the obvious methanol formed during the high temperature shift is
source being the steam system. extremely low under normal conditions and the amount
can be controlled under the low temperature shift reaction
R. RAJAMANI (Mangalore Refinery & Petrochemicals Ltd.): through kinetics. If we keep the temperature low enough
We have chloride guard catalyst on top of cobalt molyb- on our low temperature shifts, then the methanol produc-
denum catalyst. Recently, we found that chloride is escap- tion is not very high at all.
ing, from cobalt molybdenum catalyst up to .5 ppm. I
would like to know the panel’s view on what should be BARLOEWEN:
a maximum chloride content which can be tolerated by The emissions of methanol from hydrogen plants is
the reformer catalyst. increasingly a concern. Measurement of it is difficult in
the CO2 vent, and somewhat easier in the condensate.
HIGGINS: Topsoe has developed a very accurate model to predict
No response. the formation across the low temperature shift catalyst.
We compared it with one refiner and came within three
ROSS BRUNSON (United Catalysts): percent of the measured values. For a unit utilizing just
We have seen cases where you have chloride intrusion a low temperature shift, not a high temperature shift, the
from the feed gas. It shows up as a temporary poison to emissions for a 70 million standard cubic foot a day
90 Hydrogen Processing
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hydrogen plant ranged from 500 to 3,000 pounds of Determining the total make of methanol is slightly com-
methanol per day. The methanol formation as was pointed plicated because it partitions between the CO2 and the
out is sensitive to temperature. A 20 degree decrease in process condensate. The process condensate, then, itself
temperature in the operation of the low shift will decrease is often stripped and thereby leads to a vapor emission.
the methanol formation by a factor of two. It is sensitive We believe that the best means of monitoring the
to space velocity, i.e., higher space velocity will reduce byproduct methanol routinely is to take a sample of this
methanol formation. The lower the CO concentration, cooled process condensate. The water sample can be ana-
the lower the methanol formation and the more steam, lyzed by gas liquid chromatography for methanol. Fur-
the lower the methanol. thermore, the methanol in the CO2 can then be simply
Topsoe recently introduced a new low emission cata- calculated by means of well tried and trusted models.
lyst. It went into service in the past month in the West In terms of what those levels of methanol are, it depends
Coast. It reduces emissions by a factor of eight from the on gas conditions, dry gas composition, and steam to dry
typical catalyst. gas ratio. Temperature is very important and also the
quantity of catalyst volume and the catalyst age also play
JOSECK: a part.
Most of the methanol produced in hydrogen plants Finally, the inherent catalyst selectivity is the most
from low temperature shift concentrates in the process important feature of all in limiting the methanol pro-
condensate. The level in the condensate depends on the duced. For instance, potassium doped low temperature
operating condition of the low temperature shift, specifi- shift catalysts which have now been patented and are now
cally temperature, new or used catalyst, steam to carbon being further developed will give significantly lower rates
ratio, the amount of CO and CO2 in the feed. We have of methanol formation. They will do this without sacrific-
sampled the process condensate infrequently and it has ing any capacity to absorb poisons and only taking a small
ranged between 1,200 and 4,000 ppm with an average activity hit.
of 2,600 ppm. Samples were analyzed by an outside lab. We have experience already with one of these types of
United Catalyst reports levels of 400 to 600 ppm for catalysts in meeting the needs of a plant which had metha-
new catalysts and recommends higher activity catalysts to nol emissions problems.
reduce methanol concentrations. Based on recent MACT
concerns, we are in the process of reevaluating all the B. Hydrotreating
process condensate streams in the CO2 vent for methanol.
The analytical method for the vent and process condensate
is GC-FID utilizing NIOSH, method 2000 in a manner 1. Reactor Bed Plugging
consistent with U.S. EPA RM18 or SUMMA canisters Question 8.
in accordance with methods TO-12 and TO-14. Analyses What is being done upstream of hydrotreaters to mini-
performed by analytical procedures from method TO-12 mize causes of bed plugging? Please discuss metallurgy,
for NMOC and EPA RM18 for methanol. The API has corrosion control, intermediate storage and filtration.
petitioned the EPA to either (1) eliminate CO2 vents for
miscellaneous vent requirements for MACT I, (2) after Question 9.
further review of the data and if appropriate and feasible Has anyone found a reliable method for filtering solids
the EPA could add control requirements for methanol from a heavy feed, such as products from a coker, FCCU,
from hydrogen plant vents to refinery MACT II rules, or other processes? List specific micron sizes for typical
or (3) list hydrogen plants as a separate source category particulate foulants.
and evaluate the need for regulation.
Question 38.
SHOOU-I WANG (Air Products): Beyond the normal precautions of feed filtering and tank
We are currently monitoring the methanol emissions gas blanketing of feedstock to distillate/heavy oil hydro-
from one of our larger hydrogen plants in Northern Cali- treaters, what new methods are being employed to mini-
fornia. Recently we analyzed the cold process condensate mize fouling and extend run length? Has compositional
from another hydrogen plant in Pasadena, Texas. We analysis of feed streams resulted in significant findings
measured about 170 ppm methanol. The measurement relative to the mitigation of fouling?
was performed on the HP5890 gas chromatography and
used a DB wax column. BARLOEWEN:
Well, the subject of plugging and how to avoid it is a
JIM ABBOTT (ICI Katalco): perennial question. I am going to provide the base starting
We also know that a number of refineries are increas- point on avoidance. The first point is upgrade the metal-
ingly concerned to monitor and minimize their emissions. lurgy in the upstream units, particularly in the hot and
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 91
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92 Hydrogen Processing
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Although unusual, we found a few cases where corro- For napthenic acid corrosion, refiners have blended
sion actually occurs in intermediate tankage or in preheat feeds to a total acid number of less than 0.5 mil KOH
exchangers. This can be effectively addressed by either per milligram and used stainless steel grades with greater
installing a more corrosion resistant metallurgy or an than 2.5 wt% molybdnum with success. Corrosion inhibi-
effective chemical treatment program. tors have been used, but unfortunately the most effective
A well designed disperssant type antifoulant program phosphorous based inhibitors are also catalyst poisons.
can be used to effectively combat pressure drop buildup
due to inorganic foulants, but these are usually effective FOSTER:
only if they are applied before the bed fouls significantly. We produce well over 20 mbpd of coker heavy gas oil
It is also important to make sure the top of the reactor (CHGO) at our refinery. The quality is very poor, so it
bed is designed to accept the smaller dispersed particles. is essential to treat all the feed at our Cat Feed Hydrotreat-
Mr. Barloewen already covered intermediate tankage, but ers, and to maximize the run cycle. So we spend a lot of
polymerization mechanisms can also occur in the preheat time on our feed filter design. But we have found by
exchange equipment. Identifying the source of the poly- experience that no matter how good our filtration system
merization and the mechanism is critical in designing a is at our hydrotreater, it can be defeated by the sheer
proper antipolymerant program to address reactor bed quantity of fines in CHGO if the fractionator is not
fouling resulting from polymer formation. designed or run properly.
So to protect our CHGO quality, we install two redun-
CAIN: dant wash oil spray headers above the CHGO draw sec-
One other item I could add to previous comments is tion. Each spray can deliver 100% of the required wash oil,
that on the intermediate tankage be careful where your and each is designed to deliver a minimum 30% overlap.
draw point is. Your draw point could be too low and you But good design is not enough. At turnaround time
could be pulling in water and sediment. Needless to say, we require a process engineer to witness and approve the
you need to drain your tanks regularly. spray test prior to closing up the vessel. Sometimes there
I have some experience in our Delaware City plant on is an obstruction in a nozzle or other problem that prevents
a furnace oil hydrotreater. We plan to upgrade it to 316L a good spray. Even though there is intense pressure to
stainless steel when replacement is required, however it get the unit back in operation, it pays to make sure your
may not be justifiable. To reduce plugging, they have sprays are right.
installed shaped support balls and they are also using We have had some success with the installation of a
a Nalco disbursement which has been very effective in coke removal system on the coker fractionator. We filter
dispersing polymerized hydrocarbons. The shaped sup- a slip stream from the bottom of the fractionator, cool
port balls are made by Haldor Topsoe. it to about 300°F and then pass it through a standard
cloth filter. This tends to prevent coke buildup in our
FLETCHER: fractionator, as well as lower the coke fines in our HGO.
With respect to particulates, we know of several refiners
that are reliably filtering large particles greater than 25 HAHN:
microns from gas oil feeds. For smaller particles, such as In both our diesel and naphtha hydrotreaters, we expe-
FCC catalyst fines from FCC fractionator bottoms, these rienced plugging, particularly a crust that would form on
cannot be reliably filtered because of their small sizes. If the top of our beds. We do not have any gas blanketing
left in the feed, these fines will accumulate in the intersti- on our tanks or anything of that nature. We have simple
tial spaces of the hydrotreating catalyst causing pressure coalescers upstream on our crude unit rundown streams,
drop and maldistribution. mostly for water removal. Our hydrotreater feed is not
In one particular case that we know of about 7 weight pretreated in any other way.
percent of approximately 2 micron FCC catalyst fines We have found success by using the graded bed method
was measured on the spent hydroprocessing catalyst from of loading our catalyst, and we also eliminated the trash
a unit processing FCC fractionator bottoms. We believe baskets which were initially put into those reactors as part
that the most reliable method to remove these small parti- of original design. They were totally ineffective in doing
cles from the feed is to distill it, possibly in the feed of what they were supposed to do and were often a hindrance.
a DCU, or a fluid coker, or in a VAC tower. And obviously Once we removed these baskets and went to a graded
this assumes that the product streams from these units bed, we no longer had a plugging problem at all. Often
will be going to the hydrotreater. times we used to have a 50 pound pressure drop develop
With respect to polymerization, I concur with the over the life of the catalyst. Now we have none at all and
previous comments. Antioxidants have been used in the our catalyst can run until it really needs to be changed
past with some measure of success. These are usually out for catalytic reasons rather than for pressure drop
injected into the rundown to tankage. constraints.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 93
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HENKE: then did some fine tuning and found that we were missing
After experimenting with several filtration devices, we some of our backwashes. So we started looking at shorter
have concluded that in our situation, sand filters are the times in the back washing cycle and we found about half
most reliable devices for filtering solids from heavy feed of our filter elements were not being effectively cleaned.
streams such as heavy coker gas oil. Proper sizing and We have also noted that, over time, our filter elements
grading of the filtering medium is essential to optimize tend to accumulate something that does not backwash
particulate removal. We target removal of particles larger off. We therefore have a spare set. We send one set out
than 20 microns. Actual particulate balances around our for sonic cleaning to clean the residual material.
gas oil hydrotreater reactors have shown that inert solids In another refinery, we have a distillate hydrotreater,
coming from the heavy coker gas oil, smaller than 20 in which we now treat reduced crude as well as distillates.
microns, readily pass through the reactors. That unit was not designed with the filter because it was
only going to have distillate feed. We did get a significant
JOSECK: successful run, until we had an upset in the unit where
At one lube oil hydrotreater, hydrotreating gas oils and the recycle compressor had gone down. We have seen a
the deasphalted vacuum tower bottoms, 25 micron filters significant increase in reactor pressure drop in naphtha
were added and later changed to 10 micron filters improv- units as well when we have upsets with the compressor
ing the first bed fouling. The unit was revamped increasing and start back up. We get a step change in pressure drop
the hydrogen recycle from approximately 1,250 to 4,000 in the reactor.
standard cubic feet per barrel of hydrogen, improving the The last thing I would say is make sure you have a
total reactor fouling. Catalyst pressure drop no longer good vapor-liquid distribution in your reactor so you do
limits the reactor; the reactor is limited to catalyst activity. not have all the hydrogen going down one side and all
At a second hydrotreater, we have 25 micron cartridge the oil down the other causing coke formation down in
feed filters. We recently experienced a high pressure drop
the reactor bed.
in the top bed that was attributed to iron sulfide from
the reaction of iron and sulfur in the feed. The unit
processes napthenic and paraffinic feedstocks. We have SAMUELS:
since loaded high void space topping in the reactor with In fact, there is a few more things to add here. We set
promising results after seven months. Start-of-run pressure a sodium specification of 0.5 part per million on our
drop in the top bed decreased from nominal 30 psi to 65,000 barrel per day distillate hydrotreater at the Robin-
less than 10 psi. son refinery, after severe reactor fouling and some
We have had the most success when the type of bed exchanger fouling, from salt treated purchased diesel
plugging has been identified and traditional approaches
stocks. I think this would apply to any distillates that you
have been used to reduce the problem. We have had more
would be moving over salt water. This specification in
success with bed grading than scale baskets for reducing
top bed plugging. fact did eliminate the problem.
We have also used nitrogen blanket feed tanks in com- As has been mentioned many times, dissolved oxygen,
bination with size bed graded catalysts on the top bed ethers, peroxides and di-olefins will cause polymerization
for improving pressure drop. These related experiences and can cause crusting when solids either in the feed or,
support the discussion last year around the five causes of corrosion products in the preheat exchange are bound up
reactor bed plugging. That is trash, soluble iron, carbona- by the polymer. In one naphtha hydrotreater we were
ceous coke, catalyst bed coking and catalyst bed fines. actually getting about three month runs due to reactor
pressure drop where we would have to go in and skim
PETERSON: the bed due to this polymerization mechanism.
I agree with the previous comments. I would like to We solved that problem by adding an active support.
throw a little fine tuning on a couple of them. We have We are using criterion 814-Hc, cylinders and balls on
noticed that our filters plug up more if we feed resid as top of that reactor bed. Currently, we are on a nine month
vacuum tower bottoms. We see less plugging in the filters run with no pressure drop increase and are cautiously
if we feed this equivalent resid material as reduced crude, calling this a success, as the active support appears to be
before it has gone through the vacuum heater and the hydrotreating the polymer. I would also add that we do
vacuum tower, where maybe some cracking, some coking, not see much success in hot hydrogen sweeps. I think
or some other reaction has occurred. We have not isolated once you have a polymer formed or you have pluggage,
the mechanism for that yet. We run a fairly hot vacuum you pretty much have to go in and skim or dump. In
transfer temperature, about 780°F. general, Marathon has not had great success with chemical
On back washing the filters, we had set up instrumenta- treatments with antifoulants, to current hydrotreater reac-
tion and did not take full advantage of it for a while. We tor bed fouling, but we are still looking.
94 Hydrogen Processing
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 95
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PAUL FEARNSIDE (Nalco/Exxon Energy Chemicals): A second comment is about recycled backwash volume.
On upstream corrosion control, please remember that Our technology is a gas assist technology. The main fea-
when the pH of the crude unit overhead water is in excess ture of this technology is that you can achieve a very low
of 7, iron sulfide becomes insoluble and a rag layer builds. backwash volume, typically below one percent of the feed.
I cannot tell you how many times I have run into that Therefore, the quantity of the liquid you have to reprocess
rag layer continually growing and puking over, causing is extremely low.
a pretty bad pressure drop problem across the hydro-
treater reactor. PAUL SZYMBORSKI (Norton CPPC):
Moving down the tower as far as naphthanic acid As people have mentioned, many refiners have gone
corrosion control goes, to address one of the panel mem- to graded beds in addition to filtering for removing materi-
ber’s concerns on phosphorous based chemistry, we do als on hydrotreaters. It is important to note that you need
have a non-phosphorous based chemistry that is to know the source of the particles requiring removal,
extremely effective. whether it is fines, metal particulates or soluble materials
As a last ditch effort to help alleviate reactor bed pres- because that will affect the way you design the graded
sure drop, we have been 80 percent effective in reducing bed and the types of materials you use in a graded bed.
the pressure drop problem by using dispersant type chem- Norton developed macro porous rings and spheres that
istries. A typical treatment takes from 12-72 hours to we understand have been used in hydrotreater applications
complete depending on the severity of the situation. Pres- since the early 1980s. The average pore size is over 100
sure drop reductions in excess of 35 psi have been achieved. microns, thus allowing these guard beds to actually filter
out the particulates. Therefore, the particulates are not
just plated out onto the guard bed but it is actually filtered
JOHN ARNDT (Arndt & Associates): into the guard bed rings and/or spheres.
I would like to relate two things on feed filters. As Mr.
Barloewen said, cold feed can be a problem. Keep feed 2. Reactor Effluent Systems
temperature well above cloud point Ⳮ 20°F. Feeding
from cold tankage can make your filter cycle like mad. Question 10.
Watch out for periods of high cold feed rates. Has anyone observed high corrosion rates in the
Secondly, watch your back flush. Have plenty of pres- exchangers and stripper feed heaters downstream of the
sure available to get enough back flow to clean the filter LP separator in a diesel HDS unit? If so, what was the
and get the gunk out of the whole element. Insufficient cause and what materials are recommended in this ser-
back pressure will rattle the filter cake but not remove it vice to avoid such high corrosion rates? Could stripped
from the system. Upon forward flow, the filter just plugs sour water contribute to the problem?
up immediately.
SAMUELS:
High corrosion rates have been a problem in the
THIERRY DARDE (Pall Corporation): exchangers downstream of the low pressure separator,
One technology that Pall Corporation has applied in both in Marathon’s Garyville diesel hydrotreater and Rob-
many refineries worldwide is feed filtration by automatic inson’s hydrocracker. Although the configurations are dif-
self-cleaning filter. Installed on different streams such as ferent in these units, in both cases the root cause of the
coker gas oil, diesel or vacuum gas oil, Pall technology problem was under deposit corrosion from ammonium
has provided significant reactor bed protection. Pressure chloride salt formation in the 350 to 400°F temperature
drop in the reactor beds in all these applications has range. Both systems use carbon steel bundles at this point
remained fairly constant over a very long period of time. in the effluent train. In both cases the failure occurred
It was said that usually people want to remove particles on the shell side of the tubes, as a feed from the low
equal or bigger than 25 micron. One point I would like pressure separate is being preheated going to the stripper
to address is the efficiency of the removal. If you work or the debutanizer.
out a few hundred of ppm of particles in the feed and if It is suspected that minor water carry over or at least
you have a feed filtration which has an efficiency of say saturated conditions downstream of the low pressure sepa-
10 to 20 percent when compared to a filter which can rator lead to salt deposition where vaporization occurs.
deliver 99.99 percent efficiency, the difference in terms Stripped sour water if properly stripped should not con-
of solids going to the reactor can be in terms of tons. In tribute to corrosion in these exchangers. Check your
other words, one could remove 25 micron/particles with stripped sour water for chlorides, iron, calcium, total dis-
a low efficiency filter and experience reactor plugging. solve solid and total hardness in addition to ammonia,
The extremely high efficiency of Pall filters guaranties H2S and dissolved oxygen. UOP provides specifications
that no reactor plugging could occur. for this as indicated below.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 97
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98 Hydrogen Processing
TOC/INDEX
a coalescer in the feed going to that exchanger with some Ideally that is longer than your turnaround cycle. The
success on reducing the rate of corrosion in the stripper cold heat preheat shells typically do not foul a lot. Later
feed exchanger. on it is pointed out and it is mentioned in the question
that one methodology is to use some makeup gas or
HAHN: recycled gas injection into the feed to reduce fouling.
We did something quite similar. We determined that That has worked in some units, but for other units it
our salts were coming from a water carryover from the has not.
low pressure separator. We installed a demister in our Finally, at the end of that list of approaches, you are up
low pressure separator and that seems to have solved to additives and the use of antifoulants and antioxidants to
our problem. try to extend the cycle length.
Question 11. BINFORD:
Has anyone experienced fouling problems in the reactor Regarding the question about an antifoulant injection
feed/effluent preheat exchangers on an FCC pretreat unit in this service, we have used antifoulants successfully many
or MHC unit? If so, what was the cause and how was it times in these applications. More importantly, I wanted
rectified? Has anyone tried antifoulant injection in this to go through a little bit of what was not provided in
service? (Background: refiner operates with HVGO TBP this question that is really critical to understand the nature
Endpoint 1050°F, SG 0.926, CCR 0.5 wt%, ASTM Color of the fouling and then trying to design a solution around
⬍ 6.0, S&W 0.05 vol%-which comes directly from it, whether that be mechanical operational or chemical.
upstream VDU’s and from gas blanketed storage tanks. Some key information that is missing from the data
Treat gas is mixed with the HVGO upstream of the pre- provided is characterization of the feedstream itself.
heat exchangers.) Things that need to be identified and tests that should
be run are first the bromine number, which would give
PETERSON: a measure of unsaturated material since a high degree of
We have injected antifoulant in our FCC feed hydro- unsaturates may be indicative of a higher fouling rate.
treater exchange stream since day one at the very strict Filterable solids and existing gums should be measured
advice of our licensor. He also warned that if we ever on a representative sample. This would indicate a potential
take it out for any period of time, do not put it back in to deposit exchangers or carry through to the reactor bed.
again because anything that accumulated is going to Pyrolle nitrogen should be measured. This would quantify
slough off and plug up the reactor bed. Well, we have the level of nitrogen based fouling precursors which can
heeded his advice and we have experienced a four year sometimes be very significant in regards to fouling. Finally,
run. We are afraid to try anything different right now total acidity and metals content should be identified. Acids
because it has been successful. The feed to the unit com- either as a result of feedstock contamination or naturally
prises vacuum gas oil, sometimes atmospheric gas oil and occurring, and metals that may be either entrained or
light cycle oil directly from our FCC unit. dissolved in the feed can catalytically accelerate fouling.
In resid cracking season, we have fed reduced crude Trying to solve this problem or give some direction on this
and vacuum tower bottoms into the unit. All of these specific instance really needs some more characterization
feeds are direct from their units. We have at times though work on the feedstream itself before an effective chemical
had to slop some oil to a tank which, unfortunately, is solution could be applied.
not gas blanketed. So far we have been lucky. We have
not had any major problems. LLOYD WINGER (Conoco):
When monitoring for pressure drop without DP cells One of our FCC feed hydrotreaters experienced this
across exchangers where you are dealing with 0 to 3000 fouling problem, apparently due to an air leak or other
psi pressure gauges range, it is kind of hard to see a problems in the vacuum tower. We fixed the vacuum
difference in pressure drop build up from time to time. tower and have not experienced the fouling again.
We are monitoring the temperatures in the exchangers. Question 12.
The feed temperatures change depending on what the What is the industry’s experience with corrosion/erosion
feed to the unit is, so heat transfer coefficients values are effects on alloyed reactor effluent exchangers in hydro-
a little hard to calculate as well. Our hydrogen is mixed processing units? What new metallurgy (e.g., duplex
with oil downstream of the feed exchangers, but upstream stainless steels) has been tested and/or used for reactor
of the fired reactor charge heater. effluent coolers (and associated piping) to combat
ammonium bisulfide corrosion? Under what conditions
BARLOEWEN: (e.g., velocity, NH4HS concentration) have they been
Again, normally the hottest shell in the feed effluent tested or used, and what has been the experience
exchanger train will need some type of periodic cleaning. with them?
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 99
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TASKER: the carbon steel effluent coolers on our largest unit with
This question is one that has come up many times alloy 2205 duplex bundles due to repeated failures of
before during NPRA meetings in one form or another. these bundles. The shell side inlet velocities, were almost
It is often a case of economics when you are using a 40 feet per second on this unit. Use of higher grade duplex
particular alloyed effluent exchanger. This has to be justi- materials will allow higher velocities and salt concentra-
fied during the design stage. In one of our units, we have tions, however, we have not opted to do this since our
Incoloy 800 which has been used with excellent results water wash rate has been set by the requirement to have
from an erosion, corrosion standpoint. This particular 20 percent water in the liquid phase after injection. There
exchanger does not have symmetrical piping which I will have also been recent reports of entrainment of aqueous
mention in a moment and it has a three bank arrangement. water into the separator vapor outlet line at higher salt
There is perhaps some evidence of maldistribution, but concentrations. This appears to set an upper limit of
no evidence of erosion or corrosion. about ten percent ammonium bisulfide no matter what
Typically, we like to ensure that both the metallurgy the metallurgy of the coolers.
and the piping design are correct and that the standard
design criteria are followed. We strongly believe in sym- CAIN:
metrical piping. It is essential for longevity of exchanger In our Delaware City plant, the only erosion/corrosion
life when serpentine tube design is used. Box header problem we have had is on the reactor effluent exchangers.
arrangements provide quite satisfactory operation, We had to replace a bundle and pillbox due to polythionic
although we have observed both sidewall erosion and acid and corrosion. This was due to the fact that neutraliza-
corrosion in one effluent exchanger. tion was not done properly. The first three exchangers
Obviously, it is extremely important also to ensure that off the reactors are 304 stainless steel tube material. The
you have good water injection and we design for individual fourth exchanger is carbon steel followed by eight air
water injection to each pass inlet. Typically, maximum coolers. The tubes and the header boxes of the air coolers
tube velocity is around 20 feet per second at the inlet are Incoloy 800.
piping to the exchanger. The typical water injection repre- The inlet and outlet piping for the air coolers is carbon
sents about five percent of the feed flow rate with the steel. The piping configuration has been changed to a
water effluent having a maximum of about four percent concentric flow pattern. The diameter of the piping has
of ammonium bisulfide salts. Last year we heard from also been enlarged to a lower velocity. There is also water
the panel figures from two percent to eight percent, but and chemical injection in the upstream piping.
we standardize at about four. At our Louisiana plant, we experienced some erosion/
HRI and IFP have no experience with Duplex stainless corrosion in the carbon steel tubes of our reactor air
steel and we have used carbon steel, killed carbon steel, effluent coolers in one of our hydrotreaters as well. We
and that is a function of the H2S concentration. We have have successfully used E-BRITE on one train in this service
used 321, 316 and 347 stainless steel. I can say that carbon and have just ordered a new cooler made of Incoloy 825
steel is pretty bad news though. for the second train.
For the last part of the question, most of our licensees
have examined the inlet and outlet piping of the effluent FOSTER:
coolers during planned turnarounds using UT testing Since we are running high concentrations of Venezue-
methods. During operation, we recommend thermal lan crude, this is a particular problem for us. In fact we
infrared techniques to determine whether there is maldis- are performing a comprehensive review of our ammonium
tribution from both temperature and flow and we find bisulfide susceptibility. If you are contemplating, or
that there are lots of specialist companies that come in already running higher nitrogen crudes like some of those
and do that. The cheaper way, of course, is to buy your from Venezuela, I recommend performing this review
own camera, invest a few thousand dollars and do it prior to this operation if possible.
that way. We chose duplex stainless steel for the effluent air
cooler tubes for our new CFHT. While duplex stainless
ROMAN: steel is less expensive than some other alloys, the welding
Ammonium bisulfite salts will deposit in effluent cool- and fabrication is to be very carefully watched: things
ers if the product of the ammonia and H2S partial pressures like the selection of the weld procedure, the welding rod
exceeds 140 psia. This is easily attained in vacuum gas metallurgy, and qualifying procedures for the welders.
oil units and a water wash must be used to prevent Erosion-corrosion of the inlets of the carbon steel tubes
solid deposition. is a common problem for us in our older units. For these
Carbon steel is acceptable if the velocities are limited we are investigating the use of ferrules (essentially a SS
to 20 feet per second and the concentration of ammonium insert) for the inlets of the coolers, where most damage
bisulfites limited to five percent. We recently replaced takes place. Again, the devil is in the details of fabrication.
The trick here is that the ferrules have to be carefully ● Very few plants have used alloy construction for
tapered to prevent localized eddies at the end of the ferrule. REAC inlet or outlet piping.
● Two plants with outlet piping of S31803 have had
JOSECK: no problems after five years and seven years of ser-
We have a 2205 duplex stainless steel shell and tube vice, respectively.
exchanger in high pressure 3000 psig service. The ● One plant used Alloy 800 inlet piping, which failed
exchanger is separator off gas and wash water on the tube because of polythionic acid stress corrosion cracking.
side versus recycle gas. It has been serviced since 1992. ● One plant used HF-modified piping, which failed
In 1995, we pulled the exchanger offline for inspection by chloride stress corrosion cracking in three years.
due to the service change in the new application. The Alloy 800 suffers from the same shortcoming as the
inspection showed no visible corrosion or mechanical austenitic stainless steels, namely, susceptibility to inter-
defects. Velocity at the inlet is 16 feet per second and granular (polythionic acid) stress corrosion cracking if
the salt concentration in the decanted water is 0.3 used in the sensitized condition. If Alloy 800 is to be
weight percent. used for headers, the carbon content must be low (below
0.03%). Alloy 825 is a preferred choice as it contains
BOB RODDEY (Roddey Engineering Services, Inc.): stabilizing element.
I refer everybody to the Piehl article that has been
Question 13.
discussed in years past at NPRA meetings, which discusses
Are refiners inspecting the piping into and out of their
in-depth the phenomenon of velocity and salt concentra-
reactor effluent coolers? If so, what methods are pre-
tion and the K factors which affect the corrosion suscepti-
ferred?
bility to exchangers. On the injection of water, I heard
one of the panelists say that they inject water to each one MALEK:
of the bays. While that can be done very successfully, and This question deals with inspection of piping into and
it has been on some units, there have been problems in out of the reactor effluent coolers. From a design stand-
units where water injection to each bay had been tried. point, we would recommend that provision be made in
It is tough to mix water and have a three phase system the piping for corrosion probes. After the unit is in opera-
in a downflow environment. When you inject it down- tion there should be an inspection procedure established
flow, there should be a nozzle or spray. It is a lot easier to routinely inspect these pipes while the unit is operating.
to mix three phases when you have got an upflow condi- It is important to closely inspect these pipes at each turn-
tion and it is a lot easier to predict the flow regime in around to document the effects of corrosion. The patterns
an upflow condition where good mixing is achieved. I will of corrosion can be monitored, particularly if you will set
caution you about injecting into each one of those bays. up your inspection procedure to look at high turbulence
areas. The pipe should be checked for corrosion in at
CRAIG HARVEY (UOP): least four planes.
For severe service, the use of alloy tubes may be desir-
able. Alloy construction not only provides maximum ROMAN:
insurance against corrosion, but it can also allow certain We are currently relying on ultrasonic thickness mea-
design limits on velocity, Kp, and bisulfide contents to surements. We take UT readings upstream and down-
be relaxed. However, it should be noted that relaxation stream of all welds on all elbows and also at the outer
of the NH4HS design limits can have an adverse effect most point which bisects the angle of that elbow. The
on downstream piping and equipment. It should also be three phase flow which exists in these coolers makes it
noted that while alloy construction minimizes NH4HS difficult to assure even flow distribution of the water wash
erosion-corrosion problems, other forms of attack can and we generally require symmetric inlet and outlet piping
become problematic. on these exchangers to minimize flow maldistribution.
Table 1 provides recent survey data with respect to the We are also considering a new technique which would
experience with alloy construction in reactor effluent air allow us to take moving radiographic scans of this piping
cooler (REAC) service. In Table 2, these data are sorted and display it and view it digitally as opposed to on film
by material. as is done with normal x-ray techniques. This will allow
Alloy 800, S31803 (duplex), Tp 321, and Alloy 400 us to detect pitting which might be missed by spot UT
(monel) have all performed well. Alloy 825 should be a readings.
better choice over Alloy 800, but experience to date is
limited. Tp 430, S31500 (duplex), and Alonized carbon FOSTER:
steel have all failed for reasons given in the tabulation. We have used radiographic examination for many years
Survey data with respect to experience with alloy piping due to the unpredictable, localized nature of ammonium
in service downstream of the REAC is as follows: bisulfide and ammonium chloride attack encountered in
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 101
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Table 1
these systems. X-ray also allows you to examine the areas FUSSELL:
covered by insulation. UT thickness methods tends to In Port Arthur, we have a 1,600 psig UOP Unibon
get specific points and does not really allow a complete unit that hydrotreats about 40 percent of the feed to our
profile of your pipe. Automated UT scans (utilizing crawl- FCCU. We have identified the piping around the effluent
ers) can be used to give a more thorough measurement, air fan as being very critical. We use ultrasonics to inspect
but the surface must smooth for these to work. it. We inspect it once every six months and we have quite
Table 2
a few more thickness monitoring locations on this piping BILL JOHNS (Texaco R&M, Inc.):
than we would typically have in other services. I agree with the panel, i.e., x-ray and do your best to
We have had to replace portions of this piping on two look at all of those points that you feel are troublesome.
occasions. The first one was due to erosion. UOP had Also, if you have a change in process and you have not
originally installed a mixing plate downstream of the air been measuring, go back to measuring frequently the
fans which caused this erosion. I am sure that there was thicknesses of metal in and out of those air fans. Any
a good reason for the plate, but we took it out and we significant change in process will make a change.
have not had the problem again. We have also replaced On the last question, we found some tube laminations
portions due to general thinning. on 800 alloy tubes in fin fans and traced it back to
manufacturing problems. We replaced those with 825
alloy and have not seen any problems with 825 alloy. We
HAHN:
understand another refiner on the West Coast had seen
I would concur with most of what has been said already,
some laminations with 800 alloy tubes as well. So be
particularly about checking for places of high velocity and
aware of that problem.
potential erosion points. We have learned the hard way
on that a few times. In addition to the methods already 3. Catalysts and Catalyst Sulfiding
discussed, we are using sheer wave and eddy current to
inspect some of our piping. We have found that to be Question 14.
quite effective if you get an experienced specialist to do Silica uptake on hydrotreating catalysts is becoming an
your scanning for you. increasing concern. Is there a way to monitor uptake to
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 103
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effectively plan changeouts? Are there new reactor similar catalysts from other vendors are designed with
design criteria or new catalysts on the market to help high surface area to maintain activity while removing the
improve run length? silica. I would also refer you to the 1994 NPRA Q&A
transcript, page 128. It contains an excellent graph, pro-
FLETCHER: vided by Mehmet Asim of Akzo Nobel, correlating silica
The key to planning change out is accurate measure- uptake to fresh catalyst surface area.
ment of silicone in the feedstock. Because silicone is added Finally, I would like to point out that the best way to
to a delayed coker at variable rates based on the antifoam improve this situation is to reduce silicone consumption
requirements, which vary with the coking cycle, silicone at the delayed cokers. Most operators of delayed cokers
in the coker naphtha is variable. This means that spot inject more silicone antifoam than is required. New tech-
measurements of silicone content will vary widely and niques to control coke drum outage can go a long way
will not accurately represent the average silicone of the to manage and ultimately reduce silicone addition.
coker naphtha feed. Therefore, averaging a number of
spot samples taken throughout the coker cycle should JOSECK:
accurately represent the actual average silicon content. Due to a contamination in the crude, we experienced
The best measurement, however, of average silicone silicon in the straight run feed to a naphtha desulfurizer.
content of coker naphtha feedstock is the average silicone After identifying the contamination, the catalyst was
uptake over a catalyst cycle. Akzo Nobel recommends changed out four times within a six month period without
that good records be kept of spent catalyst silicone content. poisoning the downstream reformer catalyst. The unit
This is best done by obtaining three separate catalyst charge rate and daily feed analysis by atomic absorption
samples when the catalyst is discharged from the unit. (AA) were used to calculate a total silicone weight on the
These samples include: top of the main catalyst bed. This catalyst. Comparing the calculated weight to the catalyst
sample will indicate the silicone uptake capacity of the vendor estimates and analysis of the preceding catalyst, a
catalyst grade used. Second, we recommend a sample from prediction was made to plan the next catalyst changeout.
the bottom of the reactor, which identifies whether the The AA instrument was calibrated using a spike feed to
breakthrough has occurred. Third, a composite sample a 0.3 detection limit. After each catalyst change out, a
which indicates the actual silicone pickup of the unit sample of different bed locations in the reactor were ana-
during the run. If a refiner monitors the antifoam usage lyzed for metals, to determine the take up for future
at the coker over the run and measures the silicone pickup change out planning. We changed catalyst after the first
of the catalyst during the cycle, the delta between the two shut down to a higher surface area, a higher pore volume
will give a good measurement of fraction which has been catalyst for higher silica takeup based on research com-
absorbed by the catalyst. This number when applied to pleted by another refinery experiencing the same contami-
ongoing silicone antifoam usage can then be used to nation.
predict the silicone fed to the coker naphtha hydrotreater We considered inserting test plugs of different catalysts
as accurately as feed analytical measurements. in the top of the reactor for the evaluation of silica take
up versus catalyst vendor estimates per one catalyst manu-
BARLOEWEN: facturer’s recommendations.
One additional factor to give you an idea when you Our problem occurred over a year ago. We did an
are about to fall off the cliff is monitoring sulfur content extensive literature research. A technical paper presented
on the naphtha hydrotreater. Just before your silicon by Terry Reid of Akzo entitled, ‘‘Coker Naphtha Hydro-
capacity is all used up, you will start to see spikes on the processing: Solutions for Trouble-Free Operations’’ is an
nitrogen. More and more refiners are also looking at excellent resource. The paper clearly summarizes operating
nitrogen as heavier crudes are being introduced to their catalyst variables not recently available in one location
crude slate. So that is a warning that will give you about until now. The paper clearly defines guidelines, some of
two weeks before you are out of business. which we learned through painful experience.
HENKE: TASKER:
We practice those things that Mr. Fletcher mentioned. I agree with the preceding comments. Perhaps you
We monitor Silicon (Si) uptake by tracking silicone con- might want to consider having a spare charge of catalyst,
sumption at the delayed cokers and direct measurement but that is always an expensive option. One way to
of silicon in the feed to the naphtha hydrotreater. We improve the run length, of course, is to design the reactor
reconcile these values with analysis of the spent catalyst with a space velocity of about two or less.
to assist in planning future catalyst changeouts. The first consideration though is for the diolefins and
We continue to use Akzo Nobel’s KF-844 in our coker the second consideration is for hydrotreating when it
naphtha hydrotreaters with good results. This catalyst and comes to the silica poisoning. Now, our experience is that
you can probably go up to about eight weight percent of catalyst loaded into a hydroprocessing reactor? What is
silica as SIO2 with the cobalt moly catalysts before you the minimum acceptable particle length, below which
can say that the catalyst is essentially dead. The surface pressure drop and flow maldistribution problems are
area is very important to assure longevity of operation. The expected to occur?
form of the silica which affects the catalytic performance is
not fully known, but is assumed to be SIO2. It is also CAIN:
assumed that virtually all of the silica is from the antifoam As a general rule, once the length over diameter (L/
agents used in the coker operation and it generally goes D) ratio drops below three, you will see a noticeable
to the naphtha cut. The formula for that antifoam is increase in the pressure drop. Your catalyst supplier can
generally known by the antifoam manufacturer and you supply specific information on a given reactor configura-
can get some of that information from your suppliers. It tion.
is generally supplied in a polyglycol form.
FLETCHER:
For total life estimation, this has been mentioned
We believe that this answer really has three aspects.
already, but you need to know the volume of catalysts in
(1) We believe that the minimum average length for
the reactor. When you are approaching that eight percent
regenerated catalyst is about 2.5 millimeters for 1/20th
calculated number, I think you will see some bad perfor-
inch diameter catalyst. With this catalyst length the pres-
mance.
sure drop will probably not be a problem in the majority
As guidelines, we have experience with feed silica levels
of units. The average length should be greater than 2.8
of between one and two ppm in Germany and similar
millimeters which should give a satisfactorily low pressure
levels in Italy and Sweden. For U.S. domestic licensees,
drop for any unit able to use 1/20th inch diameter catalyst.
we have units designed for up to five weight ppm of silica
This minimum should be increased as the catalyst diame-
in the feed. For South American, we are looking at units
ter grows, 3.5 millimeters for 1/10th inch and an L/D
capable of handling 10 weight ppm in the feed.
of at least of at least one for larger sizes. (2) Equally
Usually for that type of situation, you need more cata-
important in determining fitness for use is the catalyst
lyst and you need a surface area of approximately 200
length distribution. The content of short catalyst particles
square meters per gram per cc. There are limits, however,
has a large impact on the pressure drop. Generally, the
and there is a need to improve the catalyst and have a
concentration of catalyst particles with an L/D of less
higher pore volume for higher tolerance. The main idea
than one should be less than 15% of the total catalyst
is to design the catalyst volume which will give you at
particles. Fines content should be less than one percent
least a two year life based on the expected feed silica
by weight. (3) Other important considerations are the
content. Watch your delta T and watch your delta P and
side crushing strength (⬎3.5 pounds per millimeter), and
you should be in good shape. A delta T of less than 40°C
the Compact at Bulk Density (CBD), (⬍10% increase
is good and you may have to recycle to keep it at this level.
compared to fresh catalyst). The CBD is directly linked
to void volume which has a large impact on pressure drop.
DAVID DiCAMILLO (Criterion Catalyst Co.):
I agree with everything the panel has said. Additionally, BARLOEWEN:
there are catalysts specifically designed for silica uptake The real issue with how much degradation and down
that will hold more than the levels Mr. Tasker mentioned. sizing of particles you can tolerate is what pressure drop
Criterion DN-140 has been analyzed at 11 wt% Si (22% you can tolerate. Every new unit is designed for a start-
SiO2) after removal from a commercial NHT treating of-run clean pressure drop and has an allowance for foul-
100% coker naphtha. ing. That fouling allowance can be used up with particu-
Depending on the age of the catalyst and the unit lates or it can be used up as you install a smaller catalyst
design, if you are spiking silica in your feed, we have and every catalyst will become somewhat smaller on regen-
observed that it can carry through even though the catalyst eration.
has not reached its normal uptake capacity. So if you One data point that we have is for a catalyst that started
have a critical service like a reformer downstream, you out as 1/16th inch catalyst with a 3:1, L/D ratio. After
might want to pay close attention to your antifoamer one regeneration, and (of course) screening out fines, the
addition and be aware that if you pass spikes through, L/D ratio dropped to 2 to 1 and that unit saw approxi-
they will get into the product. When you get back to mately a 10 percent increase in pressure drop, which was
normal addition rates, the product will be silica free again. not a problem for them.
Question 15. TASKER:
Given the reduction in L/D ratio that occurs during the Of course, this question was aimed at typical hydropro-
catalyst regeneration process, what is normally accepted cessing catalysts, and perhaps we should include the grow-
as the minimum average particle length for extrudate ing number of bottoms up grading processes such as our
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 105
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hydrocarbon accumulates in the separator downstream. Since we started this practice 17 years ago, we have
Similar to Mr. Cain’s, comment, we would use diesel to had not one incident of improperly loaded catalyst. More
flush out the heavy material in our FCC feed hydrotreater. importantly, we have had only contractor LWDI in 17
After this couple hour sweep we switch to nitrogen. years. Our success here is mostly due to the fact that we
If you have a multiple reactors in a hydrotreater and have two very high quality individuals who take pride in
are only going to change catalyst out in the lead reactor, their work. They see that not only their work but the
the hot hydrogen strip could lead to desulfiding of the work of their contractors is done safely and expertly.
other reactors if you do not have an H2S source. We have This might not be for everyone, but for a refinery of
gone to shortened times and go with nitrogen cooldown. our size, this helps our focus on catalyst issues. This allows
the engineer to focus on optimizing the operation rather
SAMUELS: than supervising catalyst handlers.
I agree, and directionally we are moving away from the
historical longer hot hydrogen sweeps. We see diminishing
returns once the hot separator level stops building. We FUSSELL:
are going to more nitrogen use. We obviously do not have as many reactors and we
use process engineers extensively to supervise both the
TASKER: unloading and the loading of all of our catalyst reactors
Most of the comments were already made. We generally in the refinery. They also work on the front end to develop
look at a guideline for hydrogen stripping of about 200 the scope of work. They help select the catalyst contractor
standard cubic feet of pure hydrogen per cubic foot of that does the job. As I mentioned, we have around the
catalyst. That seems to be quite effective. The temperature clock coverage on the unloading of the catalyst. We try
at which you do it, of course, will be a function of the to collect a good composite sample of what we are taking
feed that you have in the system because you want to get out of the reactor so that maybe we can learn some things
all of that material out, and the duration. Obviously we about it and determine if it is regeneratable. We also have
want that as minimum as possible and typically 12 hours around the clock coverage on the loading. These engineers
will do it. The nitrogen sweeping is a good way to go. do more than just technical type support. They coordinate
But, of course, that depends on your compressor. As has the work between our maintenance staff and the catalyst
been mentioned, you may want to invest that extra money handler, so it is a pretty major effort on their part.
and bring in liquid nitrogen and do the sweep as a once
through operation.
HAHN:
Question 17. We have one field engineer that follows the catalyst
What level of refinery engineering supervision is prac- loading and unloading around the clock in addition to
ticed in the loading of catalyst in hydrotreating/hydro- some of their other duties. We bring in a catalyst specialist
cracking reactors? to do our loading and unloading inert. So we do not
directly load. We just sort of monitor and make sure they
FOSTER: are loading as per our diagrams and instructions.
LYONDELL-CITGO refinery has 38 fixed catalyst
bed vessels and a working inventory of 4.8 MM pounds
of catalyst. Rather than assigning the unit engineers to FLETCHER:
manage this asset, we have centralized this under 2 Catalyst In general, we agree with the comments stated so far.
Coordinators. They do everything related to catalyst. Let Our general observation is that not enough supervision
me give you a list of their responsibilities: is being used. We have observed several cases of maldistri-
● They work with the engineering, operations, and bution in hydroprocessing units where the catalyst was
catalyst technical staff to determine best catalyst dense loaded at a slant. And in all cases, the refinery did not
selection and load configuration for each reactor. have engineering supervision during the entire loading.
● They design and maintain catalyst loading devices. In concurrence with some of the other comments, we
● They develop catalyst handling SOPs, EOPs, safety recommend that a team be formed between the personnel
procedures. These are custom developed for each from the refinery and the loading contractor. We further
catalyst job and provided to the catalyst handling recommend that evenness of catalyst levels and loading
contractor for execution. density be determined at different loading heights and
● They provide round-the-clock supervision of cata- checked with the expectations. Further, we recommend
lyst handling activities during turnarounds. that it is essential to check the reactor internals, i.e., the
● They maintain all fixed catalyst inventories, precious condition, the cleanliness, including the support, and also
metals balances, and work with financial people to look for a contractor who has available video camera
properly account for these. monitoring during the load.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 107
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bed of 8,600 cubic feet about 50 feet in depth. The give a more uniform bed density. According to the devel-
densification that we got was very close to the compacted oper, this method reduces variations in bulk density, in
bulk density as predicted by the catalyst manufacture. radial cross section of the catalyst bed, as compared to a
As far as the benefits of dense loading, these have been loading method in which a catalyst loader is fixed at the
discussed at past NPRA sessions and in various articles. top of a reactor. Some substantial increases in loading
There is some concern about the initial pressure drop of rate have been reported, especially when compared to a
the system. But we feel that the build of pressure drop fixed position dense loader. In addition, this method will
is slower with dense loading. So if you integrate it over minimize catalyst breakage and fines generation during
the whole run of the cycle, you can probably have a lower the loading which is observed in high free fall loading.
pressure drop or a longer run by not developing coked Another technology has been reported out of Japan which
areas or hot spots or having to cut short the cycle because uses laser beam technology to ensure an even bed surface
of some means other than pressure drop. As I said before, during the loading.
good dense loading does not make up for poor distribution
of liquid and vapor. You have to have everything work- Question 19.
ing properly. What analytical techniques are being used on a regular
basis in refineries to quantify aromatics reduction in
TASKER: diesel and/or VGO hydrotreaters? How accurate and sen-
Well, there are a number of specialized processes for sitive are these methods?
dense loading of catalysts and most companies have either
their own or preferred procedures. At IFP, we have the ROMAN:
catapack process and we generally get about 10 to 15 Our control labs do not measure aromatics in either
percent more extrudate in the reactors. diesel or VGO hydrotreater products routinely. Most of
For spherical catalysts, of course, it packs quite well these analyses are performed in our R&D labs. We have
by itself and the improvement is generally less due to used FIA, ASTD1319 and super critical fluid chromatog-
this characteristic. Typically, we see three to five percent raphy or SFC ASTD5186 for diesel streams. Diesel is
improvement, but we have seen up to ten with spheres. outside the recommended scope for FIA, but it is still
Our experience has been with extrudate catalysts and widely used in the industry. The reproducibility deter-
absorbants of .6 to 1.2 millimeter diameter up to three mined for gasoline samples ranges from 3.0 to 3.5 percent.
to five millimeter diameter absorbance. The extrudate However, for diesel samples, the ASTM cross check
length is typically four to six millimeters long. With program reproducibility is closer to ten percent. The color
spheres, our experience has been with three to five millime- of many diesel streams makes FIA difficult and somewhat
ter diameter spheres. subjective. The reproducibility of the FSC method is four
On vessel diameter, we have successfully dense loaded percent. Neither method does a good job in separating
catalysts into vessels up to 26 feet in diameter for absorb- multiring partially saturated molecules. They cannot gen-
ance and 13 to 16 feet diameter catalysts. We feel that erally distinguish between benzene and tetralyn for
it really does help from a channeling viewpoint and we instance. In FIA, tetralyn would be detected as aromatics
even recommend it for vessels as small as three feet in and in SFC as monoaromatics.
diameter. It is rather difficult to get a man into something For VGO or vacuum gas oil analyses at Ashland we
smaller than that. use an in-house HPLC method and this method is excel-
When you are dense loading, you have to consider lent for virgin streams including residues where a separate
what constraints you might have in the system and bed step is used to remove the asphaltenes before further
pressure drop might be one of those if you do not have analysis. The method separates the feed into saturates,
have enough recycled compressor capacity or head. We monoaromatics, diaromatics, greater than diaromatics,
find that we get better temperature distribution and overall and polar aromatics, with repeatability for each fraction
much improved operation. being three percent, two percent, one percent, two percent
On the pressure drop side, we do see the estimated and .5 percent respectively.
pressure drops which are perhaps four to eight pounds However, we have never been able to balance hydrogen
higher than sock loading, but it depends on the cata- consumption and reported aromatic ring loss across either
lyst volume. laboratory or plant hydrotreating reactors using this tech-
nique. We have concluded that the changes in ring satura-
FLETCHER: tion numbers are close to the uncertainty of the tests.
Our colleagues in Japan report a new loader developed Prior to using this method, we used mass spec method
by and called Idecat. It has a variable height that allows ASTM D3239 which, if the operator was very meticulous,
a uniform distance between the catalyst bed surface and provided excellent resolution of partially saturated multi-
the loading machine. Therefore, theoretically this would ring aromatics.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 109
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Question 21.
A number of new high-activity hydrocracking pretreat
catalysts have been introduced during the past 2 years.
What is the commercial experience with these catalysts?
HAHN:
We pilot tested several of the new hydrocracking cata-
lysts that are available and selected one based on HDN
activity. We have since loaded these and have seen quite
a bit of success. Our West Coast refineries have seen a
one to two year cycle length on these nickel moly catalysts
to date and so far they are exceeding past cycle perfor-
mances over their previous catalysts.
BARLOEWEN:
Topsoe introduced a new high activity denitrogenation
catalyst TK555 in late 1995. To date it has been installed KIRK NOVAK (Criterion Catalyst Company):
in 14 units of which six are in hydrocracking pretreat We have introduced a process called Century which
service. The first of these hydrocrackers went online in is a step out technology in manufacturing. This new
September of 1996 and the remaining were started up catalyst line produces two catalyst products, the DN190
early this year. All of them are doing very well and operat- and also HCR from UOP, part of our license catalyst
ing at lower temperatures at this point in their cycle than that we provide. The HCR was the focus of a paper from
at comparable points on previous cycles. Topsoe will be UOP at the last NPRA Annual Meeting. With the DN190
introducing another new more active catalyst in the spring and HCR we have over seven units in the industry. The
of next year. activity advantages of this catalyst are well-known in terms
of unit operations, about 136 volume metric percent activ-
ity increase.
FLETCHER:
Akzo Nobel produces many high activity hydrocracker Question 22.
pretreat catalysts, both licensed with UOP which include In choosing a spiking agent for presulfiding, what criteria
HCK, HCP and more recently HCT as well as open should be evaluated (e.g., environmental, solubility,
market grades such as KF843 and 846. UOP recently economic, toxicity, etc.)?
published a paper and presented it yesterday in our techni-
cal seminar covering the commercial performance of the BARLOEWEN:
HCP in four refineries around the world. These results We attempted to summarize some of the benefits of
show an average 25 percent increase in HDN volume various sulfiding chemicals that are used and put together
activity compared to the previous generation of catalysts in the following tables. Hydrogen sulfide is the first of
such as HCK. In one case this translated to over a 20°F these. This is fairly widely used in North America because
lower operating temperature requirement and the stability it is available in most refineries. It is cheap. On the down
was equivalent to the reference HCK. The extra activity side, one of its drawbacks is that it is rarely available in
can be used to extend cycle length or to reduce the period the rates and the pressures that you need. So, you are
of nitrogen slip commonly seen at end of run. inevitably limited in the speed at which you are able to
sulfide. And speaking from personal experience, I know
TASKER: many people get frustrated and do not do a thorough
We have seen the introduction of several higher activity job of sulfiding because of the pressure of getting their
catalysts over the last few years and there have been some unit online.
apparent marked improvements, but we have to recognize The major advantage of carbon disulfide is low cost,
that these are based on initial activities and we are waiting low decomposition temperature and high sulfur content.
right now to determine the catalysts’ longevity to make However, it is very flammable, has low auto ignition
sure that they are confirmed. temperature and high vapor pressure.
The indications are that overall life may be less than Another sulfiding catalyst, dimethyl sulfide, has been
before. But on the other hand, some of the commercial used, and is moderate in cost, moderately high in sulfur
tests have shown a lower initial activity but then very content. However, on the down side it has high vapor
stable operations with the HR348 and HR360 mild pressure and severe odor problems and has been broadly
hydrocracking catalysts. replaced by dimethyl disfulide.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 111
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Table 4
quite extensively. Its benefits are low odor, easy to handle, tities are important. UOP offers a product, SA-200
and requires no special classification and labeling. It has Sulfiding Additive, which meets all of these criteria and
disassociation temperature of around about 130° to is applicable to hydrotreating and reforming catalysts.
150°F. It is dialkyl pentosulfide. It has about 40 wt %
of sulfur on it.
JIM STONE (Louisiana Department of Environmental Quality):
Sometimes the sulfiding takes on an aspect of being a
EDWARD SMITH (UOP): test of a new material. In the Louisiana regulations, we
UOP has found in discussions with refiners that the have available a temporary exemption for testing. So if
criteria for selection typically rank as follows: safety and you get into something like this where you feel like that
handling, environmental and toxicity, supplier reliability would be useful to you, it is a way of making sure that you
and cost. This assumes the sulfiding additive has been are not going to be violating an environmental regulation
tested and/or approved by the catalyst supplier. while you are testing something new. You do have to
All of the properties listed, as well as high solubility, actually test and make a report if you use this exemption,
good low temperature handling properties, low decompo- and you have to ask for it ahead of time. (See LAC 3
sition temperature, low nitrogen and low H2S trace quan- III. 523.B)
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 113
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 115
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4. Reactor Safety and Reliability temperature measurement and so you are only looking
at a very small fraction of the reactor. You do not have
Question 26. a high assurance that you are looking at the worst spots.
What means are refiners using to extend the life of HDS Our recommendation would be to have temperature sens-
reactor vessels? ing points near the wall on the inside of the reactor.
Today’s technology allows retrofitting that quite readily
CAIN: through existing nozzles.
We have performed internal visual and dye penetrant Our recommendation would be not to vary the allow-
inspections along with acoustic emissions inspections, able gradient either in the radial direction or in the axial
sheer wave examinations. We have an outside firm to direction as the run progresses, even though coking does
perform a fit for service inspection. cause some deterioration of gradients.
The real issue that you have to deal with is process
FLETCHER: control. You want to be assured of having adequate process
The most important aspect of reaching a normal 30 control even in an upset condition. In a vertical or axial
year vessel life is a good inspection program. A plan should direction you have criteria as to maximum temperature
be in place to inspect all components on a regular schedule. rise based on your available quench gas. That is a function
The heat up and cool down cycles contribute to reactor of the recycle compressor and it may also be a function
stresses. It is important to follow the manufacturer’s rec- of the quench valve actually providing the quench.
ommended heat up and cool down rates. Avoid shock in
the reactor with water during shutdowns. FLETCHER:
Finally, failures typically occur in the attachments such The radial temperature profile is an indicator of liquid
as the internals, the outlet collectors, etc., to the reactor. flow distribution through the reactor. Liquid flow distri-
These are usually the result of poor design such as high bution is influenced by bed permeability resulting from
stress and poor materials selection. Inspections around catalyst loading and is affected by the liquid distributor
these areas is especially important. and the liquid mass velocity in the catalyst bed.
Liquid distributors can become fouled with scale and
FUSSELL: alter the liquid distribution. Irregular catalyst loading
On our Unibon unit, we follow special shutdown and tends to promote channeling or flow maldistribution. This
startup procedures to minimize any damage to the reac- can result in increasing radial temperature differentials
tors. We also use several different nondestructive testing as the catalyst cycle progresses. Units with liquid mass
methods such as acoustic emissions, replications, wet fluo- velocities less than 2,000 lb/ft2.hr are especially prone to
rescent mag particle testing, ultrasonics. We do all of this flow distribution problems.
on the reactors as well as the high pressure separator. One approach to operation is to set limits for both
radial and bed delta temperature that never change. In
Question 27. the event that variances exceed the limit, the cause for
Are bed differential and radial temperature spread limits the variance should be investigated and understood.
maintained the same from start to end of run, or are Quench and other strategies may be employed to reduce
they varied as reactor temperatures are increased to the delta temperature within the limits. If a reasonable
maintain catalyst activity? understanding of the cause of the high temperature differ-
ential is found and a risk assessment is made, there could
BARLOEWEN: be a decision to knowingly exceed these limits. In this
The question deals with radial temperature limitations case, skin temperatures and gas makes should be closely
across the reactor, and vertical, across beds of hydrotreat- observed and guide the decision process. It is critical
ing reactors. A well-designed reactor and distribution sys- that there are adequate skin temperature measurements
tem should give you a radial temperature gradient on the to make a sound decision.
outlet of the bed of ten degrees or less, and after a mixing
device, five degrees or less, with emphasis on less. SAMUELS:
The maximum radial temperature that you should be At our Robinson hydrocracker, the bed delta tempera-
able to live with is very much a function of feedstock tures are critical operating parameters and are not changed
type, processing objective, and catalyst type. For example, during the course of the run. We have reached maximum
zeolite cracking catalyst is much more sensitive and you bed delta T’s before and biased other bed temperatures
would want to apply tighter limits than on a less severe to maintain throughput and conversion without violating
service like distillate hydrotreating. critical operating parameters.
One of the problems is that most hydroprocessing We have not reached our maximum radial delta tem-
reactors, especially the old ones do not have a lot of perature of 30°F on each bed in the past. Before we would
change any temperature limitation as mentioned earlier, As reaction severity or axial rise in a hydrocracking bed
the unit quench capabilities would have to be evaluated is increased, it is generally expected that the radial spread
to ensure that in fact there is sufficient reserve quench at the bed outlet will also increase due to the accelerated
available in the event of a temperature excursion. increase in reaction rate that is experienced in the hot
Typically, the number one hydrotreater bed delta tem- zones.
perature limit of 115°F, on this hydrocracker, is the limit- As an operating cycle progresses, the relationship
ing factor on how much cracked stock can be processed. between the catalyst bed axial rise and the severity of
Hydrogen is also a limit as to how much cracked stock temperature spread at the bed outlet may change. This
can be processed. will depend as to whether the radial temperature spread
is due to poor liquid distribution, inferior quench zone
TASKER: mixing efficiency or permeability variations within the
I agree with everything people have said. For the radial catalyst bed. If the radial gradients are the result of extreme
temperature delta, we typically see in the order of 9 to bed permeability variations, then it is expected that the
11°F and feel that that is quite normal for start to end- radial gradients at a given reaction severity will worsen
of-run. as the cycle progresses. In this situation, the bulk reaction
In some cases we have seen that the delta T is consider- severity or bulk axial rise may have to be lowered as the
ably less. In one HDS unit, 11.5 feet in diameter, we cycle progresses in order to properly control reaction rates
have observed a radial delta T of less than 2°F at 1°C at all bed locations.
even with very active catalyst. In certain hydrocracking bed environments, the hydro-
genation reactions may become thermodynamically-lim-
ited as end of cycle conditions are approached. In this
ELIZABETH ALLEN (Criterion Catalyst): situation, the catalyst temperature response may change
There was a paper published by Shell in 1984 which towards end of cycle and this may result in a slight reduc-
gives details regarding the temperature profiles in trickle tion in the reaction rate in the hotter zones of the cata-
bed reactors. The paper discusses irregular flow patterns lyst bed.
which are relatively common in trickle phase hydrotreat-
ing. Their findings were that irregularities in catalyst pack- Question 28.
ing density and flows of the different phases can lead to In co-processing coker naphtha with straight-run diesel,
abnormal flow patterns. what percentages of coker naphtha have been success-
These flow patterns can lead to a situation where a fully run without using a low temperature first stage
finger of liquid channels through the catalyst causing hot pretreating reactor?
spots due to lack of gas to carry away the exotherm, and
coking as well. SAMUELS:
The paper derives an equation to calculate maximum At Robinson’s 65,000 barrel per day distillate hydro-
delta T allowed before these hot spots and coking can treater unit, we have processed up to 7,000 barrels a day
occur. The equation shows that maximum delta T is a of coker naphtha along with virgin diesel and FCC light
function of inlet temperature, activation energy, bed cycle oil since June of 1996. The unit limitation in pro-
height, gas velocity and gas density. cessing this coker naphtha has been handling the stripper
In other words, for heavy feeds with the low vaporiza- overhead naphtha production and is not related to
tion and low gas rates, the highest potential for excessive exchanger fouling or reactor exotherms.
exotherms can occur. The coker naphtha is fed hot from the cokers through
20 micron filters. Occasionally, the coker naphtha is stored
CRAIG HARVEY (UOP): prior to processing. All storage is blanketed. The stored
In hydrocracking service, good reactant distribution, feed is stripped with hydrogen, coalesced and filtered.
effective quench zone mixing and catalyst bed uniformity Along with the coker naphtha, it is common to process
are essential to minimize radial temperature spreads. An about 25 to 30 percent of the feed as FCC light cycle.
extensive temperature monitoring system must also be in The typical feed has a 32 API gravity, up to a 12 bromine
place so that the operator has detailed knowledge as to number, and an average of 0.6 weight percent sulfur.
the radial temperature profiles existing within the cata- Two parallel reactors contain over 600,000 pounds of
lyst beds. regenerated cobalt moly catalyst. There is no inner bed
The operating severity within a hydrocracking bed quenching. The typical total delta T is about 65°F with
should be limited in accordance with the severity of the a 610°F inlet start of run temperature.
radial temperature gradients. Of principal concern is the The coker naphtha itself has an API gravity of 60, a
capability to properly control reaction rates at all bed 0.5 wt % sulfur and a D3710 distillation five percent
locations in the event of an upset condition. point of 80°F and 95 percent point of 385°F.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 117
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HENKE: always optimal until the unit hits the maximum allowed
We process seven percent heavy coker naphtha in one of reactor temperature. At EOR, one typically maximizes
our diesel hydrotreaters. The coker naphtha is coprocessed the reactor WABT (inlet temperature plus 2⁄3 * bed dT) by
along with light coker gas oil, straight run diesel and FCC bringing all bed outlets to the maximum allowed reactor
light cycle oil. We see a 31⁄2 year run without any pressure temperature. Some specific cases are given below.
drop problems. Diesel Hydrotreater—More modern diesel hydro-
treater designs will have two or more beds. Usually mini-
FLETCHER: mum quench is used, but sometimes quench is used to
In addition to the routine processing of coker naphtha control reactor outlet temperature in order to keep a good
with virgin naphtha, a few refiners process coker middle product color.
distillate and/or coker naphtha with other middle distillate FCC Pretreatment—When the operating target is
streams. These units typically suffer from both silicon HDS (constant HDS operation) and insufficient hydro-
poisoning and pressure drop build up problems. The gen is available, refineries typically apply minimum
concentration of coker naphtha is usually not high, quench or control the overall exotherm not to exceed
(⬍30%). Appropriate grading at the top of the reactor liscenser’s recommendation. On the otherhand, refiners
in conjunction with low inlet temperature is usually suffi- that want more mid-distillates, usually operate in equal
cient to mitigate the pressure drop buildup tendency of the outlet temperature mode.
coker naphtha. Since a few refiners have been successful Resid Hydrotreater—Just after presulfiding, the cata-
in running coker naphtha without a guard reactor (low lysts are so active that target sulfur is attained at very
temperature diolefin saturation), it seems that the right low temperature. We recommend equal WABT mode of
catalyst system at the correct operating conditions can operation to avoid metal poisoning of the down-stream
work. HDS catalyst for the first 2-4 weeks of operation. After
that, we recommend the following settings (as an
HAHN: example):
We run about 20 percent coker naphtha combined
with virgin diesels and some coker light gas oil all in our Bed 1 (Guard Bed): Base WABT (below 720°F at inlet)
diesel hydrotreater without any problems. We do not have Bed 2 (HDM): Base Ⳮ 10-20°F in WABT
a low temperature first stage, but our first reactor bed is Bed 3 (HDS): Base Ⳮ 20-40°F in WABT
quite small, which may help us succeed in that endeavor. Bed 4 (HDS): Equal outlet of Bed 3
Question 29.
If the refiner requires high conversion, we recommend
What guidelines are used for setting bed temperature
a flat WABT for Bed 2, 3 and 4. In this case, product sulfur
profiles in multi-bed hydroprocessing reactors (e.g., increases gradually after the WABT reaches its maximum.
equal bed outlet temperatures, equal WABT’s, ascending
or descending bed outlets)? HAHN:
We run with a slight ascending temperature profile
FLETCHER: across the first two beds of our hydrotreater reactor and
The proper answer depends on many factors, and as then all the rest have equal bed temperatures.
such it is difficult to give a comprehensive answer. The
optimum reactor temperature profile for a unit wihtout
significant limits is dependent upon the feedstock, the BARLOEWEN:
goals of the hydroprocessing unit and the time on stream From a design point for a low to moderate heat release
of the unit. However, recycle gas, quench rate and/or feed, we would design for equal bed outlet temperatures.
makeup hydrogen contstraints usually significantly reduce We would adjust the bed sizes so that we have approxi-
the reactor temperature profile options. mately the same temperature rise across the beds. The
At SOR, one might decide to minimize the deactivation effect is that all of the catalyst operating at the same
in the first bed by running an ascending profile and not average bed temperature which is the most efficient from
using quench. This can also be driven by high activity in the catalyst utilization standpoint.
the first bed requiring a low inlet temperature to reduce However, when you are dealing with very reactive feeds
the temperature rise across the first bed. In other units, with olefins or very reactive sulfur aromatic compounds,
one might maximize the reactor inlet temperature by it may not be possible to live with those design goals and
operating with a descending profile. Descending profiles you may have to accept a larger temperature rise for the
are useful for maximizing the metals pickup rate of demet- first bed.
alization catalysts and maximizing aromatics saturation. Similarly, as was mentioned by Mr. Fletcher, in a resid
After the middle of a run, a descending profile is almost hydrotreater we would normally operate with temperature
profile ascending in order to spread out the metals deposi- The potential problems or risks are avoided if the
tion and guard against excessive metals laid down on the nitrogen is vaporized with the proper temperature and
lead reactor. pressure specification for your particular operation. The
The only situation, from our perspective, that we would cost of cooling down a reactor with over 150,000 pounds
recommend a descending temperature profile is where of catalyst is less than $20,000. Without nitrogen you
aromatic saturation is equilibrium limited. could triple your time to cool the reactor down.
JOSECK: FLETCHER:
There is no single answer. How you set the temperature We see liquid nitrogen cool down becoming standard
profile depends on the process objectives and whether practice for large units with significant cost of down time
multiple catalysts are in the unit. In general, our experience except during cold weather shutdowns. The economic
is to run as close to ‘‘isothermal’’ as possible. We try to benefit depends on the size of the unit and the product
keep the same ‘‘load’’ across each bed, same weighted upgrade value of having the unit onstream.
average bed inlet temperature or to control peak bed It is definitely important to stay within the metallurgi-
temperatures, where the most side reactions occur. If there cal cooling limitations for the equipment. Usually, it is
is a profile, it is usually ascending. beneficial to add the nitrogen through the furnace to
moderate temperature fluctuations. If inert entry is
TASKER: required following the cool down, further temperature
I have a fairly similar response. Each process should restrictions may be required for the comfort of catalyst
be treated according to the feed and processing objectives. handling personnel. It is actually possible to get the reactor
So there really is not a set answer to this question. Typi- too cold for inert entry.
cally, we use the classical approach depending on the
actual process, and we advise equal outlet temperatures
from each bed for distillate hydrotreaters. Similarly for FOSTER:
pyrolysis feeds we try to maintain equal outlet tempera- We have been using this practice for 15 years, with
tures and a lower inlet temperature. However, you can improvement of 2 days or more on T/A length. We also
only go so far on that. benefit from improved safety for the reactor crew-much
For residing feeds in fixed bed processors, we do use less heat-related stress, because it’s pretty cool in there
different WABTs for demetalization and desulfurization when we get done.
in order to maximize the cycle length at as low a tempera- The potential problems are compressor damage due to
ture as possible. We like to use multi-beds within reason, operating a gas for which it is not designed, and heater
of course, to minimize the delta T per bed as part of the outlet piping embrittlement due to bringing the tempera-
design criteria. ture too low at the point of liquid nitrogen injection.
For HDS operations with heavier feeds, we also use But with good management of change processes, good
equal WABT for multi-bed operation. For heavier feed- operating procedures, and a properly designed diffusion
stocks including partial residue and full residue feeds, we zone, these risks can be reduced to near zero.
have achieved two year run lengths for the lighter deed I recommend you work with your compressor experts
and over one year for the heavier feeds. It may be necessary with particular attention to the limits on compressor suc-
to relax your processing objective to be able to extend tion and discharge conditions, compressor speed, and load
the run length. For one of our units running atmospheric limitations. Also consult with your metallurgy group as
residue, we have achieved over one year run when reducing to the minimum temperature your particular piping can
the sulfur level from 4.0 percent to 0.5 percent. sustain at the point of injection. I highly recommend the
thorough use of thermocouples (encircling the piping at
Question 30. the point of diffusion). We use a stainless steel diffuser
What has been the experience with using liquid nitrogen on the heater outlet that is especially designed just for
for accelerated reactor cool down? How is this normally this purpose and is unique for each application.
done, and what are the benefits, potential problems and Once you have made the proper precautions and have
risks? How widespread is this practice? done this a few times, you can be quite aggressive. In our
case, downtime is always more expensive than nitrogen,
CAIN: so we raise the system to maximum mass circulation and
As mentioned in Question 16, normally we hook up minimum temperature on the heater outlet as quickly as
a liquid nitrogen truck to vaporize the nitrogen to 0°F we can, even if we consume a few extra pounds of nitrogen.
for a once through pass and vent to the flare. From It is a good idea to keep N2 pumper truck available
the time nitrogen is introduced, the reactor temperature all during catalyst unloading. It keeps the temperature
decreases from 180-200°F to 105°F in 12 to 18 hours. down in the vessel, which the workers appreciate, and is
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 119
TOC/INDEX
more versatile in temperature and flow rate when vacuum- dropped 10°F below target, and the injection automati-
ing, or dealing with hot spots. cally shutdown at 20°F below target. Temperature control
was not a problem. As long as the injection is in stainless
steel piping, no injection quill is needed. However, a quill
HAHN: is needed if injecting into carbon steel piping.
I think the other panelists have covered most every- The recycle gas compressor needs to be checked to make
thing. We also use nitrogen cool down as a routine process sure it was designed for or can handle 100% nitrogen. In
and we would also caution that monitoring the tempera- particular, consider the higher discharge temperature, and
tures of the piping at the inlet where your nitrogen goes motor amps. For the cooldown, we dropped pressure to
in is very important. We cool down to at least 120°F 600 psi initially (due to reactor MPT) and continued to
before inert entry. drop pressure as the motor amps increase as the recycle
gas neared 100% nitrogen. One additional precaution we
JOSECK: took was to have the Ultraformer vent H2 to flare during
We have standardized on using liquid nitrogen, cooling our cooldown to ensure that the flare was not put out
for rate limiting units. The time savings greatly outweigh with the large volume of nitrogen being purged from
the liquid nitrogen costs and the additional down time the unit. Our injection rate ranged from 400,000 to
to cool the reactor. We have also incorporated nitrogen 800,000 scfh.
cooling into the shutdown planning time line. We have
been using liquid nitrogen since the ’80s. UDAY PAREKH (Air Products):
Air Products pioneered the technology for liquid nitro-
SAMUELS: gen assisted reactor cool down in 1978 at Amoco’s Texas
UCISCO’s NICOOL process was used for the first City refinery. Since then Air Products has done more
time on the Unicracker in our March 1997 Turnaround. than 25 such cool downs in U.S. and Europe, safely and
For the first time, LEL’s were low enough to get an with significant economic benefits as several members of
immediate entry permit. Historically, nitrogen would be the panel have attested to. To ensure integrity of the
purged upflow through the reactors for approximately metallurgy, the nitrogen injection rate is controlled so
one day before an entry permit could be issued. As far that temperatures remain above a predetermined set point.
as accelerating the cooldown, it is difficult to provide an The nitrogen is injected using a custom designed coil or
exact time. At the previous turnaround we installed 12 diffuser for each application. Typically, a refinery can
additional thermocouple (GAYESCO) which provided expect to reduce cool down times by a factor of three or
skin temperature in the H-C reactor. This additional more using liquid nitrogen.
temperature monitoring showed that the catalyst and reac- In a recent case, two reactors weighing in excess of
tor walls were not cooled completely when the middle of 1.25 million pounds, that is reactor plus catalyst plus
the catalyst beds were ⬍100°F. We may have realized support weight, were cooled down from 280°F to less
approximately 4-8 hour reduction in time but achieved than 100°F in less than eight hours.
a more complete cooling compared to historical cool-
downs and an LEL free reactor. BEN GRIEB (Gay Engineering and Sales Co., Inc.):
During the accelerated cooldown, the reactor wall tem- When analyzing guidelines for setting bed temperature
peratures should also be monitored as well as the catalyst profiles in multi-bed hydroprocessing reactors, a funda-
bed temperatures. Once we started dumping the H-T mental question should be examined. ‘‘Is our current
reactor, we found that the catalyst near the reactor wall temperature measurement system capable of providing us
was still in the 150°F range when the bulk catalyst temper- with the data points necessary for making these operat-
ature was ⬍100°F. In the Hydrocracking reactor the ther- ing decisions?’’
mocouples near the reactor wall cool much slower than In many cases, traditional temperature measurement
the middle of the bed. To sufficiently cool all the catalyst, technology limits both the number and location of the
the reactor walls must also be cooled. sensors. Additionally, the use of the traditional systems
We injected the liquid nitrogen through a 1’’ valve at can detrimentally impact response time and accuracy.
the outlet of the H-T reactor heater and the H-C reactor An increasing number of refiners and process licensors
heater. The injection point was at grade level just upstream are now utilizing the ‘‘Flex-R’’ radial temperature mea-
of the check valves on the heater outlets. Liquid nitrogen surement system to provide a solution to these limitations.
was injected into the recycle gas to achieve a combined The ‘‘Flex-R’’ technology offers many attractive benefits
gas temperature of 40°F. Thermocouples were positioned for temperature profiling in reactors. Attributes such as
on the down stream piping to monitor the temperatures. faster response time, greater point density, complete reac-
Visual and Audible alarms activated if the temperature tor coverage, and improved accuracy provide the operator
with a valuable tool for setting bed profile operating from stress corrosion cracking. The reference will be put
parameters. into the transcripts.
For a full discussion of the benefits of this technology,
including user experiences, O refer you to NPRA Paper CAIN:
AM-96-63, or contact Gay Engineering and Sales Co., Normally we vacuum and neutralize with the soda
Pasadena, TX. ash solution. Although in some cases after unloading the
catalyst through the dump chute, the catalyst handling
MIKE HUNTER (M.W. Kellogg Company): specialists under fresh air clean out the catalyst pockets.
I have a followup question. Several of the panelists We then use high pressure wash with special spray nozzles
mentioned the temperatures at which they stopped the to clean and neutralize the vessel walls and hardware,
liquid nitrogen cool down. I would like to ask if that is traces, beams, etc.
a process temperature or a vessel wall temperature. Also, The spray nozzle spins 360 degrees and sprays soda
at what process temperature do you start the procedure? ash solution at 10,000 to 15,000 psig. Once finished, we
then lower a person inside and clean out any hard to
reach places with a hand-held high pressure lance. The
CAIN: vessel is then allowed to drip dry. We then discontinue
As mentioned earlier, we started at 180 to 200°F pro- the nitrogen purge. After checking for the oxygen content,
cess temperature in the reactor. We stop it at 105°F. it is ready to be entered by maintenance personnel.
JOSECK: HAHN:
On some of our heavy wall reactors, we usually go to We do not water wash our hydrotreaters. We just dump
a skin temperature and an outlet temperature due to the using an inert atmosphere by specialty contractors. They
reactor vessel metal mass. also vacuum out any remaining dust or particles from the
reactor while under inert atmosphere. We get a satisfactory
HAHN: cleaning using this mode.
The 120°F that I referred to was the process tempera-
ture (reactor inside temperature). FOSTER:
We us a high pressure orbital nozzle to spray all internal
parts with a soda-ash solution. This is to passivate 300
SAMUELS: series stainless steel parts from polythionic acid attack, of
We would start the injection at 40°F process tempera- course, but also provides initial removal of residual coke
ture and stop the process at 20°F process temperature. and scale. Once this phase is completed, contractors enter
with high pressure hydroblasting equipment for a thor-
Question 31.
ough cleaning of all internal parts—again we use soda-
What cleaning methods are used for multi-bed hydropro-
ash solution here as well. Then the liquid that remains
cessing reactors after unloading? If water is used, how
is removed by vacuum or rags. We do a final dry out
is it removed from the reactor before loading? What
with a high volume fan placed at the Rx outlet.
special methods are used to clean interbed internals and
the mesh support for the catalyst?
5. General Process
FLETCHER: Question 32.
1. Alkaline wash solution is used to protect austenetic Is anyone feeding HCGO (FCC cycle oil or heavy coker
stainless steel and other austenetic alloys from gas oil) to a hydrotreated gas oils hydrocracker/hydro-
polythionic acid stress corrosion cracking. Solution treater? If so, what are the operating conditions (WABT,
pH should be greater than nine for adequate neu- H2 partial pressure, LHSV) and yields? Are there any
tralization. These solutions may also contain an problems with FCC catalyst or coker fines? How are these
alkaline surfactant and corrosion inhibitor. hydrotreated gas oils used?
2. The recommended wash solution is a 2 wt% soda
ash. A 1.4 to 2.0 wt% soda ash solution will provide ROMAN:
a sufficient level of residual alkalinity on metal We hydrotreat RCC heavy cycle oil along with virgin
surface after the solution drains from the equip- vacuum gas oil in a vacuum gas oil desulfurizer prior to
ment. Higher soda ash concentrations (5 wt%) are feeding it into a conventional FCC unit. A maximum
desirable when the catalyst itself has wedded. gasoline yield obtained from hydrotreated heavy cycle
There is a paper from NACE (RP0170-93) that pro- oil is 60 percent compared to only 43 percent for non-
vides more details on the protection of austenetic alloys hydrotreated heavy cycle oil. We occasionally will feed
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 121
TOC/INDEX
either RCC or FCC light cycle oil into the VGO unit PETERSON:
and recrack it in the FCC if the gasoline distillate spread We treat our LCO in either the DHDS unit or the
is high enough. CFH unit as economics and available capacities allow.
The maximum gasoline yield from desulfurized RCC One of our refineries hydrotreats FCC slurrry in a 400
light cycle oil was somewhat higher at 65 percent. As psig, four bed hydrotreater. Operating conditions are as
would be expected, the sulfur in the gasoline derived from follows:
heavy cycle oil is dramatically lowered from 1,580 ppm
Feed Sulfur, wt% 1.70
to 78 ppm by desulfurizing this cut. Product Sulfur, wt% 0.95
The economics for either mode of operation are not LHSV, Hr-1 1.0
straight forward and highly dependent upon pricing, H2/HC recycle, SCFB 1,000
hydrogen availability and desulfurizer capacity. You need H2 Consumption, SCFB 350
to have a high degree of confidence in your linear program H2 Partial Pressure, psia 375
yield vectors. We have had no problems with FCC cata- Cycle Length, months 24
lyst particles. SOR WABT, F 630
EOR WABT, F 725
TASKER: In the past, cycle length had been activity limited.
I hate to steal Mr. Cain’s thunder on this one. The However, since a portion of the reduced crude feed to
convent H-Oil unit operation does include FCC heavy the FCC is typically now being hydrotreated, cycle length
cycle gas oil in the feed. Obviously, there would be some has greatly improved. Feed sulfur used to be in the 2.5
aromatic saturation taking place. But all of the recovered to 3.0 wt% range with target product sulfur content at
gas oils, treated gas oils, are recycled back to the FCC 1.0 wt%. The current cycle has nearly reached 2 years
and effectively therefore we are recycling the heavy cycle with another year to year and a half projected before a
gas oil to extinction. complete catalyst changeout is needed. A portion of the
The advantages of doing this particular operation are product can be recycled to control severity with a lower
that we improve the asphaltene solvency even though conversion per pass.
there is some partial aromatic saturation. Also when we We do not have any trouble with pressure drop as it
are heat input limited, the hydrogen consumed by the seems that the FCC catalyst fines largely pass through
heavy cycle gas oil does help us to adjust our reactor the reactor. The feed is not filtered. Dense loading is
temperatures and assist in getting the particular target critical to extending the life as sock loads suffer from
reactor temperature. regions of coke formation from poor retention of feed
There have been problems with FCC fines on occasion distribution. Catalyst pore size must also be consistent
when the filters have not functioned correctly in the with slurry molecule size as a load of small pore size
FCCU. Impeller wear on the feed pump has been experi- catalyst had a very short life. The dedulfurized slurry is
enced as catalyst fines lay down in some of the bottoms sold as No.6 fuel oil.
exchangers. Proper and good filtration therefore in the
FCC will avoid those problems.
The gas oils can be injected upstream of the reactors BARLOEWEN:
where the black oil feed can be used as quench oil in the There are a number of refineries that feed FCC cycle
downstream vessel. oils or heavy coker gas oils to hydrocrackers. These feeds,
Now, for separate processing, the heavy cycle gas oil as has been discussed, are very refractive. They are difficult
is relatively refractive and pilot testing has shown that the to treat. They put a premium on having a very high
aeromatics saturate first. It is possible to crack, but this activity denitrogenation catalyst and the higher the partial
requires quite severe conditions. pressure, the better.
The conditions will be about or 150 atmospheres of As we discussed early today, there are a number of
hydrogen partial pressure at a 0.2 to 0.3 liquid hourly problems associated with them dealing with solids han-
space velocity and a temperature of around 360°C. dling filtration. So the use of a graded bed is a big assistance
For HDS and hydrocracking operations, we do not in processing them on the long term basis.
have any commercial experience on this material , but we
think that a zeolite type catalyst would be the better choice CAIN:
of catalysts for the pretreatment that would be required. We feed the FCC heavy cycle gas oil and heavy and
Obviously, the fines would be bad news and there would light coker gas oil to a hydrocracker. We operate at 2,400
be an impact on the operation. Therefore, it might be psi with the hydrogen purity of greater than 80 percent
necessary as we have previously mentioned to design a and we target our weight average bed temperature to
guard bed and thereby increase the overall cost. achieve a 65 percent conversion.
FLETCHER: are very aromatic and require high pressure and low LHSV
Both HCGO (FCC cycle oil) and HKGO (heavy coker relative to virgin streams. We have three such hydrotreat-
gas oil) are processed by refiners in hydrocracker/hydro- ers in Japan, feeding heavy coker gas oil. Operating condi-
treater units. We will let the individual refienrs comment tions are as follows:
on conditions and yields. Suffice it to say that these oils
Company KOA OIL TOA OIL FIJI OIL
Refinery Marifu Kawasaki Sodegaura
Unit Type FCC Pretreatment FCC Pretreatment FCC Pretreatment
Feedstock
SR VGO 70-80% 70% 90%
Coker LGOⳭHGO 20-30% 30% 10%
Feedstock Properties
Density 24.5 22.0 20.7
Sulfur (wt%) 1.9 2.5 3.0
90% BP( F) 1090 1020 1010
Operating Conditions
LHSV (1/hr) 1.02 0.45 2.0
H2/OIL Ratio (SCFB) 3600 1200 3000
ppH2 (psia) 1600 670 725
Cycle Length (month) 23 23 11
Bottom Product Sulfur (wt%) 0.01 0.1 0.08-0.15
Catalyst KF901H KF901H KF901H
Question 33.
2. More active catalysts are being used. Operation
Yield estimates from hydrocracking catalyst vendors
at lower temperature reduces gas formation. In
show a decreasing trend in formation of cracked gases.
addition, yield decline (SOR to EOR difference)
Do actual commercial performance data verify this trend?
is reduced significantly.
TASKER:
3. Improved zeolites.
Choice of zeolite type catalyst over amorphous catalyst HAHN:
will result in lower formation of cracked gases. We have We replaced catalysts in two of our hydrocrackers and
observed that the recycled gas purity has remained fairly in each case we found substantial reductions in our gas
constant from start of run to end of run over a two to make. When we switched out one unit that had about a
three year cycle and relative little purging was done. This four year old catalyst in it, we reduced gas make by almost
was for a middle distillate application. For naphtha crack- half. In the other one that had eight year old catalyst, gas
ing though, we have observed an increase from start of production was reduced more than half.
run to end of run.
In one of our units, we have reached 18 months into GEORGE HADJILOIZOU (Zeolyst International):
the cycle and the deactivation has been between 4 to 5°C We have observed both commercially and in pilot plant
or 7 and 10°F. This represents a high degree of stability studies repeatedly less total gas make with our base metal
in the operation. Gas production from the start of run nickel tungsten and nobel metal hydrocracking catalyst vs.
condition to the present end-of-run condition, is very sim- competition products. Typically, we have seen at least one
ilar. to two percent less gas make depending on feed and process
conditions. We believe this is due to the type of zeolite
FLETCHER:
technology and catalyst formulation techniques that we
The yield estimates are accurate. Commercial operating employ in all of our hydrocracking catalyst products.
data verifies the improvement. The reasons for these yield
improvements are a combination of what we believe to Question 34.
be three fundamental shifts. For hydrotreaters configured with separate liquid and
1. A shift from NiMo to NiW catalysts. The NiW gas preheat, it has been suggested that a small amount
catalysts offer greater hydrogenation activity with of hydrogen be injected with the liquid feed to reduce
less over-cracking. Hence, there is also a lower fouling on the exchanger train. Does anyone do this, and
and more stable gas make over the course of the if so, what is the ratio of hydrogen to feed charge? What
catalyst cycle. other issues should be considered?
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 123
TOC/INDEX
BARLOEWEN: FUSSELL:
Some of the hydrocracking units and resid hydrotreat- We have a distillate hydrotreater in Port Arthur that
ing units designed by Unocal in the past had separate we tried this on and it did not work. Basically, what
heat exchanger trains to preheat the oil and the recycled happened was exactly what Mr. Binford described. We
gas to the hydrotreating reactor. pushed the problem into the reactor. Instead of having
For these units, it was common to add a small amount a down time after nine months just to clean some heat
of recycled gas to the oil feed upstream of the feed-effluent exchangers, we had a down time after nine months to
exchanger increasing the hydrogen partial pressure. The dump the reactor and clean the heat exchangers. So we
theory is to inhibit coking against the hot tube wall and are no longer injecting hydrogen into these heat
also incrementally increase the vapor velocity through exchangers and we are continuing to troubleshoot the
the exchanger. problem.
HENKE:
BINFORD: We inject hydrogen into the liquid feed of one our
Yes, we have seen several refiners inject hydrogen into diesel hydrotreaters at a rate of 500 standard cubic feet
the liquid feed to reduce fouling in the exchanger train. per barrel. The feed to this unit is very reactive, comprised
The primary benefit as Mr. Barloewen said is the increased of light cycle oil and light coker gas oil. Design issues
hydrogen partial pressure and the increased velocity that we consider when injecting hydrogen into liquid feed
through the exchangers, thereby reducing the deposition include total recycled gas rate, thermal design and heat
potential of material inside the exchanger tubes. You need transfer equipment, the metallurgy of the feed effluent
to make sure that the hydrogen does not result in some exchangers, the heaters and the associated piping, the
overall hydraulic limit or significant change in heat trans- reactivity and stability of the liquid feed and finally, the
fer through the preheat exchangers that may limit your stability of the flow regime. I refer you to the 1993 NPRA
heat duty. Q&A transcript page 97 Question 20. Syncrude Canada
Some units were initially designed for hydrogen injec- reported some work that their research department had
tion. So these factors have already been considered in the done concerning the chemistry of free radical saturation
design of the unit. It is also our observation, through and other items there.
feedstock characterization before and after hydrogen addi-
tion, that the hydrogen in the preheat exchangers does MALEK:
not decrease hydrocarbon polymerization in many reac- Just to reinforce some of the things that Mr. Henke
tive feedstocks. has said, we believe that the benefits of injecting hydrogen
This confirms that hydrogen is not able to saturate are primarily related to velocity effects and better heat
any of the olefinic materials in the feed until it reaches transfer coefficients, perhaps preventing some fouling in
the reactor catalyst. As a result, understanding the cause these exchangers.
of fouling is extremely important before investing in capi- However, a word of caution has been already pointed
tal to make this operational change if you do not already out. Hydrotreaters that are configured with separate liquid
have the capability. and gas preheat systems will sometimes have metallurgy
Polymerization reactions may be decreased with the that is incapable of handling H2S that may be in the
addition of hydrogen, but only if the reactions are being recycle gas. So be careful where you inject it. If there is
caused by high film surface temperatures on the exchanger no recycle gas scrubber or if it is only partially effective,
tube wall. If inorganic particulates are causing the fouling, the hot H2S corrosion can occur in some of the exchanger
adding hydrogen ahead of the exchangers to increase the equipment if it is not 300 series stainless steels.
velocity may simply push the problem downstream to the Also, potential flow distribution problems will develop
reactor bed. As a result, if the fouling mechanism is not in the multipass heaters if some of you have designs that
properly identified, hydrogen addition may accelerate do not have positive flow control and are relying on
reactor bed fouling resulting in premature catalyst symmetrical flow distribution. Two phase flow may give
changeouts or more frequent skimming of the top of you flow distribution problems across those heaters.
the bed.
TASKER:
Pushing it one stage further, we do have the capability
CAIN: in black oil processing of injecting hydrogen into the
We have been successful at Delaware City adding heater, the oil heater. We do have separate gas and oil
hydrogen to our hydrocracker feed to reduce feed side heaters. However, the idea here was to improve the overall
fouling of exchangers. We do fix the hydrogen flow rate heat transfer coefficient or the heat flux when you are
at a small rate independent of the feed rate. really pushing the unit.
It was also there to minimize the possibility of coking Biotechnology for naphtha and crude oil as well as
in the heater. However, we operate the heaters at low decanted oil desulfurization will hopefully follow shortly
enough temperature that we very seldom see any coking thereafter. We are not aware of any other company that
potential occurring in that heater. What we have seen is, is actively pursuing the development of a biological process
as already mentioned, a tendency to cause flow instability for removing sulfur from petroleum streams.
of the oil when hydrogen is injected. This facet has to
be done carefully. We have tried it but have really not EDWARD SMITH (UOP):
seen the benefit in reality. UOP also considers biodesulfurization a very exciting
Question 35. and interesting area with significant advantages and
Is biodesulfurization technology nearing commercializa- opportunities if applied correctly in the refining and petro-
tion? When do people think this might actually reach chemical industries. We have begun an active and aggres-
the refiner? sive proof of principle investigation with a partner to
determine process feasibility and to quantify some of the
HENKE:
benefits and technical challenges.
We are optimistic about the commercialization of The concept is truly in its infancy and realistically, we
biodesulfurization technology. We are working closely believe it will be at least a few more years before ‘‘true
with Energy BioSystems to incorporate Koch mixer tech- breakthrough’’ is achieved such that bulk desulfurization
nology into the design of the biodesulfurization reactor. can be offered commercially. UOP will be working on
Koch also is working closely with Energy Biosystems to specific projects in this area and we will seek refiners’
develop a biodesulfurization process for naphtha streams. feedback during the development of this technology.
We have been told by Energy Biosystems that they are
approximately 6 to 18 months away from commercial V.K. KAPOOR (Indian Institute of Petroleum):
commitment to build the first diesel biodesulfurization What level of diesel sulfurization is expected for the
unit. naphtha and diesel products particularly the diesel biode-
sulfurization process coming up in about a year?
SAMUELS:
I have similar information. Marathon believes that this HENKE:
technology will be applicable for naphtha desulfurization. For diesel it is a strong function of the residence time.
We are currently completing a joint research development You can get product sulfur down to the lower ppmw
agreement with a leading biodesulfurization concern levels with enough time in the bioreactor. As far as naphtha
involving a collaborative research effort and application of desulfurization is concerned, it is too early to tell what it
Marathon’s technology to the biodesulfurization process. will be, but I assume that they will get it down to ppmw
We estimate commercialization for naphtha desulfur- level. Again, it will be a function of residence time.
ization within three to five years and diesel biodesulfuriza- Obtaining very low product sulfur levels may not be
tion in as soon as 6 to 12 months. economically viable. One of the things we are optimistic
about is the combination of biodesulfurization with con-
SAMIR MOHAMMED HALAWANI (Saudi Aramco): ventional hydroprocessing. In this case, we would be ask-
Could we have a brief description of the biodesulfuriza- ing the biodesulfurization reactor to take out the more
tion process? refractory compounds that conventional hydroprocessing
currently has difficulty removing.
HIGGINS:
There is a paper that was presented a couple of years Question 36.
ago that had some of the introductory material on it. In start-up of hydrocracking catalyst, is anyone practicing
simultaneous presulfiding and ammonia passivation?
MIKE PACHECO (Energy Biosystems Corp.): Are there any problems controlling NH2HS formation in
As the two speakers have already stated, biodesulfuriza- the effluent piping?
tion is very near commercialization. At Energy Biosystems
in Woodlands, Texas, we are working on a process with BARLOEWEN:
several refiners to desulfurize petroleum streams with We know of one hydrocracker that used ex situ sulfided
genetically engineered microbes and air at ambient tem- catalyst to which a nitrogen containing compound had
perature and pressure. Our current focus is on the com- been added before the catalyst was loaded. This did not
mercialization of diesel biodesulfurization. We hope to completely passivate the catalyst’s cracking function since
have a commitment within the next 6 to 18 months most of the ammonia was desorbed during the startup
to announce the world’s first biodesulfurization process. and lost from the system. We would recommend separate
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 125
TOC/INDEX
sulfiding and passivation. The typical approach is to sul- product. Catalyst deactivation rates are calculated from
fide first and then proceed with passivation. Wash water these data and compared to reference curves developed
should be started before the ammonia or nitrogen contain- through pilot plant studies conducted at our research
ing compound is introduced for the passivation. center.
The DAO quality and quantity is controlled to target
GEORGE HADJILOIZOU (Zeolyst International): around a 1.7 to 2 wt % combined feed concarbon. The
We offer both base metal and noble metal hydrocrack- hydrotreater product is typically .3 to .4 wt % concarbon.
ing catalysts. We do not typically require ammonia passiv- Metals obviously, as well as concarbon, deactivate the
ation during startup or during normal operation. We have catalyst. We do not routinely test for metals, but correlate
found in our 50 plus startups that, through optimized those to concarbon. We achieve 15 month runs, but the
startup procedures, we can effectively activate and startup severity is dictated by economics. The unit has four reac-
our hydrocracking catalyst without the need to passivate. tors in parallel with a 1.45 space velocity, a 670°F start-
of-run weighted average bed temperature, and a 770°F
Question 37. end-of-run weighted average bed temperature.
What routes does the industry utilize to hydroprocess
DAO or blends including DAO? Please provide specific BARLOEWEN:
details. DAO is typically fed to FCC pretreaters. One question
to really keep in mind is the deeper you dig in your
ROMAN: deasphalting unit, the more metals will come with it.
We used to hydrotreat DAO in a vacuum gas oil Those metals are going to be quantitatively laid down on
desulfurizer and we were limited to a 50 to 55 percent your hydrotreating catalyst. So the deeper you lift or the
lift on the SDA unit to keep the concarbon down to an more you lift, the more you have to provide metals removal
acceptable level. We subsequently converted the SDA unit capacity at the front end of that hydrotreating unit, typi-
from a mixed solvent extraction operation to straight cally through the use of demet catalysts.
butane solvent operation with the goal of achieving a There also has been deasphalted oil fed to hydrocrack-
maximum lift of about 70 percent. Operation at high lift ers. However, on the particular unit that this occurred,
forced us to discontinue hydrotreating the DAO due to as they tried to raise the conversion on the DAO portion,
unacceptable catalyst life on the VGO unit. they found significant rate of deactivation and they
Some preliminary LP work as indicated that we may backed off.
have an incentive to reduce this lift and hydrotreat DAO
during the summer months if asphalt prices are high
FLETCHER:
enough.
DAO hydroprocessing resembles resid hydroprocessing
except that the metals removal load is lower and the
TASKER: Conradson carbon content is lower. Hydrotreating deacti-
We do have some experience with DAO in hydrocrack- vation rates are high relative to gas oil processing. Catalysts
ing operations. For propane DAO we find that it is easier are selected based upon the combination of high activity
to crack than HVGO. The DAO should be a purer hydro- and high metals pickup capacity. One example:
carbon with the resins and asphaltenes removed. But if
some resins are left in the DAO, then it becomes more Catalyst: KF901H-1.SE
difficult to crack and effects catalyst life. Therefore, the ppH2: 620 PSIG
ease or otherwise to process DAO will strongly depend Feed: VGOⳭ5-10% DAO
on the quality of the deasphalting operation. With the H2/Oil: 1725 2CFB
units coupled, it is possible to control the relationship LHSV: 2.6 1/H
between hydrocracking and deasphalting. Product Sulfur: 0.3 wt%
Cycle: 23 months
SAMUELS:
The Marathon Garyville refinery currently processes FUSSELL:
LVGO, HVGO and up to 20 vol% DAO in a 900 psig In Port Arthur, we have a UOP Demex unit. Our
86,000 barrel a day FCC feed hydrotreater. Rose unit colleagues at Diamond Shamrock at Three Rivers are
operation, the charge rate, solvent composition and the probably the only one that can relate to that statement.
lift provide the desired throughput of DAO according to But basically, it is a solvent extraction unit which uses
operating targets established for the hydrotreater. normal butane. We actually make three cuts off of the
These are defined by past history, current operating Demex unit.
conditions and expected catalyst performance which is We make a DMO, a resin cut and an asphalt cut. We
closely monitored by a daily sampling of the feed and run the unit at approximately 220°F softening point on
Question 39.
Drastic reductions in sulfur are required to meet Euro-
pean diesel fuel specifications or California clean air
regulations. These reductions, as well as seasonal
changes in diesel pool blend components, are making it
difficult to meet cloud, pour, lubricity, and other product
specifications. What processing, chemical treatment,
and blending options can be used to maximize diesel
the asphalt. Approximately five years ago, we started feed- pool economics in this environment?
ing the resin and the DMO to our Unibon unit. Prior
to that we were only feeding the DMO along with heavy
vacuum gas oil. We are able to get approximately 80 FLETCHER:
percent sulfur removal, 50 percent concarbon removal The simple approach is to use kerosene blending and/
and 70 percent metals removal across our Unibon unit. or additives in the diesel pool to improve the cold flow
We do have a problem on the Unibon though as a properties. The problem is using high valued kerosene or
result of running this higher asphaltene containing mate- expensive additives in the winter diesel season.
rial. That is foaming in our high pressure separator. The In Europe several refineries have selected the Akzo-
foaming has been a problem ever since we started running Fina CFI Technology and Mobil Mid-Distillate Dewax-
the resin, mostly at end-of-run. On this particular catalyst ing Technology to bring the cold flow properties of their
run that we are into right now, we seem to have a continu- diesel and heating oil into specs. The following process
ous foaming problem in the separator and we are currently options are being applied: (1) diesel dewaxing, operating
working on installing an antifoam injection system. in HDS mode during the summer and in dewaxing mode
We have done a couple of things to change the system. during the winter producing low cloud point or pour
We made some modifications in our Demex unit in point diesels with extremely low product sulfur; (2) high
November. We also changed from a Criterion catalyst conversion dewaxing. Dewaxing combined with a hydro-
system to an Akzo catalyst system on the Unibon. Now, cracking functionality which allows the conversion of
Criterion would probably say that it is that Akzo catalyst LVGO, HVGO to low sulfur, low pour point products.
system that is causing the foaming, but we really do These can be blended directly into the diesel pool; (3)
not know. MAK-LCO, a process that converts LCO into high octane
We do know that something has changed. I just want gasoline and low sulfur high cetane diesel. In many cases,
to warn everyone that you may have that problem. We these processes can be applied to existing units with only
have discussed it with UOP. They have recommended minor hardware changes.
that we install a larger high pressure separator. As you As you may have heard, Mobil, Akzo Nobel, Kellogg
might imagine, that has been very difficult to justify to and Fina have merged their MAK, CFI and Mid-Distillate
management. Dewaxing Technologies into one technology partnership,
offering the best and most flexible technology approach
to producing high quality diesel.
MIKE HUNTER (M.W. Kellogg Co.):
Within our technology alliance with Mobil, Akzo
Nobel and Fina, we have recently completed a large series BINFORD:
of pilot plant tests, looking at hydrocracking deasphalted I am going to focus on the lubricity portion of this
oil from a Rose unit in combination with vacuum gas oil. question. Mr. Fletcher effectively covered a lot of the
We have looked at blends consisting of 20 to 40 percent other issues. Severe hydroprocessing to meet sulfur and
DAO at conversion levels ranging from 20 to 70 percent aromatic specifications can result in low lubricity fuels.
in a single pass configuration. We have published the This is certainly the case with Swedish diesels and
early results of this at the 1997 NPRA Annual Meeting. CARB diesels produced to meet the ultra low sulfur and
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 127
TOC/INDEX
ten percent aromatic specification. Newly developed non- hydrotreating, although FCC performance has improved
acidic lubricity improvers are one option to improve the as well. The operating conditions are as follows:
lubricity of these fuels.
Feed Sulfur, wt % 0.60
Diesel lubricity can also be adversely affected by exces-
Reduced Crude Sulfur, wt % 1.00
sive kerosene blending to meet winter cloud or low tem-
Product Sulfur (Frac Btms), wt % 0.35
perature operability specifications, primarily due to low
LHSV, Hr-1 1.25
viscosity. The lubricity of these fuels can also safely be
Pressure, psig 800
improved with non-acidic lubricity improvers.
Recycle H2/HC, SCFB 1,670
Another option is to use a cloud point depressant and/
H2 Partial Pressure, psia 730
or low temperature operability additive to back out the
Cycle Length, months 12
kerosene. This may safely meet both lubricity and low
SOR WABT, F 650
temperature specifications. The resulting heavier fuels also
EOR WABT, F 730
typically have a higher cetane number and are more dense,
Reduced Crude Ramsbottom, wt % 2.50
resulting in better ignition properties, better cold starts,
Frac Btms Ramsbottom, wt % 1.51 to 1.88
and sometimes improved fuel economy.
Reduced crude as feed, % 45
We introduced a new cloud point depressant last year
and are currently field trialing several more new chemis- The unit has performed better than initially expected,
tries this fall to offer the refiner more choice in cloud achieving 65% reduction in sulfur and 25 to 40% reduc-
additives that can be tailored to meet the overall CARB tion in Ramsbottom carbon. Trimetallic catalyst from
diesel blend pool objectives. Akzo-Nobel is used. The feed is not filtered and most
In reference to diesel pool economics, my response in recent cycle was cut short due to pressure drop after an
Session 4, Question 42, will cover this issue. upset when the recycle compressor shut down. The pres-
sure drop across the first bed increased from 70 psi to
LINAS JOKUBAITIS (Lubrizol): 130 psi. Reduced crude was taken out of the feed and
The Lubrizol Corporation offers the refiners chemical the recycle hydrogen was reduced to get the pressure drop
treatment options to meet cloud point, pour point, lubric- below the maximum allowed 100 psi until replacement
ity and operability requirements. For example, there are catalyst could be installed. Compressor upsets in naptha
now chemistries available to thermodynamically lower hydrotreaters have also resulted in sudden increases in
cloud point. pressure drop. Our experience on our other FCC feed
hydrotreater shows filtration is quite important.
DAVID DICAMILLO (Criterion Catalyst Company):
Criterion and ABB Lumus offers Synflow as one of its BARLOEWEN:
Syn technologies. I will give you an example of how it One refiner that we worked with has been processing
can reduce cloud point. In one specific customer test, we atmospheric resid in VGO hydrotreating unit. The unit
reduced cloud point from 34° to 16°F and maintained operates at about 700 or 800 pounds partial pressure.
100 percent distillate yield in the product. When we They are able to achieve typically about 70 percent desul-
reduced distillate yield to 98 percent, the cloud point furization and 20 to 25 percent CCR reduction.
reduced further to 6°F. On this same feed, if the customer The level of CCR reduction is very much a function
cut the ten percent heaviest material out, he could have of the hydrogen partial pressure of the unit and if this
reduced the cloud point to 10°F. unit were to try to dramatically improve on that CCR
reduction, we believe that they would run into problems
Question 40. due to the lack of hydrogen partial pressure. What they
What experience have refiners had in processing atmo- are really converting are the sulfur compounds and the
spheric reduced crude with VGO in low pressure hydro- asphaltene compounds that are left in the VGO and as
treaters to produce FCC feed? What percentage of they try to get to higher conversions they have a hard
reduced crude has been processed? What levels of desul- time in that low system pressure to achieve very much
furization and CCR reduction are realized? conversion on the asphaltene portion.
PETERSON: FLETCHER:
One of our refineries processes reduced crude derived We are familiar with a number of units that are process-
from fairly sweet, light crude through a low pressure ing reduced crude in hydroprocessing units with low
distillate desulfurizer. About 45% of the reduced crude is operating pressure relative to units designed for atmo-
hydrotreated along with LCO and straight run distillates. spheric tower bottoms. In general, the cycle lengths are
FCC flue gas Sox reduction is the main purpose for the low relative to gas oil in the same unit.
Akzo Nobel is familiar with several cases in which the yield to distillate which results from commingling heavy
reduced crude is operated in 600 to 800 psia partial naphtha with the much larger middle distillate stream.
pressure hydrogen hydrotreaters. The concentration of
reduced crude is less than 50% in all cases. Up to 80% TASKER:
desulfurization and 35% CCR removal has been achieved. IFP and HRI have licensed several units to hydrotreat
This type of operation is usually only practical when full range FCC gasoline to reduce sulfur. Typically when
reduced crude sulfur, CCR and metals (Ni and V), are the unit reduces the feed sulfur from about 275 to about
relatively low (S⬍1 wt%, CCR⬍2 wt%, NiⳭV⬍5 ppm). 50 weight ppm and the feed olefin is 31 weight percent,
Even in these cases, cycle lengths of less than 12 months the road octane loss has been less than about five numbers.
are typical. Cycle length is primarily dependent upon If the feed sulfur was lowered from a level of say 4,200
operating severity (%HDS, %HDCCR and LHSV), since ppm to 420 and the feed olefin content is 24 percent,
this determines the deactivation rate due to coking. the road octane loss is less than 3.5 numbers.
The major benefit from this treatment is vanadium CAIN:
removal and the resulting reduction in required FCC We conducted a week long test at our Delaware City
catalyst purchase. In some cases, the FCC gasoline and/ plant. The inlet sulfur was reduced from 1966 ppm to
or NOx emission limits also justify the shortened cycles. 0.1 ppm. The RON was reduced from 88.8 to 77.6 and
the MON was reduced from 78.2 to 70.3.
ELIZABETH ALLEN (Criterion Catalyst Company):
A number of Criterion’s customers are processing RICHARD FOLEY (CDTECH):
reduced crudes at low pressures in VGO units. Typically, CDTECH licenses a CDHES process for reducing the
these units are processing about 25 percent resid in a sulfur content in full range FCC gasoline. Eight or ten
blend of VGO, although there are also a number of different customer feed stocks containing 2500 to 1000
customers who are processing with straight run distillates. ppm sulfur have been tested in the commercial demonstra-
Typical desulfurization levels are about 80 percent and tion unit at CDTECH. We have been able to reduce the
CCR removals up to 65 percent. At very low pressure, sulfur contents to 50 to 100 ppm level (95% desulfuriza-
let us say at around less than 1,000 pounds, the significant tion) with octane loss (RⳭM)/2 of less than 1 to 2.
deactivation of the catalyst system from coking due to the Catalytic distillation provides the opportunity to treat the
high CCR will be observed even at the low space velocities. high sulfur and high olefin fractions of full range gasoline
from the FCC unit separately, at optimum conditions,
Question 41. with lower octane loss and lower total installed cost than
Is anyone successfully hydrotreating full range FCC gaso- fixed bed processes.
line to reduce sulfur? What are the product sulfur levels
RICHARD ROSSI (Criterion Catalyst Co.):
and corresponding MON and RON octane losses. What
There are some refiners on the West Coast and a
were the initial sulfur, MON and RON levels?
couple in the midwest who are believed to be successfully
hydrotreating FCC gasoline or have done so in the recent
ROMAN: past via several different options. While one can achieve
We have done extensive work in this area. We used about 90 plus percent HDS on full range FCC gasoline
commercially available cobalt moly catalysts to minimize via conventional hydrotreatment, there will be significant
olefin loss and targeted a product sulfur level of about loss of RON and MON due to saturation of olefins in
250 ppm. The FCC naphtha experienced an octane loss the front end of the stream. With space velocities in the
of 12 octane numbers. We also performed the same test range of 5 to 8 and 92 to 98 percent HDS, a 4 to 8
on our light RCC gasoline and experienced the loss of number loss in RON and about a 1 to 3 number loss in
19 octane numbers due to its higher olefinicity. Most of MON are likely with the octane loss being more severe
the sulfur in cracked gasoline is in the 360° degree plus at the higher desulfurization rates. Because of this, many
cut. The way to minimize the severe octane loss is to refiners have considered preferentially hydrofeeding just
desulfurize the 360° degree plus gasoline only. This heavy the heavy FCC gasoline, as was mentioned before, which
naphtha can either be desulfurized in a stand alone unit is relatively sulfur rich and olefin poor and thus minimizes
or it can be dropped down into the light cycle draw in the octane loss. In this case, one can target relatively high
desulfurized and middle distillate desulfurizer or DDS HDS rates and hold RON and MON losses down to
unit. There is a three or four percent loss in total gasoline perhaps 1 to 2 numbers.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 129
TOC/INDEX
FUSSELL:
At our Port Arthur refinery, we bring our sulfuric acid
into the plant, as well as out of the plant, in rail cars to
Olin. With the spent acid, we test the concentration, we
find out what the concentration is in the acid, and then
we take a strapping on the rail car. On the fresh acid, we
use the bill of lading and we strap the rail car.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 131
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economics would have justified the additional provisions proper coalescing of the feed has a major impact on the
for light ends removal. water content in the circulating acid.
problems. The Alkat seems to have stabilized the unit improvement. It is probably justified when you weigh the
for us. additional cost of more isobutane versus the catalyst cost.
We are getting ready to do a trial using the Nalco/ The numbers that I have reviewed indicate that the use
Exxon product. We are not doing this because we have of these catalysts is cost-effective.
a problem with the Betz product; we just feel like doing
some experimenting. Question 6.
What experiences, if any, have people had using capaci-
BINFORD: tance probes to determine the settler acid level and the
The numbers that Ms. Fussell quoted are pretty typical acid-to-hydrocarbon ratio in the reactor?
of what we see with our cocatalyst product. We have
evaluated it in 21 commercial alkylation units, which FOSTER:
equates to about half of the alkylation units in the United We currently have capacitance probes on four settlers
States. Typical performance improvements quantified are and DP cells on two others.
3% to 7% improvement in unit yield; 10% to 27% We have had good experience with the capacitance
reduction in unit acid consumption; and a 0.3 to 0.7 probes. They more accurately identify where the top layer
number increase in alkylate octanes. That small value of foam exists, and they show a good trend of the acid level.
octane increase can be very valuable, but as Ms. Fussell
mentioned, it may be very hard to see in the unit, and Question 7.
hard to quantify. Reduction of undesirable side reactions We have had occasional foaming in our alkaline water
in the unit, as a result of using the co-catalyst, has also wash system. Could it be caused by poor make-up water
reduced corrosion in the downstream DIB tower and quality (TDS) or aromatics in the feed or something else?
reduced alkylate end point. Units alkylating higher levels What type of makeup water do you use (BFW, conden-
of propylene in their feedstocks or mixed propylene-butyl- sate, process water), and what is the quality? If the
ene-amylene feeds, and generally those units operating at problem is aromatics, at what level does it occur?
more severe conditions, exhibit the upper end of the
improvements I quoted before. BINFORD:
We are evaluating a new product that is specifically STRATCO has noted, in their experience, that the
targeted at higher acid reduction numbers. In our pilot alkaline water wash will have a tight emulsion when a
plant, we have seen acid reduction in the 25% to 35% surfactant enters the water wash with the olefin feed. Seal
range. We do have a commercial test on-going, and oil and lube oil leaks into the process can also cause tight
another just about ready to start. emulsions. Aromatics, ethylene, or ethyl mercaptan can
all cause a detergent or soap formation in the alkaline
CAIN: water wash at levels as low as 50 ppm in the olefin
We have conducted several trials in two of our plants feed stream.
with alkylation aids. We have been unable to quantify To prevent the formation of solids in the alkaline water
the benefits. So, we are still working with them, and we wash, they recommend that the makeup water contain
will try to get those quantified. less than 20 ppm hardness as magnesium plus calcium
carbonate. Continuous water makeup is required to main-
FOSTER: tain a conductivity in the circulating water in the range
We have done several trials of BetzDearborn’s Alkat of 5000 to 8000 micro moles per centimeter.
XL. We have seen a reduction in acid consumption of
about 9%, and an increase in alkylate yield of 3%. We CAIN:
are not sure that these results are 100% statistically sign)fi- We use clarified water as makeup water, with a total
cant, however. After the final Alkat XL trial, we intend hardness of less than 80 ppm in two plants.
to conduct a trial of the Alkat AR. I think that Mr. Binford
was talking about Alkat AR with the higher reduction in FOSTER:
acid consumption, somewhere between 25% and 30%. Mr. Binford mentioned the 5000 ppm to 8000 ppm
range for TDS. Our utility water happens to run about
MALEK: 4000 ppm, so it is a very good quality and we use util-
The data that I have reviewed on the various catalyst ity water.
systems do indicate that there is some improvement. One Condensate can also be used as makeup water, but the
refiner told me that he thought that a lot of it might hotter it is, the more it tends to absorb hydrocarbon, so
have been attributable to the fact that his engineers were it causes the TOC to go up in the water purge stream.
looking at the unit a lot closer while they were evaluating We also use an antifoam by Baker Petrolite, it is IPC
the use of the catalyst. But I really do believe there is an 5120. We use it at about 2 ppm in the caustic wash
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 133
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drum in order to control the amount of foaming in the check the source of your isobutane. It is probably coming
neutralization section. from the butane isomerization unit stabilizer. This prob-
lem is usually due to an over-injection of chloride in
HENKE: the butane isomerization unit, and to improper stabilizer
We have not experienced foaming problems due to operation. Get the licenser to review your chloride injec-
makeup water quality or aromatics in the feed. We did tion rate and make sure that you are refluxing the stabilizer
have a foaming event that we attributed to high caustic adequately, and thereby reboiling and stripping this tower
concentration in the alkaline water wash vessel. This con- properly. This tower is not an area where you should be
dition was corrected by repairing the makeup water flow trying to save reflux energy.
meter and reestablishing an adequate makeup water flow
rate. We use softened well water as makeup water to the BINFORD:
alkaline water wash. The TDS of this stream is approxi- I agree with all of Mr. Malek’s comments on the chlo-
mately 1000. ride issue. While I was researching this, I did gather a
lot of information on corrosion in the overhead of the
MALEK: depropanizer and in the debutanizer.
You would have to have a fairly large amount of aromat- Corrosion in fractionators of alkylation units is becom-
ics in your feed, probably greater than 2% to 3%, to see ing a more prevalent problem for most refineries. Many
a foaming problem. If you are using reformate to start U.S. alkylation units are running above 110 % of design
up your unit, or as a seal flush, you may have a problem capacity to meet the refiner’s need for alkylate in the
during those times. However, you should also see emul- gasoline pool. The increased loading on the reaction sec-
sion problems in your acid settler emulsion level gauges. tion creates more side reaction products, acids and neutral
esters, and acid carryover. Acids and esters carrying
HERBERT W. WIZIG (Merichem Company): through from the reactor are the most common cause of
For over 10 years, Merichem has operated a Fiber corrosion in the fractionators. Poor mixing and lower
Film娃 water wash system in Aquafining SM service which residence times in the reactor effluent treating section
is downstream of a conventional caustic wash on the allow more of these components to enter the fractionation
alkylation reactor product. We have seen extremely good section. Corrosion in the DIB comes from not aufficiently
results with this service. Merichem recommends that the neutralizing the alkyl sulfates in the water/caustic wash
makeup water to the water wash be steam condensate, upstream. The alkyl sulfates may break down to form tars
boiler feed water, demineralized water or equivalent. The and SO2. The wash needs to be at least 120°F to thermally
total dissolved solids not exceed 100 ppm weight as cal- decompose the dialkyl sulfates.
cium carbonate. Corrosion in the depropanizer on the alkylation unit
is the result of SO2 and SO3 liberation in the fractionation
STEVE MATHUR (Chevron): section. SO2 and SO3 end up in the refrigeration loop
We have found that if you have high TDS in the where they can react with water to form acids. Proper
overall alkaline water wash, higher than 10,000 ppm, you operation and sizing of the depropanizer feed treaters
will tend to carry the alkaline water with the reactor can minimize corrosion. Units without depropanizer feed
effluent to the DIB. treaters are at the greatest risk for severe corrosion. One
Hardness is another matter, however. With hardness, alkylation unit does not operate its depropanizer due to
what you do is foul up your alkaline water exchanger. If this corrosion problem.
the hardness is very high, within three weeks you will Corrosion problems in these fractionators can be effec-
end up cleaning that exchanger on a continual basis. The tively controlled through the use of chemical neutralizers.
only long term solution is to use either condensate or soft Neutralizers can be applied to the feed or the reflux of
water as makeup water to the alkaline water wash. these columns. The neutralizer used in the deisobutanizer
must be nonvolatile at the overhead conditions of this
Question 8. column so that it does not enter the reaction section with
What effects are seen in the DIB operation when chlorides the isobutane recycle. Nonvolatile neutralizers will also
come in with make-up isobutane? Has anyone experi- protect the reboilers in the fractionation section. Neutral-
enced severe tray fouling in the DIB and-or pluggage in izers used in the depropanizer should partition to the
the feed/isobutane recycle coalescer as a result of it? water phase in the overhead accumulator to prevent them
from recycling back to the reaction section.
MALEK: Reboiler fouling in the alkylation unit is typically the
If chlorides are present in your isobutane, you can be result of corrosion problems in the unit. The corrosion
assured you are going to have problems in the DIB col- products can migrate down the column and concentrate
umn. In order to make sure that you do not have chlorides, in the reboilers. Corrosion products can also come in
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 135
TOC/INDEX
STEVE MATHER (Chevron): based on the loss in ignition analysis, with the remainder
In HF alkylation plants, if you have corrosion in the being inorganics comprised of calcium and magnesium
overhead, there is a likelihood of the reboiler steam leaking carbonate. Plugging in the alkaline water wash heater is
through. If the water is reaching the overhead with the usually due to hardness in the makeup water, and thus
fluorides, it will cause low pH. It could be a very small the deposits.
leak that may not be really evident, but we have seen it.
FOSTER:
Question 14. We have found that fouling in the alkaline water wash
Has anyone experienced plugging problems on the flash heater is almost always preceded by an upset in the reactor
drum side of the suction trap/flash drum? If so, what section. If the iso/olefin ratio falls below 7 or if the spent
was the cause and/or solution? Has anyone documented acid strength falls below 88%, we tend to see polymeriza-
a case of hydrate formation? tion in the reaction section, and polymer collection in
the alkaline water wash heater. Our analysis of the material
MALEK:
in the fouled exchanger shows it to be about 60% inor-
If you are getting plugging in the flash drum side of ganic (mostly iron) and 40% organic (mostly C 4 -C 6
the suction trap/flash drum, it can be caused by ice or organic acids, C3-C9 aldehydes, and C6-C8 substituted
hydrates. This happens when water gets into the bottom alkanes).
of the depropanizer. Check the depropanizer operation
and make sure that you are not getting any carryover
HERBERT W. WIZIG (Merichem Company):
from the depropanizer feed treating section, and that you
Merichem recently replaced a conventional caustic
are running the depropanizer effectively.
wash for a major European refiner with a Fiber Film娃
BINFORD:
caustic wash ahead of the sulfuric acid alkylation unit
When a small amount of water is returned to the flash depropanizer. The unit has been on stream less than 1
drum in the depropanizer bottoms, the water will freeze year, but the benefits have been significantly reduced
at the temperatures and pressures in the flash drum, result- caustic carryover resulting in improved life of the trays
ing in plugging of the suction screens for the pumps. The and the reboiler.
solution is to increase the overhead temperature of the
depropanizer—which increases water removal poten- 3. Mechanical
tial—or to increase the pressure in the flash drum such Question 16.
that freezing does not occur. What is the experience on erosion/corrosion of nozzle
tips and candles in olefin feed distributors of alkylation
CAIN:
units? What materials and/or coatings have refiners used
We have had the same problem with water leaking
to prevent this damage? Our unit is equipped with an
into the system from an exchanger.
Alloy 20 spray nozzle on each candle with a tungsten
Question 15. carbide insert. The candle is a carbon steelpipe nipple
Has anyone experienced fouling or plugging in the alka- with a ‘‘greycoat’’ appled. Our unit is fitted with ‘‘Light-
line water wash heater or depropanizer feed heater? If ning’’ turbine type mixers.
so, what was the cause and/or solution? Was any of
the material that fouled the exchanger collected and CAIN:
analyzed? If so, what was the composition? In our Port Arthur plant during our last inspection,
we noticed some slight cracks on the feed nozzles and the
FUSSELL: spider vanes. The impellers were checked, but they showed
We have recently commissioned a caustic wash system no signs of erosion or corrosion.
upstream of the depropanizer on our alkylation unit. It
is actually upstream of the feed heat exchanger prior to 4. General
the depropanizer. We have had a lot of plugging problems
in the heat exchanger as well as in the depropanizer. We Question 17.
are slowly but surely troubleshooting our way out of these What are the panelists’ thoughts on preneutralizing the
problems. We have determined that the plugging has been spray mitigation water? Has anyone used sodium silicate
caused by the caustic salts. in this service?
BINFORD: ROMAN:
Some analysis provided by STRATCO, based on their We think the best approach is to allow the runoff
experience, is that the foulant is typically 50% organics, flow to a nearby impoundment area where it can be
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 137
TOC/INDEX
subsequently neutralized with lime. If there is no local Higher molecular weight sulfur compounds can also
impoundment area adjacent to the unit, we would recom- come through if your Merox system has some problems.
mend installing a pump pit and pumping the overflow Isobutane consumption increases not only from the alkyl-
into a nearby diked area, again, for subsequent neutraliza- ation of the olefin, but also because of the significant
tion. Pre-neutralization would be our last choice due to hydrogen transfer that occurs with amylene. Again, this
its high cost and problems associated with spray nozzle is all a balance between what you really want to do with
plugging. RVP reduction and these other operating costs. The iso-
pentane and normal pentane are going to end up in the
ROBERT E. DAVIS (R.E. Davis Chemical Corporation): gasoline pool anyway. But maybe you would rather have
Years ago, I worked for a company that manufactured them go there with the FCC gasoline as opposed to the
HF. One of the products used for any spills was sodium alkylate, depending on how you are using your alkylate
silicate. It forms a sodium silica fluoride, which is totally for octane optimization.
insoluble and can be swept up and disposed of.
SAMUELS:
Question 18. I like some of the things Mr. Peterson said here. With
What is the current ‘‘best’’ practice for washing the resid- amylenes, of course, you usually have a large amount of
ual H2SO4 from an alkylation unit after draining for turn- dienes which, if not removed, will form light ASO in the
around? Is a neutralizing circulation used, or is deluging alkylating unit. Also, the C5 mercaptans are harder to
with water to the sewer a common practice? If a circulat- treat in a standard Merox unit. Selective hydrogenation,
ing basic water wash is used, what is the typical flow operated to remove sulfur, can have the added benefits
diagram for it, and how is the pH of the water monitored of saturating diolefins and converting 1 butene to 2-
and controlled? butene to improve alkylate quality. So there are some
advantages there. It should also be noted that to get the
CAIN: amylenes, a lot of saturated pentane must typically be
We inject 50 baume caustic into the wash, carefully taken. Normal pentane lowers alkylate octane while iso-
time the wash, check pH to determine whether to add pentane increases the vapor pressure. Also, for refiners
more caustic or stop, and then check to make sure that who have ether units, if you have not prefractionated,
the pH is in a safe and legal range to drain. We dump you are going to make TAME and dilute your ether with
from one settler to another to conserve the caustic. unconverted C5’s.
PETERSON:
We are still using the temperature indication method
in the Ardmore Refinery to control level in our HF regen-
erator. Our Alma Refinery, however, is a little more
advanced than we are on this. They have a radiation
and alarms. The quasi-mass spectrometer pulls ambient system aimed diagonally across the level control region
air into a cleaning and drying system, and actually analyzes of their regenerator, and they have seen some very encoura-
the air. This instrument can detect Zero ppm to 10 ppm ging results from this. They do not overdraw too low, so
of hydrofluoric acid. The philosophy in selecting the sen- they are able to save some acid. They can also stabilize the
sors was to get inexpensive, proven sensors for general operation, because they know where the level is, instead
monitoring, and get a more sophisticated instrument for of waiting for a temperature to indicate-almost like a
monitoring areas which are more likely to experience batch system.
a leak.
SAMUELS:
Question 21.
Now that some of the new vapor suppression additive
In Robinson’s HF alkylation unit, we successfully oper-
systems have started up, what has been the experience
ate a Texas Nuclear fixed source detector level indicator
with their performance?
at the bottom of the acid regenerator. Temperature indica-
tors above and below this instrument act as a backup
HAHN:
system.
In July, 1997, Texaco and UOP completed the latest HAHN:
field test on a new, more cost effective additive called At E1 Dorado’s HF alkylation unit, they also found
Alkaid, at Texaco’s El Dorado refinery. This test was very that temperatures and DP cells were not very reliable.
encouraging. The main objective was to determine the They also have installed nuclear detection devices, and
increased operating costs, if any. There were no substantial have found them to be much more reliable.
increases in operating costs as far as they could determine.
The flash chamber testing of the unit circulating acid Question 23.
sample taken during the additive operation shows substan- For HF alkylation systems, what instruments are refiners
tial reductions in aerosol formation, in comparison to the using to indicate acid settler levels other than sight
circulating acid without the additive operation. glasses and DP cells?
We are very encouraged by these test results, and intend
to conduct a more extensive field test this fall. After a SAMUELS:
successful field testing period, we intend to go commercial At Marathon’s Garyville Phillips HF unit, we use an
with this product next year. OHMART nuclear level indicator to monitor the acid
level in the settler. The instrument continuously measures
LARRY W. SHOEMAKER (Phillips Petroleum Company): the density in the settler and physically travels from the
Phillips started up their reduced volatility alkylation top to the bottom of the vessel about every 1.5 hours.
process (ReVAP) at the Woods Cross Refinery near Salt The instrument plots the density versus level in the vessel.
Lake City, Utah, in early August. Since that time, the The difference in density between the acid and the hydro-
process has worked extremely well. The alkylate product carbons is very distinct making this a very useful level
quality and yields have been observed to be equal to or indicator. To date, the instrument itself has been very
maybe slightly better than that seen with traditional HF reliable, but has been somewhat subject to mechanical
catalysts. The operability and the reliability of the unit problems, due to the physical nature of the instrument,
have been good, with only one minor piece of mechanical e.g., the detector moving up and down.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 139
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We also have purchased and are in the process of installing unit. We used our multivariable predictive control soft-
an Applied Automation FTNIR analyzer. We hope to ware, OPC (Optimal Predictive Control), to control reac-
have that installed by year end. It will model RON, tor weighted-average reactor temperature and inlet tem-
benzene, aromatics, and RVP. Also, in our Port Arthur perature profile by manipulating furnace outlet tempera-
plant, they have been using advanced control since 1985, tures. Furnace tube temperatures are constraint variables:
and are in the process of starting up an on-line optimizer. the controller will attempt to meet the desired temperature
profile through the reactors while respecting maximum
limits on tubeskin temperatures. For optimization, like
PETERSON: the alkylation model I discussed yesterday, we used our
One of our refineries introduced advanced controls in CRO (Closed-loop Reconciliation and Optimization)
the semiregenerative reformer about 10 years ago, and software to perform an economic optimization using a
they have worked quite well. They do inferential octane first-principles, non-linear chemical engineering model of
controls by looking at the WABT, the feed rate, and other the entire plant. The model is in simultaneous equation
variables. They minimize the hydrogen recycle ratio in form, so the same model is used for a full reconciliation
both the reformer side and at the hydrotreater side. They and parameter update, followed by an economic optimiza-
minimize pressure in the reactor section, all, of course, tion. What is unique about this reformer application is
relative to the constraints of the catalyst system. that the model starts at the crude unit atmospheric tower
In the stabilizer system, pressure is minimized to match and includes the hydrotreater and the naphtha splitter.
a predetermined allowable off-gas rate. Reflux ratios and The current crude slate is known, so the optimizer rigor-
pass balancing controls on the towers are used. The big ously calculates the naphthenic and paraffinic content of
the reformer feed and calculates the change in weighted
key to making this successful is to make sure the operators average temperature required to maintain a target octane.
understand what the systems are doing. Operators tend The crude slate changes every 3 days and the octane target
to really get concerned when they see an automatic system changes twice weekly. The optimizer also computes and
start changing the pressure on a tower. implements the optimal feed 95% point on the atmo-
spheric column, and the optimal feed 5% point on the
ROMAN: naphtha splitter. New values are calculated for up to 25
Ashland has had good experience with reformer setpoints and sent to the controllers every 45 to 60
advanced controls. General advanced control design calls minutes. The application has shown high uptimes and
had a payout in the range of 6 to 9 months
for control of the reformate octane by resetting reactor
weight average inlet temperatures against both charge and LEE E. TURPIN (Honeywell Hi-Spec Solutions):
interheater constraints. A bed profile controller maintains Advanced process controls on catalytic reformer units
an operator-entered specification and temperature profiles have been very effective in stabilizing unit operations and
across the bed. Reactor liquid hourly space velocity is pushing constraints such as feed rate, equipment limits
used as a feed forward parameter in reformate octane and carbon make. We have installed on-line closed-loop
predictive controllers. Most success has been found in optimization on several units, including multiple reformer
those systems using Ashland’s NIR on-line technology to simultaneous operations.
measure reformate octane. Some reformers rely upon a I would like to point out that the flat profile of profit
calculated octane value, which is updated with laboratory versus operating conditions may result in an optimizer
values. Optimization parameters include temperature pro- eventually downgrading to just a constraint pusher, some-
file across the beds, final reformate octane, and the amount thing that needs to be watched very closely. I would
of naphtha, which bypasses the reformer to achieve an like to note another problem: we see some optimization
problems have been put on reformers where the unit is
overall octane demand, as dictated by gasoline blending. varying octane as an independent variable, which is a local
The quality of the feed being introduced into the optimization, but it does not fit into the refinery’s general
reformers is also an optimization parameter, which is, of operating plan and results in a non-optimization of the
course, controlled by the split at the dehexanizers or naph- plant. The summer edition of Hydrocarbon Technology
tha splitters upstream of the units. Quarterly contains an article I wrote that reviews the
All of our CCR units have on-line equations which different operating parameters for optimization of reform-
are used to calculate coke on catalyst, which is based upon ers, and includes some economic data on the impact of
an oxygen balance around the regenerator. moving independent variables.
PARIMAL KANTI BISWAS (Indian Oil Corporation Limited):
H. C. KLIESCH (Treiber Controls Inc.): For a semiregenerative type of reformer, with the oil
We have implemented advanced control and on-line, plate heat exchanger, how are feed and effluent leaks
closed-loop unit optimization on a catalytic reforming detected?
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processes. We try to maintain the water level to about making water and deactivating the isomerization catalyst.
15 ppmw to 25 ppmw, and the HCL levels between 1 This is not easy for us to find.
ppmw to 2 ppmw. The ratio of water to chlorine is You can try to Drager tube for CO, but hydrogen in
therefore usually in the range of 10:1 to 25:1. The real the system interferes in the test. So we have actually had
target is to maintain a chloride level on the catalyst to send samples off to places that can find the CO in the
between 0.9 wt% and 1.1 wt% of chlorine. recycle gas.
On the question of type and age, we do not generally
differentiate between catalysts. But there is a difference ANGELO FURFARO (UOP):
on age, since the chlorine retention ability reduces with For semiregenerative operation, UOP generally recom-
age. Therefore, we should maintain a higher chloride level mends effective feed stripping (to less than 1 ppmw H2O)
with a lower ratio of about 20 to 25 for fresh catalyst and injection of 4 ppmw H2O into the feed. This practice
and a 10 to 15 ratio on the other aged catalysts. The normally results in 15 mol ppm to 20 mol ppm H2O in the
targets in the recycle gas stream are dependent upon the recycle gas. Some moisture is recommended to facilitate
type and the age of a catalyst being used. Chloride reten- chloride distribution, but more than 30 mol ppm in the
tion is determined by two main factors: the type of impuri- recycle gas has adverse selectivity and stability effects. The
ties that are in the alumina used to make the catalyst, chloride (HCl) content of the recycle gas depends on
and, of course, the surface area of the catalyst. catalyst type and age, but generally varies from a trace to
For control, it is important to be able to sample cor- 1 mol ppm to 2 mol ppm. The chloride injection rate is
rectly. This calls for a sampling device, or a sample thief, varied according to catalyst type, reactor temperatures,
which can be used to extract samples. Then, the chloride performance indications, experience, and analytical results
levels on the catalyst can be measured, and the operations if made possible by catalyst sampling devices.
adjusted. If there is no sampling device, then the control Cyclic units tend to have high and variable moisture
becomes more of a black art. as a result of freshly regenerated catalyst being returned
As an alternative to sampling the catalyst, normally the to service at intervals. There is rarely if ever a need to
water and chloride levels are controlled by measuring the inject H2O into a cyclic unit. The variability of recycle
water and the HCL in the recycle gas and adding the gas moisture content and varying amounts of chloride
appropriate amount of alcohol and/or chloriding agent. being released from freshly regenerated reactors makes
To achieve a constant water to chloride balance, it is chloride control very difficult and the recycle gas HCl
important to keep a constant moisture level in the feed. concentration highly variable. The catalyst age and type
If the moisture level in the feed varies, then you will also affect the recycle gas HCl concentration. UOP does
always be chasing that water to chloride balance. not design cyclic units.
There continues to be difficulty in measuring or in For CCR platforming units, there is no need to inject
getting instrumentation for proper analysis of the water H2O or chloride into the reactor section, except for periods
content. However, we have to be very careful with the of extended regenerator downtime. The regenerated cata-
instruments requiring re-calibration. With the CCR pro- lyst chloride content is controlled by injection into the
cess, it is not required that a sample has to be taken from regeneration tower to a target value which depends on
the reactor, since a sample can be taken at the regenerator. catalyst type. The spent catalyst chloride content is slightly
This sample device can be mounted on the 4 in. dump lower due to loss of chloride in the reactors. The amount
line. of chloride lost is a function of catalyst residence time in
the reactors, the recycle gas moisture content, and the
PETERSON: reactor temperatures, but is normally relatively small. Nor-
I would agree with the comments and the general mally, there is sufficient moisture from the regeneration
ranges of control and the means of control. I would stress so that no water injection is necessary. Recycle gas HCl
that taking a sample of the catalyst be used to calibrate your concentration depends on catalyst type, catalyst age and
licenser’s recommendations as to correlating moisture and recycle gas moisture content, and can vary from less than
chloride content in recycle gas. It is far better to know 1 mol ppm to as high as 8 mol ppm or 9 mol ppm if
what you really have than to be thinking that you are the catalyst surface area is very low and/or the recycle gas
doing okay. moisture is abnormally high. UOP’s surface areas stable
We had also another case where we had poor stripping catalysts help to limit chloride loss.
of the carbon oxides from the CCR catalyst coming back
into the system. The carbon oxides were apparently under- Y.K. KUCHHAL (Indian Institute of Petroleum):
going the shift reaction and making some water in the The water content of recycle gas for S-R bimetallic
reformer, which was making moisture control more diffi- catalyst is targeted in the range of 15 ppmv to 20 ppmv.
cult there. This carbon monoxide was also getting over For this value of moisture, chloride dosing may be done
to our isomerization unit where it was shifting there and intermittently to maintain chlorine content in the catalyst
at around 1.0 wt%. For recycle gas moisture of 20 ppmv exchangers. I am unaware of a safer or better method at
to 30 ppmv the chloride in the feed is kept at 1 ppmw. this time.
It is further increased to 2 ppmw for recycle gas moisture
of 30 ppmv to 45 ppmv. For higher moisture content in PETERSON:
recycle gas, the reactor inlet temperatures are reduced as We normally wait for a breakthrough in our sulfur
per the advice of the catalyst supplier. When the moisture guard bed. We detect this either with laboratory analysis
content increases, it becomes necessary to look into strip- of the splitter bottoms, the heavy naphtha, which is not
per operation. always real precise at these low sulphur levels that you
In order to meet a minimum target of 15 ppmv mois- see out of a sulphur guard bed. A more reliable test, but
ture in recycle gas, it may be desirable to inject water with a little time lag, is to look for the H2S in our debutan-
with feedstock (3 ppmw to 5 ppmw). Water injection is izer offgas. This gets magnified in the Ardmore Refinery,
done after thoroughly confirming the moisture content because we recycle this gas back to the reactor effluent
of the recycle gas. system for LPG recovery.
As far as catalyst sampling down the bed in the sulfur
SAMIR HALAWANI (Saudi Aramco): guard bed goes, we had installed catalyst samplers designed
What is the latest technology in moisture analyzers on after the method used for the vapor phase reformer catalyst
a recycle gas for a semiregenerative reformer? samplers. This did not work very well on the liquid system,
so we have abandoned use of those.
CAIN: As for chloride traps, we have one on the LPG from
Dupont 560 the reformer going down to the saturated gas fraction-
Sensitivity: 0.5 ppm by vol. ation. That was put in to help control corrosion in the
Accuracy: Ⳳ10% of reading or 2 ppm, whichever is line to the saturated gas and in the saturated gas unit itself.
greater, on all ranges. We probably have grossly oversized this vessel, because it
Repeatability: Ⳳ3% of reading or 0.5 ppm, whichever has run about 3 years, and it was designed for 9 months.
is greater. But the reason for that is probably the difficulty of actually
Calibration: Has a built in moisture generator for cali- pinning down how much HCl is in an LPG stream. It
bration. is not real easy to do that with Drager tubes.
Note: Very accurate, and dependable.
Range: Normal running zero ppm to 50 ppm moisture. TASKER:
Used for normal running on the CRU because of the Well, as you heard, and based on our experience, most
low concentration of moisture in the gas. operators do wait for breakthrough to replace their sulfur
Ranarex Moisture Analyzer Model XMA-72 1 B and chloride guard beds. There are other techniques which
No specifications in the manual on accuracy or repeat- are involved, including monitoring the pickup and so
ability. on, but those methods tend to be somewhat inaccurate.
Calibration: using a separate moisture generator source. Acreon Catalysts has helped to resolve this problem by
Range: 0 ppm to 1000 ppm moisture. allowing companies to have a spare charge of material
The larger range allows us to utilize this meter during on-site at no charge until it is placed into service.
startup. Also, the reading on this meter is usually 5 ppm
to 6 ppm lower than the Dupont meter when the concen-
BARLOEWEN:
tration falls down to normal operations. Plan to replace
this one with a Meeko moisture analyzer. I agree with the comment that most people, in fact all
people that I know, go to breakthrough. I would echo
Question 29. Mr. Peterson’s comment that the debutanizer offgas is a
Do operators wait until breakthrough on their sulfur and real sensitive indicator when you are starting to see sulfur
chloride guard beds to decide when to change out the breakthrough. It is magnified, and you will see a detectable
beds? Is there a better method? change there faster than anywhere else.
HENKE: CAIN:
Our strategy with chloride guard beds is to wait for In Port Arthur, we have two guard reactors in series.
breakthrough. We recently began to monitor both organic Once we spot a breakthrough in the lead reactor, we
and inorganic chlorides using Sensidyne tubes (these are switch to the lag reactor, then change the catalyst out in
model #14L for hydrogen chloride, 0.2 ppm to 40 ppm). the lead. We monitor the Delta T across the second guard
We found that Draeger tubes only detect the inorganic bed as the first line of defense against breakthrough. If
chlorides. This is an important distinction since the the Delta T becomes too large, it is time to change out
organic chlorides also contribute to fouling in hydrotreater the lead guard bed. Furthermore, if the nitrogen in the
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deposition can occur, you need the sublimation curve for of chlorides being carried out of the reduction zone into
ammonium chloride. This is based on the product, of the reactor and on through the system. I believe UOP
course, as I mentioned a minute ago, of the ammonia did modify their design to correct that problem.
and HCl partial pressures. UOP has a good graph of this.
These partial pressures can be reasonably estimated from BARLOEWEN:
knowing the nitrogen content in the reformer feed and I just wanted to put in a pitch to keep the chloride
the HCl concentration in the hydrogen recycle. You check in the reformer via traps, and do not export it to the
where this sublimation condition coincides with the tem- hydrotreater where it is going to cause plugging and corro-
perature conditions in the reformer, then you can deter- sion, as well.
mine where the precipitation will take place. If you are
increasing the nitrogen content of your feed, or if you CAIN:
suffer a nitrogen upset or a chloride upset, this precipita- At our Louisiana plant, our problems show up in our
tion will tend to occur in the cooler regions of your absorber de-ethanizer tower, so we take an opportunity
reformer. to wash our tower whenever we can. At Port Arthur,
As far as pressure is concerned, lower pressure can move the depropanizer is occasionally affected by deposition of
the deposition to the cooler part of the system, and higher ammonium chloride, and we have a caustic wash tower
pressure can move the deposition to a hotter part of the to remove the chlorides in this propane stream.
system. It all depends on where the least painful place to
deposit your salts is. Most of us do not have that much JOSECK:
room to move on pressure, and yield considerations usu- We have noticed problems downstream of the semire-
ally dictate where we run our pressures. generative reformer with precipitation of ammonium
chloride in the stabilizer shortly after start-up and mid-
FUSSELL: cycle. The salts were attributed to high nitrogen in the
We have experienced some ammonium chloride salt feed. The ammonium chloride was removed by injecting
plugging in our refinery on the reformer. The first place water into the stabilizer feed—a very simple procedure.
we have seen this is in our depentanizer on our reformer. We have ammonium chlorides in the recycle during regen-
We periodically have to do an on-line water wash to clear eration which are washed out after the regeneration pro-
this up. It is pretty obvious when we need to do this; the cess. We have not encountered ammonium chloride
tower starts acting up. So we wash it and everything lines deposits in the reformer during the high nitrogen in the
out fairly well. feed associated with salts in the stabilizer. We have ammo-
We have also had problems in our downstream hydro- nium chloride in one of two hydrogen booster compres-
processing units. Specifically, we have a toluene dispropor- sors. The ammonium chlorides are predominantly in the
tionation unit, and the compressor on that unit has a booster compressor operating at a lower cylinder jacket
suction screen. The compressor quit operating—basically temperature. Ammonium chloride problems in the
quit working. We pulled the screen and discovered a good reformer are a nitrogen problem. There are usually enough
layer of salt on that screen. We went back to our reformer chlorides available in the system to react with all the
and discovered that we had some blocked valves around nitrogen in the feed. The temperature at which ammo-
our chloride bed that were partially open, and that we nium chloride sublimes is a function of the concentration
were actually bypassing material around it. Once we got of HCl and ammonia. It is also a function of the water
those blocked in, we no longer had that problem. We in the vapor phase. If the salt is present on the pipe
also periodically feed reformer hydrogen as fuel gas to upstream of the compressor, and if the mole fraction of
our gas turbine. We have also seen some salt deposits on water increases in the recycle, the salt can and does move.
the filter on the fuel gas upstream of that gas turbine. It can vaporize and then form again downstream. As
I believe that the cause for the salt is, as Mr. Foster operating pressure increases, the temperature at which
mentioned, in large part due to the nitrogen in the feed sublimation occurs also increases, thus making the salt
to the reformer. We do not analyze for this nitrogen, so problem worse. In our case, the sublimation is occurring
I would be very interested in hearing about how his in a booster compressor operating at a low temperature.
analyzer works out. I know that we run more nitrogen
in our feed than UOP would recommend, and that is PETERSON:
something that I am going to continue to work on, as Our biggest problem is in the debutanizer stabilizer,
far as getting that nitrogen down. and we occasionally have to do a water wash. On the
As far as the chloride side of it, I believe that the causes water wash, we reduce the temperature so that the brine
of the chloride carrying through on a CCR are more can leave the bottom of the tower. Otherwise, we just
related to the design of the unit. Our particular unit was may rearrange where the salt is if we do not let the salts
designed in the mid-to late 70s, and it does have a problem go out the bottom. When you are done with this, you
want to make sure that you get all of the water out of C5Ⳮ yield benefits have been on average 2 vol% to 4
your overhead receiver, so that you do not have new vol% points over the incumbent catalyst. The hydrogen
HCl coming up and forming a very low pH and highly yield benefits have, on average, been about 150 scf/bbl
corrosive situation in the receiver. to 300 scf/bbl above the performance of the incumbent
We would agree that good denitrification is important. catalyst.
We do not have a real good naphtha hydrotreater. We For lower pressure operation with this catalyst, the
have a 300 psi separator, so we have to be quite careful more the difference is enhanced. In other words, there is
in what crudes we buy and how much nitrogen is in the a greater yield benefit. However, this could be masked
naphtha portion. by more catalyst deactivation by coke which occurs more
rapidly, of course, at the lower pressure. The least that
ROMAN: could be said about the unit operating pressure is that it
We occasionally get problems on our recycle compres- has not affected the RG-582 catalyst yield benefits.
sors due to deposition of ammonium chloride salts. We
will inject a small amount of naphtha on the run to try FLETCHER:
to wash them out or redistribute them. On occasion, we One customer reports recently loading UOP R-72 and
have even used a couple of gallons of water for a wash. having seen a 1.5% increase in liquid volume yield. They
Obviously, that has to be done through a quil so that it feel the catalyst has lived up to its promise.
is properly dispersed.
ANGELO FURFARO (UOP):
HERBERT W. WIZIG (Merichem Company): UOP offers high yield catalyst systems for both CCR
SM
Merichem offers Chlorex technology with a Fiber platforming and semiregenerative platforming units. In
Film娃 contactor to remove hydrochloric acid and ammo- CCR platforming, one unit is operating with UOP’s R-
nium chloride upstream of the stabilizer by means of an 170 series high yield catalyst. This catalyst met perfor-
alkaline water wash. We have four units operating on mance guarantees and matches predicted performance.
CCRs in Japan. The results have been a significant There are now 27 platforming units operating with UOP’s
decreased fouling of the stabilizer trays and the reboiler. R-72 staged loading catalyst system which provides a yield
advantage without sacrificing stability. The expected yield
THIERRY DARDE (Pall Corporation): advantage has been observed commercially. For either
We have installed several of our very high efficiency catalyst system, there is no significant effect of pressure
liquid gas coalescers on the recycle gas line on reformers, on the yield advantage within typical operating ranges.
both in the U.S. and in Canada. Installing these high
efficiency liquid gas coalescers results in dramatically MICHEL ROY (Petro Canada Products):
improved reliability of the compressor by removing the We have been using RG582 for 2 years now. It has
ammonium chloride. lived up to expectations. We have seen the higher hydro-
gen yield. Also, I would like to comment on the robustness
Y.K. KUCHHAL (Indian Institute of Petroleum): of the catalyst. We operated it severely and it still survived.
Ammonium chloride in the recycle gas can deposit It has gone through major sulfur and humidity upsets
in coolers, separators, stabilizers cold trays and recycle and its activity recovered quickly.
compressor creating fouling, under deposit corrosion or Catalyst loading was done using a proprietary catalyst
mechanical problem. It is worth remembering that 0.5 dispenser supplied by the manufacturer. Yield predictions
ppmw of organic nitrogen in the feed leads to approxi- were conditional to this type of loading.
mately 2 tons per year of NH4Cl for a million ton plan. We are presently in our second cycle with RG582.
The regeneration procedure for this catalyst has been
Question 32. simplified compared to our past experiences. The catalyst
Have the high yield catalysts lived up to their expecta- was regenerated successfully and is again performing
tions? What yield improvements have been realized? within the yield projections. These results were obtained
Does the yield improvement decrease at lower pres- despite periods of higher than normal N2 in our feed and
sures? a 15% increase in unit charge. Compared to selectivity
projections, we have seen an increase for certain aromatics
TASKER:
which has benefitted our operation.
There is a publication on the RG-582 promoted bime-
tallic catalyst. This catalyst has been very successful. The Question 33.
publication is by ProCatalyse and Acreon. What are the problems associated with reducing the
This particular publication summarizes the overall pressure in either a CCR or cyclic reformer, and do the
yields obtained. The high yield 582 catalyst has met per- yield benefits justify the lower pressure operation for a
formance expectations in all of the units to date. The gasoline or an aromatics unit?
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in service for 12 years. In 1995, we had a major turnaround We do not have the GC detection method. We use a
on the unit, and we strongly considered pulling these beta particle generator and a little ammeter that measures
exchangers. We actually put together a pretty detailed the electron absorption by the sulfur hexafluoride tracer
plan on how to pull them. But as we got closer and closer in the system. This system had also been used in one of
to the day of the turnaround, we decided against pulling our refineries to find reactor bypass in a reformer. We
them for several reasons. Number one, they would take were able to determine that, yes, we had to get in these
up space, and the equipment required to pull them would reactors and seal the tops of the beds.
also take up space required for other activities during the Our turnaround cycles on the exchangers themselves
turnaround. We made phone calls to UOP and to other are in the 3 year to 7 year range.
refiners and determined that very few people have actually
pulled these exchangers. ROMAN:
So, instead of doing that, we did a pretty extensive Our experience is the same. These are the exchangers
inspection. We did acoustic emissions; we also did ultra- that never get pulled. We have not had any leaks. They
sonics. We removed the insulation and did ultrasonic do not foul.
testing in order to determine that the exchangers were fit One further item on the leak detection, we have used
for service. We have not seen any heat transfer loss on these all three methods: radioactive tracers, helium, and sulfur
exchangers, so we have never really had any requirement to hexafluoride. We stopped using radioactive detection due
pull them for cleaning reasons. to the handling problems. If you have the capabilities, the
sulfur hexafluoride is much more sensitive than helium.
HAHN:
We also have two vertical feed exchangers in service. SAMUELS:
One is 8 years old in our service, and it was a second- In our Robinson refinery, we have not pulled the
hand to us, so it has several prior years service in addition exchangers in their 16 years of service. However, due to
to our service. Another unit has an exchanger that is over loss of heat transfer prior to a spring turnaround this year,
10 years old now. The only problem we experienced was we did try to chemically clean the shell side of these
one leaking baffle, about 2 years ago. Now we inspect exchangers without pulling them. We used a potassium
the bellows about every 5 years during turnaround. There permagenate solution and an acidizing wash. Coming
are manufacturers recommendations for how to pull these back on-line, we actually lost heat transfer. We believe
bundles. We studied these but we decided that we could the problem was due to lack of velocity of the circulating
not justify it, either. We have not seen any heat loss either. solution, and we think we moved some of the deposits
around. So we do, in fact, plan to pull those bundles in
MALEK: the near future. The way we intend to do this is to actually
Our experience with these exchangers with our clients build a superstructure at the unit site and suspend the
has been very good, also. As a matter of fact, one mainte- bundles for cleaning, rather than laying them down.
nance supervisor recently told me that his exchanger had Since the Q&A session, we have pulled and cleaned
already outlasted four refinery managers. these bundles. The primary cause of fouling was tube-
side pluggage of heavy hydrocarbons. The tubes had been
PETERSON: hydroblasted without dropping the tubs and tube-side
We have 17 years of operation on our feed/effluent internals. This is a must for hydroblasting the tubes.
exchanger. We have had three leaks of the expansion Hydrocarbon on both tube and shell sides was poly nuclear
bellows at the bottom end. The first time one was found, aromatics, with a higher molecular weight on the shell
we were successful at weld repair for a while, but that side than on the tube side.
weld repair later failed again. The last time that we had
the exchanger open, we replaced the bellows. We have R. RAJAMANI (Mangalore Refinery and Petrochemicals Ltd.):
never pulled the exchanger to look at the inside of the Did this question address only the non-Packinox
shell or to look at the outside of the tubes. We did do exchangers?
acoustical emissions testing to help us determine that
the shell did not have any active indications (to use an ANGELO FURFARO (UPO):
inspector term). The CCR platforming process unit at Mangalore has
We had some heat transfer loss this last time, and we a Packinox welded plate exchanger. Those exchangers
were overjoyed when we took the dollar plate off the top have, in CCR platforming service, shown excellent non-
to see that we had a bunch of tubes plugged. We were fouling operation.
able to wash that out and get all of our heat transfer back. However, in regard to this specific question, the life
As far as looking for leaks on-line, Mr. Roman pre- of VCFE’s is similar to that of other process equipment.
viously mentioned using the sulfur hexafluoride method. Typical life can extend well past 15 years, but that can
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 153
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be shortened by internal vibration (especially in early some testing on the spent Sulfolane to check the chloride
vendor designs), improper maintenance, corrosion, and content, and then I can compare notes with Mr. Cain.
so on. Inspection generally consists of pulling the shell
cover, dropping the floating head and dye checking the JASON NOE (UOP):
bellows. Exchanger component metal thickness readings Traditionally, UOP has removed chloride from the
are also taken. In fixed bed reforming service, corrosion solvent systems by passing a slipstream of solvent through
can occur at the bottom inside surface of the shell cover single stage vacuum distillation or single stage steam strip-
(a dead area) if this area is not regularly drained during pping. More accurately, we allow mostly chloride salts
regeneration and unit restart. Also, there is another poten- to accumulate in the bottoms material of this type of
tial area for corrosion on the outside diameter of the tubes equipment which is manually removed intermittently.
at the very bottom, just above the floating head tubesheet. UOP recommends the injection of monoethylamine
You can see this without pulling the bundle. UOP does (MEA) to neutralize the acid contaminants that can form
not require the pulling of this bundle unless necessitated in extraction units as a result of the breakdown of the sol-
by process reasons (fouling), or dictated by the regulatory vents.
agencies, company policy or a real need to do so. If the Some operators have used ion exchange to remove ionic
bundle is pulled, proper support of this piece is mandatory species in general from the process units. This appears to
to avoid damage when handling or placing the bundle in be a very efficient method for those who have difficulty
the horizontal position. maintaining a clean solvent stream, but this practice is
not the norm for the majority of process units.
D. Aromatic Extraction A slipstream processing of solvent through activated
carbon has also been pursued by some operators, but this
method, also, does not appear to be widely-practiced, and
Question 37. would tend to produce more solid waste than the previous
What methods are available for removing chloride from two strategies.
a solvent system?
CAIN: E. Polymerization
In our Delaware City plant, we operate a solvent vac-
uum regenerator on a continuous basis to remove chlo-
Question 38.
rides from the solvent. We target approximately 100 ppm
Where is Dimersol catalyst injected, and what ratio of
chloride level in the solvent.
alumina to nickel do you maintain?
TASKER:
In HRI’s sulfolane aromatic extraction process, we do TASKER:
have a continuous slipstream to solvent regeneration. The The Dimersol process uses two different types of cata-
amount that you put through is a function of just how lysts. One catalyst is injected into the feed line and the
well you are controlling your pH and oxygen ingress into other is routed to the recycle stream before entering
the recovery tower. the reactor.
In one of our licensed processes in Japan, we have run The ratio of these catalysts is somewhat proprietary
18 months with water white sulfolane, which is most information, but the range is typically in the order of 12
unusual. It is an extremely tight unit. The two things to 16 on a molar basis.
that affect solvent degradation most are the build-up of The injection points have been changed. Injection is
acidic compounds due to high temperature operation and after the pumparound system at the coldest point of the
the oxygen ingress. You get acidic compounds forming loop. The nickel ‘‘soap’’ is injected to either the suction
quite readily when you have oxygen leaking in. It is often or the pumparound pump or into the feed. The nickel
very difficult to detect the oxygen ingress except by looking ‘‘soap’’ is usually where the highest concentration of pro-
at the degraded solvent that you pull from your continuous pylene in the feed occurs. We have found that quill injec-
on-line regenerator. tion is the best method for mixing. Previous use of static
We generally advocate removal of a small quantity mixers has been dropped from our designs.
every few weeks, like up to 5 gallons, but this is directly
a function of how well you are operating the unit. We PETERSON:
are not specifically looking at the chloride content as such. Our EADC is injected in the air cooled reaction recycle
We are just maintaining good pH control in a carbon or pumparound cooler with the outlet returned back to
steel system, and we see no corrosion. So one thing, based the reactor. Our aluminum to nickel ratio is currently
on the question, that I am going to do is explore doing being run within the range that Mr. Tasker mentioned.
Question 39. minutes every shift through the pumpout line to the
Has anyone had problems with forming sludge in Dimer- caustic treating section.
sol pumparound coolers? If so, how have you con-
trolled it? STEVE MATHUR (Chevron):
What we have found is that sludge is a way of life with
TASKER: a Dimersol circulation loop. I suggest that if you are
Some of our licensees have problems with sludge in the seeing a lot of sludge, and your catalyst consumption is
Dimersol pumparound cooler. IFP and HRI recommends high, especially the EADC, then you probably have a
purging some of the reactor bottom stream to the down- problem with the molecular sieve driers. Check the regen-
stream neutralization section, occasionally, to minimize eration cycle, the state of molecular sieves, the regeneration
the sludge deposits. temperature, etc. That is where we found our problem,
In efforts to improve the overall situation, we are now and were able to reduce the catalyst consumption by half.
proposing a slightly different and new philosophy. We
now look at having the process fluids in the tubes for Question 40.
high velocity. However, this may not meet the client’s How frequently do you check for contaminants (ammonia,
requirements and therefore, we may have water on the water, diolefins) in Dimersol feed? What test methods
tube side in the U.S.A. This is a client choice. are used?
In addition, the design and type of the pumparound
cooler is important. It is important to avoid the dead HENKE:
areas which occur in the box headers in air coolers, since We have an on-line water analyzer that checks moisture
this is where sludge can accumulate. Our experience is in the discharge of our feed dryers. This analyzer can be
that sludge comes from impurities in the C3 feed. The switched to sample the dryer inlet as well. We only check
main contributors are water and dienes and, therefore, for ammonia occasionally with Draeger tubes, and have
driers can be justified. Levels of contaminates which can only had one or two minor upsets with ammonia in the
cause problems are about 5 ppmw with diene and the last several years. Generally, if the water is kept out, the
saturation level of water, which is about 1000 ppm in ammonia will not be a problem.
the C3 feed. So, the solvent needs to be dry. Therefore, We have not detected diolefins in our Dimersol feed.
in start-up procedures, a lot of emphasis is placed on While diolefins are difficult to detect and measure, we
ensuring that the unit is as dry as possible before operation. have found gas chromatography to be a reliable method.
Corrosion has been a problem in the units, as well When testing for contaminants in the laboratory, we
as erosion. use ion chromatography for ammonia, and Karl-Fischer
titration for water.
PETERSON:
We are one of the units that has a problem with sludge PETERSON:
formation. We see it in our recycle cooler, or pumparound We probably do not analyze as often as we should for
cooler. This is an air cooler, so we do have the material some of these contaminants. We do try to control the
on the tube side of the exchanger. About once a year, we amount of diolefins that get into the system by running
have to shut the unit down and clean the cooler, the lines, our C3/C4 splitter in such a way that quite a bit of the
and the reactor. We determine the need to shut down propylene goes down the tower, so that we do not have
by a decrease in recycle flow and a decrease in the cooling a very good chance of getting any of the diolefins going
capacity of the system. up the tower into the Dimersol. We do have driers on
A basket strainer has been installed in front of the the system, and we try to keep the operation of the
cooler, and I do not know how much of a change this depropanizer or the splitter, the drier, the Merox system,
has made to the situation. The cleaning is done by hydro- and the LPG aiming system running very steady, and just
blasting, and because the system is intolerant of water, try to mind our business there to keep the dirt out of
we do a hot nitrogen purge or strip of the system to the system.
get all residual moisture out of the system before we
reintroduce the feed and catalyst. CAIN:
We have on-line analyzers for water and diolefins. We
CAIN: use a Panametrics analyzer for water and a GC for the dio-
We monitor our feed quality for diolefins, sulfur, and lefins.
moisture. We regenerate our molecular sieve driers every
24 hours, and we have lowered our reactor temperature TASKER:
from 125°F to 110°F, which seems to have helped. We I agree with everything that has been said. You can
also blow down our reactors, about 50 bbl/hr, for 5 use an ASTM method to check for ammonia. IFP and
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 155
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HRI recommend testing the feed for contaminants on a attractive revamp opportunity for improving the perfor-
daily basis. For the moisture, the DuPont and Panametric mance of existing oncethrough zeolitic units and TIP
type have been quite good for measuring the moisture in units.
the Dimersol feed. For diolefins, we recommend the IFP
D2-77 method to test the diolefins. Question 42.
Have any refiners experienced excessive yield loss in
isomerization units? To what has this loss been attrib-
F. Isomerization uted?
than 12 pH, they are going to be in trouble in a few a backup system that we use in case something happens
hours, so they change the caustic right then. That has or the laboratory analysis is showing too high a number
worked very successfully for 7 years. We have not had an
additional leak since we started looking at the pH. G. Etherification
Startup procedures are very important to follow, as far
as making sure we get rid of all the water in the system
before we cut the reactors in is concerned. We did have Question 44.
some corrosion in the stabilizer overhead receiver a few What are the experiences with advanced controls on
years ago resulting from trying to start up a little too ether units? What are the key control parameters?
soon. The time you save in starting up is not worth the
problems of having to go back and full weld and change CAIN:
the operation of your unit. We recently installed DMC controllers in both the
MTBE and TAME units, and have had great success in
SAMUELS: controlling these units. The key control parameters are
Concerning corrosion, I certainly agree with Mr. methanol, and optimization of the depentanizer on the
Peterson’s comments on the startup, particularly for the TAME, as well as controlling the purity on both units.
fractionation section. You must get it dried out.
We have had problems in the Penexate rundown piping BRIAN JOHNSON (UOP):
with actual pipe failures. Several producers of MTBE have used advanced pro-
To solve the problem, we use a corrosion inhibitor in cess control (APC) to augment the control of the butane
this rundown line to combat chloridebased corrosion. The MTBE column. The azeotropic mixture formed between
corrosion appears to be caused by trace chlorides in the methanol, the various C4s, and MTBE, enhances the diffi-
stabilizer bottoms where the wet regenerant stream from culty in controlling the separation of the C4s and methanol
the feed driers combines with this rundown stream. Since from the MTBE. APC has been used to adjust the column
we do not see corrosion at dew point in the piping from pressure, the reflux rate, and the reboiler duty. This opti-
the driers to the rundown line, we do not believe that mizes the MTBE purity and minimizes MTBE carryover
the source of chlorides is coming from the regeneration into the overhead.
of the hydrogen driers. The platformer wet gas wash tower
does a reasonable job of removing Penex feed gas chlorides. Question 45.
We are replacing carbon steel with hastalloy in some of What impact does feed sulfur content (particularly
the piping, particularly in the product stabilizer overhead dimethyl sulfide) have on MTBE catalyst life? What solu-
around the water boot area. tions exist for reducing the impact of sulfur in the feed?
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 157
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 159
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Garyville Refinery currently has particulate filtration on in the amine stream is to provide an adequate rich amine
the rich MDEA system plantwide and has had good suc- flash drum upstream of the lean/rich amine exchangers.
cess with 3M bag filters. The Robinson Refinery also uses
3M bag filters upstream and downstream of all the carbon CAIN:
beds in the system. Additionally, it is highly recommended At our Port Arthur plant, we use a 95% MDEA solution
to water wash the refinery fuel gas upstream of your plus 5% of MEA for CO2 control. We try to maintain
fuel gas absorbers to remove impurities such as hydrogen our heat stable salt level below 3 wt%. We are fortunate
cyanide, thiosulfuric acid, naphthenic acids, formic acids, because we have two flash drums in the rich amine return
and oxygen. All of these, of course, form heat stable salts. to the regenerating units, plus two 10,000 bbl rich amine
The problem with heat stable salts, is foaming and fouling. tanks to allow a residence time for any hydrocarbons to
The type of salt that you have in your system will impact settle out. We try to keep the rich amine temperature
the absolute number—the percentage that you can toler- below 120°F to prevent amine stress corrosion.
ate. We typically keep our salt level below 2%, and that
has been reasonably successful for us. There is a lot of FUSSELL:
vendor information on this to guide people. The only thing I would add is the importance of having
When it comes to SCOT amine systems the key is someone in your facility that is responsible for these amine
making sure that you have excess hydrogen on your tail treaters. We are a small facility; we do not have a lot of
gas reactor effluent and no SO2 in that system. When engineers and these units tend to be the last things that
heat stable salts are present, you generally also have degra- people want to worry about. As a result, approximately
dation of the amine in solution. This can cause corrosion 5 to 6 years ago we got ourselves into a tremendous
problems also, and should be carefully considered before amount of trouble with the EPA, because we were not
purchasing reclaimed amine. Our Garyville Refinery has paying enough attention to these units. Since we do not
tried both vacuum distillation and ion exchange reclama- have a large engineering staff, we changed our amine
tion of their amine, on-line. While both work, Garyville supplier and went with Union Carbide. We have seen a
feels that the ion exchange offers advantages when dealing major turnaround in the performance of our amine
with low levels of contaminants, and in controlling the treaters.
reclaiming process.
THOMAS R. BACON (Dow Chemical Company):
We have also tried sodium hydroxide to neutralize heat
We agree with everything that has been said. The points
stable salts. We do not think this was very successful as
are well covered. I would take issue with the question
it does not really remove heat stable salts; it just tends to
itself as it suggests that tertiary amines have more degrada-
make them less corrosive. From our experience, other
tion than primary and secondary. That is not true. From
than the above, corrosion can result from excessive high
a chemical point of view, the tertiary amines have fewer
amine loadings, high temperature, certainly, high velocity,
reactions, and, therefore, should have less degradation.
H2S flashing out of solution, and improper metallurgy.
So, I would suggest that all of the comments made apply
to any amine system no matter who your supplier is or
HENKE:
what you are using.
Fouling caused by corrosion is often controlled by
using special alloy metals, primarily series 300 stainless SAMIR HALAWANI (Saudi Aramco):
steel, in highly corrosive areas. These would include the Could I have some more details on the water wash of
lean/rich exchanger, the reboiler, the reboiler vapor return the tail gas prior treating?
line, the rich amine feed line, and the overhead condensers.
A very important part of reducing corrosion is the proper SAMUELS:
regeneration of the amine. This is especially true when The refinery fuel gas water wash removes impurities
CO2 is present in the system. Target regeneration effi- that cause the formation of heat stable salts in the amine.
ciency should be at least 90% for primary and secondary The contactor is located directly up-stream of the fuel
amines, and at least 95% for the tertiary amines. gas amine treaters. At the Robinson Refinery 2mm SCFH
Heat stable salts in all amine systems, including tertiary of fuel gas is washed with 50 gpm of circulating stripped
amines, are usually caused by acids in the feed stream to sour water in a 26 foot tangent to tangent, 7 foot diameter,
the amine contactor. Water washing is the best method packed column, (1 pall rings are used). Enough make-
to remove most of these acidic compounds which create up stripped sour water is added to compensate for satura-
heat stable salts. tion losses.
Hydrocarbon contamination is best controlled by
maintaining the lean amine feed temperature to the con- MARK O. WIMBERLY (Union Carbide Corporation):
tactor 15°F above the incoming gas or liquid stream. The design of any amine system should include equip-
Another practice to reduce hydrocarbon contamination ment to remove feed stream contaminants, such as water
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 161
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wash towers, coalescers, and particulate filters. Also, the the system after the conversion, and to minimize cost.
formation of corrosion products and heat stable salts can Four vendor proposals were reviewed in detail. UCAR-
be mitigated by eliminating oxygen incursions, but for SOL威 LE713, which is an MDEA with some additives,
the most part, heat stable salts do not result from oxidative was selected because of the projected product perfor-
degradation of the amine. Also, use high quality makeup mance, cost, and Union Carbide’s experience with on-
water and avoid the use of inhibitors and additives that line conversion. Basically, the on-line conversion was a
are incompatible with the amine. Furthermore, Union plug flow exchange of MDEA with MEA. Twelve tempo-
Carbide has technology for removing heat stable salts on- rary tanks were piped up to the system and a 45 wt%
line. This is the UCARSEP威 process which employees solution of LE713 was blended in several of the tanks.
electrodialysis. With respect to hydrocarbons fouling, we In order to minimize mixing in the system, the olefin
usually can control that by skimming the flash and and LPG absorbers were emptied and bypassed and other
reflux drums. system vessel levels were minimized. Pumping rates of
the LE713 into the system and the MEA out of the system
to the remaining tanks were matched. Union Carbide
CHARLES T. ORLANDO (Pall Corporation): had predicted that a measurable pH change would be
Foaming and fouling in amine systems is caused by seen when the LE713 was leaving the unit versus the
hydrocarbons and particulate matter in the system. The MEA. The conversion was successful and safely completed
hydrocarbon itself creates the foam; the particulate in the in 3 hours from the beginning of the swap. There were
system will stabilize that foam and help make it foam no environmental violations, no unit upsets, the resultant
over. By handling it by a two stage approach, namely a MEA quantity was 4.3% of the unit solution after the
high efficiency liquid gas coalescer before the amine sys- conversion.
tem, will allow you to remove the hydrocarbon in its A lesson learned for those who are going to try this,
aerosol form prior to it ever getting into the amine system is not to expect plug flow even if you do the things
and causing the foaming problem in the first place. How- that we have described and try to minimize your system
ever, if it is in there, the removal of the particulate material volumes. Expect a good deal of wasting of your new
will allow the foam not to become stable and, therefore, amine, particularly if you are desiring a low percentage
eliminate a lot of the problems within the system. Usually of the old amine. We would recommend that you hard
if you bring the particulate level down to 1 ppm or less, pipe your temporary piping. You can use carbon steel
it will not stabilize the foam. In every system where we put screwed piping. We had some problems with stainless steel
high efficiency cartridge filters to remove the particulate flex hose; not from the amine itself, but just mechanical
material down to this level, there was no foaming. problems with the hoses. I would just hard pipe it to
begin with.
The expected pH change was never seen, in fact, the
Question 3. greatest pH change that we saw was 0.2, which led to
What has been the experience with using higher capacity more LE713 losses than planned.
amines (MDEA, DIPA) to increase refinery sulfur handling Another lesson learned is that the temporary storage
capacity, and what success have refiners had in convert- tanks that we filled from the unit were filled in parallel,
ing to these amines from non-compatible amine (such just for ease of operation. We should have filled those in
as MEA) on the run? What advice can be shared on the series. Because of the unit mixing, it would have allowed
conversion process? us to segregate the amines as they came out of the unit
for better disposal. The final solution contained 17%
MEA and 14.5% LE713. Although the refiner that was
SAMUELS: scheduled to take the waste amine finally did accept it,
Mr. Bacon may not agree with my first statement make sure that you have a contingency plan if the waste
here, but in our experience high capacity amines tend to amine contains a higher quantity of MEA than you have
perform as advertised. The down side, for us at least, has advertised. Disposing of the amine as a waste could be
been controlling the higher potential losses of the tertiary extremely expensive. And lastly, make sure that you can
amines. Converting from MEA to MDEA on the run operate at these low levels. We did have some problems.
was necessary at the Robinson Refinery in order to take If you push amine levels out of your carbon beds, for
advantage of capital investments we had made to allow instance, you are going to push some hydrocarbon into
the refinery crude sulfur to be raised from a 0.75 wt% to your system, which will introduce foaming. Below is a
1 wt%. The refinery’s objectives in this on-line conversion table which is on 30 minute intervals the percentage of
were no environmental violations or injuries during the MEA and UCARSOL威 LE713 leaving the unit, so that
conversion, no process upsets, less than 5% MEA left in you can get a feel for the extent of mixing that takes place.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 163
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ROMAN:
We have converted most of our reheat burners to steam
reheaters. Where we still have the burners, the reheat
burner itself is the only thing that shuts down, on loss
of flame.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 165
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reliability with it. I am not going to go into all the details CAIN:
of what controls what and what trips what. As has just At our Delaware City plant, our pilot ignition system
been mentioned in the previous two answers, the logic is very reliable. It was put in by Technical Applications
system is independent from our DCS system, with just from Brumal, Pennsylvania. At Louisiana, we use John
the basic information getting back in to the board man. Zink igniters on our SRUs and tail gas treating units. We
We did have one brief shutdown this year, and that was find that they work very well for hot starts, but we have
a short in a 110 volt trip system—bare wire onto conduit. difficulty getting light off from a cold start situation. One
Other than that, we have no problems. common problem is wet fuel gas. Natural gas should be
used, and the system should be checked for water prior
CAIN: to initiating the lighting sequence.
At our Port Arthur plant we use an Allen-Bradley PLC
logic for shutdown and alarming conditions critical to HENKE:
operations. These conditions are then input back to our Yes, there are pilot burners that actually work. I suspect
TDC Honeywell system for alarm summaries and opera- that this question arises from the ignitors, not the pilots
tor notifications. themselves. It is hard to believe that the pilot burner does
not work. We have had very good success with flame-
HAHN: front generator ignitors in our sulfur recovery units. As
I agree with what has already been said on most things. an additional point, we are experimenting with a new
Our shutdown logic is also separate from our DCS system. spark plug type igniter from John Zink which will actually
Having the right bypasses so that you can check the spark in a bucket of water.
shutdowns on-line is very important. That has been our
biggest difficulty, i.e., making sure that our Instrument STEVE FENDERSON (Goar, Allison & Associates, Inc.):
technicians thoroughly understand the system, so that We have had good success also on some plants that
when they say they are going out to check the instruments, use the direct ignition type spark that Mr. Henke referred
they do not accidentally shut you down. We have had a to. In addition to Zink, two other companies that offer
few such accidental shutdowns but these give our opera- that type of unit are Peabody and Forney. There are also
tors a chance to practice restarting the unit. It is usually some European companies.
not too serious a condition for us because we have dual
trains, so we have a little safeguard there. R. RAJAMANI (Mangalore Refinery and Petrochemicals Ltd.):
We have pilot burners in the incinerator which were
Question 8. not functioning properly more due to the sensor problem.
Has anyone found SRU or TGU pilot burners that actually These are of ionization type. Once the hydrogen content
work? We have used several types and are not pleased in tail gas goes beyond 70% then it does not function
with the reliability of any of them. properly. Otherwise the pilot burners are functioning
alright.
FOSTER:
We could have very well asked question number 8. A Question 9.
year ago we were having a lot of problems with pilots. How are sulfur plants protected from overpressure
The good news on that one is in the past year we have caused by higher utility pressures (e.g., nitrogen or
had some success. We found that the stack match DRAM steam purges)? Do units have relief valves on the vessels
(standing for dual range air mix) pilots can be very reliable or exchangers in the reaction zone?
in sulfur plant service. They make a retractable lighter
that has a high intensity spark, but the best feature is that JOSECK:
it has a shielded recessed secondary pilot within the main We have relief valves on the steam and nitrogen header.
pilot. That shielded pilot has its own flame verification, We have a high pressure shutdown on the sulfur plant.
and because of the recessed nature of the pilot the Stack- We do not have relief valves on the exchangers or the
match is much less sensitive to turbulence and much less vessels. The diplegs off the exchangers enter the sulfur pit.
sensitive to improper combustion mixture. Two of our
Claus plants have been retrofitted to Stackmatch, and we MALEK:
plan on having the third Claus unit retrofitted with a I would agree that you would not have relief valves on
Stackmatch at our next shutdown. They light the first the reactors. However you should have relief valves on
time, every time. the utility systems into the sulfur plant. Piping should be
We also have recently installed two Stackmatch pilots protected by relief valves down stream of utility let down
in one of our flares that has been giving us some trouble stations in order to prevent overpressure of the equipment
too, so we are going to see how it works in flare operation. during purging.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 167
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the potential for buildup if you have a failure of your reaction furnaces with cooling between the two furnaces.
sweep system. It improves the safety during loading, trans- While this process has been operating successfully since
portation, and unloading. It removes the odor from the 1990 at KOA Oil in Japan, a new approach has increased
SRU area, from the loading operations, etc. It also can the flexibility and expanded potential applications.
be used to reduce the overall emissions, because some of The API refinery in Italy has been using the BOC
the systems provide the capability of returning the gases SURE Double Combustion process for about one year.
to the process. It lessens the corrosivity of the sulfur itself, However, at API both the #1 and #2 waste heat boiler,
and provides a superior solid product if you are going to and a new #1 sulfur condenser are all housed in the same
solidify the product sulfur. Goar, Allison does have a new vessel. Further, the extended head of this heat exchanger
degassing system that contacts the product sulfur with air also acts as the #2 reaction furnace. Thus, a single skid
in a pressurized vessel outside of the pit. The first of these consisting of a burner, reaction furnace (#1), and the
units has been in operation for over 12 months and has multi pass heat exchanger provide a complete new front
achieved less than 10 ppm residual H2S in the sulfur end to either of two parallel Claus sulfur plants. Either
without the use of a catalyst. plant can be increased in capacity by a factor of 2 to
provide redundancy as well as increased throughput when
JIM LEWIS (TPA, Inc.): both trains are operating.
TPA has designed vapor recovery systems on sulfur Based on the successful operation at API, a major
pits that educt the pit vapors back to the front end of U.S. refiner has elected a similar approach. A new skid,
the SRU which helps reduce the overall emissions from consisting of a new burner, reaction furnace, and multi
the facility, since the H2S is not fed to the incinerator. pass heat exchanger, including a second reaction furnace
Additionally, we have designed pressurized sulfur tanks, in the extended head, will replace the existing burner,
in lieu of a concrete pit, in high water table areas that furnace and reaction furnace. The new facility will have
use tail gas as the sweet medium. That tail gas is then a capacity of 250% of original capacity while maintaining
fed directly back to the feed heater of the tail gas treater turn down to current minimum throughput. This is
for processing. achieved by a fully flexible operation based on air, oxygen
enriched air, or 100% oxygen. Moderate temperatures
Question 11. are maintained in the reaction furnace through all regimes,
What new developments are being applied in the area and the process is easy to control.
of SRU oxygen enrichment technology? In addition to the above, improved burner technolog-
ies, from BOC based on extensive pilot studies and C.F.D.
MALEK: modeling, allows one to enhance sulfur handling capacity
There are quite a few refiners now who are operating up to 70% with a burner change alone.
with oxygen enrichment routinely in the 28% to 30% At the time that the Schendel/Hull response was sub-
range. These installations, primarily, have been put in to mitted (pre-submitted prior to actual Q&A session), BOC
get additional capacity out of existing units. Goar, Allison was not in a position to identify the major U.S. refiner
and Air Products have applied their technology on that will also be using the new Double Combustion tech-
extremely high oxygen enrichments. The Lurgi process, nology. Today, we can tell you that the U.S. refiner is
which has been applied successfully by Pritchard, has Shell Oil. The Shell refinery at Anacortes, Washington,
operated in excess of 60% oxygen. I do not really believe will be using a new variation of the double combustion
that this technology is necessarily competitive compared process. That plant will be fully flexible. It will be able
to conventional air fired plants, if you consider the cost to go from 100% air to 100% oxygen. It is currently in
of oxygen. the design phase. The minimum throughput will be equal
to the current minimum. The maximum throughput on
CAIN:
air will be equal to the current maximum, and the maxi-
At our Louisiana refinery we have been using TPA’s mum throughput on oxygen will be 2.5 times the cur-
oxygen injection technology since 1989 on all five units. rent maximum.
With regard to the request for comments on the use
We have seen a significant increase in capacity as limited
of oxygen in new plants, I can report that we are currently
by front reactor and boiler outlet temperature limits. building a plant in Italy for a gasification project that will
be designed for the use of 100% oxygen from day one.
RON SCHENDEL/RANDY HULL (BOC Gases):
The BOC SURE Double Combustion process allows STEVE FENDERSON (Goar, Allison & Associates):
refinery Claus plants to be expanded to 250% of original I would like to comment further on the Goar, Allison-
capacity, by operating at up to 100% oxygen. Even with Air Products COPE娃 Process. From a refining stand-
high levels of oxygen, moderate temperatures are main- point, I guess this could almost be considered new technol-
tained in the Reaction Furnace (2500° F) by using two ogy. The first unit started up 12 years ago at Conoco,
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 169
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The only problem with lining up to the tail gas unit a Management Systems Review is performed to test our
is that, if unattended, the quench water pH will drop overall compliance with company policies and procedures.
drastically if your SO2 breaks through. So, to prepare for Reviews are addressed in a timely manner. System reviews
this, we go to maximum purge and makeup on the quench are performed by corporate internal auditors.
water, and we maximize ammonia injection. At the same Every three years, Environmental and Safety Industrial
time, we also station an operator at the filters, because Hygiene Reviews are performed. These reviews check
of the scale formation due to pH swings and also the salt compliance with federal, state, and local EH&S regula-
formation that you are always going to have. They change tions. Audit teams are comprised of headquarters EH&S
out filters nonstop for about 15 minutes to 30 minutes. personnel, EH&S personnel from facilities other than
We are normally able to keep that well under control, the one being audited, and, optionally, outside EH&S
and we have had good success with that method. consultants. Additionally, some of our refineries are add-
ing a third level of review which is called self auditing.
STEPHEN BLASHKA (CRI International): Facility EH&S personnel not normally assigned to a given
To reduce SO2 emissions further, you may also consider area audit that EH&S area’s compliance with regulatory
using ex situ presulfurized tail gas catalyst if the catalyst requirements.
is being changed out. One Gulf Coast customer used ex
situ presulfurized catalyst in their tail gas treater and FOSTER:
completed the sulfiding in only 10 hours. Conventional Our procedures are pretty similar to those Mr. Cain
in situ sulfiding, on the other hand, typically takes 24 just mentioned. We have a full time Health, Safety and
hours or longer to complete. During the sulfiding, addi- Environmental (HSE) audit function at LYONDELL-
tional sulfur compounds are being vented to the incinera- CITGO Refining. We employ two full time internal audi-
tor, so if you can complete the sulfiding more quickly, tors who perform about 12 HSE audits a year, and they
it will help reduce emissions on start up. work off of a 5 year audit plan which is updated annually.
The things they cover are not just the strict compliance
JAMES STONE (Louisiana Department of Environmental Quality): with particular rules, but also they cover areas like manage-
With Title V coming on line, why do you not take ment system issues, procedures for the management of
the permit and describe the startup that you want, of this HSE, accountability structure, and organizational struc-
unit in the permit? Then make it a permit condition to ture. Each audit follows a written protocol that is devel-
start it up in the sequence that you want it started up oped and approved before the audit begins. Audit findings
for safety. That eliminates the problem of being out of are then published in a final report which identifies a
compliance during the startup. responsible individual for each and every finding. Usually,
this individual is a plant manager level. The HSE audit
B. Environmental Management group also maintains a tracking system which is reviewed
by senior management and executive management once
Question 13. a month.
Beyond the required recordkeeping and reporting
requirements, what approach does your organization use HAHN:
for performing internal audits to check regulatory compli- Texaco also has a 3-year cycle auditing program that
ance of environmental and OSHA regulations? we go through. The first year we conduct a corporate
compliance Environmental Health and Safety audit, and
BARLOEWEN: this is done at a site. It takes about one week, and 8 to
I am going to comment on this from a catalyst manufac- 10 people are involved in the audit. There are 6 or 8
turing perspective. We do not have a regular schedule for from corporate headquarters, two from another location
conducting internal audits. We do, periodically, hire an that is not being audited, and then the plant’s own EH&S
external consultant to do an audit of our own activities department personnel. In year 2 of the cycle, we do a
in the environmental field. And, we have even used a management systems assessment, similar to what Mr. Fos-
local university and had them use us as a class exercise ter was speaking about. That is completed with three
to do an audit. people from headquarters, and they also come for a week
and work with the plant. Then in year 3, we do a facility
CAIN: site assessment. This is a smaller group of corporate audi-
Our organization uses a two tier approach for Environ- tors who come in and help. We also review recently
mental, Health and Safety (EH&S) compliance reviews. completed multimedia audits and their findings, hoping
We perform EH&S Management Systems reviews, and to learn from them, pick up some different techniques,
EH&S Compliance Assurance Reviews. Every two years, or what is a more acceptable manner to stay in compliance.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 171
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 173
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FUSSELL:
BINFORD: We work with Scaltech Industrial Services to recover
Information given on the sludge in question indicates our solid waste. The end result is that it is sent to a
that it is a water continuous slurry. Discounting the water, cement kiln. The solid waste is collected and it is sent
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 175
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charge heater which is all radiant heat transfer. I wish I climates, the proximity of the sweet fuel gas knockout
could tell you that I had skin thermocouples before and drum to the furnaces must also be considered. Other areas
after and tell you what the difference is, but we came for consideration in reducing burner tip fouling include
close to this. We installed skin thermocouples and we particulate filters and optimized burner tip design.
have a sister heater in the same cabin and the side that
is coated is noticeably dark, and the side that is not coated
is bright from all the material on the tubes, the old ash BINFORD:
and scale. So, it appears as if the coating has done some I think Mr. Henke covered most of the points. Most
good from emissivity and heat transfer. Even if it has not of this fouling, when we get involved in a system like
done some good that way, the exercise of sandblasting this, is either coming from upsets in the amine system or
the tubes and putting a ceramic coating on probably is from iron sulfide scale sloughage that is not properly
going to keep them from oxidizing again. So, in that caught in dip legs, knockout pipes, or trash pipes. It is
standpoint, we view that as being successful. Skin thermo- very important that these ‘‘catch’’ systems are operating
couples between the coated heater and the uncoated heater properly and that they are periodically maintained. Good
show a difference of about 100°F between the two, both housekeeping practices in the amine unit, which are cov-
on the peak temperature and average temperature with ered in detail in the amine section, are a real key to
the coated heater being colder. We are considering doing keeping your fuel gas systems clean. If these measures
some additional heaters in the refinery to help even out are still not effective, chemical antifoulant programs can
heat flux, as well as improve efficiency in the heaters. So effectively mitigate the deposition of trace contaminants
far it looks like it has been successful for us. at the burner tips. This is one area of the refinery where
antifoulants have been used successfully for clean-up pur-
ASHUTOSH GARG (Furnace Improvements): poses. For a program to be successful, it needs to be
As a designer of fired heaters, refractory emissivity does tailored to address the fouling mechanism, specifically
not figure anywhere in the radiant section calculations. based on deposit analysis. We usually use deposit analysis
We have changed the refractory lining of several heaters rather than fuel gas analysis, because, most of the time,
from castable to ceramic fiber, and the radiant section fouling is incidental in nature, so that a spot fuel gas
performance was never affected. But, coating on ceramic analysis will not give a representative indication of the
tubes will definitely make some minor differences, because true fouling components.
emissivity of the tubes does come into play.
CAIN:
LLOYD WINGER (Conoco Inc.): We are in the process of installing fuel gas filters at
We have installed ceramic coatings on four heaters: each heater down stream of the fuel gas knockout drum.
reformer feed hydrotreater reboiler crude feed and coker We are addressing our amine carryover problems as well.
feed. We have observed more heat transfer in the radiant
section. However, the net benefit is difficult to quantify
due to numerous other changes to the process units HAHN:
involved. Very similar to Mr. Cain’s answer, we feel that most
of our fuel gas plugging problems were related to amine
Question 25. problems, and we are addressing those. But, we also put
What experience has the industry had with magnetic in filters on our fuel gas system, and that took care of
devices installed in furnace fuel gas piping to improve the problem very nicely for us in most cases.
heater efficiency?
Question 26. RONALD BREDEHOFT (KTI Corporation):
What are refiners doing to control or eliminate fouling In addition to what the panel has addressed, I would
of burner tips? We suspect that most of the fouling results add that some of our clients have insisted on a 3/32 in.
from amine system carryover. minimum drilling on their burner tips to avoid or mini-
mize this plugging.
HENKE:
Complete separation of amine from fuel gas is a critical
element in elimination of burner tip fouling. Most of our CHARLES T. ORLANDO (Pall Corporation):
fouling events can be traced back to poor amine contactor I would just like to add to the panel’s discussion that
operation. Much can be done to improve the separation a high efficiency coalescer will take either the hydrocarbon
of amine from fuel gas in the sweet fuel gas knockout or the amine, or both, down to levels less than 0.01 ppm,
drum. Proper distribution of the inlet stream and installa- and the particulate levels down to 0.3 micron absolute.
tion of coalescing devices are just a few. In cold weather It is very important to protect the burner tips.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 177
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Question 27. soot blowers can be loud during their cycle. The soot
Has anyone tried controlling fuel gas flow to process blower vibration frequency should be selected to fit the
heaters on a mass basis (software CEMS or other techno- application. Two infrasonic soot blowers were recently
logies) to compensate for rapid fluctuations in BTU con- installed in the superheat section and economizer section
tent to the furnace, or to better measure actual fired/ of a 200,000 lb/hr 600 lb steam CO boiler on Robinson’s
absorbed duty, or emissions impact ? catalytic cracker. Actually, this was done in 1994. Low
frequency soot blowers were selected because they do a
FOSTER: better job at removing particulates. Previously, we had
In some services, we do use a calorimeter value as a two retractable 600 lb steam soot blowers in the superheat
feed forward into a temperature controller for duty control section, and 12 smaller fixed 150 lb steam soot blowers
application. We do not use CEMS, but we are using in the economizer section. The steam soot blowers caused
PEMS, predictive emissions monitoring system. In fact, problems with opacity spikes, steam drum level upsets,
we are implementing that even as we speak on our new and occasional tube failures due to tube impingement.
crude unit and on our new coking unit heaters to comply The infrasonic soot blowers generate a low frequency
with new permit requirements. This technology can accu- 22 hz wave for 60 seconds every 2 to 3 minutes. This
rately predict emissions and is recognized as a viable tech- provides a multidirectional effect knocking catalyst off
nology by our regulators in Texas. the tubes, even upstream of the fire box section of the
The step testing is expensive because we were required, boiler. Tube cleaning is more effective; opacity spikes
as part of the step testing, to run at less than optimum and drum upsets have subsided, and required equipment
rates on the heaters in order to gather the emissions data maintenance is less compared to the old soot blowers.
that were required for predicting the emissions. But, I Vibration has not been a problem, even though the boiler
expect that the predictive system is going to be a cheaper, skin is very thin in the economizer section. One hundred
more cost-effective, and more accurate system in the long psig plant air in a surge tank drives the soot blowers.
run, because it will require less maintenance and it will The blowers themselves consume 1000 scf/min in the
be more reliable. incinating mode and 200 scf/min in the idling mode.
One lesson we learned in the installation of these soot
HAHN: blowers is that you do want, particularly in the CO boiler,
At one time, we had a relatively sophisticated control to put a knife valve between the horn of the blower and
system on our fuel on one of our new heaters. It had the boiler itself for maintenance, because you have positive
BTU on-line analyzers which are based on chromatograph draft there.
results, but we found that the on-line analyzer loop feed-
back was too slow to keep up with the changes in the ROMAN:
fuel gas composition. So, the feed forward was not effec- We have installed sonic soot blowers in both the air
tive. We could never get it tuned properly, so we finally preheater and the radiant section of one of our large crude
abandoned that whole system. We do, however, under- heaters. A small high frequency sonic soot blower operated
stand that lately some people are now putting mass meters at 150 hz to 250 hz in the air preheater and it was
on their fuel gas system, and are using them, apparently successful, but its effective cleaning area was limited. The
successfully, to control their fuel gas. You may want to talk large low frequency sonic soot blower operated at 20 hz
with some of the suppliers of those types of instruments for in the radiant section and dislodged and damaged refrac-
specific examples. tory in that heater. We have also tried sonic soot blowers
on the dirty side of a pulse jet bag house module, and
CAIN: severe bag damage occurred.
We have feed forwards on our fuel gas gravity and feed
gas flow, as well as the steam flow. These feed forwards 2. Exchangers
work well for us.
Question 29.
Question 28. What is the experience with twisted tube heat exchangers
Are there any new developments in soot blowing? What and with tube inserts? Has anyone had success with
has been the success with continuous sonic soot these in crude oil service?
blowers?
HENKE:
SAMUELS: The twisted tube experience base is rapidly expanding.
There is a distinction between sonic soot blowers and Over 135 twisted tube heat exchangers have been sold
infrasonic soot blowers in that infrasonic soot blowers by Brown Fintube in the past three years. Twenty-nine
operate at a frequency below audible sound, while sonic of these have been sold to refiners; 18 of the 29 are
currently in service. All of these are performing as pre- improves the service U-value. The measured total fouling
dicted, or slightly better. actors on many crude versus diesel and HVGO pumpar-
One refiner, this year, put six twisted tube bundles in ound exchangers is in the range of 0.02 to 0.05 hr/btu-
a high fouling overhead condenser service to increase ft2-F.
capacity, reduce fouling, and improve cleanability. They A major concern with the inserts are their impact on
pulled one of the bundles after 90 days in service; no crude charge hydraulics. In principle, the inserts should
fouling was detected. Ninety days had, historically, been have less pressure drop in a fouled condition than a fouled
their cleaning interval with the conventional tube bundles. exchanger without inserts. This assumes the mechanism
The track record on these has convinced Koch Refining of fouling is not salt, inorganic deposition, or other hard
to utilize twisted tube technology in crude service. fouling material. Downstream of the desalters the filter-
We are planning to install eight twisted tube bundles able solids, ‘‘dirt’’, and salts should be low relative to the
in crude service early next year in our own refineries. whole crude. A caution in using the insets is when the
The tube bundles were designed to fit within existing crude charge hydraulics are limiting without the inserts.
exchanger shells. These replacement tube bundles will There is no margin for increased pressure drop. If parallel
provide an on-line increase of unit capacity, and improve exchangers trains are available, then the inserts can be
vacuum gas oil yield through increased heat transfer effi- tested in one of the services.
ciency and reduced pressure drop on both sides of the
exchangers. We expect to see a 30% increase in heat Question 30.
transfer, a 90% reduction in shell side pressure drop, and What best practices are used to track crude preheat
a 25% reduction in tube side pressure drop. exchanger fouling rates? Are any adjustments made
based on projected run lengths between turnarounds?
SAMUELS: What techniques are being used currently to reduce
I have data from four refineries, five applications in all, exchanger fouling?
which indicate that the projected or design heat transfer
performance for each application was exceeded for these BINFORD:
refiners. As a matter of fact, in one case, the refiner Regarding the first part of the question, we consider
achieved up to three times the original heat transfer with the best practice we consider for monitoring crude preheat
no increase in surface area. Each application was used in exchanger fouling rates to be either heat duty or U coeffi-
a different service, and they were initiated for different cients for each separate exchanger. Obviously, in some
reasons. Two were initiated to reduce fouling, and that crude preheat configurations, the instrumentation is not
was achieved. In four of the five applications, the pressure there to do such a detailed analysis. Alternatively, monitor-
drop also exceeded the prediction, as well as the heat ing across the whole train and then verifying with heater
transfer. None of these applications were in crude service. inlet temperature, (corrected for flow and feedstock) can
In our Garyville Refinery, we are installing some twisted also be effective. This can be accomplished by either
tube exchangers in our FCC debutanizer overhead conde- inclusion of the heat transfer parameters on the DCS
nsors, and, as Mr. Henke mentioned, we are able to install system itself, or automatic data dump to a dedicated heat
these in the existing shells which significantly reduces the transfer calculation package on a remote PC terminal. If
investment. The design numbers indicate that we should this is not practical, then manual data entry of the heat
get a twofold increase in duty, from 12 million btu/hr transfer parameters can be put into a number of software
to 22.8 million btu/hr with a surface area increase of packages designed for monitoring of crude preheat transfer
25%, a mass flow increase of 27%, and an overall heat parameters. We have developed our own programs that
transfer coefficient increase of 30%. include linear, exponential, polynomial, and neural net-
works to curve fit historical data into a predictive modeling
ANDREW W. SLOLEY (Process Consulting Services Inc.): monitoring tool, these can be supported by either DCS,
Exchanger inserts have been used for several years to remote PC, or inputting the data by hand.
improve the exchanger service U-value. In a recent case Regarding adjustments made during the run, this is
we are familiar with the inserts were used in both diesel very typical. Those adjustments may be made based on
pumparound-to-crude and the HVGO pumparound-to- crude slate mix, such as the asphaltene content of the crude
crude services. The inserts were on the crude side of the slate. Other considerations, such as amount of caustic
exchangers. The inserts increase the heat transfer through injection in the desalted crude if caustic is used, and
two mechanism. First they create more turbulence and desalter operations are very critical. BS&W and filterable
reduce the fouling factor. Since crude side fouling controls solids in the desalted crude are two key variables. Finally
the service U-values on most of the crude preheat there is the monitoring of the program with a heat transfer
exchangers, the major effect of the inserts is reduced foul- model to have an ongoing idea of what your fouling curve
ing. Reducing crude side fouling by 50% significantly looks like.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 179
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Answering the last part of the question, the first tech- start-of-run and design data to predict heat exchanger off-
nique being used currently to reduce exchanger fouling line cleaning for turnarounds. The preheat train hydraulics
is mechanical. Installation of redundant heat exchangers limit run lengths before thermal performance. This is
is one option, if only a few exchangers are fouling on a due to excess heater capacity from improvements to the
consistent basis. Installing blocks and bypasses on critical preheat train configuration efficiency. Run lengths on the
exchangers to allow on-line cleaning without unit shut- preheat exchangers have been significantly extended by
downs is certainly another option, if you can do this improving desalter operations and limiting vaporization.
effectively without limiting throughput because of a pres- We did find that without double blocks and bleeds we
sure drop or crude furnace duty limit. Redesigning criti- were not able to take exchangers off when we redesigned
cally fouling exchangers to run at higher velocities and the crude preheat train to verify the previous comment.
minimize solids deposition may be another option, if
solids deposition due to low velocities is one of the causes MALEK:
of fouling. (When evaluating this option, it is important With respect to the monitoring of exchanger perfor-
that you are not just moving the problem down stream.) mance, this is sometimes complicated by the fact that the
Also, the erosion potential of running at higher velocities crude slate is changing and the fluid on the other side of
should be considered. Turbulent vibrators have been the exchanger is also changing due to the changing product
installed in exchangers to knock loose fouling material, but slates. I would recommend that your engineers use the
we have seen some problems with these devices actually simulation programs that are out there, such as Hisym,
providing a trap for foulant to accumulate on. Covered and Sim-Sci, and the Aspen programs. They do an excel-
in the previous question, was installation of twisted tube lent job of rating exchangers rigorously. They can deter-
bundles which seems to be an up-and-coming technology. mine heat transfer coefficients for changing fluid condi-
Regarding the process, optimizing the crude slate mix tions across the exchanger. It is thereby possible to monitor
to avoid crude incompatibilities is important, as are opti- the heat transfer coefficient and implied fouling rates very
mizing desalter and caustic injection rate. Finally, the use accurately. It is also beneficial to track the pressure drops
of chemical antifoulant programs has been proven to be in addition to the fouling rates.
very successful in controlling fouling and maximizing run
lengths with minimum capital investment. A.W. KRUEGER (Spirelf System):
We have had the Spirelf exchanger insert systems intro-
CAIN: duced in the U.S. for about 8 years now, initially on a
I do not have much more to add to that, except that test and trial phase. In the meantime, there are about 10
we are using HEXTRAN to track our fouling rates in refineries in the U.S. and Canada that are using this
one of our refineries. We are also using antifoulants in system. Typically, it is being used in the hot part of the
two refineries with good success. preheat train, so this is of particular interest to what has
be described by some operators as being a problem area.
FUSSELL: In principle, there are two effects from the system. One
On very rare occasions, we will reduce the rate on our is that you reduce the fouling; you have, typically, a tube
crude unit, and when we do, we have the ability to take side fouling reduction of about 80%. By virtue of the
some of our exchangers off-line in order to maintain fact that our system is a moving and not stationary system,
sufficient velocities in the exchangers that are still in ser- you also create a higher turbulence in the flow. That, in
vice. We also designed our newest crude unit with the itself, can about double the inner heat transfer rate. As a
ability to take exchangers out of service on-line for clean- consequence, you have less fouling, you have better heat
ing as Mr. Binford discussed. Our biggest problem has transfer, you have, as a primary effect, improved energy
been in our hot section of our preheat train. Taking these efficiency or energy savings.
exchangers out of service on-line has been a disaster. There are also two other aspects that come into play
Blocked valves will not hold, and it takes forever to actually when looking at those systems. One is, when there are
get the exchangers out of service for cleaning. We have limitations to furnace capacity, that by better heat transfer
a turnaround coming up in 1998, and we are going to you can maintain your crude flow rates over a long time.
actually install double block valves hoping that they will The second point is that simply by reducing fouling you
allow us to block in these exchangers on-line for cleaning. can eliminate several cleaning operations. Some refineries
have to clean exchangers maybe once a year. By using
JOSECK: inserts you might be able to extend your run time to 3,
We continuously trend heat exchanger heat transfer 5, and in some cases even 7 years. Additional aspects
coefficients in upper level software from the DCS for that should lead a refinery to consider the inserts are:
the crude preheat train. Exchanger pressure surveys are enhancement of crude throughput capacity. This can be
routinely completed once per month and compared to achieved by increasing the crude inlet temperature
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 181
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is economical to carry out a cleaning, although the require a field survey. These are rarely performed, there-
global pressure drop is reasonable and allows a fore, a true test of anti-foulant effectiveness is typically
regular throughput of crude. not performed. Prior to using a long term anti-foulant
c) The reaching of the end of the life time of the program (they are expensive) a rigorous field test should
devices when fouling is not very high. As for any be conducted. The rigorous field test will determine anti-
spring, there is a fatigue of the device and an over foulant effectiveness.
stretching could then occur. Life time depends on
the material (our special alloy has the best resistance 3. Steam Systems
against fatigue) and on the localization of the
exchanger. On the hotest exchangers, life time is Question 31.
shorter due to higher temperature and to the even- What consultants and software programs are available
tual fluid hammer coming from water vaporization. to aid refineries in optimizing and controlling refinery-
The cycle duration is generally multiplied by 2 some- wide steam systems? Please include on-line/real time,
times by 3, which translates to 2-3 times less cleanings, optimization programs, as well as ‘‘design’’ support.
as indicated in the following summary:
SAMUELS:
Cleaning frequency Service time of Spirelf devices
Marathon contracted with Veritech to develop an
before Spirelf or new cleaning frequency if
Excel-based steam system model called ‘‘ESTEAM’’. The
equipment chemical cleanings are not
model is linked to the refinery plant information system
used
to collect data. The model is not truly a real-time model,
6 months 1 year to 1.5 years (depending but can be run on intervals using archived plant data.
on the tube diameter, the We use the model for case study work, and to evaluate
fouling degree. . .) different operating configurations. Veritech’s ESTEAM
program is a powerful steam simulation program for
1 year 2 years minimum for carbon
Microsoft Excel which brings unprecedented levels of
steel and stainless steel devices;
steam system analysis to the spreadsheet environment.
2 ⳮ3 years for special alloy
Using rigorous steam property data add-ins based on the
devices
ASME 1967 Formulation, and Excel’s powerful built-in
18 months 3 years for carbon steel and data base and VBA capabilities, complete steam systems
stainless steel devices; 3 years can be constructed without having to manually construct
minimum for special alloy heat and material balance equations. These are all handled
devices automatically with the model formulation. Systems with
unlimited number of users and process units can be han-
R. RAJAMANI (Mangalore Refinery and Petrochemical Ltd.): dled automatically for sites with up to six major steam
They recently used Sim-Sci flowsheet model for check- pressure levels. Sites with greater complexity can be
ing the fouling of exchangers in the preheat train, and quickly customized.
we were fairly successful in predicting the fouling. When- The model performs rigorous heat and material bal-
ever we had to clean it we lowered crudes and then came ances at all levels and allows full flexibility for specifying
down on load and isolated stream-by-stream. We then condensate return, flash steam, blowdown and deaeration
cleaned both the shell side and tube side and were suc- schemes, letdown arrangements and desuperheating con-
cessful. figurations—all automatically, without the need to manu-
ally construct the balance equations.
ANDREW W. SLOLEY (Process Consulting Services Inc.): Included in the economic module is the ability to
The total exchanger fouling is calculated by a rigorous specify boiler efficiency vs. load profiles and operating
heat exchanger network model using measured exchanger logic to more accurately model actual boiler house fuel
temperatures. Typically, the exchanger fouling factors will consumption. Important ancillary boiler costs for services
increase to 80% of their end-of-run fouling factor in about such as boiler feed water (BFW) an make-up water pump-
30-60 days from start-up (after exchanger cleaning). Also, ing, forced draft fan operation, BFW chemicals and cool-
exchanger pressure drop will increase from the start-of- ing water costs for condensing turbine surface condensers
run pressure drop to approximately 150-200% of the are also included to more accurately reflect true steam
clean value. Once the water wash system and desalter generation costs.
performance is optimized, the two means to reduce fouling The interactive user interface uses build in forms and
are anti-foulants and inserts. When testing the effective- dialog boxes to make input of steam system details very
ness of anti-foulants, both the fouling factors and pressure simple. An interactive drill-down feature for program nav-
drop should be measured. Pressure drop measurements igation provides a multi-layered viewing capability ranging
from a complete system overview, to individual plant have different steam levels, different steam costs, and if
units to individual steam users. you have ever had the pleasure of presenting a capital
The steam functions included with the model can be budget to your executives and tried to explain why you
utilized with any Excel workbook and feature 52 steam are using different steam costs for four different refineries
property functions together with functions to calculate you will appreciate what I am saying. It provides you the
steam turbine power from steam rate, turbine steam rate technical backup for that.
from power, turbine outlet conditions, and deaerator Lenhoff-March also has developed a steam system mod-
water make-up and steam requirements as native Excel eling program called ‘‘Steam 97’’ which is available com-
functions. mercially. It is somewhat similar to Veritech’s bon services
Options include an additional cogeneration module are not as reliable. On average, these machines are available
featuring built-in gas turbine performance characteristics, for operation in our refineries all but two days per year.
off-design performance prediction, and heat recovery A five year average for maintenance costs is $6,500 per
steam generator performance simulation and rating capa- machine. This is mainly due to seal work and occasional
bilities. overhaul of the last stages in the turbine. The return on
Additionally, Veritech has an excellent steam costing investment is good, provided the turbin is sized properly.
program. It provides a true thermodynamic cycle evalua-
tion of steam use and associated costs. The steam is classi- CAIN:
fied by path between the generator and user, and by the We had a terrible experience with one of these turbines,
type of user, such as live steam, heat, or work. What I like and removed it from the unit. Safety was the major con-
most about this software program is that it is a universally cern. We had a seal failure where H2S gas was released, and
applicable engineering tool. Every refinery is going to we had many mechanical problems and high maintenance.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 183
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 185
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counteracts the higher olefins yield. This is done by reduc- There was a very good article published on this subject
ing the pressure drop from the reactor to the compressor, just recently in Hydrocarbon Processing by J.V. Albano
normally by packing the main fractionator. On the other and K.M. Sundaram with ABB Lummus. This appeared
hand, lowering the overhead receiver temperature reduces in the July 1997 Hydrocarbon Processing.
the wet gas rate as well. This can be achieved by modifying
the main fractionator heat balance or changing its design, Question 4.
such as by installing a top pumparound in the tower to How much advantage in selectivity have some of the
unload the overhead condensing system. newer acetylene removal catalysts shown in commer-
For the gas concentration unit fractionation towers, cial operation?
the higher internal vapor and liquid loads can be handled
TASKER:
with high performance trays. This is generally more eco-
nomical than building new columns or packing existing IFP has promoted LD catalysts that bring significant
columns. The heat integration between the pumparounds ethylene selectivity. These catalysts are supplied by Acreon
in the main fractionator and some of the gas concentration in North America and ProCatalyse outside of North
unit reboilers also results in the need to adjust the heat America. As important as the catalysts, process set up and
balance or redesign some of the sections in the main operating conditions allow you to maximize catalyst cycles
fractionator. and yields. IFP has developed a new process named
‘‘Acetex,’’ and, in this process the bulk of the acetylene
hydrogenation is carried out in the mixed phase reactor.
B. Ethylene As for the MAPD hydrogenation, the liquid phase
washes the catalyst, dissolves oligimers as they are formed,
Question 3. therefore stopping the polymerization catalyst fouling.
What new techniques are being developed to minimize The liquid phase is obtained by a liquid solvent readily
coking in the new generation ethylene furnace techno- available in a petrochemical complex. The Acetex is partic-
logies? ularly attractive for feeds containing high acetylene con-
centrations of about 1.5 wt%. Ethylene yield increases in
MALEK:
the range of about 1%, can be achievable. Existing units
In the new generation ethylene furnaces, the continuing could be revamped to the Acetex process with modest
trend in the design has been: raising temperatures, lower- investments.
ing the pressure drop, and shortening residence time. MALEK:
Thanks to metallurgical advances, tube metal tempera- Just to reinforce something along the same lines, the
tures in pyrolysis furnaces now are in the range of 2000 ° high severity operations have increased acetylene yields
to 2100°F. As is well documented in the literature, there up considerably in pyrolysis furnaces. Proper acetylene
are certain catalytic effects that occur inside the tubes at hydrogenation is very critical. These new catalysts have
these temperatures. These catalytic effects lead to coke the selectivity to hold the formation of the green oils to
formation and more frequent decoking cycles. There have a minimum level. This will extend the catalyst life. I think
been alloying techniques, sulfiding techniques, and other this is one of the more important advances that has been
approaches to minimize these effects. made recently.
I would like to comment on one of the design efforts
that are being worked on for minimizing coking. Since Question 5.
the coking rate goes up dramatically as temperatures rise, What is the best way to ensure that pyrolysis gasoline
the ability for coke to form can be minimized by shorten- does not carryover into the water used in the dilution
ing the residence time. It is very important that dead zones steam system in an ethylene plant?
be completely eliminated in the piping and transition
sections. There has been some interesting work in chang- BINFORD:
ing the geometry of the various piping tubes, manifolds, The quench water/oil water separator or settling drum
transition sections, and entries into the transfer line should remove virtually all of the pyrolysis gasoline from
exchangers to accomplish this. There are sophisticated the quench water used in the dilution steam generator.
computer analysis tools now available that can do three Proper operation of the quench settling drum will mini-
dimensional flow analysis inside of these tubes. These mize breakthrough. Pyrolysis gasoline quench water emul-
analyses allow the geometry to be modified such that the sions that will not resolve on their own in the quench
velocities can held to extremely high levels. All the dead settling drum can be resolved by feeding a small amount
zones, for all practical purposes, are eliminated. This will of reverse emulsion breaker, typically less than 5 ppm,
go a long way toward minimizing coke formation and into the quench water feeding the separator. These chemi-
extending the life of the run on the pyrolysis furnace. cals are typically net cationic solution polymers. The use
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 187
TOC/INDEX
188 Memorandum
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PANEL BIOGRAPHIES
ALEX E.M. BARLOEWEN—Executive Vice President, Haldor Topsoe, Inc., Houston, Texas.
Alex joined Haldor Topsoe in 1996 as Vice President of its Refining Technology Division
responsible for worldwide licensing and design of Haldor Topsoe Hydroprocessing Technology,
and is currently responsible for Haldor Topsoe’s North American subsidiary. He previously
worked for Fluor Daniel as Executive Director, Process Engineering, and for Unocal in operating,
planning and engineering assignments. His final Unocal Refining assignment was as General
Superintendent of Operations at the 150,000 bb/d refinery in Nederland, Texas. Alex received
a Bachelor of Applied Science degree in Chemical Engineering from the University of British
Columbia.
❖ ❖ ❖ ❖ ❖
❖ ❖ ❖ ❖ ❖
❖ ❖ ❖ ❖ ❖
RAY FLETCHER—Regional Technical Service Manager, Akzo Nobel Catalysts, Houston, Texas.
Ray is responsible for providing technical support in the FCC catalyst division of Akzo Nobel
Chemicals. This includes unit monitoring, optimization, trouble-shooting, and training on the
FCC. Ray spent the first seven years of his career with Texaco Refining & Marketing Inc. and
the Shell Oil Company. He has worked as a process engineer on most refinery units including
the fluid catalytic cracker, catalytic reforming, hydrotreating, alkylation, catalytic polymerization,
and LP modeling. Ray holds a Bachelor of Science degree in Chemical Engineering from the
University of Washington.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 189
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❖ ❖ ❖ ❖ ❖
BECKY L. FUSSELL—Operations Support Supervisor, Fina Oil & Chemical Company, Port
Arthur, Texas. In her current position, Becky is responsible for providing technical service to the
Port Arthur Refinery. She joined Fina in 1982 and has held various assignments in technical
service, process control, and process design. She holds a Bachelor of Science degree in Chemical
Engineering from Lamar University and is a registered Professional Engineer in the State of Texas.
❖ ❖ ❖ ❖ ❖
❖ ❖ ❖ ❖ ❖
❖ ❖ ❖ ❖ ❖
BEN L. MALEK—Executive Vice President, PCI International, Inc., Houston, Texas. Ben has
30 years of experience in the energy and processing industries, which includes 29 years in
management consulting and related engineering design. He has been involved in project manage-
ment, engineering and procurement for over 30 major process construction projects. Prior to
joining PCI, he served as a Senior Process Consultant with The Pace Company, and an operations
Manager/Process Engineer with Dow Chemical Company. Ben holds a Bachelor of Science degree
in Chemical Engineering from the University of Texas.
❖ ❖ ❖ ❖ ❖
❖ ❖ ❖ ❖ ❖
❖ ❖ ❖ ❖ ❖
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 191
TOC/INDEX
PARTICIPATION INDEX
Abbott, Jim, 88, 91 Fletcher, Ray, 13, 31, 33, 45, 47, 50, 53, 54, 57, 58, 61,
Albert, Brian D., 23, 77, 79 65, 66, 68, 70, 71, 86, 93, 104-107, 109, 110-112,
Allen, Elizabeth, 117, 129 114, 116, 118, 119, 121, 123, 126-128, 146, 149,
Alverson, Ed, 10 156, 171, 174, 176, 184
Anderson, Sidney, 62 Foley, Richard, 129
Arndt, John, 97 Forero, Patricia, 174
Azzouz, Ziyad, 71, 146 Foster, David, 9, 14-16, 20, 21, 26, 27, 29, 34, 36, 39,
Bacon, Thomas R., 83, 161, 163 43, 46, 71-74, 80, 86, 93, 100, 101, 106, 107, 114,
Barloewen, Alex, 12, 28, 83, 86, 87, 89-91, 96, 98, 99, 119, 121, 130, 133, 135-137, 147, 151, 166, 167,
104, 105, 110, 111, 116, 118, 122, 124-126, 128, 169, 170, 178
143, 148, 152, 170, 176 Fredrick, Cyndie M., 12, 16
Fritsche, Ray, 96
Bartholic, David B., 55, 56, 59
Furfaro, Angelo, 152, 144, 149, 151, 153, 158
Biggs, Donald, 41
Fussell, Becky, 17, 33, 34, 36, 43, 49, 62, 71, 86, 102,
Binford, Mark, 9, 11-15, 18, 19, 22, 24, 25, 27-30, 34, 107, 110, 114-116, 124, 126, 131, 132, 135-138, 142,
41, 44, 49, 54, 67, 68, 72, 76-78, 81-83, 92, 96, 99, 143, 146, 148, 150, 152, 156, 161, 174, 175, 180
124, 127, 130, 132-137, 152, 159, 167, 173, 175, Garg, Ashutosh, 74, 177
177, 179, 184, 186 Gray, Stuart, 151
Birnbaum, Rick W., 160, 164 Grieb, Ben, 120
Biswas, Parimal Kanti, 141 Hadjiloizou, George, 123, 126
Blashka, Stephen, 170 Hahn, Suzanne, 24, 31, 32, 34-36, 38, 39, 41, 44, 58,
Bothe, Michael, 28 70, 74, 75, 78, 90, 93, 99, 103, 106, 107, 111, 115,
Bredehoft, Ronald, 177 118, 120, 121, 123, 130, 135, 139, 147, 153, 163,
Brunson, Ross, 90 165-167, 170, 174, 177, 178
Cain, Glenn, 9, 14-16, 18, 22, 25, 29, 31, 33-36, 38, Halawani, Samir, 18, 49, 51, 66, 72, 96, 142, 145, 160,
43-45, 47, 49, 56, 58, 61, 62, 65, 66, 68, 73-75, 78, 161, 163, 174
79, 83, 86, 87, 89, 93, 98, 100, 105, 106, 116, 119, Haley, John, 71
121, 122, 124, 129, 130, 133, 135, 137, 138, 140, Halford, Tom, 23
143, 145, 146, 148, 152, 154, 155, 157, 161, 163, Hallauer, Greg, 131
164, 166, 168, 170-173, 175, 177, 178, 180, 183 Harrell, Jack, 78
Canziani, Carlos, 25 Hart, Brian, 32, 34-36
Chlapik, Ken, 90 Hartley, Daniel, 37, 44
Choy, Ed, 80 Hartman, Edward L., 185
Cuadros, Elkin Carmona, 14, 23 Harvey, Craig, 95, 101, 117
Cullon, Lana, 55, 63 Heimbaugh, William, 9
Darde, Thierry, 68, 97, 130, 146, 149, 152 Henke, Kevin, 15, 23, 31, 33, 36-38, 43, 44, 47, 49, 58,
Davis, Robert E., 138 61, 65, 73, 75-78, 81, 84, 89, 94, 104, 106, 108, 110,
Dergregorian, Heros, 59, 68, 146, 147 118, 124, 125, 131, 134-136, 142-145, 155, 159, 161,
DiCamillo, David, 105, 128 164, 166, 169, 172, 177, 178
Higgins, Terrence, 23, 68, 80, 88, 90, 125, 146, 158,
Dougan, Tim, 59
171
Dreyfuss, Corey, 174
Hill, Randy, 168
Eaton, Paul, 82 Howerton, Amanda, 15, 17
Elvin, Frank, 55 Hunter, Mike, 121, 127
Fahey, Bill, 29, 31, 96 Johns, Bill, 103
Fearnside, Paul, 10, 15, 97 Johnson, Brian, 140, 147, 156, 157
Fearon, Eric, 88 Jokubaitus, Linas, 43, 128
Fenderson, Steve, 165-168 Joseck, Eric, 11, 12, 20-22, 25, 30-32, 35, 37-39, 43, 44,
Ferrall, Kevin, 152 53, 60, 64, 85, 89-91, 94, 101, 104, 106, 108, 110,
Fischer, Steven M., 38 112, 119, 120, 121, 147, 148, 166, 171-173, 176, 180
Fisher, Paul, 143 Juno, Edward F., 28
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 193
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 195
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Topic Index
1997 NPRA Q&A Session on Refining & Petrochemical Technology
ADDITIVES Hydrotreating Procedure for Unloading Spent Cat.; Dry vs. Wet 115-97
Cloud Point Experience With Depressants 41-97 Hydrotreating Uptake of Silica on Catalyst 104-97
Desalter Fouling of Preheat from Emulsion Polymers 9-97 Isomerization Performance of High Activity Systems 155-97
Gasoline Sulfur FCC Cat. Additive to Reduce 70-97 MTBE Effect of Sulfur on Cat. Life; Ways to Reduce 157-97
Heavy Crudes Polymers to Process without Diluents 10-97 Particle Length Minimum Average Length for Reactor 105-97
HF Vapor Suppression Additive 139-97 Poly Unit Where Cat. Injected in Process 154-97
Pyro. Gasoline Anti-Polymerant Blends 184-97 Presulfiding Criteria for Choosing Spiking Agent 111-97
Tight Emulsions Breaking in Heavy Crudes 10-97 Spent Catalyst Audit Trail for Recycling 176-97
Use Control Metering Pumps; Other Methods 30-97 Spent Catalyst Recyclers 176-97
Reactor Loading Level of Refinery Engineering Supervision for Job 107-97
AIR POLLUTION CONTROL Reactor Loading New Developments in Dense Loading 108-97
H2 Plants Organic Contaminants in CO2 Vents 172-97 Steam Reformer Chlorine Guard for Low Temp. Shift Cat. 89-97
MACT II Technologies for Reforming & FCC 172-97 Waxes For Color Improvement 19-97
NOx Emissions Reduce FCC Throughput to Cut Emissions 51-97
NOx Emissions Way to Reduce from FCC Regenerator 50-97 CHARGE STOCKS
NSPS Vapor Recovery Control System 171-97 Base Oil For Saturate Levels 22-97
Passivation Effect on SOx, NOx Additives 55-97 Co-Processing Crude & Condensate 19-97
Separators Use of Floating Covers for API Separators 171-97 Deasphalted Oils Hydroprocessing Routes for DAO & Blends 126-97
Steam Reformer Methanol Emissions & Way to Control 90-97 FCC Feed Impact on Yield of Diesel In Feed 65-97
Gas Condensate Problems When Processing 40-97
ALKYLATION HCGO Conditions, Problems When Hydroprocessing 121-97
Corrosion In Alkylate Splitter Tower Overhead System 136-97 High Sodium VGO Dealing With 12-97
H2, H2SO4 Acids Water Content of Circulating Acid 132-97 Naphthenic Crudes Dealing With in Downstream Units 13-97
Optimization Results With Kinetic & Statistical Computer Models 33-97 Naphthenic Crudes Effect in Downstream Units 13-97
Software For Optimization 33-97 Nat. Gasoline Problems When Processing 40-97
—HF ALKYLATION —FAILURE
Acid Settler Instruments to Indicate Settler Levels 139-97 Furnace Steam Reformer Heater Tube 87-97
Amylenes Problems Caused When Alkylating 138-97
Eductor New Alternative to Pumps 140-97 CHEMICALS & CHEMICAL ELEMENTS & METALS
HF Regenerator Instrument to Control Level in Column Bottoms 139-97 Chlorides Removal from Aromatic Extraction Solvent 154-97
HF Vapor Vapor Suppression Additive 139-97 Mercury In Crude Oil; Problems 24-97
Pumps Magnetic vs. Sealless 140-97 NH4Cl Deposition During Cat. Reforming 148-97
—H2SO4 ALKYLATION Nitrogen In Cat. Reformer Feed 147-97
Acid Wash Testing for Acid in Effluent 135-97 Presulfiding Agents Criteria For Choosing Spiking Agent 111-97
Acid Wash Troubleshooting Electrostatic Precipitator 135-97 Sulfides Amount Causing Copper Strip Failure 18-97
Chloride Corrosion, Fouling in DIB 134-97 Sulfides Coping With Contaminated Naphtha 18-97
Co-Catalysts Benefits of Using 132-97 Sulfur Recovery O2 Enrichment Developments 168-97
Distributors Erosion/Corrosion in Olefin Feed Distributors 137-97 Sulfuric Acid Metering Transfer of Spent & Fresh Alky Acid 130-97
Effluent Benefits from Treating With Bauxite 136-97 —SULFUR & MERCAPTANS & SULFUR COMPOUNDS
Feed Coping With Light Ends in Feed 131-97 Mercaptan Treating Oxidizing with NH4 17-97
Feed Freeze Problems With Recycle Iso-Olefin Feed 130-97
Feed Levels of Light Ends That Can Be Tolerated 131-97 CLAY TREATING
Foaming Causes of in Alkaline Water Wash System 133-97 Design Criteria Clay Life, Disposal 12-97
Foaming Causes of in Spent Acid Tanks 135-97
COKE (COKE PRODUCTION)
Fouling In Heaters 137-97
Antifoam Threat to Coker Naphtha HDT 104-97
Hydrogenation Selective Units: Product Strippers or Flash Separators 131-97
Cycle Times Lower Limits; Time for each Activity 79-97
Neutralization Preneutralizing Spray Mitigation Water 137-97
Drum Life Period & Effect of Operating Factors 72-97
Plugging Flash Drum Side of Suction Trap 137-97
Drum Inspection Tools & Prediction of Repairs or Remaining Life 73-97
Probes To Determine Acid Level, Acid/Hydrocarbon Ratio 133-97
Foam Control Grade Silicone Antifoam & Type Carrier Oil 77-97
Space Velocity Experience Running 0.6 Olefin Space Velocity 139-97
Foam Control Non-Silicone Antifoam 79-97
Sulfuric Acid Metering Transfer of Spent & Fresh Acid 130-97
Fouling Results & Use of Antifoulant in Preheat Train 82-97
Washing Acid ‘‘Best Practice’’ for Washing Residual Acid From Unit 138-97
Fractionators Grid/Structured Packing; Results, Objectives 79-97
Run Length On-Line Spalls 74-97
ANALYSIS (TESTING & ANALYTICAL METHODS) Run Length Period Achieved & Ways to Increase 73-97
Aromatics Reduction Ways & Accuracy for VGO, Diesel Units 109-97 Sludge Fouling Ways to Stop It 76-97
Cat. Reforming Analyzer for Moisture in Recycle Gas 147-97 —DELAYED COKING
Copper Strip Test Failure Due to Sulfide in Naphtha 18-97 Decoking Tubes Pigging vs. Stream/Air; Results 74-97
Crude Assay Sources & Quality of Assays 44-97 Drum Pressure Ways to Reduce 77-97
Gasoline NIR for Blend Certification 30-97 Drum Pressure Yields, Liquid Distribution at Lower Pressure 76-97
In Crude Injection Not Feasible to Prevent Fouling 19-97 Feed Highest Concarbon Feed; Heater Run Lengths 80-97
Moisture H2O in Cat. Reformer Recycle Gas 145-97
Nitrogen Detection in Cat. Reformer 147-97 COKING (FOULING)
Poly Unit Testing for Contaminants in Feed 155-97 Antifoulants Results & Use, In Coker/Visbreaker Preheat Trains 82-97
Ethylene New Techniques to Reduce Furnace Coking 186-97
ASPHALT
Emulsion For Dust Suppressant 22-97 COMPUTER CONTROL
Processing Various Schemes 22-97 Alkylation Unit Kinetic & Statistical Computer Models 33-97
Data Software Reconciled Data for Plant, Units, & Accounting 31-97
CATALYSTS Process Control DCS Instrumentation & Extent of Control 36-97
Acetylene Catalyst for Removal 186-97 Reconciled Data For Information, Monitoring & Optimization 31-97
Alky. Co-Catalysts Benefits of Using 132-97 Scheduling Software Tools & Their Benefits 35-97
Cat. Reforming Performance of High Yield Catalysts 149-97 Training Operators Using New Process Control Systems 39-97
Cat. Reforming Target Chloride/H2O Levels in Recycle Gas 143-97
CCR Cat. Density Grading to Recover Contaminated Cat. 143-97 CORROSION & EQUIPMENT PROBLEMS
CCR Cat. Ex Situ Regeneration of ‘‘Heel’’ Cat. 143-97 Alky Unit In Alkylate Splitter Tower Overhead System 136-97
Cobalt Moly Cat. Big Deviations in Recommended Volumes for H2 Plant 89-97 Amine Plant Causes 161-97
Ex Situ Presulfided Avoiding Exotherms in Large Units 114-97 Cat. Reformer Stress Cracking in Regen System 152-97
FCC Best Deactivation Simulation 70-97 Crude Oils Effect of Crude Compatibility 14-97
FCC Metal Contamination, Strategies to Combat 54-97 Crude Oils Strategy to Address Naphthenic Acids 15-97
FCC Reliability of MAT, Fluid Bed, & Pilot Plant Tests 69-97 Diesel Desulfurizer Causes of High Corrosion in Exchangers & Heaters 97-97
FCC Slurry Settling, Removal, Disposal 67-97 Diesel Desulfurizer High Rates in Exchangers & Heaters 97-97
FCC Strippers Design Conditions & Evaluating Performance 63-97 FCC Monitoring Methods, H2 Permeation 71-97
FCC Strippers Design, Operations, Performance, Revamps 60-97 H2 Plant Stainless Steel Cracking 83-97
FCC Strippers Important Cat. Variables in Stripping Hydrocarbons 61-97 H2 Plant Ways to Reduce 83-97
FCC ZSM-5 Levels, Limits, Conditions, Results 68-97 Heater Erosion Reason For, Material to Cope With 14-97
H2 Stripping Procedure in Preparation for Dumpting 106-97 Hydroprocessing On Alloyed Reactor Effluent Exchangers 99-97
Hydrocracking Catalyst Type Decrease Cracked Gas Formation 123-97 Hydrotreating Bed Plugging 92-97
Hydrocracking Cat. Experience With Ex Situ Presulfided 114-97 In DIB Chloride Problem 134-97
Hydrocracking Pretreat Experience With High-Activity Cat. 111-97 Isomerization Salt Deposition & Corrosion 157-97
Hydrotreating Influences of Size, Shape on Activity & Pressure Drop 110-97 Lube Extraction NMP Corrosion Treatment 22-97
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 197
TOC/INDEX
HYDROTREATING REFORMING
Aromatics Reduction Ways to Quantify; Accuracy for VGO, Diesel Units 109-97 —CATALYTIC
Bed Plugging Factors that Cause 91-97 Catalyst Performance of High Yield Catalysts 149-97
Bed Plugging Feed Filtration & Devices to Minimize 91-97 Chloride/H2O Target Levels in Recycle Gas 143-97
Bed Plugging Ways to Minimize 91-97 Controls Experience With Advanced Process Controls & Optimizers 140-97
Bed Temp. Guideline for Setting in Multi-Bed Reactors 118-97 Corrosion Stress Cracking in Stainless Steel Regen Systems 152-97
Catalysts Uptake of Silica on Cat. 104-97 Effluent Leaks Leak Detection 141-97
Coker Naphtha Percent in Mix With Diesel Treated 117-97 Extraction Way to Remove Chloride for Aromatic Extraction Solvent 154-97
Unloading Cat. Procedures; Dry vs. Wet 115-97 Feed Exchanger Life of Vertical Combined Feed Exchanger 152-97
H2 in Feed Ratio to Reduce Fouling in Exchangers 123-97 Guard Beds When Sulfur, Chloride Guard Beds Changed 145-97
Resid Ⳮ VGO Processing to Produce FCC Feed 128-97 H2 Purity CCR Process Add-Ons to Further Improve 143-97
Waxes Catalysts for Color Improvement 19-97 H2 Purity Variables That Can Improve 143-97
H2 Recycle Effect of Heavy Hydrocarbon in H2 146-97
INCINERATION ‘‘Heel’’ Catalyst Density Grading to Recover Contaminated CCR Cat. 143-97
Caustic Experience With Caustic Incineration 174-97 ‘‘Heel’’ Cat. Ex Situ Regeneration 143-97
Moisture Analyzer for Moisture in Recycle Gas 147-97
INSPECTION Moisture Analyzers for H2O in Recycle Gas 145-97
Hydroprocessing Methods for Piping In & Out of Reactor Effluent Coolers 101-97 NH4Cl Where Deposition is Problem; Effect of Pressure 147-97
Nitrogen Analysis for Level in Feed 147-97
INSTRUMENTATION (METERING, MONITORING, & CONTROL) Pressure Benefits of Lower Pressure in Cyclic & CCR Units 149-97
Cat. Reformer Advanced Process Controls & Optimizers 140-97 Salt Build-Up Ways to Control in Recycle Compressor 151-97
Chemical Additives Methods to Control & Optimize 30-97 Vent Gas Scrubbing CCR Regeneration Vent Gas 158-97
DCS Instrumentation Extent of Process Control 36-97 —STEAM
Etherification Advanced Control & Key Parameters 157-97 Chlorine Guard Protection for Low Temp. Shift Cat. 89-97
HF Alkylation Acid Level in Regenerator 139-97 Desulfurizer Big Deviations in Recommended CoMo Cat. Volumes 89-97
HF Alkylation Instruments to Indicate Settler Levels 139-97 Furnaces Ways to Avoid Overheating 87-97
Sulfur Plant Claus & Scot Unit Shutdown 165-97 Methanator High Temp. Trip Strategy With Aging Catalyst 88-97
Methanol Emissions Levels & Ways to Monitor 90-97
ISOMERIZATION Sulfur In Feed Ways to Monitor 89-97
Catalysts Performance of High Activity Systems 156-97
Salt Ways to Cope With Deposition & Corrosion 156-97 SAFETY & INDUSTRIAL HYGIENE
Yield Loss Caused by Benzene Destruction, Prevention 156-97 Sour Water Tank Overpressure, Containment 37-97
Sour Water Tank Rupture Precautions 37-97
JET FUEL
Caustic Treating Life of Clay in System, Disposal 12-97 SLUDGE
Dimersol Problem in Pumparound Coolers 155-97
KEROSENE
Color Precursors Role of Merox Process 11-97 SLURRY
Color Precursors Ways to Reduce 11-97 Disposal Ways & Technologies to Dispose of 175-97
Color Problem Reasons & Solutions 29-97 FCC Cat. Settling in Slurry, Removal, Disposal 67-97
Naphthenic Acids Maintaining Quality With Acid Crudes 15-97
SOFTWARE
LUBE OILS (AS PRODUCTS) Reconciled Data Uses for Data 31-97
Base Oils Saturate Levels & Feedstocks 22-97 Steam Software & Models for Refinery-Wide Optimization 182-97
Hot Waxes Catalysts for Color Improvement 19-97
Light Neutrals Addressing Volatility Specs 20-97 SPECIFICATION
Light Neutrals Volatility Specifications 20-97 Volatility In Light Neutrals 20-97
NMP Losses, Decomposition & Corrosion 22-97
START-UP
MATERIALS Steam Reformer Monitor Heater Tubes in the Field 87-97
Acid Corrosion Metallurgy to Cope With 14-97
STEAM
MATHEMATICAL MODELS Optimization Programs for Refinery-Wide Systems 182-97
FCC Application, Feasibility of Cold Flow Modeling 63-97
LP Planning Checking Accuracy 33-97 STAFFING
Steam Optimization Refinery-Wide 183-97 Work Processes Teams & Operator Tasks 39-97
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 199
TOC/INDEX
References
The next several pages provide a list of references by ‘‘U.S. refiners must increase alkylation capacity to meet
subject from the publications Chemical Engineering, demand,’’ Oil & Gas Journal, Aug. 22, 1994, p. 49.
Hydrocarbon Processing, and Oil & Gas Journal. The Sub- Rhodes, Anne K., ‘‘Searches for new alkylation catalysts,
ject Index for the References is organized as follows: processes forge ahead,’’ Oil & Gas Journal, Aug. 22,
1994, p. 52.
I. Alkylation
Rhodes, Anne K., ‘‘New process schemes, retrofits, fine tune
II. Hydrocracking
alkylation capabilities,’’ Oil & Gas Journal, Aug. 22,
III. Catalytic Cracking
1994, p. 56.
IV. Hydrotreating/Hydrorefining
Sheckler, John C., Ross, Larry J., and Comey, Kenneth R.
V. Reforming
III, ‘‘New process additive reduces HF cloud-forming
VI. Treating and Desalting
potential,’’ Oil & Gas Journal, Aug. 22, 1994, p. 60.
VII. Crude Distillation
‘‘Refining Processes ’94,’’ Hydrocarbon Processing, Vol. 73,
VIII. Petrochemical
No. 11, Nov. 1994, p. 83.
IX. Delayed Coking
‘‘Alkylation safety major topic at Oil & Gas Journal semi-
X. Environmental Controls
nar,’’ Oil & Gas Journal, Jan. 16, 1995, p. 33.
XI. Instrumentation, Product Blending, and
‘‘Petrochemical Processes ’95,’’ Hydrocarbon Processing,
Quality Control
Vol. 74, No. 03, Mar. 1995, p. 89.
XII. Miscellaneous
Dobis, J.D., Clarida, D.R., and Richert, J.P., ‘‘Survey reveals
XIII. Lube Oil and Waxes
nature of corrosion in HF alky units,’’ Oil & Gas Journal,
XIV. Maintenance
Mar. 6, 1995, p. 63.
XV. Piping
‘‘Portuguese refiner starts up new gasoline complex,’’ Oil &
XVI. Furnaces & Heat
Gas Journal, Mar. 13, 1995, p. 95.
XVII. Storage and Transfer
‘‘European gasoline survey shows decreasing lead, MON,’’
XVIII. Corrosion
Oil & Gas Journal, Oct. 2, 1995, p. 77.
XIX. Energy Conservation
‘‘New HF detector accepted for use by refining consortium,’’
XX. General
Oil & Gas Journal, Feb. 19, 1996, p. 46.
XXI. Light-Oil Cat Processing
‘‘Pilot-plant results in on fixed-bed alkylation process,’’ Oil
XXII. Isomerization
& Gas Journal, Apr. 1, 1996, p. 69.
XXIII. Aromatics Extraction
‘‘NPRA Q&A—2: Catalyst issues stir interest at technology
XXIV. Visbreaking
meeting,’’ Oil & Gas Journal, June 24, 1996, p. 45.
XXV. Hydrogen Production
Rao, Pradip, and Vatcha, Sorab R., ‘‘Solid-acid alkylation
XXVI. Sulfur Plant Operations
process development is at crucial stage,’’ Oil & Gas Jour-
XXVII. Polymerization
nal, Sept. 9, 1996, p. 56.
XXVIII. Hydrogen
Schneider, Donald F., Musumeci, Joseph, and Chavez, Rick,
‘‘Analysis of alky unit DIB exposes design, operating
I. ALKYLATION
considerations,’’ Oil & Gas Journal, Sept. 30, 1996, p. 41.
Pescarollo, E., et al., ‘‘Etherify light gasolines,’’ Hydrocarbon ‘‘Refining processes ’96,’’ Hydrocarbon Processing, Vol. 75,
Processing, Vol. 72, No. 02, Feb. 1993, p. 53. No. 11, Nov. 1996, p. 87.
Sloley, Andrew W. and Golden, Scott W., ‘‘Analysis key to Rhodes, Anne K., ‘‘Environmentally advanced refinery nears
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‘‘New HF alky unit key to Navajo’s $50-million expansion,’’ Inomata, Makoto, Sato, Kyohei, Yamada, Yu, and Sasaki,
Oil & Gas Journal, June 14, 1993, p. 42. Hajime, ‘‘Engineering firm has designed refinery of the
‘‘Spanish refinery starts up HF alky unit,’’ Oil & Gas Journal, future,’’ Oil & Gas Journal, Apr. 28, 1997, p. 56.
Nov. 22, 1993, p. 77. PERF, ‘‘New refinery stream profiles available,’’ Hydrocar-
Jezak, A., ‘‘C5 alkylate: a superior blending component,’’ bon Processing, Vol. 76, No. 08, Aug. 1997, p. 63.
Hydrocarbon Processing, Vol. 73, No. 02, Feb. 1994,
p. 47. II. HYDROCRACKING
‘‘NPRA Q&A: Refiners focus on FCC, hydroprocessing, Ladeur, Peter and Bijwaard, Harry, ‘‘Shell plans $2.2-billion
and alkylation catalysts,’’ Oil & Gas Journal, Mar. 28, renovation of Dutch refinery,’’ Oil & Gas Journal, Apr.
1994, p. 41. 26, 1993, p. 64.
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TOC/INDEX
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‘‘NPRA Q&A: Refiners exchange experiences on FCC prob-
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 201
TOC/INDEX
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Oct. 24, 1994, p. 80. Dahlstrom, Bud, Ham, Kevin, Becker, Myron E., Hum,
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No. 11, Nov. 1994, p. 83. REVAMP—Conclusion: Canadian refiner gets 2-year
Aguilar-Rodriguez, Enrique, Ortiz-Estrada, Ciro, and Aguil- payout with FCC revamp,’’ Oil & Gas Journal, Aug. 12,
era-Lopez, Matin, ‘‘Thermal analysis finds optimum 1996, p. 77.
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Golden, Scott W., Lieberman, Norm, and Martin, Gary R., Krishna, Ashok S., Arndt, John H., Kuehler, Chris W.,
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fractionators,’’ Oil & Gas Journal, Nov. 21, 1994, p. 72. approach to catalyst selection,’’ Oil & Gas Journal, Oct.
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14, 1996, p. 44.
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1995, p. 61. ‘‘Experts reveal catalyst-selection methodologies,’’ Oil &
Benton, Steve, ‘‘FCC catalyst increases isobutylene yield at Gas Journal, Oct. 14, 1996, p. 50.
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p. 98. valve differential pressure,’’ Oil & Gas Journal, Oct. 14,
Bullerdiek, Edward A., and Hobbs, James W., ‘‘Advanced 1996, p. 56.
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Menon, Raghu, Chou, Ting, Tamhankar, Satish, Ramachan-
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dran, Ram, Hull, Randall, and Watson, Richard, ‘‘FCC
O2 ENRICHMENT—1: Proper choice of O2 supply Inomata, Makoto, Sato, Kyohei, Yamada, Yu, and Sasaki,
enhances enrichment benefits,’’ Oil & Gas Journal, Feb. Hajime, ‘‘Engineering firm has designed refinery of the
26, 1996, p. 54. future,’’ Oil & Gas Journal, Apr. 28, 1997, p. 56.
Tamhankar, Satish, Menon, Raghu, Chou, Ting, Ramachan- Netzer, D., ‘‘Economically recover olefins from FCC off-
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O 2 ENRICHMENT—Conclusion: Enrichment can 1997, p. 83.
decrease NOx, SOx formation,’’ Oil & Gas Journal, Mar. 4, PERF, ‘‘New refinery stream profiles available,’’ Hydrocar-
1996, p. 60. bon Processing, Vol. 76, No. 08, Aug. 1997, p. 63.
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Dahlstrom, B.F., Ham, Kevin, Becker, Myron E., Hum, p. 67.
Tom P., Lacijan, Larry, and Lorsbach, Tom, ‘‘FCC McCarthy, Steve J., Raterman, Mike F., Smalley, Chris G.,
REVAMP—1: Feed injection, riser-termination systems Sodomin, Joe F., and Miller, Rik B., ‘‘Refiner improves
replaced in fast-track revamp,’’ Oil & Gas Journal, July FCC yields using latest process technologies,’’ Oil & Gas
29, 1996, p. 83. Journal, Aug. 18, 1997, p. 56.
202 References
TOC/INDEX
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Toman, Jerry J., and Beckman, Robert F., ‘‘Visbreaker hard- 1995, p. 118.
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 203
TOC/INDEX
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No. 11, Nov. 1996, p. 87. July 3, 1995, p. 48.
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1996, p. 41. former turnaround costs,’’ Oil & Gas Journal, Sept. 18,
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Dickenson, R.L., et al, ‘‘Refiner options for converting and lysts,’’ Oil & Gas Journal, Oct. 2, 1995, p. 35.
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Vol. 76, No. 02, Feb. 1997, p. 57. Oil & Gas Journal, Oct. 2, 1995, p. 37.
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Hydrocarbon Processing, Vol. 75, No. 02, Feb. 1996,
V. REFORMING p. 59.
Al-Mutaz, I.S., ‘‘How to implement a gasoline pool lead
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‘‘OGJ international refining-catalyst compilation,’’ Oil & ‘‘Program predicts reformate properties, including octane,
Gas Journal, Oct. 11, 1993, p. 44. vapor pressure, and gravity,’’ Oil & Gas Journal, Sept. 9,
Ancheyta-Juarez, Jorge, and Aguilar-Rodriguez, Enrique, 1996, p. 68.
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Oil & Gas Journal, Jan. 31, 1994, p. 93. 1996, p. 43.
Christensen, T.S. and Primdahl, I.I., ‘‘Improve syngas pro- Krishna, Ashok S., Arndt, John H., Kuehler, Chris W.,
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1994, p. 51. 1996, p. 43.
Anon, ‘‘Gas Processes ’94,’’ Hydrocarbon Processing, Vol. 73, Rhodes, Anne K., ‘‘Environmentally advanced refinery nears
No. 04, Apr. 1994, p. 67. start-up in Germany,’’ Oil & Gas Journal, Mar. 17,
Jeanneret, J.J., et al., ‘‘New strategies maximize para-xylene 1997, p. 49.
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June 1994, p. 43. bon Processing, Vol. 76, No. 08, Aug. 1997, p. 63.
Aguilar-Rodriguez, Enrique, and Ancheyta-Juarez, Jorge,
‘‘New process model proves accurate in tests on catalytic VI. TREATING AND DESALTING
reformer,’’ Oil & Gas Journal, July 25, 1994, p. 80.
‘‘Refining Processes ’94,’’ Hydrocarbon Processing, Vol. 73, ‘‘Filtration method efficiently desalts crude in commercial
No. 11, Nov. 1994, p. 83. test,’’ Oil & Gas Journal, May 17, 1993, p. 59.
204 References
TOC/INDEX
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1993, p. 82B. Feb. 1996, p. 63.
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Monticello, D.J., ‘‘Biocatalytic desulfurization,’’ Hydrocar- Alverson, Ed and Mullenix, Andrew J., ‘‘New process
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Anon, ‘‘Gas Processes ’94,’’ Hydrocarbon Processing, Vol. 73, Journal, May 20, 1996, p. 75.
No. 04, Apr. 1994, p. 67. Harruff, Lewis G., and Bushkuhl, Stephen J., ‘‘Activated
‘‘NPRA Q&A: Auxiliary equipment, corrosion focus of carbon passes tests for acid-gas clean-up,’’ Oil & Gas
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Stewart, E.J. and Lanning, R.A., ‘‘Reduce amine plant sol- Lunsford, K.M., ‘‘Advantages of brazed aluminum heat
vent losses, Part 1,’’ Hydrocarbon Processing, Vol. 73, exchangers,’’ Hydrocarbon Processing, Vol. 75, No. 07,
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Stewart, E.J. and Lanning, R.A., ‘‘Reduce amine plant sol- Depew, C.A., and Nielsen, R.B., ‘‘Dynamic simulation for
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Tamburrano, F., ‘‘Disposal of heavy oil residues, Part 1,’’ Gothenquist, Carol A., and Rooker, Karen M., ‘‘Carbon
Hydrocarbon Processing, Vol. 73, No. 09, Sept. 1994, adsorption system protects LPG storage sphere,’’ Oil &
p. 79. Gas Journal, July 1, 1996.
Tamburrano, F., ‘‘Disposal of heavy oil residues, Part 2,’’ Harris, J.R., ‘‘Use desalting for FCC feedstocks,’’ Hydrocar-
Hydrocarbon Processing, Vol. 73, No. 10, Oct. 1994, bon Processing, Vol. 75, No. 08, Aug. 1996, p. 63.
p. 77. Stanger, C.W., et al, ‘‘Hydroprocessing/FCC synergy,’’
‘‘Refining Processes ’94,’’ Hydrocarbon Processing, Vol. 73, Hydrocarbon Processing, Vol. 75, No. 08, Aug. 1996,
No. 11, Nov. 1994, p. 83. p. 69.
Ernest, J.B. and Depew, C.A., ‘‘Use dynamic simulation to Spears, Michael L., Hagan, Kathy M., and Michalik, Carl
model HPU reactor depressuring,’’ Hydrocarbon Process- J., ‘‘Converting to DEA/MDEA mix ups sweetening
ing, Vol. 74, No. 01, Jan. 1995, p. 72. capacity,’’ Oil & Gas Journal, Aug. 12, 1996, p. 63.
Abry, R.G. and DuPart, M.S., ‘‘Amine plant troubleshooting Suarez, F.J., ‘‘Pluses and minuses of caustic treating,’’ Hydro-
and optimization,’’ Hydrocarbon Processing, Vol. 74, carbon Processing, Vol. 75, No. 10, Oct. 1996, p. 117.
No. 04, Apr. 1995, p. 41. ‘‘Refining processes ’96,’’ Hydrocarbon Processing, Vol. 75,
Kafesijan, A.S. and Dewey, R.C., ‘‘Demonstrating tail-gas No. 11, Nov. 1996, p. 87.
treater reliability reduces costs,’’ Hydrocarbon Processing, Absi-Halabi, M., et al, ‘‘Trends in catalysis research to meet
Vol. 74, No. 04, Apr. 1995, p. 53. future refining needs,’’ Hydrocarbon Processing, Vol. 76,
Collins, C., et al, ‘‘Liquefaction plant design in the 1990s,’’ No. 02, Feb. 1997, p. 45.
Hydrocarbon Processing, Vol. 74, No. 04, Apr. 1995, Dickenson, R.L., et al, ‘‘Refiner options for converting and
p. 67. utilizing heavy fuel oil,’’ Hydrocarbon Processing,
Cook, P.J. and Losin, M.S., ‘‘Membranes provide cost-effec- Vol. 76, No. 02, Feb. 1997, p. 57.
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Vol. 74, No. 04, Apr. 1995, p. 79. cut method,’’ Hydrocarbon Processing, Vol. 76, No. 03,
Guida, J.W. and Fruge, D.E., ‘‘Improve wastewater treat- Mar. 1997, p. 79.
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1995, p. 55. one step,’’ Oil & Gas Journal, Mar. 17, 1997, p. 80.
Price, J. and Burns, D., ‘‘Clean amine solvents economically Bourdon, J.C., ‘‘Improve operations and enhance refinery
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No. 11, Nov. 1995, p. 107. 1997, p. 83.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 205
TOC/INDEX
‘‘Fina/Total’s U.K. refinery starts up CHP project,’’ Oil & Campagne, W. v. L., ‘‘Use Ponchon-Savarit in your process
Gas Journal, May 5, 1997, p. 58. simulation, Part 2,’’ Hydrocarbon Processing, Vol. 72,
Quinlan, Michael P., Echterhoff, Linda W., Leppin, Dennis, No. 10, Oct. 1993, p. 63.
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recovery processes studied,’’ Oil & Gas Journal, July 21, Part 1,’’ Hydrocarbon Processing, Vol. 72, No. 10, Oct.
1997, p. 54. 1993, p. 71.
Colbert, G.L., et al, ‘‘Make boiler feedwater with lower Rhodes, Anne K., ‘‘Northwest Australia’s Saladin crude
risks,’’ Hydrocarbon Processing, Vol. 76, No. 08, Aug. assayed,’’ Oil & Gas Journal, Oct. 18, 1993, p. 50.
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total residue destruction,’’ Hydrocarbon Processing,
Vol. 72, No. 11, Nov. 1993, p. 52.
VII. CRUDE DISTILLATION Golden, S.W., et al., ‘‘Revamping FCC main fractionator
energy systems,’’ Hydrocarbon Processing, Vol. 72, No. 11,
Sarathy, P.R. and Suffridge, G.S., ‘‘Etherify field butanes,
Nov. 1993, p. 43.
Part 1,’’ Hydrocarbon Processing, Vol. 72, No. 01, Jan.
Cassata, J.R., et al., ‘‘Modeling of tower relief dynamics,
1993, p. 89.
Part 2,’’ Hydrocarbon Processing, Vol. 72, No. 11, Nov.
Sarathy, P.R. and Suffridge, G.S., ‘‘Etherify field butanes,
1993, p. 69.
Part 2,’’ Hydrocarbon Processing, Vol. 72, No. 02, Feb.
Capps, R.W. and Thompson, J.R., ‘‘Statistical safety factors
1993, p. 43.
reduce overdesign,’’ Hydrocarbon Processing, Vol. 72,
Pescarollo, E., et al., ‘‘Etherify light gasolines,’’ Hydrocarbon
No. 11, Nov. 1993, p. 77.
Processing, Vol. 72, No. 02, Feb. 1993, p. 53. Miquel, J. and Castells, F., ‘‘Easy characterization of petro-
Rhodes, Anne K., ‘‘EXPORT CRUDES FOR THE ’90s: leum fractions, Part 1,’’ Hydrocarbon Processing, Vol. 72,
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Oil & Gas Journal, Feb. 15, 1993, p. 73. Miquel, J. and Castells, F., ‘‘Easy characterization of petro-
Golden, S.W., et al., ‘‘FCC main fractionator revamps,’’ leum fractions, Part 2,’’ Hydrocarbon Processing, Vol. 73,
Hydrocarbon Processing, Vol. 72, No. 03, Mar. 1993, No. 01, Jan. 1994, p. 99.
p. 77. Ghoshal, P.C. and Mukhopadhyay, S., ‘‘Improve glycol
Toman, Jerry J., and Beckman, Robert F., ‘‘Visbreaker hard- dehydration unit efficiency,’’ Hydrocarbon Processing,
ware has alternate uses in low-sulfur fuel era,’’ Oil & Gas Vol. 73, No. 03, Mar. 1994, p. 75.
Journal, Mar. 22, 1993, p. 66. Rhodes, Anne K., ‘‘Lyondell, Citgo join for heavy oil upgrade
Fair, J.R., ‘‘How to design baffle tray columns,’’ Hydrocarbon project at Houston refinery,’’ Oil & Gas Journal, Mar.
Processing, Vol. 72, No. 05, May 1993, p. 75. 21, 1994, p. 60.
French, Eddie C., ‘‘New inhibitor reduces crude-unit corro- Rhodes, Anne K., ‘‘Two offshore Australian crudes assayed,’’
sion problems at lower pH,’’ Oil & Gas Journal, May 24, Oil & Gas Journal, May 9, 1994, p. 76.
1993, p. 45. Rhodes, Anne K., ‘‘Yemen’s light, sweet Alif crude assayed,’’
Roberts, D.A., et al., ‘‘Recover additional distillate from Oil & Gas Journal, May 23, 1994, p. 78.
vacuum residue,’’ Hydrocarbon Processing, Vol. 72, Rhodes, Anne K., ‘‘Benchmark West Texas Intermediate
No. 07, July 1993, p. 75. crude assayed,’’ Oil & Gas Journal, Aug. 15, 1994, p. 88.
Golden, S.W., et al., ‘‘Troubleshoot vacuum columns with Daubert, T.E., ‘‘Petroleum fraction distillation interconver-
low-capital methods,’’ Hydrocarbon Processing, Vol. 72, sions,’’ Hydrocarbon Processing, Vol. 73, No. 09, Sept.
No. 07, July 1993, p. 81. 1994, p. 75.
Lieberman, Norman P., ‘‘Four steps solve crude-tower over- Tamburrano, F., ‘‘Disposal of heavy oil residues, Part 1,’’
head corrosion problems,’’ Oil & Gas Journal, July 5, Hydrocarbon Processing, Vol. 73, No. 09, Sept. 1994,
1993, p. 47. p. 79.
Campagne, W. v. L., ‘‘Use Ponchon-Savarit in your process Rhodes, Anne K., ‘‘Danish North Sea crude assayed,’’ Oil
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Rhodes, Anne K., ‘‘GUIDE TO WORLD CRUDES: Two Martin, G.R., et al, ‘‘Understand vacuum system fundamen-
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206 References
TOC/INDEX
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 207
TOC/INDEX
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Oil & Gas Journal, Mar. 29, 1993, p. 60. ‘‘Naphtha cracker starts up in Taiwan,’’ Oil & Gas Journal,
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208 References
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Oct. 2, 1995, p. 30. ‘‘Union Texas slates ethylene unit at Geismar,’’ Oil & Gas
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Catalyst suppliers consolidate further, offer more cata- Rhodes, Anne K., ‘‘New ammonia process, catalyst proven
lysts,’’ Oil & Gas Journal, Oct. 2, 1995, p. 35. in Canadian plant,’’ Oil & Gas Journal, Nov. 11,
‘‘China’s refining/petrochemical industry continues expan- 1996, p. 37.
sion,’’ Oil & Gas Journal, Oct. 9, 1995, p. 78. Shanley, Anges, ‘‘Ammonia’s on the upswing,’’ Chemical
Williamson, Michelle, ‘‘WORLDWIDE CONSTRUC- Engineering, Nov. 1996, p. 30.
TION UPDATE: Petrochemicals,’’ Oil & Gas Journal, ‘‘China downstream investment focus shifting,’’ Oil & Gas
Oct. 16, 1995, p. 79. Journal, Dec. 2, 1996, p. 46.
Summers, Daniel R., McGuire, Peter J., Resetarits, Michael ‘‘Enhanced solvent recovery process boosts PTA production,
R., Graves, Caryn E., Harper, Steven E., and Angelino, saves energy,’’ Oil & Gas Journal, Dec. 16, 1996, p. 44.
Salvatore J., ‘‘High capacity trays debottleneck Texas C3 ‘‘New Borealis unit uses metallocene catalyst, ‘‘Oil & Gas
splitter,’’ Oil & Gas Journal, Nov. 6, 1995, p. 45. Journal, Dec. 30, 1996, p. 33.
‘‘Tennessee facility to obtain methanol from coal syngas,’’ ‘‘Ethylene consumption seen doubling by 2015,’’ Oil & Gas
Oil & Gas Journal, Nov. 6, 1995, p. 23. Journal, Jan. 13, 1997, p. 31.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 209
TOC/INDEX
‘‘Borealis expands polypropylene interests,’’ Oil & Gas Jour- IX. DELAYED COKING
nal, Feb. 3, 1997, p. 35.
‘‘Shell France first French refiner in 12 years to cut capacity,’’ Thorpe, Wilson A. and Sivaraman, Srini, ‘‘Simple techniques
Oil & Gas Journal, Feb. 17, 1997, p.26. reduce coke inventory, sales measurement errors,’’ Oil &
‘‘Petrochemical capacity expansions abound,’’ Oil & Gas Gas Journal, Jan. 18, 1993, p. 44.
Journal, Feb. 24, 1997, p. 40. ‘‘DOE: New process cuts ethanol cost,’’ Oil & Gas Journal,
‘‘Volatility to rule olefins, styrene markets to 2001,’’ Oil & Aug. 15, 1993, p. 48.
Gas Journal, Mar. 17, 1997, p. 39. ‘‘Latest coker designs increase liquid yields, reduce emis-
Radler, Marilyn, ‘‘WORLDWIDE CONSTRUCTION sions,’’ Oil & Gas Journal, Nov. 8, 1993, p. 82.
UPDATE: Petrochemicals,’’ Oil & Gas Journal, Apr. 14, Schulman, B.L., et al., ‘‘Bottom-of-the-barrel upgrading
1997, p. 67. moves aggressively,’’ Hydrocarbon Processing, Vol. 73,
Rhodes, Anne K., ‘‘World ethylene capacity jumped 5 mil- No. 12, Dec. 1993, p. 100C.
lion mt/y, or 6.5% in past year,’’ Oil & Gas Journal, May ‘‘Bonner & Moore sees gain in U.S. delayed coking capacity,’’
19, 1997, p. 45. Oil & Gas Journal, Dec. 27, 1993, p. 30.
Glauthier, Tad, Kalkstein, Harold, and Williamson, Robert, Sloan, H.D., ‘‘Refinery expansion/upgrading means lighter,
‘‘Petrochemical producers gain advantage with novel busi- quality products,’’ Hydrocarbon Processing, Vol. 73,
ness strategies,’’ Oil & Gas Journal, May 19, 1997, p. 54. No. 01, Jan. 1994, p. 82C.
Bansal, B.B., et al., ‘‘Improve your coking process,’’ Hydro-
‘‘Ethylene survey,’’ Oil & Gas Journal, May 19, 1997, p. 59.
carbon Processing, Vol. 73, No. 02, Feb. 1994, p. 63.
Picciotti, Marcello, ‘‘ETHYLENE TECHNOLOGIES-1:
Rhodes, Anne K., ‘‘Lyondell, Citgo join for heavy oil upgrade
Novel ethylene technologies developing but steam crack-
project at Houston refinery,’’ Oil & Gas Journal, Mar.
ing remains king,’’ Oil & Gas Journal, June 23, 1997,
21, 1994, p. 60.
p. 53.
‘‘NPRA Q&A: Refiners exchange experiences on FCC prob-
Picciotti, Marcello, ‘‘ETHYLENE TECHNOLOGIES-
lems, coking operations,’’ Oil & Gas Journal, May 2,
Conclusion: New ethylene routes are available, but eco-
1994, p. 110.
nomics inhibit their use,’’ Oil & Gas Journal, June 30,
‘‘Oman, India team up for proposed fertilizer plant,’’ Oil
1997, p. 71.
& Gas Journal, Aug. 15, 1994, p. 33.
‘‘South Korea’s refining/petrochemical capacity expansion ‘‘Refining Processes ’94,’’ Hydrocarbon Processing, Vol. 73,
push continues to gather momentum,’’ Oil & Gas Journal, No. 11, Nov. 1994, p. 83.
July, 7, 1997, p. 19. Golden, Scott W., Lieberman, Norm, and Martin, Gary R.,
‘‘Chem Systems: outlook strong for Asian petrochemicals,’’ ‘‘Correcting design errors can prevent coking in main
Oil & Gas Journal, July 7, 1997, p. 46. fractionators,’’ Oil & Gas Journal, Nov. 21, 1994, p. 72.
‘‘Statoil, Conoco dedicate giant Norwegian methanol plant,’’ Bennett, Robert P., Blevins, H.J. (Jim), and Cuevas, H.J.
Oil & Gas Journal, July 14, 1997, p. 26. (Joe), ‘‘New chemical reduces coke dust emissions at
‘‘Thailand’s petrochemical demand grows,’’ Oil & Gas Jour- Mississippi refinery,’’ Oil & Gas Journal, Dec. 26,
nal, July 21, 1997, p. 34. 1994, p. 74.
‘‘W. Australia eyeing petrochemical complex,’’ Oil & Gas Swain, Edward J., ‘‘SULFUR, COKE, AND CRUDE
Journal, Aug. 4, 1997, p. 32. QUALITY—1: Coke, sulfur recovery from U.S. refineries
‘‘Global petrochemical markets to get tougher,’’ Oil & Gas continues to increase,’’ Oil & Gas Journal, Jan. 2,
Journal, Aug. 11, 1997, p. 28. 1995, p. 33.
‘‘BP cracks polymer recycling technique at Grangemouth,’’ Stefani, A., ‘‘Choosing a coke recovery system,’’ Hydrocarbon
Oil & Gas Journal, Aug. 18, 1997, p. 18. Processing, Vol. 74, No. 09, Sep. 1995, p. 61.
‘‘BP to expand olefins capacity in Southeast Asia,’’ Oil & Golden, S.W., et al, ‘‘Refinery analytical techniques optimize
Gas Journal, Sept. 15, 1997, p. 27. unit performance,’’ Hydrocarbon Processing, Vol. 74,
Aitani, Abdullah M. and Hamid, Syed Halim, ‘‘DOWN- No. 11, Nov. 1995, p. 85.
STREAM IN THE PERSIAN GULF-2: The Persian Parks, S.B. and Schillmoller, C.M., ‘‘Use alloys to improve
Gulf’s petrochemical industry is proliferating,’’ Oil & Gas ethylene production,’’ Hydrocarbon Processing, Vol. 75,
Journal, Sept. 22, 1997, p. 73. No. 03, Mar. 1996, p. 53.
‘‘Petrochemical deals mark European shakeout,’’ Oil & Gas Rhodes, Anne K., ‘‘Venezuelan refiner completes $2.5 billion
Journal, Sept. 29, 1997, p. 50. refinery expansion,’’ Oil & Gas Journal, Mar. 18,
Aitani, Abdullah M. and Hamid, Syed Halillm, ‘‘DOWN- 1996, p. 51.
STREAM IN THE PERSIAN GULF-Conclusion: To Stefani, A., ‘‘Debottleneck delayed cokers for greater profit-
diversify its petrochemicals portfolio, GCC needs liquid ability,’’ Hydrocarbon Processing, Vol. 75, No. 06, June
feeds,’’ Oil & Gas Journal, Sept. 29, 1997, p. 96. 1996, p. 99.
210 References
TOC/INDEX
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‘‘Refining processes ’96,’’ Hydrocarbon Processing, Vol. 75, Lin, Sheng H. and Yeh, Kuo L., ‘‘Looking to treat wastewa-
No. 11, Nov. 1996, p. 87. ter? Try ozone,’’ Chemical Engineering, May 1993, p. 112.
Alveal, Enrique Dávila and Karpenski, Martin J., ‘‘Partners Blair, Hugo, ‘‘The Environmental pluses of diaphragm
assume risks, lower finance costs of delayed coker-cogen- pumps,’’ Chemical Engineering, May 1993, p. 118.
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1997, p. 111. 1: Federal, state efforts force reexamination of glycol-
‘‘Phillips, Pdvsa ink coker, crude sale deal,’’ Oil & Gas reboiler emissions,’’ Oil & Gas Journal, May 17, 1993,
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True, Warren R., ‘‘GLYCOL-REBOILER EMISSIONS—
2: Glycol mass-balance method scores high for estimating
X. ENVIRONMENTAL CONTROLS BTEX, VOC emissions,’’ Oil & Gas Journal, May 31,
1993, p. 54.
‘‘EPA issues clarification on rule governing benzene emis-
Stubblefield, Fred, Jr., ‘‘Get topnotch performance from
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‘‘Tests show limits on oxygen content to be unwarranted,’’
Jespersen, Chris, Jerger, Douglas and Exner, Jurgen, ‘‘Bior-
Oil & Gas Journal, Jan. 18, 1993, p. 46. emediation tackles hazwaste,’’ Chemical Engineering, June
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Chemical Engineering, Feb. 1993, p. 74. Felten, J.R., et al., ‘‘Residual fuels in a clean-fuels environ-
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Petchonka, J., et al., ‘‘How CAA impacts polymer process- 1993, p. 97.
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Kotcher, Raymond L., ‘‘Turn a permitting challenge into an Conclusion: PC program estimates BTEX, VOC emis-
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‘‘Diesel fuel quality is improving in most European coun- mental waste problems,’’ Hydrocarbon Processing, Vol. 72,
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Gas Journal, Mar. 22, 1993, p. 32. Hydrocarbon Processing, Vol. 72, No. 07, July 1993,
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1993, p. 95. No. 08, Aug. 1993, p. 55.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 211
TOC/INDEX
Callahan, B. and McCaw, P.A., ‘‘Risk assessment alleviates Fewel, Kenneth J., and Conroy, John H., ‘‘Design guidelines
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Vol. 72, No. 08, Aug. 1993, p. 61. Oil & Gas Journal, Nov. 29, 1993, p. 56.
Anon, ‘‘Environmental Processes ’93,’’ Hydrocarbon Process- Sweetland, Kirk, ‘‘Dealing with lead in the workplace,’’
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Bergmann, E.P., ‘‘Approximate risk assessment prioritizes Goldblatt, M., ‘‘How to justify water conservation projects,’’
remedial decisions,’’ Hydrocarbon Processing, Vol. 72, Hydrocarbon Processing, Vol. 72, No. 12, Dec. 1993,
No. 08, Aug. 1993, p. 111. p. 65.
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abandonment,’’ Hydrocarbon Processing, Vol. 72, No. 08, for refineries, Part 1,’’ Hydrocarbon Processing, Vol. 72,
Aug. 1993, p. 149. No. 12, Dec. 1993, p. 73.
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‘‘Glycol reboiler emissions control process tested,’’ Oil & Davis, Gregory B., Goss, Michael L., Schoemann, Pete, and
Gas Journal, Aug. 23, 1993, p. 44. Tyler, Susan S., ‘‘Crude oil tank-cleaning process recovers
‘‘Witco: new diesel grade meets California specs,’’ Oil & oil, reduces hazardous wastes,’’ Oil & Gas Journal, Dec.
Gas Journal, Aug. 30, 1993, p. 24. 13, 1993, p. 35.
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olefin plant’s spent caustic,’’ Hydrocarbon Processing, Engineering, Feb. 1994, p. 147.
Vol. 72, No. 09, Sept. 1993, p. 61. Radigan, M.J., ‘‘How to select a continuous emission moni-
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No. 09, Sept. 1993, p. 76C.
‘‘Dutch refinery remediating contaminated soils on site,’’
‘‘Ashland produces low sulfur diesel for highway use,’’ Oil
Oil & Gas Journal, Feb. 7, 1994, p. 62.
& Gas Journal, Sept. 20, 1993, p. 42.
Higgins, Thomas and Thom, James, ‘‘Solvents: Know your
Miller, M. and Jackson, R., ‘‘New valve packing technology
options,’’ Chemical Engineering, Mar. 1994, p. 92.
extends service life,’’ Hydrocarbon Processing, Vol. 72,
Gorry, Matthew, Amin, Pradeep and Richardson, D. Wayne,
No. 10, Oct. 1993, p. 105.
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1993, p. 139. La Russo, Anthony, ‘‘Audit your environmental contrac-
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Laczko, Lawrence P., ‘‘H2S IN EOR—Gas processing ‘‘Russian refiner tests new one-stage H2S removal process,’’
for CO2 EOR involves sulfur removal,’’ Oil & Gas Journal, Oil & Gas Journal, Mar. 7, 1994, p. 81.
Nov. 15, 1993, p. 61. AL-Tell, Nasser, and Lueders, Richard, ‘‘Texas refiner starts
‘‘Stepwise approach selects most effective remediation alter- up new waste water treatment plant,’’ Oil & Gas Journal,
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Johnson, J.E., Tzap, Stephen J., Kelley, Robert E., and Anon, ‘‘Gas Processes ’94,’’ Hydrocarbon Processing, Vol. 73,
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Nov. 29, 1993, p. 50. refiner,’’ Oil & Gas Journal, May 30, 1994, p. 43.
212 References
TOC/INDEX
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 213
TOC/INDEX
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1995, p. 32. Ferry, Robert L., and Kissell, J. Randolph, ‘‘New equation
Smith, Bruce R., ‘‘Monitoring wet scrubber performance,’’
estimates emissions from tank turnovers,’’ Oil & Gas
Chemical Engineering, June 1995, p. 96.
Journal, Sept. 25, 1995, p. 75.
Manuele, Vincent O., ‘‘Avoid dangerous surprises during
Isaacs, Mark, Heywood, Nigel, Blake, Nigel, and Alderman,
site cleanups,’’ Chemical Engineering, June 1995, p. 125.
Neil, ‘‘Getting a grip on sludge,’’ Chemical Engineering,
Goyal, R. and Ramirez, R., ‘‘Reduce power outages,’’ Hydro-
Oct. 1995, p. 80.
carbon Processing, Vol. 74, No. 06, June 1995, p. 71.
Carnell, Peter J.H., Joslin, Ken W., and Woodham, Peter Hassebrock, F., ‘‘Reduce losses through smarter valve selec-
R., ‘‘Fixed-bed processes provide flexibility for COS, H2S tion,’’ Hydrocarbon Processing, Vol. 74, No. 10, Oct.
removal,’’ Oil & Gas Journal, June 5, 1995, p. 52. 1995, p. 53.
Byers, Bill, ‘‘Zero discharge: A systematic approach to water Rhodes, Anne K., ‘‘WORLDWIDE CATALYST REPORT:
reuse,’’ Chemical Engineering, July 1995, p. 96. Catalyst suppliers consolidate further, offer more cata-
Cappos, Steve, ‘‘Membrane minimize liquid discharge,’’ lysts,’’ Oil & Gas Journal, Oct. 2, 1995, p. 35.
Chemical Engineering, July 1995, p. 102. ‘‘OGJ international refining-catalyst compilation—1995,’’
Boffardi, Bennett P., and Smith, Alan L., ‘‘Chemical treat- Oil & Gas Journal, Oct. 2, 1995, p. 37.
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ing, July 1995, p. 106. Oil & Gas Journal, Oct. 2, 1995, p. 77.
Shaikh, A. and Lee, C.J., ‘‘Minimize flaring during ethylene ‘‘Controversy over U.S. RFG still alive,’’ Oil & Gas Journal,
plant startup,’’ Hydrocarbon Processing, Vol. 74, No. 07, Oct. 9, 1995, p. 40.
July 1995, p. 89. ‘‘Tank-cleaning method removes, processes F037 waste,’’
Crow, Patrick, ‘‘WATCHING GOVERNMENT: EPA’s Oil & Gas Journal, Oct. 9, 1995, p. 86.
tale from the crypt,’’ Oil & Gas Journal, July 10, McKenna, Joshua, and Pickering, Edward, ‘‘Testing contam-
1995, p. 36. inated soil,’’ Chemical Engineering, Nov. 1995, p. 175.
Carr, David M., ‘‘Where sealless pumps make sense,’’ Chemi- Hennessey, P.M., et al, ‘‘Use coalescing methods to solve
cal Engineering, Aug. 1995, p. 78. emulsion problems,’’ Hydrocarbon Processing, Vol. 74,
Netzel, James, Pecht, Glenn, and Kalodimos, Mike, ‘‘Gas No. 11, Nov. 1995, p. 107.
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214 References
TOC/INDEX
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1995, p. 111. Tamhankar, Satish, Menon, Raghu, Chou, Ting, Ramachan-
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Wasilewski, Marek, ‘‘Make your process water pay for O 2 ENRICHMENT—Conclusion: Enrichment can
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Geiger, G.E., ‘‘Improve corrosion and deposition control 4, 1996, p. 60.
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No. 01, Jan. 1996, p. 105. ‘‘Automakers’ fuel specs trouble U.S. refiners,’’ Oil & Gas
Gabriel, R. and Lundy, W., ‘‘Industry initiative sets stan- Journal, Mar. 25, 1996, p. 37.
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Spencer, C. and Tolpa, G., ‘‘Use computer-based design
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Croom, Miles L., ‘‘New development in filter dust collec-
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‘‘Gas Processes ’96,’’ Hydrocarbon Processing, Vol. 75,
Hilaly, Ahmad, and Sikdar, Subhas, ‘‘Process tools for pollu-
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 215
TOC/INDEX
McManus, Anne Marie, ‘‘Get the most from environmental Crumpler, D.K. and Whittle, D.K., ‘‘How to effectively
audits,’’ Chemical Engineering, June 1996, p. 143. revalidate PHAs,’’ Hydrocarbon Processing, Vol. 75,
Straitz, III, J.F., ‘‘Improve flare safety and reliability to meet No. 10, Oct. 1996, p. 55.
ISO-9000 stds.,’’ Hydrocarbon Processing, Vol. 75, Emerson, G., ‘‘Improve safety with pilot operated relief
No. 06, June 1996, p. 109. valves,’’ Hydrocarbon Processing, Vol. 75, No. 10, Oct.
‘‘WATCHING GOVERNMENT: World Bank urges lead 1996, p. 67.
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‘‘WATCHING GOVERNMENT—NRC: More studies tions,’’ Hydrocarbon Processing, Vol. 75, No. 10, Oct.
required on MTBE,’’ Oil & Gas Journal, June 17, 1996, p. 85.
1996, p. 25. Tripathi, Paul, ‘‘Pinch technology reduces wastewater,’’
Ebadat, Vahid, ‘‘Electrostatic hazards in the CPI,’’ Chemical Chemical Engineering, Nov. 1996, p. 87.
Engineering, July 1996, p. 141. Hohl, Howard M., ‘‘Flameless thermal oxidation reduces
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Underground storage,’’ Chemical Engineering, July 4, 1996, p. 77.
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Anderson, R., et al, ‘‘Use proactive permitting to expand wide compliance,’’ Hydrocarbon Processing, Vol. 75,
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1996, p. 65. ‘‘Refining processes ’96,’’ Hydrocarbon Processing, Vol. 75,
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safeguard wastewater systems,’’ Hydrocarbon Processing,
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Thurman, J., ‘‘Do you manage your environmental risks
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‘‘Environmental Processes ’96,’’ Hydrocarbon Processing, effectively?,’’ Hydrocarbon Processing, Vol. 75, No. 12,
Vol. 75, No. 08, Aug. 1996, p. 85. Dec. 1996, p. 99.
Rhodes, Anne K., ‘‘Kansas refiner starts up coke gasification Stokman, Sofia K., Sogorka, Brian J., ‘‘Soil contamination:
unit,’’ Oil & Gas Journal, Aug. 5, 1996, p. 31. Dealing with petroleum spills,’’ Chemical Engineering,
‘‘In situ remediation cleans hydrocarbon-contaminated soil,’’ Jan. 1997, p. 113.
Oil & Gas Journal, Aug. 26, 1996, p. 56. Zetter, M.S. and Gethner, J.S., ‘‘Use software to power-
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Chemical Engineering, Sept. 1996, p. 116. Jan. 1997, p. 83.
Ferrantd, John and Verdibello, Mario S., ‘‘Services with a Mandel, S.B., ‘‘What is the total cost for emissions monitor-
global accent,’’ Chemical Engineering, Sep. 1996, p. 147. ing?,’’ Hydrocarbon Processing, Vol. 76, No. 01, Jan.
‘‘Texas facility treats, recycles refinery, petrochemical 1997, p. 99.
wastes,’’ Oil & Gas Journal, Sept. 16, 1996, p. 49. Saunders, Barbara, ‘‘U.S. refiners must piece together RFG,
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Ledbetter, D., ‘‘Reduce accidental releases of hazardous Miller, L.R. and Kroll, T.R., ‘‘Minimize environmental
materials,’’ Hydrocarbon Processing, Vol. 75, No. 09, impacts when replacing underground pipe,’’ Hydrocar-
Sep. 1996, p. 113. bon Processing, Vol. 76, No. 02, Feb. 1997, p. 85.
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No. 09, Sep. 1996, p. 121. 1997, p. 57.
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216 References
TOC/INDEX
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 217
TOC/INDEX
Lipták, Béla G., ‘‘Level measurement with problem liquids,’’ Lines, B., et al., ‘‘Polyethylene reactor modeling and control
Chemical Engineering, Mar. 1993, p. 130. design,’’ Hydrocarbon Processing, Vol. 72, No. 06, June
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Hydrocarbon Processing, Vol. 72, No. 03, Mar. 1993, Hodgson, Steve and Holden, David, ‘‘Scaling new heights
p. 77. in plant automation,’’ Chemical Engineering, July 1993,
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Forsell, K.A., ‘‘Protect motors with solid-state overloads,’’ Hydrocarbon Processing, Vol. 72, No. 07, July 1993, p. 41.
Hydrocarbon Processing, Vol. 72, No. 03, Mar. 1993, Stoll, K.E., et al., ‘‘Simplify fuzzy controller implementa-
p. 100. tion,’’ Hydrocarbon Processing, Vol. 72, No. 07, July
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Visigalli, R., et al., ‘‘Predict AGO quality,’’ Hydrocarbon
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Hussain, M.S., ‘‘Improve planetary gear vibration analysis,’’ Valleur, M., ‘‘Integrate offsites management with informa-
Hydrocarbon Processing, Vol. 72, No. 05, May 1993, tion systems,’’ Hydrocarbon Processing, Vol. 72, No. 11,
p. 105. Nov. 1993, p. 63.
DiFoggio, Rocco, Sadhukhan, Maya, and Ranc, Martha Pugh, T., et al., ‘‘Improve heat exchanger leak detection,’’
L., ‘‘Near-infrared techniques for octane analysis have Hydrocarbon Processing, Vol. 72, No. 11, Nov. 1993,
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218 References
TOC/INDEX
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1993, p. 74. McPherson, Lori, ‘‘Understanding ORP systems,’’ Chemical
Bayard, Pete, ‘‘Improved, integrated yield-accounting system Engineering, Mar. 1994, p. 143.
saves time and money,’’ Oil & Gas Journal, Nov. 22, Albers, J.E., ‘‘Data reconciliation with unmeasured vari-
1993, p. 67. ables,’’ Hydrocarbon Processing, Vol. 73, No. 03, Mar.
Wentworth, Craig E., ‘‘Guidelines useful for incorporating 1994, p. 65.
DCS in existing process plant,’’ Oil & Gas Journal, Nov. ‘‘Meters to answer needs for low cost EFM, energy measure-
29, 1993, p. 74. ment,’’ Oil & Gas Journal, Mar. 7, 1994, p. 49.
Smithline, Herb, ‘‘Practical guidelines for temperature mea- Trosper, Robert L., Stubbs, Robert G., and Carver, Darrell,
surement.’’ Chemical Engineering, Dec. 1993, p. 78. ‘‘New Mexico gas plant operator automates field control,’’
Lewis, Clifford W., ‘‘Accuracy in temperature measure- Oil & Gas Journal, Mar. 7, 1994, p. 54.
ments,’’ Chemical Engineering, Dec. 1993, p. 85. Stark, Stephen T., and Heuer, Richard D., ‘‘Testing paves
Early, P.L., Jr., and Miller, J., ‘‘Fieldbus: How a worldwide way for electronic flow monitoring system,’’ Oil & Gas
standard will benefit the HPI,’’ Hydrocarbon Processing, Journal, Mar. 7, 1994, p. 58.
Vol. 72, No. 12, Dec. 1993, p. 107. ‘‘European diesel fuel quality continues to improve,’’ Oil &
Wittliff, M., et al., ‘‘Improve plant reliability with informa- Gas Journal, Mar. 14, 1994, p. 68.
tion systems,’’ Hydrocarbon Processing, Vol. 73, No. 01, Morgan, S.W., et al., ‘‘Improve process training with
Jan. 1994, p. 63. dynamic simulation,’’ Hydrocarbon Processing, Vol. 73,
Page, E.A. and Berggren, J.C., ‘‘Improve predictive mainte- No. 04, Apr. 1994, p. 51.
nance with HFE monitoring,’’ Hydrocarbon Processing,
Treiber, S., et al., ‘‘Optimize control of natural gas plants,’’
Vol. 73, No. 01, Jan. 1994, p. 69.
Hydrocarbon Processing, Vol. 73, No. 04, Apr. 1994,
Faust, E., ‘‘Pressure calibration standards: How accurate
p. 63.
should they be?,’’ Hydrocarbon Processing, Vol. 73,
Poynter, Wesley G., and Barrios, Roy J., ‘‘Coulometric Karl
No. 01, Jan. 1994, p. 79.
Fischer titration simplifies water content testing,’’ Oil &
Rhodes, Anne K., ‘‘U.S. reformulated gasoline rule complex,
confusing,’’ Oil & Gas Journal, Jan. 17, 1994, p. 16. Gas Journal, Apr. 11, 1994, p. 53.
‘‘When a refinery stops making JP-4,’’ Oil & Gas Journal, Ziegler, J.G. and Connell, J.R., ‘‘For optimum control:
Jan. 17, 1994, p. 17. Modify the process, not the controls-Part I,’’ Chemical
Morris, William E., Smith, William E., and Snee, Ronald D., Engineering, May 1994, p. 132.
‘‘Interaction blending equations enhance reformulated McCracken, Philip G., ‘‘Technical audits and crucial clues,’’
gasoline profitability,’’ Oil & Gas Journal, Jan. 17, Chemical Engineering, May 1994, p. 161.
1994, p. 54. Iscovici, R.S., ‘‘Kinetic model solves visbreaker constraint
‘‘California refiners’ RFG worries compounded by dual control problem,’’ Hydrocarbon Processing, Vol. 73,
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‘‘GPM Gas Corp. brings New Mexico plant on line,’’ Oil Boyes, Walt, ‘‘Look at your process non-invasively,’’ Chemi-
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Lee, Anthony L., Feldkirchner, Harlan L., Gamez, Jorge P., Edwards, L.A. and Kipper, J.P., ‘‘Computerization: prob-
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31, 1994, p. 90. Semwal, Prem B., and Varshney, Ram G., ‘‘New pour point
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Hydrocarbon Processing, Vol. 73, No. 02, Feb. 1994, Oil & Gas Journal, June 6, 1994, p. 89.
p. 69. ‘‘New correlations predict diesel cold-flow properties accu-
Radigan, M.J., ‘‘How to select a continuous emission moni- rately,’’ Oil & Gas Journal, June 20, 1994, p. 51.
toring system,’’ Hydrocarbon Processing, Vol. 73, No. 02, Welch, William T., Bain, Michael L., Maggard, Steven M.,
Feb. 1994, p. 73. and May, Jack M., ‘‘Experience leads to accurate design
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 219
TOC/INDEX
of NIR gasoline analysis systems,’’ Oil & Gas Journal, Bakker, Andre, Smith, John M., and Myers, Kevin J., ‘‘How
June 27, 1994, p. 48. to disperse gases in liquids,’ Chemical Engineering, Dec.
Ziegler, J.G. and Connell, J.R., ‘‘For optimum control: 1994, p. 98.
Modify your process- Part 2,’’ Chemical Engineering, July Friedman, Y.Z., ‘‘Tuning averaging level controllers,’’
1994, p. 107. Hydrocarbon Processing, Vol. 73, No. 12, Dec. 1994,
Wilson, David H., ‘‘Automate bulk-solids delivery with feed- p. 101.
back control,’’ Chemical Engineering, Aug. 1994, p. 87. San, Yip Poh, Landells, Keith, and Mackay, David C.,
Brenner, Raul, ‘‘Nuclear radiation sees it all,’’ Chemical Engi- ‘‘INFERENTIAL CONTROL—Conclusion: Crude
neering, Aug. 1994, p. 118. unit controls reduce quality giveaway,’’ Oil & Gas Journal,
Cunningham, D.B., ‘‘Adaptive control of sulfur recovery Dec. 5, 1994, p. 56.
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Book, Neil, Sitton, Oliver, et al., ‘‘The road to a common Cohen, M.H. and Arzenheimer, M., ‘‘Benefits of advanced
Byte,’’ Chemical Engineering, Sept. 1994, p. 98. process control maintenance,’’ Hydrocarbon Processing,
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information system,’’ Hydrocarbon Processing, Vol. 73, Stobbe, A.W., ‘‘Manage leak detection and repair programs
No. 09, Sept. 1994, p. 43. cost-effectively,’’ Hydrocarbon Processing, Vol. 74, No. 01,
Michalek, T.F., et al, ‘‘Using a relational database for blend Jan. 1995, p. 101.
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Sept. 1994, p. 47. Hydrocarbon Processing, Vol. 74, No. 02, Feb. 1995,
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Sept. 1994, p. 51. tion,’’ Hydrocarbon Processing, Vol. 74, No. 02, Feb.
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No. 09, Sept. 1994, p. 65. Alexander, R.E. and Vickers, A.K., ‘‘Use new detectors to
Daubert, T.E., ‘‘Petroleum fraction distillation interconver-
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Vol. 74, No. 02, Feb. 1995, p. 93.
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Padalkar, Samir, Karsal, Gabor, et al., ‘‘Online diagnostics
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Giacone, G.D. and Logue, D.A., ‘‘Updated advanced con- Riner, J.L., Hashemian, H.M., et al., ‘‘Online testing assures
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Processing, Vol. 73, No. 10, Oct. 1994, p. 103. 1995, p. 84.
Espinosa, Alain, Sanchez, Michel, Osta, Sebastien, Boniface, Richard, L., et al, ‘‘Advanced control improves MHC-VGO
Christian, Gil, Jose, Martens, Andre, Descales, Bernard, unit operation,’’ Hydrocarbon Processing, Vol. 74, No. 03,
Lambert, Didier, and Valleur, Marc, ‘‘On-line NIR analy- Mar. 1995, p. 163.
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Williams, A.K., et al, ‘‘Reformer model improves control,’’ refiner benefits from advanced control,’’ Oil & Gas Jour-
Hydrocarbon Processing, Vol. 73, No. 11, Nov. 1994, nal, Mar. 20, 1995, p. 70.
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Oil & Gas Journal, Nov. 28, 1994, p. 76. Parker, Sarah, ‘‘On the level. Measuring liquids: A guide
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Siegell, J.H., ‘‘Control valve fugitive emissions,’’ Hydrocar- Sasson, Richard and Pate, Robin, ‘‘Retraying and revamp
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Cresswell, L.W., ‘‘Refining in the Former Soviet Union,’’ nal, Aug. 2, 1993, p. 71.
Hydrocarbon Processing, Vol. 76, No. 08, Aug. 1997, Connell, David E., Horth, Paul, and Powell, R.H.W., ‘‘Anal-
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 223
TOC/INDEX
‘‘Syngas plant eyes anhydrous ammonia increase,’’ Oil & ‘‘Texas JV to burn residue gas in cogen unit,’’ Oil & Gas
Gas Journal, Mar. 13, 1995, p. 31. Journal, Sept. 23, 1996, p. 43.
Butts, R. Clark, Chou, Kelley, and Slaton, Barbara, ‘‘Nitro- ‘‘Work starts on S. African TAME unit,’’ Oil & Gas Journal,
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Gas Journal, Mar. 13, 1995, p. 92. Hohl, Howard M., ‘‘Flameless thermal oxidation reduces
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Rhodes, Anne K., ‘‘Texas refiner optimizes by integrating ‘‘Conoco inaugurates new unit at its U.K. Humber refinery,’’
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Festen, Leo J.F.M., Bronneberg, Joseph P.A., Brugman, 1996, p. 43.
Wilfried P.T., Hartmann, David W., and Huber, Brian ‘‘New etherification process commercialized in Finland,’’ Oil
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 225
TOC/INDEX
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TOC/INDEX
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 227
TOC/INDEX
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carbon Processing, Vol. 76, No. 08, Aug. 1997, p. 79. Hydrocarbon Processing, Vol. 73, No. 08, Aug. 1994,
Weaver, C.E., ‘‘Applying FT-IR in chemical cleaning,’’ p. 121.
Hydrocarbon Processing, Vol. 76, No. 08, Aug. 1997, Morran, Don, ‘‘How to design stressless steam lines-Part
p. 97. II,’’ Chemical Engineering, Oct. 1994, p. 88.
Bloch, Heinz, ‘‘Automatic lubrication saves money,’’ Chemi-
Moustakakis, B., ‘‘Pitfalls of piping flexibility analysis,’’
cal Engineering, Dec. 1997, p. 125.
Hydrocarbon Processing, Vol. 73, No. 10, Oct. 1994,
Ray, Rudolf K., ‘‘Taking the guesswork out of plant upkeep,’’
p. 99.
Chemical Engineering, Jan. 1998, p. 68.
Broyles, R.K., ‘‘Improve high-temperature expansion joint
Garcia-Borras, Thomas, ‘‘Improving boilers and furnaces,’’
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Chemical Engineering, Jan. 1998, p. 127.
1994, p. 55.
Gomez, Jose Vicente, ‘‘New equation predicts viscosity of
XV. PIPING unknown hydrocarbon vapors,’’ Oil & Gas Journal, Feb.
Lindley, Nancy L. and Lloyd, Joe C., ‘‘Piping systems: How 6, 1995, p. 60.
installation costs stack up,’’ Chemical Engineering, Jan. Cochran, T.W., ‘‘Simplifying piping network analysis,’’
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Kroupa, Ralph, ‘‘Selecting valves for tough conditions,’’ Kreder, R.A., and Berwanger, P.C., ‘‘Making safety data
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Spock, Thomas, ‘‘Control fugitive emissions from valves,’’ Montgomery, G., ‘‘How to predict temperatures during gas
Chemical Engineering, Feb. 1993, p. 82. depressuring,’’ Hydrocarbon Processing, Vol. 74, No. 04,
Stubblefield, Fred, Jr., ‘‘Get topnotch performance from Apr. 1995, p. 85.
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228 References
TOC/INDEX
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 229
TOC/INDEX
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databases accelerate process design & costing,’’ Chemical bon Processing, Vol. 74, No. 05, May 1995, p. 99.
Engineering, July 1994, p. 139. Realff, Matthew J. and Sommerfeld, Jude T., ‘‘Drain heating
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for hydrogen production,’’ Hydrocarbon Processing, 1995, p. 121.
Vol. 73, No. 07, July 1994, p. 69. Martin, G.R. and Sloley, A.W., ‘‘Effectively design and
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Ganapathy, V., ‘‘Understand boiler performance characteris-
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Grosboll, M.P. and Stover, L., ‘‘Avoid flow maldistribution
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Buecker, Brad, ‘‘Beware of condenser fouling,’’ Chemical No. 11, Nov. 1995, p. 55.
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Golden, S.W., et al, ‘‘Refinery analytical techniques optimize
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TOC/INDEX
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 231
TOC/INDEX
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232 References
TOC/INDEX
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1995, p. 89. 1996, p. 84.
Badrock, John, Coutu, Robert, Johnson, Norman, and Mar- Gothenquist, Carol A. and Rooker, Karen M., ‘‘Carbon
tin, Andrea, ‘‘Bulk, heating cleans paraffinic bottoms from adsorption system protects LPG storage sphere,’’ Oil &
crude tanks,’’ Oil & Gas Journal, Feb. 20, 1995, p. 66. Gas Journal, July 1, 1996.
Gupta, Dinesh and Rafferty, Bob, ‘‘Proven tools and tech- Caruthers, Steve, ‘‘Here are guidelines for inspecting AST
niques for electric heat tracing,’’ Chemical Engineering, terminals,’’ Oil & Gas Journal, July 8, 1996, p. 52.
May 1995, p. 104. Grainawi, Lorri, ‘‘Aboveground storage, Part 1: Decoding
True, Warren R., ‘‘First year of AGA’s weekly storage survey shop-built tanks,’’ Chemical Engineering, Aug. 1996,
suggests useful patterns,’’ Oil & Gas Journal, July 17, p. 98.
1995, p. 50. Braune, Steven, Thorpe, Greg, et al, ‘‘Aboveground storage
Carr, David M., ‘‘Where sealless pumps make sense,’’ Chemi- tanks—Part II: Fielderected tanks,’’ Chemical Engineer-
cal Engineering, Aug. 1995, p. 78. ing, Aug. 1996, p. 104.
Netzel, James, Pecht, Glenn, and Kallodimos, Mike, ‘‘Gas
Bays, Joseph N., ‘‘Minimizing wastes from vacuum pumping
lubricated seals change pump choices,’’ Chemical Engi-
systems,’’ Chemical Engineering, Oct. 1996, p. 123.
neering, Aug. 1995, p. 82B.
Siegell, J.H., ‘‘Control VOC emissions,’’ Hydrocarbon Pro- Cameron, Donald B., ‘‘How fluid properties affect hydrau-
cessing, Vol. 74, No. 08, Aug. 1995, p. 77. lically balanced metering pumps,’’ Chemical Engineering,
Ferry, Robert L., and Kissell, J. Randolph, ‘‘New equation Nov. 1996, p. 100.
estimates emissions from tank turnovers,’’ Oil & Gas Hummel, Bob, ‘‘Lining aboveground storage tanks,’’ Chemi-
Journal, Sept. 25, 1995, p. 75. cal Engineering, Dec. 1996, p. 116.
Isaac, Mark, et al, ‘‘Getting a grip on sludge,’’ Chemical Prang, Allan J., ‘‘Selecting multiphase pumps,’’ Chemical
Engineering, Oct. 1995, p. 80. Engineering, Feb. 1997, p. 74.
‘‘Tank-cleaning method removes, processes F037 waste,’’ Vella, Philip, ‘‘Improved cleaning method safely removes
Oil & Gas Journal, Oct. 9, 1995, p. 86. pyrophoric iron sulfide,’’ Oil & Gas Journal, Feb. 24,
Shuai, Xiaoshan, and Meisen, Axel, ‘‘New correlations pre- 1997, p. 65.
dict physical properties of elemental sulfur,’’ Oil & Gas Berto, Frank J., ‘‘TANK GAUGING-1: Review of tank
Journal, Oct. 16, 1995, p. 50. measurement errors reveals techniques for greater accu-
Kusha, A.A., ‘‘Lessons learned from relocation,’’ Hydrocar- racy,’’ Oil & Gas Journal, Mar. 3, 1997, p. 68.
bon Processing, Vol. 74, No. 12, Dec. 1995, p. 85. Berto, Frank J., ‘‘TANK GAUGING-Conclusion: Auto-
Cochran, T.W., ‘‘Calculate pipeline flow of compressible matic gauging technologies have advanced, but better
fluids,’’ Chemical Engineering, Feb. 1996, p. 115. accuracy is needed,’’ Oil & Gas Journal, Mar. 10,
Aglitz, John, Bhatnager, Rajender K., Bolt, Donald E., and 1997, p. 63.
Butzbach, Thomas L., ‘‘Installing liquid-ring vacuum Krenek, M.R., ‘‘Improve global competitiveness with supply-
pumps,’’ Chemical Engineering, Nov. 1995, p. 132. chain management,’’ Hydrocarbon Processing, Vol. 76,
Crossley, N. Graeme, ‘‘Converting LPG caverns to natural- No. 05, May 1997, p. 97.
gas storage permits fast response to market,’’ Oil & Gas Early, P.L., et al, ‘‘Integrated terminal operations improves
Journal, Feb. 19, 1996, p. 39. profitability,’’ Hydrocarbon Processing, Vol. 76, No. 05,
Monroe, Perry C., ‘‘Pump installation: Penny pinch at your May 1997, p. 101.
own risk,’’ Chemical Engineering, Mar. 1996, p. 88. Karlsson, Per, ‘‘Put steel belts to work,’’ Chemical Engineer-
Reynolds, John A., ‘‘Use minimum flow data to prolong ing, Sept. 1997, p. 124.
centrifugal pump life,’’ Chemical Engineering, Mar. Tolan, William A., ‘‘Get to know your application,’’ Chemi-
1996, p. 92. cal Engineering, Jan. 1998, p. 78.
Whitmire, Kent, ‘‘Installing and maintaining gear pumps,’’
Chemical Engineering, Mar. 1996, p. 96.
Heng, Thomas, ‘‘A pump for high-value products,’’ Chemical XVIII. CORROSION
Engineering, Mar. 1996, p. 110.
Baker, R.W. and Jacobs, M., ‘‘Improve monomer recovery Sumbry, Louis C. and Bogner, Ben R., ‘‘Lining tank bottoms
from polyolefin resin degassing,’’ Hydrocarbon Processing, to extend service life,’’ Chemical Engineering, Jan.
Vol. 75, No. 03, Mar. 1996, p. 49. 1993, p. 131.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 233
TOC/INDEX
Schwinn, V. and Streisselberger, A., ‘‘Avoid H2S corrosion in Khaladkar, Pradip, ‘‘Fight corrosion with plastic,’’ Chemical
refinery vessels,’’ Hydrocarbon Processing, Vol. 72, No. 01, Engineering, Oct. 1995, p. 94.
Jan. 1993, p. 103. Kane, R.D. and Cayard, M.S., ‘‘Improve corrosion control
Gallaher, Dale M. and Malhoney, Michael J., ‘‘MOBILE in refining processes,’’ Hydrocarbon Processing, Vol. 74,
BAY—1: New technologies used in development of sour No. 11, Nov. 1995, p. 129.
Fairway gas,’’ Oil & Gas Journal, Feb. 22, 1993, p. 57. Groce, Bernard C., ‘‘Chemical, mechanical treatment
Gallaher, Dale M. and Malhoney, Michael J., ‘‘MOBILE options reduce hydroprocessor fouling,’’ Oil & Gas Jour-
BAY—Conclusion: Fairway sour gas development proves nal, Jan. 29, 1996, p. 81.
new materials, monitoring,’’ Oil & Gas Journal, Mar. 1, Wharry, Samuel R., ‘‘Transfer heat in a resin sheath,’’ Chemi-
1993, p. 76. cal Engineering, Feb. 1996, p. 74.
Miller, W.A., ‘‘How to choose a fluoropolymer,’’ Chemical Hohmann, F.W., ‘‘Improve steam reformer performance,’’
Engineering, Apr. 1993, p. 163. Hydrocarbon Processing, Vol. 75, No. 03, Mar. 1996,
DuPart, M.S., et al., ‘‘Understanding corrosion in alkano- p. 71.
lamine gas treating plants, Part 1,’’ Hydrocarbon Process- Rooney, P.C., et al, ‘‘Effect of heat stable salts on MDEA
ing, Vol. 72, No. 04, Apr. 1993, p. 75. solution corrosivity,’’ Hydrocarbon Processing, Vol. 75,
DuPart, M.S., et al., ‘‘Understanding corrosion in alkano- No. 03, Mar. 1996, p. 95.
lamine gas treating plants, Part 2,’’ Hydrocarbon Process- ‘‘Gas Processes ’96,’’ Hydrocarbon Processing, Vol. 75,
ing, Vol. 72, No. 05, May 1993, p. 89. No. 04, Apr. 1996, p. 103.
French, Eddie C., ‘‘New inhibitor reduces crude-unit corro- Brooks, Kevin and Martin, Mark W., ‘‘Ceramics stand up
sion problems at lower pH,’’ Oil & Gas Journal, May 24, to acid service,’’ Chemical Engineering, Oct. 1996, p. 77.
1993, p. 45. Wessel, James K., ‘‘Breaking tradition with ceramic compos-
Lieberman, Norman P., ‘‘Four steps solve crude-tower over- ites,’’ Chemical Engineering, Oct. 1996, p. 80.
head corrosion problems,’’ Oil & Gas Journal, July 5, Hummel, Bob, ‘‘Lining aboveground storage tanks,’’ Chemi-
1993, p. 47. cal Engineering, Dec. 1996, p. 115.
Brown, R.L., Jr., and Wines, T.H., ‘‘Improve suspended Rooney, P.C., et al, ‘‘Effect of heat stable salts on MDEA
water removal from fuels,’’ Hydrocarbon Processing, solution corrosivity, Pt. 2,’’ Hydrocarbon Processing,
Vol. 72, No. 12, Dec. 1993, p. 95. Vol. 76, No. 04, Apr. 1997, p. 65.
Wu, Yiing-Mei, ‘‘Calculations estimate process stream depo- Turner, J., ‘‘Control corrosion in washwater systems,’’
sitions,’’ Oil & Gas Journal, Jan. 3, 1994, p. 38. Hydrocarbon Processing, Vol. 76, No. 06, Jun. 1997,
Babaian-Kibala, Elizabeth, ‘‘Phosphate ester inhibitors solve p. 87.
naphthenic acid corrosion problems,’’ Oil & Gas Journal, Weiss, W.H., ‘‘Designing and maintaining plant piping and
Feb. 28, 1994, p. 31. valve systems,’’ Hydrocarbon Processing, Vol. 76,
Kohley, Bill, ‘‘Consider plastic spray nozzles,’’ Chemical No. 07, Jul. 1997, p. 59.
Engineering, Apr. 1994, p. 147.
Anon, ‘‘Gas Processes ’94,’’ Hydrocarbon Processing, Vol. 73, XIX. ENERGY CONSERVATION
No. 04, Apr. 1994, p. 67.
‘‘NPRA Q&A: Auxiliary equipment, corrosion focus of Ganapathy, V., ‘‘Effective use of heat-recovery steam genera-
refiner meeting,’’ Oil & Gas Journal, Apr. 4, 1994, p. 62. tors,’’ Chemical Engineering, Jan. 1993, p. 102.
‘‘Study scheduled on fouling of refinery units,’’ Oil & Gas Ganapathy, V., ‘‘Recovering heat when generating power,’’
Journal, May 23, 1994, p. 41. Chemical Engineering, Feb. 1993, p. 94.
Buxton, L. William, ‘‘Get the most out of plastic lined pipe,’’ Burger, Robert, ‘‘Cooling towers: The often over-looked
Chemical Engineering, Sept. 1994, p. 133. profit center,’’ Chemical Engineering, May 1993, p. 100.
Fultz, Benjamin S., Rogers, Robert H., Young, J.S., ‘‘Take Nutter, Darin, Britton, Angela and Heffington, Warren,
the guesswork out of plastics selection,’’ Chemical Engi- ‘‘Conserve energy to cut operating costs,’’ Chemical Engi-
neering, Oct. 1994, p. 84. neering, Sept. 1993, p. 126.
Hendrix, D.E. and Carucci, V.A., ‘‘Improve storage tank Hahn, Glenn E., ‘‘Get the most out of steam,’’ Chemical
inspections,’’ Hydrocarbon Processing, Vol. 74, No. 01, Engineering, Jan. 1994, p. 80.
Jan. 1995, p. 89. Power, Robert B., ‘‘Pump up your energy savings,’’ Chemical
Dobis, J.D., Clarida, D.R., and Richert, J.P., ‘‘Survey reveals Engineering, Feb. 1994, p. 120.
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Mar. 6, 1995, p. 63. Laird, T.L., ‘‘On-line power plant optimization improves
Buecker, Brad, ‘‘Beware of condenser fouling,’’ Chemical Texas refiner’s bottom line,’’ Oil & Gas Journal, May 16,
Engineering, Apr. 1995, p. 108. 1994, p. 53.
Shahani, G.H., et al, ‘‘Increase TPA production,’’ Hydrocar- Nelson, Kenneth E., ‘‘A practical guide to energy account-
bon Processing, Vol. 74, No. 05, May 1995, p. 99. ing,’’ Chemical Engineering, Sept. 1994, p. 122.
234 References
TOC/INDEX
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 235
TOC/INDEX
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Hydrocarbon Processing, Vol. 72, No. 03, Mar. 1993, Dahl, Carol and Garcia, Wolfgang J., ‘‘Reformulated gaso-
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236 References
TOC/INDEX
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No. 10, Oct. 1993, p. 95. Kerridge, A.E., ‘‘Project-manage the owner/client,’’ Hydro-
‘‘Supplying low sulfur diesel no great hurdle for U.S. refin- carbon Processing, Vol. 72, No. 12, Dec. 1993, p. 49.
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‘‘Catalyst suppliers further consolidate business units,’’ Oil Hydrocarbon Processing, Vol. 72, No. 12, Dec. 1993,
& Gas Journal, Oct. 11, 1993, p. 41. p. 57.
‘‘OGJ international refining-catalyst compilation,’’ Oil & Winston, R.E., ‘‘Rapid method for capital investment deci-
Gas Journal, Oct. 11, 1993, p. 44. sions,’’ Hydrocarbon Processing, Vol. 72, No. 12, Dec.
Bell, Laura, ‘‘WORLDWIDE CONSTRUCTION 1993, p. 132.
REPORT—Refineries,’’ Oil & Gas Journal, Oct. 18, Rhodes, Anne K., ‘‘World crude capacity stays flat while
1993, p. 59; Apr. 11, 1994, p. 65. conversion capability rises again,’’ Oil & Gas Journal,
Bell, Laura, ‘‘WORLDWIDE CONSTRUCTION Dec. 20, 1993, p. 37.
REPORT—Petrochemicals,’’ Oil & Gas Journal, Oct. Bell, Laura, ‘‘WORLDWIDE REFINING REPORT,’’ Oil
18, 1993, p. 71; Apr. 11, 1994, p. 78. & Gas Journal, Dec. 20, 1993, p. 46.
1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 237
TOC/INDEX
Chieu, J. and Foster, S., ‘‘Improve storm water management Wallace, S.J. and Hunter, B.L., ‘‘Optimize facility-siting
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No. 01, Jan. 1994, p. 83. May 1994, p. 85.
Bruce, S.R., ‘‘Who’s leading your process safety efforts?,’’ Fesharaki, F., ‘‘Oil prices in a new light,’’ Hydrocarbon Pro-
Hydrocarbon Processing, Vol. 73, No. 01, Jan. 1994, p. 89. cessing, Vol. 73, No. 05, May 1994, p. 143.
Foo, K.W., ‘‘Size steam tracers quickly, Part 1,’’ Hydrocarbon ‘‘China’s refiners face massive overhaul, expansion to meet
Processing, Vol. 73, No. 01, Jan. 1994, p. 93. demand growth, crude slate,’’ Oil & Gas Journal, May
Boutte, F.D., et al., ‘‘Optimize project execution, Part 1,’’ 9, 1994, p. 36.
Hydrocarbon Processing, Vol. 73, No. 01, Jan. 1994, Rhodes, Anne K., ‘‘Two offshore Australian crudes assayed,’’
p. 116. Oil & Gas Journal, May 9, 1994, p. 76.
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Foo, K.W., ‘‘Size steam tracers quickly, Part 2,’’ Hydrocarbon & Gas Journal, May 23, 1994, p. 43.
Processing, Vol. 73, No. 02, Feb. 1994, p. 91. Rhodes, Anne K., ‘‘Yemen’s light, sweet Alif crude assayed,’’
Mehall, J.R., ‘‘State of worldwide refining,’’ Hydrocarbon Oil & Gas Journal, May 23, 1994, p. 78.
Processing, Vol. 73, No. 02, Feb. 1994, p. 96A. Bartholomew, Calvin H. and Hecker, William C., ‘‘Catalytic
Myers, Philip E., ‘‘OSHA confined-space reg interpreted for reactor design,’’ Chemical Engineering, June 1994, p. 70.
storage tank operations,’’ Oil & Gas Journal, Feb. 14, Wu, K. and Dorian, J.P., ‘‘China’s petrochemical outlook,’’
1994, p. 84. Hydrocarbon Processing, Vol. 73, No. 06, June 1994,
Carroll, J.J., ‘‘Converting amine concentrations,’’ Hydrocar- p. 50B.
bon Processing, Vol. 73, No. 03, Mar. 1994, p. 91. Olstead, C.E., et al., ‘‘Objectives Matrix: A practitioner’s
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Oil & Gas Journal, June 13, 1994, p. 54.
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‘‘Worldwide gas-processing survey,’’ Oil & Gas Journal, June
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Derr, K.T., ‘‘Oil and its critics: The facts and the future,’’
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Hydrocarbon Processing, Vol. 73, No. 04, Apr. 1994,
Coker, A.K., ‘‘Selecting and sizing process compressors,’’
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No. 04, Apr. 1994, p. 141. Fusaro, P.C., ‘‘Asia Pacific refining: What’s next?,’’ Hydrocar-
‘‘Russian refineries tap western technology,’’ Oil & Gas Jour- bon Processing, Vol. 73, No. 07, July 1994, p. 66C.
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Vervalin, C.H., ‘‘A view of ACHEMA ’94 conference,’’ bon Processing, Vol. 73, No. 07, July 1994, p. 83.
Hydrocarbon Processing, Vol. 73, No. 05, May 1994, DeSilva, Francis, ‘‘The ion exchange deal,’’ Chemical Engi-
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Peterson, F.M. and Johnson, J.E., ‘‘What’s ahead for propyl- Molad, C., ‘‘New way to swap engineering data,’’ Hydrocar-
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238 References
TOC/INDEX
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 239
TOC/INDEX
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 241
TOC/INDEX
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Jan. 8, 1996, p. 42. ‘‘Siberian company starts up modular refinery,’’ Oil & Gas
Strozier, Robert W., ‘‘Unocal’s patent of gasoline formulas Journal, Mar. 18, 1996, p. 68.
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‘‘Toxicity, emissions test results in for RFG,’’ Oil & Gas Journal, Mar. 25, 1996, p. 37.
Journal, Jan. 8, 1996, p. 34. ‘‘Economic forces push down selling prices of U.S. refiner-
‘‘U.S. gasoline plagued by economic, technical uncertainty,’’ ies,’’ Oil & Gas Journal, Mar. 25, 1996, p. 82.
Oil & Gas Journal, Jan. 8, 1996, p. 29. Plotnikov, Valeri S., Avgerinos, Gabriel F., Dvorets, Nikita
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Gas Journal, Jan. 29, 1996, p. 38.
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Beedie, M., ‘‘Energy waste: A process quality defect?,’’ Hydro-
No. 04, Apr. 1996, p. 82F.
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Hydrocarbon Processing, Vol. 75, No. 02, Feb. 1996,
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p. 147.
‘‘Changes due in Russian petroleum product mix,’’ Oil & Oil & Gas Journal, Apr. 1, 1996, p. 40.
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‘‘Texas plant treats natural gas for use as alternative fuel,’’ Williamson, Michelle, ‘‘WORLDWIDE CONSTRUC-
Oil & Gas Journal, Feb. 19, 1996, p. 38. TION UPDATE: Gas processing,’’ Oil & Gas Journal,
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Oil & Gas Journal, Feb. 19, 1996, p. 47. Williamson, Michelle, ‘‘WORLDWIDE CONSTRUC-
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TOC/INDEX
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 243
TOC/INDEX
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244 References
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 245
TOC/INDEX
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‘‘DOE plans gas-to-liquids conventional transportation proj- ‘‘Merger of Venezuelan refineries delayed,’’ Oil & Gas Jour-
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TOC/INDEX
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No. 08, Aug. 1997, p. 87. STREAM IN THE PERSIAN GULF-1: Gulf countries
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1997 50th Anniversary NPRA Q & A Session on Refining and Petrochemical Technology 247
TOC/INDEX
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