Professional Documents
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Sudan Refinery
Sudan Refinery
Table of Contents
1. Unit Introduction
2. Manual Structure
1. Unit Introduction
1.1. General
Continuous Catalytic Reforming Unit (CCR) of Khartoum Refinery Company is built
under the expansion project of the refinery, phase II. The unit is designed by
Sinopec Engineering Incorporation. The process utilizes Axens's "State of the art"
moving catalyst bed with continuous catalyst regeneration.
The unit is designed to process 400,000 metrics tons per year and to operate at a
severity of RON 98 with an on-stream factor of 8000 hours/year.
2. Manual Structure
The design information and operating instructions of the Continuous Catalytic Reforming
Unit (unit71) are covered by six different volumes as follow:
1. Basis of Design
2. Unit Description
3. Chemistry
1. Basis Of Design
Density d4 0.7224
Composition (wt %)
2. Unit description
The naphtha coming from GDHT unit first of all enters the pretreatment feed surge drum
D-71100, after which it is pressurized by the pretreatment feed pump P-71101A/B.
Naphtha will be blended with the hydrogen rich gas that comes from the pretreatment
recycle compressor K-71101A/B, and then enters the pretreatment reactor R-71101 after
exchanging heat with the reactor product in E-71101A/B and heated to the reaction
temperature by the heating furnace F-71101. With the action of the catalyst; sulfur,
nitrogen and unsaturated olefins in the naphtha will react with hydrogen to give rise to
hydrogen sulfide, ammonia, and saturated hydrocarbons. While the metal impurities will
be adsorbed onto the catalyst. After the reaction effluents has exchanged heat with the
feed and has been cooled by the air condenser A-71101, it will enter the separator drum
D-71101, and the hydrogen rich gas from overhead line will return to the inlet of the
pretreatment recycle compressor K-71101A/B to be pressurized and circulated, and then
reused. The liquid at the drum bottom will be sent to the stripper C-71101, which will draw
the slight amount of lighter components out of the tower top and eliminate such impurities
in the oil as sulfur, ammonia, and water. After exchanging heat with the column feed in F-
71102, the oil at the bottom of the stripping tower C-71101 will become the refined
naphtha, reformer feed. After being condensed and cooled by the surface evaporation air
cooler A-71102, the product at the top of the stripping tower C-71101will enter the reflux
ISSUE DATE: 20/03/06 -3-
KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0
drum D-71103 of the stripping tower. Some of the H2S and NH3 will be discharged along
with the gas from the top of the drum D-71103 and enter the fuel gas piping network of
the unit; water is discharged from the drum boot. Light Naphtha from reflux drum bottom
is pressurized by the reflux pump P-71103A/B, some of it will be charged back into the
top of the stripping tower as reflux, while another part of it will be sent into the catalytic
cracking unit as the sulfur-containing light naphtha. A reboiler F-71102 will input heat into
the stripping tower using the fuel gas.
The pretreatment process will use the recycle hydrogen flow. Because the reaction
process only consumes a very slight amount of hydrogen, therefore a slight make-up of
hydrogen rich gas from the reforming section will be added to the inlet of the pretreatment
recycle compressor. After the hydrotreating process, a slight amount of waste hydrogen
will be vented into the fuel gas piping network through the top of the separator drum D-
71101. The pretreatment reaction pressure is controlled at the top of the separator drum.
The process flowchart of the pretreatment section is shown in B9701-71-PR1/1..
3. Chemistry
REACTANTS PRODUCTS
Note that the molecular weight of these chemicals is 84g for thiophene, 2g for
hydrogen, 58g for butane and 34g for H2S, respectively.
Action required to
Characteristics Trends
increase conversion
Exothermic reaction Temperature increase Temperature
decrease
Decreasing number of Pressure decrease Pressure increase
moles from 5 (reactants) to (if vapor phase)
2 (products)
Reaction consuming Decrease in Increase in hydrogen
hydrogen hydrogen concentration of the
concentration of the medium
medium
Reaction producing H2S Increase in H2S Decrease in the H2S
concentration of the concentration of the
medium medium
3.2. Kinetics
Several reactions occur in the hydrotreating (HDT) process, which aim is to prepare
the naphtha feed for the downstream aromizing unit (avoid the poisoning of the
aromizing catalyst). The main purpose of the process is the removal of sulfur
compounds (desulfurization). In parallel, many other reactions take place such as
denitrification (nitrogen compounds removal), deoxygenation (oxygen compounds
removal), olefins hydrogenation (or saturation), and at a lower extend
demetallation (organometallic compounds removal).
Note that mercaptans are acid components and have an obnoxious smell.
The chemical reactions related to the removal of mercaptans are
described below:
For example:
Sulfides
In these compounds the sulfur is linked to two hydrocarbon radicals. The
sulfur therefore forms an intermediary between the two radicals. Sulfides
have the following general formulas:
For example:
Thiophenic compounds
Thiophenic compounds are found typically in cracked naphtha (especially
heavy fractions). They derive from thiophene:
These compounds are not acid. However, the desulfurization of the ring is
more difficult, since this implies the opening of the ring, before the
hydrogenation of the radical and the release of the hydrogen sulfide.
An example of desulfurization of the methyl thiophene reaction is
presented hereafter:
The heat released by the denitrification reactions is also negligible, owing the
small amounts of nitrogen compounds (even fewer than sulfur compounds).
Note that the C – N bond is much more difficult to break than the C – S bond.
Consequently, the denitrification occurs to a much lower extent than
desulfurization.
The surface area available for contact between catalysts and reactants may be as
high as several hundreds of square meters per gram. The supports commonly used
are alumina (Al2O3) or silica (SiO2).
The catalytic reaction can be broken down into three successive steps:
adsorption of reactant molecules on certain available sites on the surface,
known as "active sites"
chemical reaction in the surface-adsorbed phase. This step is usually very fast,
since the chemical species formed by association with properly selected sites are
far more reactive than non-adsorbed molecules
Furthermore, the catalyst brings together these reactive species locally in the
adsorbed phase, thereby considerably increasing their probability of meeting,
which also helps accelerate chemical change.
desorption of products formed by the reaction, thereby releasing the active sites
for re-use
The products migrate through the pores to the outside of the grain towards the liquid
or the gas homogeneous phase.
These various elementary steps in catalysis are summarized in the following
diagram.
Use of the solid catalyst in such a mechanism involves the following requirements:
its surface must be easily accessible to the reactants, and products must be
able to move away quickly to allow maximum use of active sites
the chemical nature of these same active sites must be appropriate for the
reactions to be catalyzed, which explains the wide variety of chemical formula for
catalysts
The metal which constitutes the active phase of the catalyst must promote the
desired reaction as selectively as possible.
Since heterogeneous catalysis is a surface phenomenon, the active metals are
those which can chemisorb all the reactants
Nevertheless, this chemisorptive condition is not sufficient because the reactants
must be neither too weakly nor too strongly adsorbed.
If adsorption is excessively weak, very few molecules are activated on the catalyst
surface and the reaction rate is very slow. If the adsorption is too strong, the
hydrocarbon and the catalyst form a very stable complex, which produces a
poisoning effect.
Reference RS-1
Supplier RIPP
Composition Cobalt (CoO) ≥0.04 wt %
Tungsten (WO3) ≥19 wt %
Nickel (NiO) ≥2 wt %
Presentation Trifoliate - Diameter: 1.4 mm
Surface area ≥130 m2/g
Pore volume ≥0.22 cm3/g
Bulk density 0.75-0.80 t/m3
Bulk crushing strength ≥16 N/mm
3. Catalyst Loading
3.1. Preparation Before Catalyst Loading
3.1.1. Prior to catalyst loading, the startup work such as line flushing, run-in pumps
and motor, compressor commissioning, fire heater dry-out and leaking test
should be finished. The reactor should be cleared up and free from rust,
welding, water which can contaminate the catalyst. The blinds should be added
to prevent nitrogen and gas entering the reactor section. All instrument valves
should be in good condition.
3.1.2. Prepare the loading tools, such as one crane, one forklift, two transfer hoppers,
explosion-proof light, ceramic gasket to protect reactor manway, canvas as
protection against rain, loading socks of correct diameter and sufficient length,
wooden boards, a vacuum eductor, dust masks, measuring tape, chalk, ladder,
communication facilities, fresh air mask, etc.
3.1.3. Before reactor loading, personnel must enter the reactor to mark the wall for
each layer of the ceramic balls and catalyst according to design height.
3.1.4. The bolts of outlet basket at the bottom of reactor should be fixed and the blank
flange of unloading nozzle should be installed before reactor loading. The
explosion-proof light should be installed inside the reactor.
3.1.5. The loading area and reactor platform should be clean and free from
obstruction.
3.1.6. To avoid chaos and accident, personnel who will load catalyst should be
organized and undertake their own responsibility.
3.1.7. Insert a temporary hose into reactor and supply air to it. This can provide the
protection for the personnel who enter the reactor.
3.2. Notes
3.2.1. During catalyst transferring, care should be taken to put down and unload
catalyst gently.
3.2.2. Catalyst loading should be in fine day.
3.2.3. Catalyst drums should not be opened until the catalyst will be loaded
immediately. The rate of loading should be as quick as possible within
allowance to reduce exposing time of catalyst in the air which can affect
catalyst with damp.
3.2.4. Catalyst scattered on the ground or contaminated should not be loaded into
reactor.
3.2.5. While loading the catalyst, the end of the socks shall be, at any time, kept
within one meter away from the catalyst level.
3.2.6. Personnel who will load catalyst must wear clean clothes and workers in
reactor should button cuff and clean pockets to avoid something dropping into
reactor.
3.2.7. During catalyst loading, the sock should be kept moving in figure “8” pattern to
prevent the catalyst forming hills or craters. When loading each layer of ceramic
balls, the previous layer of balls should be not disturbed. And after each one-
meter level loading, the catalyst bed should be smoothly raked to keep it as
level as possible so that the loaded catalyst density is uniform throughout the
catalyst bed.
3.2.8. To avoid static producing, catalyst crashing or becoming bridged in catalyst
bed, the loading rate should be controlled. Typically the rate is about 2- 4 tons
of catalyst per hour.
3.2.9. Personnel who enter the reactor should stand on wooden boards to avoid
treading down the catalyst.
3.2.10. Retain 10ml of catalyst sample from each drum loaded for future reference.
bed (see figure 1). After this, the distributor basket temporary covers should be
removed.
3.3.6. Place the inlet distributor and bolt up the reactor inlet top cover.
Next to catalyst loading, catalyst will undergo the following operations which is
discussed in next document KRCIM 71100.04
Inerting
Air tightness test
Catalyst Drying
Presulfiding
ISSUE DATE: 20/03/06 - 19 -
KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0
4. Catalyst Regeneration
4.1. Introduction
It is defined as nitrogen-air regeneration that coke accumulated on spent catalyst is
burnt off with recycle nitrogen and air. During catalyst regeneration, the nitrogen is
circulated in reactor section, and the air is gradually added to it. Catalyst is
regenerated by controlling air flow rate and reactor temperature increasing rate.
4.2. Neutralization of Acidic Gases
4.2.1. Regeneration Reaction
Because the spent catalyst is the sulfide type catalyst containing much coke, a
lot of CO, CO2, SO2, SO3 will be formed during catalyst regeneration.
The main reactions of catalyst regeneration are shown below:
These acid gases formed during burning of coke can react with water at low
temperature location of reactor section. These reactions are listed below:
.
The equipments of reactor section would be seriously corroded by sulfuric acid,
sulfurous acid, carbonic acid and nitric acid at low temperature, so caustic
neutralization should be adopted during catalyst regeneration.
At the same time, injected ammonia can also react with CO2 in regeneration
gases as following:
Typically the caustic solution is added to the upstream of air cooler. The NaOH
containing in fresh caustic solution should be at 4-5w% and the PH of
circulating caustic solution should be at 8-10. To hold the PH of circulating
caustic at 8-10, there will be a continuous injection of fresh caustic at proper
rate and a continuous withdraw of spent caustic.
4.3.1.8. Pressurize the reactor section to 1.0 MPa and commission the recycle gas
compressor after the displacement has been finished. When the
compressor run well, detect the concentration of hydrogen and
hydrocarbon in recycle gas. If it can not meet the above requirement, the
reactor section needs to be displaced again.
4.3.2. Preparation
4.3.2.1. The injection system of ammonia, caustic solution and soft water should
be clean and all equipments should be in good condition.
4.3.2.2. Prepare the caustic solution containing 30% NaOH, which is mixed with
soft water to produce solution of 4~5% NaOH, anhydrous liquid ammonia,
corrosion inhibitor, which is mixed with soft water and added into caustic
solution to produce solution containing 30 μg/g of corrosion inhibitor.
4.3.2.3. Establish the catalyst regeneration flow.
4.3.2.4. Install oxygen analyzers at inlet and outlet of reactor, which should be
calibrated and ready to work.
4.3.2.5. Notify the analysis department to prepare to analyze following items:
4.4.3.6. Slowly adjust the air injection rate so that the oxygen content in the
recycle gas is 0.6 v% or the maximum temperature in catalyst bed is
440°C, whichever comes first.
4.4.3.7. While the second burning wave is passing through the catalyst bed,
continue to hold conditions constant, including the oxygen level in gas to
reactor, until the reactor outlet drops back to the temperature T1
measured in step(5). A reduction in air injection rate will be required.
4.4.3.8. Continue to raise the reactor inlet temperature at a maximum rate of
15°C/h to 440 °C, adjust the air injection rate so that the oxygen content of
the recycle gas is 1.0 v% or the maximum temperature in catalyst bed is
less than 450°C, whichever comes first.
4.5. Notes
4.5.1. Do not increase reactor inlet temperature and oxygen content of recycle gas
simultaneously, otherwise, the temperature in catalyst bed is easy to exceed
the limited value.
4.5.2. During catalyst regeneration, especially when reactor temperature is being
increased, an oxidizing atmosphere should be maintained at all times. If the
oxygen concentration in the gas to reactor drops to zero, it is possible that
some catalyst reduction can occur due to the presence of CO2.
4.5.3. In order to prevent caustic cracking, the temperature of caustic injection point
should be less than 200°C and between for 140~150°C.
4.5.4. During catalyst regeneration, the maximum temperature of catalyst bed should
be less than 480 °C.
5.1. Cool the reactor beds to less than 65°C. At the temperatures above this level,
combustion of iron pyrites is greatly accelerated and difficult to control. If the catalyst
is to be screened during unloading, the catalyst should be cooled to less than 50°C.
5.2. After cooling the catalyst beds to 65°C, the unit should be purged with N2 at least
twice. The unit should then be properly isolated and a small N 2 purge established at
the compressor discharge or preferably at the inlet to reactor. Do not open the
reactors at the top until all catalyst has been unloaded.
5.3. Be sure that several CO2 extinguishers are available.
5.4. Use only metal drums for unloading, and dump directly into drums if possible. Each
drum should be either purged with N2 during unloading or a piece of dry ice placed at
the bottom of each drum. Do not seal the drum air tight since this could result in
sudden rupture of the drum when combustion occurs. Burning of catalyst in the drum
is not serious and can be quickly extinguished with nitrogen or CO2.
5.5. When the catalyst should be screened at the same time as it is being dumped from
the reactors, nitrogen need to be purged through the dumping nozzle to the top of the
first screen to provide additional protection from pyrite ignition.
5.6. It is expected that some "sparking" of the pyrites will take place in any event.
Therefore, all workmen in the area must be supplied with face and eye protection. In
addition, they should wear long sleeve shirts with collars and cuffs tightly buttoned.
5.7. Maintain a positive flow of N2 out of the unloading nozzle throughout the unloading, if
the catalyst becomes bridged in the unloading nozzle or is not free flowing, break the
plug with a blast of N2. Do not allow air to be drawn into the reactor.
5.8. If ignition of pyrite takes place inside a reactor, stop unloading in that reactor and
increase the N2 purge to maximum until burning is stopped.
Contents: This instruction outlines the procedure for the start-up and shutdown of the
CCR regeneration Unit. The text includes:
1. Start-Up Requirement
2. Unit Purging
3. Initial Leak Test
4. Unit Drying
5. Catalyst Loading
6. Air Freeing and Leak Testing
7. Catalyst Drying
8. Catalyst Presulfiding
9. Establish Normal Operation
10. Normal Shutdown Procedure
1. Start-Up Requirement
1.1. All overhaul activities and technical modifications influencing Start-up are completed.
All units, removal of equipment and pipeline blinds conform to process requirements.
1.2. Pressure gauges and safety valves are checked. Replacement work and installation
is completed.
1.3. All chemical raw materials are ready and sufficient.
1.4. All process lines and equipment has been purged, qualified in pressure test and
undergone final inspection according to the following procedures.
1.5. Disassembled or replaced equipment flanges are padded and screwed uniformly.
1.6. Safety valves in good condition and its set pressure meet the requirement.
1.7. Close all atmospheric relief valves and drain.
1.8. Verify all instruments are in good condition.
1.9. Utilities services are working normal.
1.10.Ensure complete fire appliances, place inflammables and explosives in fixed area,
clean sundries on site.
1.11.Contact dispatch, maintenance department, fitters, electrical maintenance and lab.
Complete corresponding support work.
1.12.Complete and examine all Start-up schemes, planning diagrams, all related
procedures sheet and work permits.
1.13.All maintained and revamped equipment has acceptance qualification sheet.
1.14.Inspection of the unit is done according to “Plant Inspection” procedure in (KRCIM
71300.04)
2. Unit Purging
2.1. Purging objective
2.1.1. Eliminate welds rods and slags, abrasive dusts, oxides and in general other
substances which might impede the normal unit operation or damage the
equipment (valves, pumps, compressors, turbines, etc.)
2.1.2. Timely find existing problems through process line. Ensure system operability.
2.1.3. Make operators further understand field flow path.
→100-P-711033→FV-1013 bypass →Flanges upstream non-return valves on P-71103A/B outlet and drain points discharge steam
→SN-71102 purges and discharges steam to the flare drum
→FT-1021 bypass →80-P-711080→FV-1014 bypass →light naphtha boundary limit line 8-shaped
blind plate discharges steam
→150-P-711024→drain downstream E-71103A tube side and slops line 8-shaped blind plate discharge steam
→drain downstream E-71103B/C tube side and slops line 8-shaped blind plate discharge steam
→150-P-711020→FV-1029 and its bypass →150-P-711019 line 8-shaped blind plate discharges steam
→25-P-711073→D-71102 bottom 8-shaped blind plate discharges steam
→FV-1007 bypass →100-P-711087→P-71101A/B outlets drain and flanges upstream non-return
valves discharges steam
→150-P-711005 →SN-71101 discharges steam
→HV-1001 discharges steam
→FV-1003 discharges steam
→100-P-711060→discharges steam upstream FV-1003
→150-P-711020/1 →150-P-711002→100-SLO-711024→8-shaped blind plate discharges steam
→100-P-712096/3→8-shaped blind plate discharges steam
→100-P-711052→100-P-711051→drain upstream E-71109 and slops line 8-shaped
blind plate discharges steam
→150-P-711002→LV-1001 bypass →FT-1001 crossover line→naphtha comes from
hydrogenation line, 8-
shaped blind plate
discharges steam
→150-P-711001/1→
naphtha from tank field,
8-shaped blind plate
discharges steam
→100-P-711001/2→
naphtha from SCR, 8-
shaped blind plate
discharges steam
→150-P-711002→D-71100→tank bottom discharges to underground drain
→top vent discharges steam
→PG-1001 discharges steam
After D-71102 top inlet is purged to clean, connect it and enter the next blowing-up port. At D-71101 top hydrogen line,
remove flange and install temporary nozzle; the blowing-up flow is: 0.8MPa nitrogen from 40-GN-711001 enters K-
71101A/B inlets respectively→150-P-711021 and 150-P-711021/1→D-71102 top outlet →D-71102→150-P-
711018→150-P-711015→D-71102 top inlet. Close other connected pipelines valves for isolation;
A secondary procedure is: Fill D-71101 with steam before installation of instrument devices and purge according to the
following flow: 150-P-711015→150-P-711018→D-71102→150-P-711021 and 150-P-711021/1 and discharge steam before K-
71101A/B inlets. Close other connected pipelines valves for isolation
At R-71101 reactor top, turn the inlet elbow to atmosphere; the blowing-up flow is: 0.8MPa nitrogen to 40-GN-
711001→40-GN-711002→100-P-711022→200-P-711008→E-71101B/A shell side 250-P-711010→F-71101→250-P-
711013→R-71101 reactor top. Close other connected pipelines valves for isolation;
3.4.1. Pressure boosting speed should be slow and air tightness test pressure should
comply with the regulations strictly without overpressure.
3.4.2. Any leak source found should be marked in time and the maintenance
personnel should be contacted for handling.
3.4.3. Pay attention to inspect whether there is interflow between systems and avoid
equipment overpressure strictly. Watch out for gas expansion in the system
and consequent equipment overpressure because of ambient air temperature
change.
3.4.4. During air tightness test, commands should be given uniformly and personnel
in all areas should contact with each other.
3.4.5. During air tightness test of each system, at least two pressure gauges should
be used to observe pressure with required pressure gauge precision of
magnitude 0.4, 1.5-2 times of the highest air tightness pressure.
3.4.6. Handling of leak sources under pressure is not allowed.
3.5.1. Initial leak tests will be performed under KRC or Engineering company
responsibility and the general instructions hereunder shall only be used as a
reminder.
3.5.2. The initial leak tests can be performed using air or nitrogen depending upon
local facilities. The test pressure will be the air or nitrogen system pressure or
the unit (or section of unit) design pressure, whichever is the lower.
3.5.3. The unit is isolated with blinds from adjacent sections containing hydrocarbons
(liquid or gaseous), and from utilities systems where pressure is lower than air
(or nitrogen) pressure.
3.5.4. The pressure rise must be checked on several manometers and possibly
checked on a pressure recorder. Leaks must be carefully located and
tightened. Their location must be recorded.
3.5.5. The leak test is satisfactory when the pressure decrease is lower than
0.005 MPa/hour over a period of 4 consecutive hours.
3.5.6. The air (nitrogen) used for leak tests should be purged out of the unit using low
points drains to remove free water, if any.
When introducing vaccuum, close all pressure gauges and pressure lead wires.
Install vacuum gauge at D-71101 to start up ejector. When introducing vaccuum in
prehydrotreatment system, it is up-to-standard when D-71101 pressure reaches
0.003KPa (gauge pressure); then, introduce nitrogen slowly to break the vacuum.
After vacuum test, blind the vacuum line blind plate; then, prepare positive pressure
airtightness.
4. Unit Drying
4.1. Drying Objective
4.1.1. To avoid damaging the catalyst with water
4.1.2. To shorten the duration of the low severity operation after first oil in.
4.1.3. Unit dry out is conducted simultaneously with the heater refractory drying,
which can save commissioning time.
4.1.4. The objective of furnace drying is to remove the natural water, crystallines.
Drying will calcinate materials contained in the furnace refractory. Accordingly,
intensity and service life of refractory materials will increase.
4.1.5. Furnace drying and system drying should be done simultaneously, namely,
using nitrogen circulation method. On one hand, nitrogen flow through the
furnace tubes will ensure no tubes overheating will occur; on the other hand,
circulating this hot nitrogen through the unit will remove excess moisture which
might have remained from the construction and flushing.
4.1.6. During furnace drying and system drying, potential internal and external
expansion problems will be discovered. Moreover, the plant operability will be
confirmed.
.
4.3. F-71102 Furnace Drying (Note: Same procedure is be used for F-71205 drying)
4.3.1. Preparation work
Flushing and purging of heat carrying system finishes.
Electricity, instrument air, steam, nitrogen, and gas are smooth and enough
supply is guaranteed.
Strictly read and follow KRCIM 71200.07
5. Catalyst Loading
Please refer to chapter 3 of KRCIM 71100.03
7. Catalyst Drying
7.1. Preparations
7.1.1. Prehydrotreatment hydrogen-system inerting is fulfilled. Oxygen content <0.5%,
D-71101 pressure reduced to 0.8MPa.
7.1.2. Prepare one 1000ml measuring flask and one 5 liter water flask.
7.1.3. Make sure that sufficient nitrogen supply is available and analyze nitrogen
purity in advance. It is required that the content of water in the nitrogen rich gas
should be less than 300µg/g, total hydrogen and hydrocarbons content less
than 0.3v% and oxygen content less than 0.3v%
7.1.4. H2, gas and all kinds of hydrocarbons should be isolated from the reactor
during catalyst drying. Accordingly, make sure blinds are located at:
H2 inlet into the unit (50-P-712050/3)
Fuel gas line at top of D-71101 (50-P-711061)
All feedstock inlets to unit
7.1.5. F-71101 ignition according to regulations, control temperature in every stage
according to following requirements. Meanwhile, under the conditions of N 2
environment, pressure as 0.8MPa, full circulation of compressor K–71101.
Drain water every hour at D-71101& D-71102 and complete measurement.
7.3. Procedure
The drying procedure includes three phases:
8. Catalyst Presulfiding
8.3.3. When the hydrogen circulation is stabilized and the highest temperature in the
catalyst bed is less than 150°C, introduce carrier oil into the reactor.
8.3.4. Gradually adjust the charge rate according to unit condition until LHSV comes
up to 3.0 h-1
8.3.5. Within first 2 hours, if the resultant oil is dirty, drain the oil directly to the waste
oil tank and then divert the clean oil to feed surge drum to establish oil
circulation.
8.3.6. Raise reactor inlet temperature at the rate of 20°C /h until the highest
temperature in the catalyst bed reaches 175°C. Then start injection of DMDS
and hold the temperature at 175°C for 2 hours.
8.3.7. The presulfiding procedure and sulfiding agent rate are shown in the table
below.
8.3.9. Notes
When the reactor inlet temperature reaches 230°C, the H2S concentration
should be in the range of 500 - 5000 ppm (v).
Analyze H2S content of recycle gas twice per hour and hydrogen purity
every 4 hours, which should be over 80v%.
1. Operating Conditions
2. Process Variables
3. Troubleshooting
4. Analysis Control
1. Operating Conditions
1.1. Reaction System
Design feed rate: 61, 897 kg/h
Air speed: 6h-1
Hydrogen oil volume ratio: 150
Reaction temperature: 280-340˚C
D-71l01Temperature: 40˚C
D-71l01Pressure: 2.2MPa
1.2. C-71101
Temperature top / bottom: 125/220˚C
Tower top pressure: 1.2MPa
Feed temperature: 141˚C
Feed rate: 59560
Reflux ratio (feed) 1.86
Reflux temperature: 40˚C
Tower bottom heat load: 6132 KW
Tower bottom product rate: 50, 000 kg/h
2. Process Variables
2.1. Reaction System
2.1.1. Reaction temperature
Reaction temperature is a major approach to regulate oil quality generated from
prehydrotreatment reaction, and it is an adjustable operation parameter. Too
low temperature, will not guarantee hydrotreating depth and remove impurities.
Accordingly generated oil will be disqualified. High temperature facilitates
removing impurities and olefin saturation. However, over high reaction
temperature will intensify hydrocracking reaction, cause catalyst carbon deposit
and reduce activity and life time as well as increase energy consumption.
Reactor inlet temperature can be lowered in SOL(Catalyst Start of Life) due to
higher catalyst activity. Catalyst activity will falloff after some time indicating
EOL(Catalyst End of Life); reaction temperature can be increased.
In actual operation, reactor inlet temperature shall be properly regulated
according to product and feedstock quality.
Always ensure small temperature fluctuations in operation. 2 – 3˚C every time
when lifting temperature.
ISSUE DATE: 20/03/06 - 44 -
KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION NORMAL OPERATION
CCR UNIT KRCIM 71100.05 REV.0
2.2. C-71101
2.2.1. Pressure
Tower pressure is maintained through controller PICl004 to control the pressure
of reflux drum D-71103. During operation, if tower top pressure is reduced,
temperature rises and tower bottom oil get heavier; otherwise, tower bottom oil
get lighter.
2.2.2. Temperature
Fractions quality takes regulating parameters as a major approach. In case of
column depressurization, properly reduce tower bottom temperature, otherwise
initial boiling point of tower bottom oil will rise.. Meanwhile, timely regulate
according to the change of feed quality and control tower bottom temperature
through F-71102 outlet temperature.
3. Troubleshooting
3.2. Cascade control between R-71101Inlet temperature and fuel gas pressure
Influencing factor Remedies
Fuel gas composition change According to composition change,
regulate fuel gas flow rate
Unsteady Feed Investigate. Find whether filter is
clogged. Stabilize feed
Unsteady hydrogen flow rate Check whether K-71101 fails and
troubleshoot
Feed contain water Enhance tank dehydration or change
feeding tank
Unsteady D-71101 pressure Use PV1002 and hydrogen make-up
control line to control D-71101 pressure
ISSUE DATE: 20/03/06 - 46 -
KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION NORMAL OPERATION
CCR UNIT KRCIM 71100.05 REV.0
3.3. C-71101 pressure controlled with pressure control valve PV1004 on D-71103
gas outlet
Influencing factor Remedies
Feed rate fluctuation Control liquid level and stabilize feed
rate
Feed property change Regulate operation and check water
Tower bottom temperature Stabilize reboiling furnace operation,
fluctuation stabilize tower bottom temperature
Reflux rate unsteady Check reflex pump normal or not,
regulate reflux rate
A-71102A/B cooling effect Check air cooling belt and regulate
poor cooling water rate
3.6. Arsenic, lead & copper content exceed limits in hydrotreated naphtha
Influencing factor Remedies
Too high arsenic, lead & Contact dispatch, change feedstock
copper content in feedstock
Catalyst activity falls Increase reaction temperature.
E-71101A/B Feed Feed reformer with desulphurized naphtha and
exchanger leak treat the exchanger leakage
Low reaction temperature Increase reaction temperature or pressure
or pressure
Test analysis error Contact lab for reanalysis
4. Analysis Control
4.1. Recommended Methods And Frequency
The frequencies given here below are related to routine operation.
Table of Contents
1. Unit Introduction
2. Manual Structure
1. Unit Introduction
1.1. General
Continuous Catalytic Reforming Unit (CCR) of Khartoum Refinery Company is built
under the expansion project of the refinery, phase II. The unit is designed by
Sinopec Engineering Incorporation. The process utilizes Axens's "State of the art"
moving catalyst bed with continuous catalyst regeneration.
The unit is designed to process 400,000 metrics tons per year and to operate at a
severity of RON 98 with an on-stream factor of 8000 hours/year.
would lead to very short cycle length. Hence CCR unit involves continuous catalyst
regeneration.
Continuous regeneration eliminates the need of shutdown for regeneration of the
earlier fixed bed reformers. It also minimizes the amount of catalyst in the unit, while
allowing high reformate yield and quality.
2. Manual Structure
The design information and operating instructions of the Continuous Catalytic Reforming
Unit (unit71) are covered by six different volumes as follow:
1. Basis Of Design
2. Unit Description
1. Basis Of Design
Composition, wt P N A
%
C5 - 3.74 0.37 0.00
C6 8.93 0.14
2.27
C7 13.32 4.81 0.90
C8 17.32 7.00 2.00
C9 15.98 5.59 2.25
C10 8.99 2.12 0.94
C11 + 3.12 0.19 0.00
Total 71.42 22.35 6.23
1.2.1. Impurities
The reforming catalyst is a high purity alumina based catalyst, impregnated with
platinum and promotors. It is highly sensitive to impurities in the feedstock.
Some are considered reversible poisons, others irreversible.
Following table lists the maximum allowable limits of impurities in the feed. It is
critically important than the performance of the naphtha hydrotreating is such
that the impurity levels in the reforming feed do not exceed these levels.
Discussions regarding feed poisons and their effects will be discussed further in
this book.
Contaminant wt ppm
Sulphur 0.5
Nitrogen (organic) 0.5
Water 5
Arsenic 5 ppb
Olefins 0
Diolefins 0
Metals 5 ppb
Halogens (F, C1) 1
1.4.1. Reformate
The reformate is the product collected at stabilizer bottoms which the
specification is shown in the following table:
SOL/EOL
Spgr 0.796
RVP, kPa 33.1
RON C 98
MON C 88
C4 content, wt% 1.0 maxi
ASTM distillation, °C
IBP 45
10% 70
50% 127
90% 165
EBP 205
Flowrate (kg/h) SOL 44 082
EOL 43 379
1.4.3. LPG
Composition, wt %
SOL EOL
C2- 5.6 5.4
C3 26.6 24.8
C4 66.9 68.9
C5+ 0.9 0.9
Total 100.0 100.0
Spgr 0.536 0.538
Flowrate (kg/h) 1 157 1 615
Pressure Temperature
Medium pressure
Minimum 3.3 MPa g 380°C
Normal 3.5 MPa g 400°C
Maximum 3.7 MPa g 420°C
Low pressure
Minimum 0.9 MPa g 220°C
Normal 1.0 MPa g 250°C
Maximum 280°C
1.6.3. Water
Cooling water - supply
Minimum: 0.40 MPa g 32°C
Maximum: 0.50 MPa g 32°C
1.6.4. Air
Pressure Temperature
Plant Air
Minimum: 0.60 MPa g
Normal: 0.80 MPa g
1.6.5. Nitrogen
1.6.6. Fuel
Fuel gas
Minimum: 0.30 MPa g
Normal: 0.35 MPa g
Maximum: 0.40 MPa g
SOL EOL
Reforming reactors inlet/outlet temperature
st
1 reactor R-71201 514/393 529/418
*
Space velocity, WHSV h-1 1.9 1.9
1.7.4. Yields
The estimated ex-reactors yields are expressed including recycle gas :
SOL, wt % EOL, wt
%
H2 5.34 5.02
METHANE 1.08 1.37
ETHANE 1.38 1.75
PROPANE 2.68 3.38
NBUTANE 3.41 4.29
IBUTANE 2.18 2.75
NPENTANE 2.53 2.50
IPENTANE 4.84 4.77
NHEXANE 2.46 2.40
IHEXANES 7.65 7.48
METHYLCYCLOPENTANE 0.75 0.73
CYCLOHEXANE 0.00 0.00
BENZENE 2.13 2.07
C7 PARAFFINS 7.45 7.23
C7 NAPHTENES 0.07 0.06
TOLUENE 8.91 8.63
C8 PARAFFINS 3.97 3.84
C8 NAPHTENES 0.04 0.04
C8 AROMATICS 17.56 16.98
C9 PARAFFINS 0.68 0.66
C9 NAPTHENES 0.01 0.01
C9 AROMATICS 16.93 16.36
C10+ PARAFFINS 0.00 0.00
C10+ NAPHTENES 0.00 0.00
C10+ AROMATICS 7.94 7.68
C5+ 83.92 75.29
Total 100.00 100.00
2. Unit Description
2.1. Introduction
Naphtha feed to a Catalytic Reforming unit typically contains C6 to C10 paraffins,
naphthenes and aromatics. The purpose of this reforming process is to produce
aromatics from naphthenes and paraffins either for use as a high octane gasoline
blending component or as a source of specific aromatic compounds.
Naphthenes convert rapidly and efficiently to aromatics. Paraffins do not, requiring
higher severity conditions and even then conversion is slow and inefficient.
In this process, conversion is achieved by passing the naphtha over a slow moving
bimetallic catalyst bed in three adiabatic reactors, in the presence of hydrogen at
relatively high temperature and low pressure. Operating under these conditions of
low pressure and high temperature, the rate of coke laydown on the catalyst is
relatively high. A semi-regenerative type process is impractical in this case, a
continuous catalytic regeneration unit is necessary. In this process, catalyst is
withdrawn from the reaction section at a fixed rate, regenerated in the continuous
catalytic regeneration unit and returned fresh to the reaction section.
The rate of catalyst withdrawal and regeneration ensures a consistently highly active
catalyst with a low carbon content and controlled chloride/water content. This
maximises yields of both reformate and high quality hydrogen off-gas.
Vapor from D-71205 is routed to fuel gas under pressure control. This stream is
predominantly light ends i.e. C1 and C2's and this controls the stabilizer
operating pressure. Separated liquid from this drum is pumped by P-71204
through the stabilizer feed/bottom exchanger E-71208 to enter the stabilizer C-
71201. The stabilizer operating at an average of 1.70 MPa g, reduces the C4 in
the reformate to less than 1.0 wt %. The stabilizer is reboiled with a fired
reboiler F-71205, circulating with reboiler pump P-71202, with temperature
control on stabilizer.
C-71201 overheads are partially condensed in air cooler A-71202 and
subcooled to collect in D-71204, the stabilizer reflux drum. The overhead vapor
is routed back to D-71205 for LPG recovery. The separated liquid is pumped by
P-71203 under flow control back to the top of C-71201 as reflux. A split stream
of the liquid is withdrawn as LPG from P-71203, discharge under level/flow
control and is routed to LPG battery limit.
Bottoms from the stabilizer after partial cooling in the stabilizer feed/bottom
exchanger constitutes the reformate which is sent under flow control with level
reset to battery limits.
Contents: The aim of the information given in this document is to provide enough
theoretical basic background to support the instructions given in the
chapters that follow: Startup of the unit, Operation of the unit, Shutdown
of the unit.
The objective is to help the operators to better understand the reasons
of the operating instructions and enable them to make wise decisions,
should the circumstances deviate from what is covered in the operating
instructions.
2. Chemical Reactions
The heat of the reactions mentioned hereafter as well as their relative rate are
necessary to understand the process. They are listed for the ease of reference in
Table 1, below. A catalyst is being used to promote the desirable reactions at the
expense of the adverse ones through its action on reaction kinetics.
TABLE1
Reforming reactions heat of reaction - relative rate of reaction
Reactions Heat of reaction Relative rate
(1) KCAL/MOLE (2) approx.
Naphthenes dehydrogenation - 50 30
Paraffin dehydrocyclization - 60 1 (base)
Isomerization: Paraffins +2
3
Naphthenes +4
Cracking + 10 0.5
(1) Heat of reaction < 0 = endothermic reaction.
(2) For pressure below 1.5 MPa.
Naphthenes dehydrogenation
Naphthenic compounds i.e. cyclohexane, methylcyclohexane,
dimethylcyclohexane up to C10 naphthenes are dehydrogenated respectively
into benzene, toluene, xylenes, C9 and C10 aromatics with the production of 3
moles of hydrogen per mole of naphthene.
The cyclohexane reaction, for instance, writes as follows:
CH CH
2
HC CH HC
2 2 CH
+ 3H
2
HC CH HC CH
2 2
CH CH
2
Cyclohexane Benzene
Cyclohexane Benzene
At the selected operating conditions the reaction is very fast and almost total. It
is promoted by the metallic function of the catalyst. Since it yields a high octane
product, promoting this reaction is most desirable. Refer to octane number
below:
RON MON
Cyclohexane = 83 77.2
Methylcyclohexane = 74.8 71.1
1.3 dimethylcyclohexane = 71.7 71.
Benzene = 114.8 > 100
Toluene = 120 103.5
m-Xylene = 117.5 115.
RON: Research Octane Number
MON: Motor Octane Number
Paraffins dehydrocyclization
This is a several step process which applies either to the normal paraffins
(linear) or ISO-paraffins (branched). It involves a dehydrogenation with a
release of one hydrogen mole followed by a molecular rearrangement to form a
naphthene and the subsequent dehydrogenation of the naphthene. The
molecular rearrangement to build a naphthene is the most difficult reaction to
promote but the subsequent aromatization of the naphthene yields a noticeable
octane increase.
CH CH CH CH CH CH
2 2 2 2 2
+H
CH CH CH CH CH CH CH 2
3 2 2 3 3 CH 2 3
C H C H
7 16 7 14
CH CH
2 2
CH CH CH CH
2 2
H C CH
2 3
CH CH CH CH
3 2 3 CH CH
2 2
Met hylcyclohexane
CH CH CH CH
2 2
C
H C CH CH
3 HC CH + 3H
2 3 2
CH CH CH CH
2 2
T oluene
C H
7 16 C H
7 16
These reactions are fast, slightly exothermic and do not affect the number of
carbons. The thermodynamic equilibrium of isoparaffins to paraffins depends
mainly of the temperature (see table hereafter). The pressure has no effect.
Iso-N paraffin equilibria
Carbon atom C4 C5 C6 C7 C8
% Isoparaffin at 44 58 72 80 88
500°C
Napththenes isomerization
The isomerization of an alkylcyclopentane into an alkylcyclohexane involves a
ring rearrangement and is desirable because of the subsequent
dehydrogenation of the alkylcyclohexane into an aromatic. Owing to the
difficulty of the ring rearrangement, the risk of ring opening resulting in a
paraffin is high.
The reaction is slightly endothermic. The reaction can be summarized as
follows:
RON MON
Ethylcyclopentane = 67.2 61.2
Methylcyclohexane = 74.8 71.1
Toluene = 120 103.5
Cracking
Cracking reactions include hydrocracking and hydrogenolysis reactions.
Hydrocracking affects either paraffins (normal or iso) or naphthenes. It involves both
the acid and metallic function of the catalyst. It is, to some extent, a parallel reaction
to paraffin dehydrocyclization.
It can be schematized by a first step of dehydrogenation which involves the metallic
function of the catalyst, followed by a breakage of the resulting olefin and the
hydrogenation of the subsequent short chain olefin. The second reaction is
promoted by the acidic function of the catalyst.
(m)
+H
2
C H C H
7 16 7 14
(a)
+
+H
2
C H
7 14 C H C H
4 8 3 8
(m)
+H
2
C H C H
4 8 4 10
The first reaction involves the same reactants as the dehydrocyclisation and is
likewise catalysed by the metallic function.
Hydrocracking also affects the naphthenes, the overall reaction can be
summarized as follows:
+H
2
C H
6 14
CH - C H
3 5 9
or
+H
2
C H
CH - C H 7 16
3 6 11
Hydrogenolysis
This undesirable reaction has some similarity with hydrocracking since it involves
hydrogen consumption and molecule breakage. But it is promoted by the metallic
function of the catalyst and leads to lighter hydrocarbon C1 + C2 - even less
valuable than LPG (C3 + C4).
It can be schematized as follows:
+H CH +
4
2
C H C H
7 16 6 14
or
+H C H +
2 6
C H 2
7 16 C H
5 12
Like hydrocracking it is exothermic and favored by high pressure and high
temperature.
Both hydrogenolysis and hydrocracking may induce runaway reactions owing to their
exothermicity.
Hydrodealkylation
Hydrodealkylation is the breakage of the branched radical (-CH3 or -C2H5) of an
aromatic ring.
Xylene (two radical groups) can be dealkylated into toluene (one radical group)
which in turn can be dealkylated to benzene.
The standard representation is:
+H + CH
4
2
Xylene T oluene
+H + CH
4
2
T oluene Benzene
Hydrodealkylation consumes hydrogen and produces methane. It is favored by high
temperature and high pressure and promoted by the metallic function of the catalyst.
At the operating conditions and with the selected catalyst this reaction is not
significant.
Alkylation
Alkylation is a condensation reaction which adds an olefin molecule on an aromatic
ring. It results in an aromatic with an increased molecular weight. The reaction writes
as follows:
CH
3
+ CH = CH - CH HC
2 3
CH
3
Benzene Propylene Isopropylbenzene
This reaction, promoted by the catalyst metallic function, is not hydrogen consuming.
But it leads to heavier molecules which may increase the end point of the product. In
addition the high molecular weight hydrocarbons also have a high tendency to form
coke. This reaction must be avoided.
Dismutation
Two toluene rings (one branched CH3 radical) can dismute to produce one benzene
ring (no branched radical) and one xylene ring (two branched radicals), as shown:
+ +
Coking
Coke formation on the catalyst results from a very complex group of chemical
reactions, the detailed mechanism of which is not fully known yet.
Coke formation is linked to heavy unsaturated products such as polynuclear
aromatics (or polycyclics which can be dehydrogenated) resulting either from the
feed or from the polymerization of aromatics involved in some of the reforming
reactions (dehydrocyclisation, dismutation,...). Traces of heavy olefins or diolefins
may also result from the reforming reactions (dehydrocyclization, alkylation, for
instance) and promote coke formation.
A high end boiling point of the feed likely means greater amount of polyaromatics
and then a higher coking tendency. Since polymerization is promoted by high
temperature, poor distribution in a reactor favors local high temperatures and coke
build up.
Coke deposit on the catalyst support reduces the active contact area and greatly
reduces catalyst activity.
Low pressure unfortunately favors coke formation (see Fig. 1). This is why a low
pressure reforming (which has a lot of advantages) requires a continuous
regenerated catalyst. In CCR the continuous catalyst regeneration loop maintains a
controlled low coke content on the catalyst while operating at low pressure.
The effect of the main operating conditions on the rate of the reactions involved in
the reforming process using the selected catalyst (Refer to “Catalyst selection and
description”) is summarized below.
Figure 1 show, with a logarithmic scale, the relative rate of the various reactions
as a function of hydrogen partial pressure. The dehydrogenation rate is used as
reference and taken at 100 (Log 100 = 2). Other reaction rates are measured
against this reference.
At 1.0 MPa hydrogen partial pressure, the dehydrogenation of naphthene is
about 10 times, faster than isomerization, 30 times faster than
dehydrocyclization and 50-60 times faster than cracking (hydrocracking and
hydrogenolysis).
At relatively high pressure (above 2.0 MPa) the rate of coking is low compared
to the other reactions but it increases noticeably at lower pressure.
To sum up, figure 1 shows that there is an incentive to operate at low
pressure: cracking rate will be reduced and dehydrocyclization rate
increased.
On another hand thermodynamics also favors low pressure for
dehydrogenation and dehydrocyclization. The only drawback of low pressure is
the high coking rate but this is compensated by continuous catalyst
regeneration.
The kinetic study of the chemical reactions becomes even more complicated
owing to the presence of molecules with different numbers of carbon atoms.
As is the case for thermodynamic equilibriums, it appears that the rates of the
reactions are affected by the length of the chain of the reactant. Figure 3
presents the rates of dehydrocyclization and cracking of C6 to C10 paraffins
related to that of n-heptane, as a function of the number of carbon atoms of
reactant.
Figure 3 shows that the cracking reaction rate, (the curve represents in fact the
sum of hydrocracking and hydrogenolysis), increases regularly with the number
of carbon atoms, whereas dehydrocyclization rate exhibits a sudden increase
between hexane and heptane as well as between heptane and octane, while
the variation between the higher homologues remains relatively slight.
To sum up, the dehydrocyclization of C6 paraffins to benzene is more
difficult than that of C7 paraffin to toluene, which itself is more difficult
than that of C8 paraffin to xylenes. Accordingly the most suitable fraction
to feed a reforming process is the C7-C10 fraction.
CONCLUSIONS:
From the above analysis it can be concluded:
Dehydrogenation reactions are very fast, about one order of magnitude
faster than the other reactions.
Low pressure favors all desirable reactions and reduces cracking. To
compensate the detrimental effect of low pressure on coking, low
pressure reformer requires continuous catalyst regeneration.
An increase in temperature favors the kinetics of dehydrogenation,
isomerization, dehydrocyclization, but accelerates the degradation
reactions (cracking, coking) even more. Consequently an increase in
temperature leads to an increased octane associated with a decrease in
reformate yield.
The reaction rates of such important reactions as paraffins
dehydrocyclization increase noticeably with the number of carbon atoms.
Cyclization is faster for C8 paraffin than for C7, and for C7 than for C6.
Consequently the C7 - C10 fraction is the most suitable feed.
taking account of the feed quality (PNA, distillation range ...) and product
requirement (octane).
Owing to the great endothermicity of the most important and desirable reactions
(naphthenes dehydrogenation and paraffins dehydrocyclization) this optimum
temperature cannot be sustained through out the whole catalyst volume. In addition,
dehydrogenation is also, by far, the fastest reaction, which means that the
temperature drops very sharply over the first part of the catalyst. In order to restore
the catalyst activity, when temperature has dropped to a certain level which depends
upon the reactions involved, the reactor feed is reheated. To achieve this, the
catalyst is distributed in three reactors and intermediate heaters are provided.
Figures 4 and 5 illustrate this question, Figure 4 shows for a given feed (Paraffins:
45% LV, Naphthenes 45% LV, Aromatics 10% LV) the profile of the amount of P.N.A
along the catalyst volume. In this case there is no need to have more than 20% of
the catalyst in the first reactor because the naphthenes dehydrogenation results in a
temperature too low to sustain the reaction any longer. The reactor effluent is
reheated to allow for the naphthenes hydrogenation to continue and the paraffin
dehydrocyclization to start. Over the next 30% of catalyst, distributed in the 2 nd
reactor, temperature drops again to a level where reheating is required to enable the
paraffin hydrocyclization to proceed.
The catalyst distribution in this case is:
R1 = 20%
R2 = 30%
R3 = 50%
Each specific case has, obviously, a specific catalyst distribution.
In a somewhat simplified but practical way, for operational guidance, the main
reactions take place in the various reactors in the following order:
1st reactor:
Dehydrogenation
Isomerization
2nd reactor:
Dehydrogenation
Isomerization
Cracking
Dehydrocyclization
3rd reactor:
Cracking
Dehydrocyclization
3. Catalyst
3.1. Activity, Selectivity, Stability
The main characteristics of a catalyst other than its physical and mechanical
properties are:
The activity which expresses the catalyst ability to increase the rate of the reactions
involved. It is measured by the temperature at which the catalyst must be operated
to produce a reformate of a given octane number, for a given feed and given
operating conditions.
The selectivity expresses the catalyst ability to favor desirable reactions rather than
others. It is practically measured by the C5+ reformate and hydrogen yields, for a
given feed and octane number, and given operating conditions.
The stability characterizes the change with time of the catalyst performance (i.e.
activity, selectivity) when operating conditions and feed are stable. It is chiefly the
coke deposit which affects stability, through its inhibition of the catalyst acidity and
decrease of metal contact area. Traces of metal in the feed also affect stability
adversely.
Stability is generally measured by the amount of feed treated per unit weight of
catalyst (i.e. m3 of feed per kg of catalyst). C5+ wt reformate yield at steady
conditions is also an indirect measure of the stability.
OH Cl OH OH
elution
Al Al + H 20 Al Al + ClH
chlorination
O O
The simplified theory, generally accepted today, is that the optimum acidity
level (which varies with the requested performance) is a function of ratio of the -
OH bonds to the Cl- bonds, which are adsorbed at the catalyst surface. This
ratio, in turn, is a function of the water and HCl content in the recycle gas,
because of the equilibrium which exists between water and HCl in the recycle
and OH- and Cl- bonds on the catalyst.
Good acidity of the catalyst is controlled by the balance between H 2O and HCl.
An excess of water in the recycle will shift the balance towards excess of OH-
and thus reduce the activity.
Conversely, if the amount of water in the recycle is too low (an infrequent
case) the catalyst is reputed too dry, and the OH- to Cl- balance is shifted
towards Cl-. In other words, the catalyst is over-chlorinated, which means its
TABLE 2
Decrease of acidic Increase of acidic Decrease of metallic
function function function
Pt + H2S PtS + H2
and consequently it reduces the activity of the catalyst while decreasing the
metallic contact area.
The same type of reaction occurs with H2S towards the other catalyst
promoters, and further reduces the catalyst activity.
Effect of sulfur contamination
Sulfur contamination inhibits the metal function of the catalyst. This is indicated
by:
A decrease in hydrogen and liquid product yields
A decrease in recycle purity
An increase in hydrocracking (LPG yield increase)
A reduced temperature drop in the reactors
Prevention and causes of contamination
Sulfur removal is achieved by pretreating the naphtha feed, which results in
H2S production. Poor operation of the pretreater is generally the cause of sulfur
poisoning of the reforming catalyst:
Either low activity of the hydrotreater catalyst
Or too low hydrotreater reactor temperature
which leads to an insufficient sulfur removal. Unsatisfactory operation of the
hydrotreater stripper can also result in dissolved H2S being fed to the reforming
unit.
An additional protection to avoid H2S upsets to the reforming unit is to provide
a sulfur guard reactor on the feed.
Detection
Analytical methods are available to detect sulfur in the unit feed. A very easy
way, however, is to check sulfur content in the recycle gas using Draeger
tubes. The H2S content in the recycle which corresponds to the 0.5 ppm wt in
the feed, is approximately 1 ppm (volume).
Remedies:
When the sulfur content in the recycle gas increases, the reactor inlet
temperature must be reduced.
Typically for an H2S level of 5 vol. ppm in the recycle the reactor inlet
temperature must be lowered to 480°C ; the reformer feed must be reduced
accordingly to maintain product quality (octane number). These conditions must
be maintained until the cause of the upset has been found and corrected.
The high severity operating conditions can only be resumed when the H 2S
content in the recycle gas is lower than 1 ppm vol.
Nitrogen
Nitrogen is less frequently present in the reforming feed than sulfur. Scarcely
present in straight run naphtha, nitrogen is a usual impurity of cracked naphtha
and may also result from injection of amine based corrosion inhibitors.
The maximum allowable concentration in the feed is 0.5 wt ppm expressed as
organic nitrogen.
Mechanism
In fact, organic compounds containing nitrogen are responsible for inhibition but
nitrogen gas itself (N2) has no detrimental effect.
Contamination is due to NH3 formed by decomposition of compounds
containing organic nitrogen, on the catalyst. Then NH3 which is alkaline, reacts
with chlorine decreasing the acidic function of the catalyst and producing
ammonium chloride NH4Cl. This compound is volatile in the conditions of the
reactors and is eliminated inducing a loss of chlorine.
The reaction can be schematized as follows:
Cl OH Cl Cl OH OH
NH3 + H O2 + Al Al Al
Al Al Al + HCl + NH
3
O O O O
and HCl + NH NH Cl
3 4
Effect of nitrogen contamination
Nitrogen contamination reduces the acidic function and is indicated by:
A decrease in octane
An increased hydrogen production
A reduced reactor temperature drop
On top of this, ammonium chloride in the recycle gas can deposit in coolers,
separators compressors etc. creating mechanical problems.
It is worth remembering that 0.5 ppm wt of organic nitrogen in the feed leads to
approximately 2 T/year of NH4 Cl for a 1 106 T/y unit.
Prevention and causes of contamination
Organic nitrogen removal is also achieved by naphtha pretreating of the feed.
But it shall be emphasized that nitrogen removal is more difficult than sulfur.
Efficient nitrogen removal often requires the use of a specific catalyst, also
active for desulfurization, but generally operating at higher hydrogen partial
pressure. Naphtha, with high nitrogen content must not be fed to a pretreater
not designed for it.
Detection
Since water contamination is a major concern of the operator, on line analyzer
is usually provided in the recycle gas line.
Operating experience shows that the optimum water content in the recycle gas
must be within a range of 15 to 25 ppm (vol.). The associated chlorine level will
then be between 1 to 2 ppm vol.
Above 50 ppm vol. of water, the reactor inlet temperature must be lowered to
reduce the chlorine elution from the catalyst. The following figures are generally
accepted:
50 ppm water Temperature < 480°C
100 ppm water Temperature < 460°C
Below 10 ppm of water in the recycle gas, the catalyst acidic function is
enhanced. Water injection must be used: 1 ppm wt in the feed results in an
increment of 2 to 5 ppm vol. in the recycle.
Remedies
In case of water upset,
Adjust chlorine injection to make up for the increased chlorine loss
Decrease reactor inlet temperature as indicated above
Restore operating conditions upstream of the unit to reduce water
contamination
Check amount of oxygenated compounds in the feed
TABLE 3
Poisons Max. level (wt) Source
Arsenic 5 ppb max Cracked Naphthas
Lead 5 ppb max Recycled slops
Copper < detection limit Corrosion
Mercury 5 ppb max Naphtha - condensates
Iron < detection limit Corrosion
Silicon < detection limit Additives (foaming)
Nickel < detection limit Corrosion
Chromium < detection limit Corrosion
Mechanism
Most metals poison the metal function (platinum and promoter) of the catalyst.
Metal poisons tend to affect the first reactor, then to break through and affect
nd
the 2 reactor. The first reactor is typically the reactor where the poisoning is
first detected.
Effect of metal contamination
Metal contamination is characterized by:
A dramatic decrease of the T in the first reactor associated with an
increased T in the second reactor
A decrease in octane number
An increase in liquid product yield
In addition, mechanical problems may result from the collection of
corrosion products (scale, rust...) in the first layer of the first catalyst bed,
or the accumulation of scale, rust in the dead ends, of the first reactor
Prevention and causes of contamination:
The contaminants and the source of contamination are listed in Table 3 above.
Prevention consists of adequate hydrotreating and appropriate material
selection to limit corrosion.
Metal poisons are generally partially retained on the upstream hydrotreating
catalysts. However the retention capacity is limited and breakthrough may
occur. Such a breakthrough would result in a very harmful situation for the unit
since theses poisons would not be eliminated by the catalyst regeneration.
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PRODUCTION & OPERATION PROCESS THEORY
CCR UNIT KRCIM 71200.03 REV.0
S wt ppm = ~ 300
Pb wt ppm = ~ 200
As wt ppm = ~ 200
Zn wt ppm = ~ 400
Co wt ppm = ~ 400
Cr wt ppm = ~ 400
Mo wt ppm = ~ 400
Cd wt ppm = ~ 400
Cu wt ppm = ~ 400
Fe wt ppm = ~ 3000
Si wt ppm = ~ 400
Na wt ppm = ~ 300
Ca wt ppm = ~ 300
K wt ppm = ~ 300
High selectivity offering maximum C5+ and hydrogen yield at very low
pressure.
Low coke make offer the possibility to increase throughput without revamping of
regenerator.
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PRODUCTION & OPERATION PROCESS THEORY
CCR UNIT KRCIM 71200.03 REV.0
4. Process Variables
4.1. Independent Variables
The process variables are:
Pressure
Temperature
Space velocity
Hydrogen partial pressure or H2/HC recycle ratio
Quality of the feed
The above are independent variables: each of them can be fixed by the operator -
within the operating range of the equipment - independently from the others.
For one set of independent variables, there is only performance of the unit i.e. one
set of values for:
Product yields
Product quality (octane)
Catalyst stability (coke make)
In this chapter we examine the effect on the unit performance of each independent
variable taken separately.
4.1.1. Pressure
Hydrogen partial pressure is the basic variable because of its inherent effect on
reaction rates. But for the ease of understanding total reactor pressure can be
used. Reactor pressure is most accurately defined as the average catalyst
pressure. Due to catalyst distribution in the reactors, it is usually close to the
last reactor inlet pressure.
All the hydrogen producing reactions i.e. dehydrogenation, dehydrocyclisation
are enhanced by low pressure.
The lower the pressure the higher the yields of both reformate and hydrogen for
a given octane number. This is the reason for minimizing unit pressure drop
and operating at the lowest practical pressure. Low pressure however
increases the coke make.
Operators action on pressure is limited:
Operating pressure rise is limited by equipment design pressure
Operating pressure lowering is limited by recycle compressor design
power and intake volume
4.1.2. Temperature
Catalyst activity is directly related to reactor temperature. Thus the most direct
operating variable available for the operator, to control product quality and
yields, is the reactor inlet temperature.
In the CCR unit the coke amount on the catalyst is maintained at a constant low
level through the continuous regeneration. Consequently a temperature
adjustment is required only:
To change the reformate octane
To process a different feed quantity
To process a different feed quality
To balance a temporary loss of activity due to a temporary poisoning
To balance catalyst ageing which occurs slowly over several years
An increase of the reactor inlet temperature results in :
An increased conversion of the non aromatic compounds of the feed
mainly the paraffins
But since the hydrocracking reaction is more favored than the cyclization of
paraffins, the end result is:
An increased octane but a decrease in reformate yield
An increase of the coke deposit
The inverse of the liquid hourly space velocity i.e. (LHSV)-1 is linked with the
residence time of the feed in the reactor. The space velocity then affects
directly the kinetics of the reforming reactions.
A decrease in the space velocity means an increased residence time, hence a
higher severity which results in increased octane, lower reformate yield, higher
coke deposit.
When changing feed rate, an important recommendation derives from the
above:
Always decrease reactor inlet temperature first and decrease feed flow
rate afterwards.
Always increase feed flow rate first and increase temperature afterwards.
Hence, for a required octane number, the lighter the feed the higher the
required severity or, conversely, at constant severity, low initial boiling point
results in lower aromatic and hydrogen yields.
In recent years, the restriction of benzene content in gasoline has resulted in
selecting feed with IBP above 82°C (180°F) to eliminate cyclohexane.
Heavy fractions have a high naphthenic and aromatic hydrocarbons content,
thus they need a lower severity to obtain good yields. But these fractions
contain also polycyclic compounds which produce a high coke deposit on the
catalyst. High final boiling point of the feed is favorable up to a certain level,
detrimental above. An end boiling point above 180°C (350°F) is generally not
recommended.
Chemical composition
The detailed chemical composition of the feed is determined by gas
chromatography analysis. This analysis is necessary to predict the aromatics
and hydrogen production as well as the severity of the operation.
Even if not sufficient for a complete prediction, an index of characterization of
the feedstocks related to the actual and potential aromatics content of the feed,
proved very useful. N + 2A has long been used (N and A volume % of
naphthenes and aromatics in the feed). AXENS now uses 0.85 N + A which is
found to be more representative.
The higher this index, the lower the severity of operation to meet the same
product specifications. The lower this index (i.e. the higher the paraffins
content), the higher the severity of operation to meet the same product
specifications as the dehydrocyclization of paraffins becomes important.
Impurities in the feed
The catalyst activity can be reduced, either temporarily or permanently by
poisons contained in the feed (refer to “Catalyst contaminants”). Table 4
specifies the maximum allowable amount of each contaminant.
TABLE 4
Maximum allowable impurities (wt) in the feed
4.1.6. Summary
Table 5 summarizes the theoretical effect on the unit performance of each
independent process variable taken separately.
TABLE 4
EFFECT OF PROCESS VARIABLES
Pressure
Temperature
Space velocity
H2/HC ratio
A + 0.85 N
Naphtha
End boiling point
Quality
5. Supplements
1. Plant Inspection
2. Cleaning of Piping and Equipment
1. Plant Inspection
The plant should be carefully checked to assure that it is constructed according to the
applicable plans, drawings and specifications. A check against the P&ID's is done for
piping, equipment and instrumentation. A, "punch list" of missing, incomplete, or incorrect
items is then prepared for correction.
This check is carried out during the final stages of construction work, under the direction
of the Pre-commissioning group in charge of the unit. Typically, this checking (which can
be called conformity to P&ID's check) is useful when construction progress is 70% or
above. Several checks can be made simultaneously depending upon the completeness of
each section or system of unit at that time.
Smooth Start-Up will depend on a large degree on the thoroughness with which the unit is
checked out beforehand. Every installation details must be checked against the design
specifications and standards and for good construction practice.
General Inspection
A general inspection of the equipment is made against the design drawings
after erection. This check includes:
Verification of temperature/pressure and vacuum rating on nameplate
Verification of lining condition (if applicable)
Nozzle location, size, flanges face
Thermowell location and length of immersion
Cleanliness
Sliding Supports
When equipment experiences a temperature change it undergoes thermal
growth. Supports are provided to allow and guide this growth. It is therefore of
great importance that all supports are inspected and special attention is given
to large horizontal vessels and heat exchangers
Internal Inspection
Drums and vessels will be inspected internally by observation with a light. The
bottom manhole should be left open in case tools or other materials are
accidentally dropped down
Check that no scaffolding or trash remains in the vessel
Vessels and tower internals must be inspected carefully and checked
against the design documents to ensure that the installation was
properly carried out. This check should include:
Trays: number, location, type, spacing, levelness, weir height,
downcomers, valve number and operation, support bolting.
(Tightness testing is usual for chimney trays). Especially check
that all valves on valve type tray are clean and free to move.
Check that weep holes, where provided, are not plugged.
Distributors: location, alignment, size and number of openings.
Vortex breakers: type, size and orientation
Demisters: size, material and support
Check that baffles in the bottom of the columns are correctly fitted, type,
orientation and levelness
Check that instrument nozzles are clear. Check those, which are
accessible from inside the vessel, on the aeration air. Those, which are
accessible only from the outside, will be checked during the air tightness
test that will be implemented prior to inerting by observing that the
instrument vent valve is passing air
Cleaning
All vessels, columns, drums, tanks, etc. have to be inspected and cleaned if
required, before final closure, boxing-up.
The Pre-commissioning team witnesses the final cleaning, especially if the
relevant vessel has been integrated in a cleaning sequence.
If the capacity is used as a buffer capacity, make sure that air is evacuated
from the vessel to lines and not reverse.
When the vessel is used as "collecting device", it must be finally closed only
after cleaning.
Vessel cleaning is normally performed in different ways according to the
equipment materials.
Equipment internal materials are generally the following:
Carbon steel
Stainless steel
Carbon steel lined with different coating material
Final Inspection
Vessels final closure (boxing-up) will occur after blowings/flushings are
implemented during the precommissioning phase. Therefore, a vessel may be
required, after a first inspection for conformity against design and drawings, to
be closed temporarily by the precommissioning group until final inspection.
After blowing/flushing (if required), cleaning and dryout, a final vessel
inspection should be done.
Carefully inspect for cleanliness. After a positive final inspection result, vessel
shall be immediately closed, and a "Final Box Up Certificate" will be signed
1.1.2. Pumps
1.1.2.1.7. Temporary strainers are provided for the suction of each pump to be
installed on the pump side of the suction block valves. These
strainers should be installed after the suction lines are flushed. These
should be cleaned frequently to keep lines free of foreign matter. The
strainers should be cleaned frequently by alternating pumps where
possible. Except on severe services, which may require installation of
fine mesh on both pumps A and B, it is normally sufficient to equip
only one pump with fine mesh (on all "A" pumps for instance).
Consequently, "A" pumps will be the ones preferentially started
during initial startup.
1.1.2.1.8. Then when temporary strainers are not anymore required they should
be removed and only the permanent strainer installed to prevent
further possible pump damage
1.1.2.1.9. Pumps are not field hydrostatically tested.
1.1.2.2.7. Check that the seal does not leak (if packed seal check that packing
nuts are not too slack) and that the seal flushing and cooling water
connections are correctly made.
1.1.2.2.8. Rotate centrifugal pump shaft by hand to test for free rotation but
never if the starter switch is not locked.
1.1.2.2.9. Confirm that the alignment check has been made on the pump shaft,
driver shaft and coupling.
1.1.2.2.10. Check that the coupling guard is secured over shaft.
1.1.2.2.11. Check that the grounding clip and wire is secured from motor to
grounding point.
1.1.2.2.12. Check that a discharge pressure gauge is installed and functioning.
1.1.2.2.13. Check that the electrician has tacked the pump power supply in
substation.
1.1.2.2.14. Check that if a pump is on a closed recirculation loop from a vessel,
the vessel is vented to atmosphere to prevent any possibility of
damage by pulling vacuum. A specific procedure will be issued with
marked down PID's for pump running with water prior to actual
start-up.
1.1.2.2.15. When a run with water has been planned the loop system should
be carefully isolated from the rest of the sections. The water make-
up should be sufficient to fill the whole loop and still leave a good
head available to the pumps.
1.1.2.2.16. Check arrangements to vent the pump for priming, if the pump is
not self venting.
1.1.2.2.17. Verify that special connections such as bleeds and drains are
properly installed.
1.1.2.2.18. Strainers must be installed before aligning pumps. A strainer is
provided for each pump suction line during start-up. To avoid pump
damage during flushing with water the strainers may be lined
temporarily with 20 mesh screens or as specified by the pump
manufacturer. Remove this temporary screen after water flushing is
completed and fit the permanent one.
1.1.2.2.19. To prevent equipment damage multistage centrifugal pumps in light
product service (specific gravity less than about 0.8) should not be
running with water.
1.1.2.2.20. All valves in the loop should be opened except for control valves
(manually closed from the control room) and the discharge valve of
the pumps. The operator at the control panel should then be
informed that the system is ready for operation.
1.1.2.2.21. If possible do not start the motor on a centrifugal pump with the
discharge valve open as this also throws an excessive load on the
motor (except if specified to start with fully open valve as auto start
cases).
1.1.2.2.22. When a hot pump is being kept hot by circulation of a stream
through it from an adjacent pump, the shaft of the motor may be
turning slowly in the direction opposite to normal rotation. If a pump
is running in this manner and is started up, an excessive load is
thrown on the motor. Therefore, if a standby pump is already slowly
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CCR UNIT KRCIM 71200.04 REV.0
1.1.4.9. Check that the correct motor oil has been put in and the storage protection
(light) oil removed if any.
1.1.4.10. Check the fan motor for proper rotation and grounding (never when the
motor is energized)
1.1.4.11. Set the fan blade pitch as per manufacturer's specification. Once the fan
is in operation, if motor amperage is too high or too low, pitch
readjustment may be required.
1.1.4.12. Set the vibration shutdown switches to give the permitted safe vibration
level
1.1.4.13. If the fan is belt driven adjust the drive belts for proper tension and check
belt condition. Confirm that the fan safety shields are in place.
1.1.4.14. Remove protection plywood that may have been laid on the tubes.
1.1.4.15. Check operation of louvers (if any).
1.1.4.16. When all above checks have been made, proceed to a 4 hours (except
otherwise agreed duration) test run and check the following points:
1.1.4.17. Check that the amperage of the motors is in the normal range.
1.1.4.18. Check for any noise from the bearings or other.
1.1.4.19. Check for any screeching or abnormal noises from the pulleys (belts
may be too tight, which will affect bearings).
1.1.4.20. Check that all belts remain on the pulleys (belts that constantly come off
could indicate offset pulley).
1.1.4.21. Check that air fan blades are not making any abnormal noise.
1.1.4.22. Check that air fans on the same cell are all turning at approximately the
same speed
1.1.4.23. Stop the air fans one by one and stand underneath to observe and
check the following:
1.1.4.24. Check that no abnormal noise occurs on the rundown.
1.1.4.25. Check that the air fans slowly come to a stop in a smooth manner.
1.1.4.26. Check by hand that the motor has not overheated.
1.1.4.27. If the motor is inside the safety screen cover and if motor overheating is
suspected or another intervention on the fan is required never remove
the safety screen by yourself.
1.1.4.28. Inform the Electrical Specialist which will follow the normal safety
procedure of electrical isolation in the substation by tagging off and
locking shut the electrical breaker for the motors.
1.1.4.29. Complete the run-in before using the air cooler condenser for any heat
transfer duty.
Instrumentation
1.1.5.1. Controllers, regulators, and recorders for flows, pressures and
temperatures: correct zero adjustment or designed values, normal
position, connections.
1.1.5.2. Thermocouples: length, location, and correct connection of cables.
1.1.5.3. Connections for controls (pressures, temperatures) and sampling.
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PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0
1.1.5.4. When not being used, connections should be closed off with threaded
plugs or blind flanges.
1.1.5.5. Carry out tests on all instruments that are part of the safety control
system.
1.1.5.6. Ensure that the necessary checking of the burners control system has
been performed.
1.1.5.7. Ensure that minimum stop positions have been set up on fuel gas and
combustion air systems (if any).
Stack Damper
1.1.5.8. The full-open and the minimum opening position of the damper should be
checked visually. The movement of the damper must be free and
unobstructed. Incorrect positioning will materially affect furnace operation
and may result in a great deal of difficulty in firing at higher rates.
1.1.5.9. Check the pneumatic actuator controls for proper operation (if any).
1.2.1. Commissioning of instruments will be carried out as the plant comes on stream.
Most attention will be directed towards liquid flow measurements: differential
pressure instrument piping must be drained to eliminate accumulated dirt and
water and the instrument zero must be adjusted to obtain a correct zero reading
on the scale on the control board instrument. Controllers must be tuned;
interface level transmitters must be zero checked; scale, weld slag and trash
must be removed from stricking control valves; other malfunctions must be
corrected. Inspection and commissioning of analyzers should include attention
to sample line lengths, analyzer enclosures, auxiliary equipment, such as
carrier gas for chromatography and other items as indicated in the instruction
manual for the particular analyzer.
1.2.2. Analyzers should be inspected, calibrated and commissioned in accordance
with procedures and instructions in the instruction manual for the analyzer. An
instrumentation engineer has to review installation and supervise calibration
and initial start-up. A vendor representative might be required for some specific
analyzers.
1.2.3. Chromatographs should be inspected to make sure that all external piping and
wiring are complete and that no parts have been lost or damaged in shipment.
1.2.4. Functional test for instrument loops have to be done prior to start-up to ensure
correct
1.2.5. operation of safety devices. ESD system interlocks and local/remote actions.
1.2.6. Proceed to the following checking. First, before energizing field instrumentation
and proceed to energized loop checks, confirm that the following static checks
are actually
1.2.7. implemented:
1.2.8. Clean air lines before connecting to instruments
1.2.9. Clean the instrument air supply headers by blowing with clean, dry air, and
check them for leak tightness.
1.2.10. Verify that pneumatic tubing is hooked up, that instrument air is available at
the instrument.
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PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0
1.2.11. Check piping from instruments to process piping and equipment for leak
tightness.
1.2.12. Isolate or remove in line components such as control valves, positive
displacement meters and turbine meters for pressure and leak testing if
specified tight shut off (already done in workshop normally.)
1.2.13. Reinstall these items after successful testing of the system.
1.2.14. Check orifice plate bore diameters versus documents.
1.2.15. Install orifice plates after completion of testing, draining, flushing and cleaning
of lines.
1.2.16. Isolate or remove inline components for flushing and cleaning operations.
Reinstall and/or reconnect after completion of cleaning and flushing
operations.
1.2.17. Verify correct positions and installation of inline instrumentation (control valve
flow direction and fall position, orifice plate installed in correct relation to flow
etc).
1.2.18. Perform all non-operating tests that ensure instrument operability: remove
shipping stops, check pointer travel, verify and adjust the instrument's
capability to measure, operate, stroke etc., in the direction and manner
required by the process application (direct or reverse controllers etc).
1.2.19. Perform functional loop checks and demonstrate correct operation (a
precommissioning record sheet with the relevant loop diagram).
1.2.20. Fully pressurize and energize the transmitting and control signal systems by
opening process connections at primary sensors and regulators and by
making control mode settings for automatic operation of equipment as the
process unit is charged and brought on stream.
1.2.21. On the DCS check operability of the system and interfaces to other
subsystems.
1.2.22. Thermocouple wiring should be inspected for proper polaring at the
thermocouple head. Point-by-point verification or the switch identification at
the temperature indicator on the operator's board can be accomplished by
selecting a point to be checked, opening the circuit at the thermocouple head
and checking the temperature indicator to see if it drives upscale or otherwise
indicates an open circuit. The same applies for temperature recorder
controller instruments on the control board. Loop checking involves checking
inputs and should be simulated at the transmitter and the control board
instrument should be watched for response. The controller output should be
adjusted manually and the control valve watched for response. Special
attention should be given to split-range loops and complicated systems
(machinery/DCS interface, etc).
1.3.1. Verify conformity of the installation with drawings, specifications, safety rules,
supplier instructions.
1.3.2. Verify the free rotation of fans and motors.
1.3.3. Verify the correct installation of anti-vibrations mountings and sealing
compound of fire dampers, if any.
1.3.4. Verify that leakage and blades of dampers run freely.
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PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0
1.4. Telecommunications
1.4.1. Inspection of all telecommunication equipments is performed to ensure
compliance with specifications, drawings, Codes of Practice, regulations and
manufacturer's particular requirements. In general, inspections should ensure
satisfactory jointing and continuity of all conductors, satisfactory alignment and
tightness of bolting, acceptance levels of insulation, and a high standard of
cleanliness.
1.4.2. Main telecommunication systems are:
Message switch system
Radio communication system
Telephone network.
(if applicable) until no more collected fragments In the strainers at the pump
suction.
2.1.8. Even if water flushing method would be foreseen, it is impossible to have the
proper and required velocity to clean lines over a certain size with water,
without unreasonably sized temporary facilities (process pumps do not allow
such flows).
2.1.9. The cleaning of lines and associated equipment, which forms the various
systems to be mechanically completed and made ready for start-up, will be
treated during the construction and precommissioning phases in two steps:
(1) During the construction phase, preliminary pipes protection and checking is
implemented to avoid pipelines retaining construction materials until the actual
cleaning takes place when practically feasibly and applicable with the required
efficiency.
(2) Then to reach the readiness for start-up, a cleaning is implemented for each
system/subsystem. This cleaning will use efficient methods, which could be
implemented only after part of the plant is available.
As a summary, only step 1 above can be implemented at the hydraulic test
stage of the work. The cleaning at step 2 of course will be performed as soon
as the site facilities allow for it, the optimum being that both are implemented in
sequence.
2.1.10. To make easier the understanding, the sequence of events, the cleaning
steps that will be applied are the following:
The prefabricated piping spools will be transferred to the site for
installation duly protected at all open ends with plastic
caps/wrapping.They will be visually checked for any foreign material as
tools, gloves, etc, which will be removed.
For big lines, construction group carries out inspection after each spool is
welded, and a manual rubbing/wiping is performed, if necessary.
After the hydrotest, the hydrotesting medium (mainly water) is drained,
through drain valves or one open flange at the maximum rate, so that dirt
is as much as possible removed.
When a system or part of the hydrotested system (so called Test Pack) is
released, a provisional reinstatement is implemented. This is with
exceptions list agreed by precommissioning group and construction to
allow the use of permanent facilities (columns/vessels/pipes themselves)
to perform the actual cleaning to meet the precommissioning cleanliness
requirement.
Some of this cleanings may need the utilities, (such as instrument air,
utility air, service water, etc.). In this case of course utilities should have
been precommissioned before with the normal required checks.
Above step is the period of time where the unit is actually cleaned and is
followed by final reinstatement and conformity to PID checks, air tightness
test, etc.
Targets made from aluminum sheet will be inserted, on temporary vent only
after that three-four blowings (depending on the experience on site) have
been carried out and the steam appears to be clean.
Other steam piping and steam piping to turbine less than 4"
Piping system blowing will be considered completed when steam at the exit
of vent point will appear clean. (The steam has not to be orange dust color).
When blow down of the steam system is completed, traps and other
equipment that were removed prior to the blowdown may be reconnected.
The system can then be reheated and placed in service, after it has passed
the steam test.
Pickling Procedure
Pickling is not required for Stainless Steel Piping. The pickling (or chemical
cleaning) of the carbon steel piping which follows cleaning or degreasing may
be carried out by the following recommended procedure.
Procedure for Carbon Steel
Immerse the piping in an acid pickling bath containing a 10 % wt
solution of hydrochloric (muriatic) acid in water. Rodine, Pyridine or
other suitable inhibitors should be added to the solution in accordance
with the Supplier's instructions to prevent the piping from rusting
quickly when removed from the acid bath.
Piping and/or solution is agitated to ensure the flow of solution through
the piping.
The bath temperature should be between 60 and 70°C and the time of
immersion required to remove all scale and rust will depend on the
strength of the solution and condition of the pipe. Normally, 12 to 14
hours are required and 6 hours should be taken as a minimum.
Remove piping from acid bath, drain it and immediate wash with cold
water to remove all traces of acid.
Neutralizing Procedure
Without allowing the piping to dry, immerse in a hot neutral solution of
0.75 to 1,5%wt of soda ash in water maintained at a pH value of 9 or
above. The temperature of the bath should be about 70/80°C.
Piping and/or solution is agitated to ensure the flow of solution through
the piping.
pH paper may be used to check the wet surface of the piping to
determine than an acidic condition does not exist. If the check shows
acidity then the neutralizing treatment must be repeated.
Rinse piping with cold water, drain thoroughly and blowout with service
air until dry.
Contents: This instruction outlines the procedure for the start-up of the CCR
reforming unit up to the stage where the catalyst is being loaded. The
text includes:
1. Start-Up Requirement
2. Unit Purging
3. Initial Leak Test
4. Unit Dryout
5. Catalyst Loading
6. Second Leak Test And Partial Inerting
7. Supplements
1. Start-Up Requirement
1.1. All overhaul activities and technical modifications influencing Start-up are completed.
All units, removal of equipment and pipeline blinds conform to process requirements.
1.2. Pressure gauges and safety valves are checked. Replacement work and installation
is completed.
1.3. All chemical raw materials are ready and sufficient.
1.4. All process lines and equipment has been purged, qualified in pressure test and
undergone final inspection according to the following procedures.
1.5. Disassembled or replaced equipment flanges are padded and screwed uniformly.
1.6. Safety valves in good condition and its set pressure meet the requirement.
1.7. Close all atmospheric relief valves and drain.
1.8. Verify all instruments are in good condition.
1.9. Utilities services are working normal.
1.10.Ensure complete fire appliances, place inflammables and explosives in fixed area,
clean sundries on site.
1.11.Contact dispatch, maintenance department, fitters, electrical maintenance and lab.
Complete corresponding support work.
1.12.Complete and examine all Start-up schemes, planning diagrams, all related
procedures sheet and work permits.
1.13.All maintained and revamped equipment has acceptance qualification sheet.
1.14.Inspection of the unit is done according to “Plant Inspection” procedure in (KRCIM
71200.04)
2. Unit purging
2.1. Purging Objective
2.1.1. Eliminate welds rods and slags, abrasive dusts, oxides and in general other
substances which might impede the normal unit operation or damage the
equipment (valves, pumps, compressors, turbines, etc.)
2.1.2. Timely find existing problems through process line. Ensure system operability.
2.1.3. Make operators further understand field flow path.
2.4.4.1.1. Firstly, inspect to confirm that all branched lines of 2.5MPa nitrogen of CCR unit and the boundary valve of
GDHT unit are fully closed.
2.4.4.1.2. Introduce 2.5MPa nitrogen into the system, then, introduce nitrogen into the end of the CCR unit pipeline and
disconnect the blind flange at the end for blowing-up purging until the discharge is clear and the purging
requirements are met. Reinstall the blind flange.
2.4.4.1.3. Then, use nitrogen for purging and blowing-up purging to all branch lines respectively.
2.5MPa nitrogen →80-GN-714001→20-GN-711007 →purge at the disconnected location (disconnect D-71107 nitrogen inlet orifice plate) (remove top cover of D-71107 for water
washing)
→after D-71107 is washed to be up-to-standard →25-CL-711001→remove inlet filter of M-71101 to empty water flushing →after washing, re-
connect pipeline well → pump P-71106→25-CL-711004→to the location hand valve downstream
flange disconnects where pipeline 200-P-711003 is connected, flush with water
→25-CL-711001→20-CL-712010→flush P-71206A/B inlet pipelines with water (firstly, remove
pump inlet filter screen and flush with water, when it is up-to-standard, re-connect filter screen
well) → pump inlet drain discharges
→25-CL-711001→20-CL-712010→20-CL-712009→flush water in the location where 20-CL-
712007 line disconnects with 150-P-711044 line (simultaneously, flush water into pump outlet
line, discharge at pump outlet drain)
→after D-71107 is washed to be up-to-standard, re-connect D-71107 inlet pipeline to purge tank D-71107 with nitrogen, discharge from low
point on tank bottom outlet line→25-CL-711001→remove M-71101inlet filter for purging re-connect D-71107→ pump P-71206A/B line, purge,
discharge from the location where pump outlet line disconnects and low points on pump outlet and inlet lines
2.5MPa nitrogen →80-GN-714001→40-GN-711001→25-GN-71100→flange downstream first valve to K-71101A/B inlet nitrogen lines disconnects
→flange downstream first valve to K-71101A/B outlet nitrogen lines disconnects
→to the location where K-71101A/B instrument air blind plate disconnects
→40-GN-711003→ 8-shaped blind plate disconnects on D-71103 nitrogen line
→25-GN-712010→ 8-shaped blind plate disconnects on D-71204 nitrogen line
→25-GN-712008→ 8-shaped blind plate disconnects on D-71206A nitrogen line
→25-GN-712009→ 8-shaped blind plate disconnects on D-71206B nitrogen line
→25-GN-712007→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71202A/B 1st outlet line (300-P-712030)
→25-GN-712007→25-GN-712007/1→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71202A/B 2nd outlet line 200-
P-712039
→25-GN-712004/1→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71202A 2nd inlet line (300-P-712033)
→25-GN-712005/1→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71202B 2nd inlet line (300-P-712033/1)
2.5MPa nitrogen →80-GN-714001/1→80-GN-711001→25-GN-713028→GN-713067→Inlet of M-71302
→GN-713068→Inlet of M-71303
2.4.4.2.1. Firstly, inspect to confirm that all branched lines of 0.8MPa nitrogen of CCR unit and the boundary valve to GDHT
unit are fully closed
2.4.4.2.2. Introduce 0.8MPa nitrogen from the system, then, introduce nitrogen to the end of reforming unit pipeline,
disconnect the blind flange at the end for blowing-up purging until the discharge is clear and the standard is met.
Reinstall the blind flange.
2.4.4.2.3. Then, use nitrogen for purging and blowing-up purging to all branch lines respectively
0.8MPa nitrogen →100-GN-714001/2→50-GN-712001→ 8-shaped blind plate disconnects on nitrogen line that connects with K-71201 outlet and inlet lines.
→25-GN-712004→ 8-shaped blind plate disconnects on nitrogen line that connects with K-71202A 1st inlet line.
→25-GN-712005→ 8-shaped blind plate disconnects on nitrogen line that connects with K-71202B 1st inlet line.
→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71202B inlet line.
→25-GN-712103→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71201 outlet and inlet lines.
→25-GN-713064→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71302A outlet and inlet lines.
→25-GN-713064/1→ 8-shaped blind plate disconnects on nitrogen line that connects with K-71302B outlet and inlet lines.
→25-GN-713063→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71301A outlet and inlet lines.
→25-GN-713063/1→ 8-shaped blind plate disconnects on nitrogen line that connects with K-71301B outlet and inlet lines.
→15-GN-719001→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71303 outlet and inlet lines.
→25-GN-714002→ flange downstream first valve of D-71405 disconnects.
→25-GN-714003→ flange downstream first valve of D-71404 disconnects.
→40-GN-713004→ 8-shaped blind plate disconnects at the joint of T-71303 oxychlorination zone line 40-GN-713005.
→to all hose stations
2.4.4.6.1. Firstly, inspect to confirm that all demineralized water branched lines of the reforming unit and hand valve to
hydrogenation unit boundary valve are fully closed
2.4.4.6.2. Introduce demineralized water from the system into reforming unit pipeline terminal; then, disconnect the blind
flange at the end for blowing-up purging until the discharge is clear and the standard is met. Reinstall the blind
flange. Then, use demineralized water to flush all branched lines respectively. Introduce demineralized water into
following positions respectively to flush:
Introduce demineralized water →150-SW-714001→40-SW-711006→to A-71101 water tank, then, empty from water tank for discharging.
→40-SW-711008→to A-71102 water tank, then, empty from water tank for discharging.
→50-SW-712006→to A-71201 water tank, then, empty from water tank for discharging.
→40-SW-712011→to A-71202 water tank, then, empty from water tank for discharging.
→40-SW-712009→to A-71203 water tank, then, empty from water tank for discharging.
→40-SW-712013→to A-71204 water tank, then, empty from water tank for discharging.
→100-SW-71501→to WHB
→40-SW-713008→to regeneration part oxychlorination water injection tank T-71302, empty from water tank for discharging.
→50-PW-713003→to P-713044 where flange disconnects
→40-SW-711001→to prehydrogenation water injection tank D-71106, then, empty from water tank for discharging.
→25-SW-712001→to reforming water injection tank D-71211, then, empty from water tank for discharging.
→50-SW-719010→to regeneration compressors house water station inlet where flange disconnects, after discharging to clean, re-connect flange.
Then, empty from water tank for discharging.
→to hydrogen compressor water station inlet where flange disconnects, after discharging to clean, re-connect flange. Then, empty from water tank
for discharging
→50-SW-713001→to P-71305A/B inlets where flange disconnects
2.4.4.7.1. Introduce circulating water into unit, (only open one-side boundary area circulating water inlet and outlet valve)
open bypass valves of all equipment using circulating water, close hand valves of inlet and outlet equipment
2.4.4.7.2. Then, introduce circulating water into all branched lines in turn to flush until the gas discharged from where all
branched lines disconnect is clear and meets the requirements. Then open another-side boundary area
circulating water valve.
2.4.4.8.1. Firstly confirm that fuel gas boundary hand valve is closed. Confirm that E-71401 bypass valve is opened; inlet
and outlet E-71401 hand valves are closed. Confirm that PV4303 bypass valve is opened; inlet and outlet
PV4303 hand valves are closed.
Introduce steam into →50-LS-714012→PV4303 bypass →300-GF-714001
→E-71401 shell side inlet where flange disconnects
→E-71401 tube side outlet where flange disconnects
→D-71401 fuel gas inlet where flange disconnects→purge to clean and then, re-connect flange
→D-71401 fuel gas tank bottom outlet and top flange downstream hand valve disconnects for discharging.
→50-LS-714013→D-71401 fuel gas top hand valve downstream flange disconnects for discharging.
→300-GF-714004→50-GF-711001→solenoid valve UV1001/B disconnects for purging →purge to be up-to-standard and then re-connect→PV1006 bypass →
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→50-GF-711001→25-GF-711002→solenoid valve UV1001/A disconnects for purging →purge to be up-to-standard and then re-connect→filter
disconnects for purging →purge to be up-to-standard and then re-connect→PCV1001 disconnects for purging →purge to be up-to-standard and then re-connect→
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→80-GF-711005→solenoid valve UV1002/B disconnects for purging →purge to be up-to-standard and then re-connect→PV1007 bypass →
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→80-GF-711005→25-GF-711006→solenoid valve UV1002/A disconnects for purging →purge to be up-to-standard and then re-connect→filter
disconnects for purging →purge to be up-to-standard and then re-connect→PCV1002 disconnects for purging →purge to be up-to-standard and then re-connect→
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→50-GF-712017→solenoid valve UV2004 disconnects for purging →purge to be up-to-standard and then re-connect→PV2110 bypass →
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→50-GF-712017→25-GF-712018→solenoid valve HV2004 disconnects for purging →purge to be up-to-standard and then re-connect→filter
disconnects for purging →purge to be up-to-standard and then re-connect→PCV2112 disconnects for purging →purge to be up-to-standard and then re-connect→
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→100-GF-712001→solenoid valve UV2001/1 disconnects for purging →purge to be up-to-standard and then re-connect→PV2007 bypass →
burner flame arrester upstream flange disconnect for purging
→purge to be up-to-standard and then re-connect→purge to burner
2.4.4.9.1. Close reforming unit and confirm that all hand valves into D-71403 pipeline have been closed.
Introduce 1.0MPa steam into →500-NF-714001 (purge the main pipeline into D-71403) and discharge from bottom
1.0MPa Steam →500-NF-714001→D-71403→500-NF-714002 unit boundary 8-shaped blind plate disconnects
→80-SLO-714006 downstream valve flange disconnects
→150-NF-711003→Upstream D-71100 safety valves A/B and downstream bypass valve where flange disconnects
→80-NF-711006→Upstream D-71101 safety valves A/B and downstream bypass valve where flange disconnects
→50-NF-714008→the location where flame arrester FA-71402 disconnects (remove flame arrester)
→50-NF-714007→the location where flame arrester FA-71401 disconnects (remove flame arrester)
→150-NF-711017→Upstream C-71101 safety valves A/B and downstream bypass valve where flange disconnects
→80-NF-711011→Upstream K-71101A safety valve and downstream bypass valve where flange disconnects
→80-NF-711014→Upstream K-71101B safety valve and downstream bypass valve where flange disconnects
→450-NF-712005→Upstream D-71201 safety valve and downstream bypass valve where flange disconnects
→300-P-712025→D-71201 top where 8-shaped blind plate disconnects
→200-NF-712007→Upstream K-71201 safety valve and downstream bypass valve where flange disconnects
→150-NF-712009→Upstream D-71202 safety valve and downstream bypass valve where flange disconnects
→150-NF-712011→Upstream K-71202A 1st safety valve and downstream bypass valve where flange disconnects
→150-NF-712017→Upstream K-71202A 2nd safety valve and downstream bypass valve where flange disconnects
→150-NF-712016→Upstream K-202B 1st safety valve and downstream bypass valve where flange disconnects
→100-NF-712021→Upstream K-202B 2nd safety valve and downstream bypass valve where flange disconnects
→100-NF-712027→Upstream D-71203 safety valve and downstream bypass valve where flange disconnects
→80-NF-712029→Upstream D-71205 safety valve and downstream bypass valve where flange disconnects
→50-P-712069→the location connecting with line 50-P-712068 from D-71204 to fuel gas tank where 8-shaped blind plate disconnects
→100-NF-712023→Upstream D-71206A safety valve and downstream bypass valve where flange disconnects
→100-NF-712025→Upstream D-71206B safety valve and downstream bypass valve where flange disconnects
→40-P-712059→the location connecting with line 40-P-712058 from D-71205 to fuel gas tank where 8-shaped blind plate disconnects
→40-P-713057→ to T-71303 where flange downstream first valve disconnects
→100-NF-712031→Upstream C-71201 safety valve and downstream bypass valve where flange disconnects
→50-NF-711007→Upstream D-71101 safety valve and downstream bypass valve where flange disconnects
→40-NF-714009→ the location connecting with E-71401 steam inlet line where 8-shaped blind plate disconnects
→40-NF-714010→D-71401 bottom where 8-shaped blind plate disconnects
→100-NF-712040
→20-NF-712037→SN-71210 to first outlet valve where rear flange disconnects
→20-NF-712036→SN-71209 to first outlet valve where rear flange disconnects
→20-NF-712035→SN-71208 to first outlet valve where rear flange disconnects
→20-NF-712034→SN-71201 to first outlet valve where rear flange disconnects
→20-NF-711004→SN-71101 to first outlet valve where rear flange disconnects
→20-NF-711018→SN-71102 to first outlet valve where rear flange disconnects
→20-NF-711020→SN-71103 to first outlet valve where rear flange disconnects
→20-NF-711028→SN-71104 to first outlet valve where rear flange disconnects
→20-NF-711030→D-71105 to first outlet valve where rear flange disconnects
→50-NF-711021→D-71103 to first outlet valve where rear flange disconnects
→20-NF-711029→D-71107 to first outlet valve where rear flange disconnects
→100-P-712050/2→D-71206 reforming hydrogen exits where 8-shaped blind plate disconnects
→100-NF-714006→Upstream D-71401 safety valve and downstream bypass valve where flange disconnects
2.4.4.11.1. Introduce 0.8MPa nitrogen downstream inlet flange of underground oil collection drum D-71404 (disconnect
flange for purging until purge to be up-to-standard and then re-connect). Inject nitrogen into D-71404. If bottom
discharge is up-to-standard; then purge pipeline 80-SLO-714003 through its end flange. Disconnect the flange
for purging until up-to-standard and re-connect. Then, purge all branched lines respectively.
0.8MPa N2→25-GN-714003→D-71404→80-SLO-714003→40-SLO-712001→D-71201 bottom drain
→40-SLO-712003→D-71202 bottom drain
→40-SLO-712002→D-71207 bottom drain
3.4.1. Pressure boosting speed should be slow and air tightness test pressure should
comply with the regulations strictly without overpressure.
3.4.2. Any leak source found should be marked in time and the maintenance
personnel should be contacted for handling.
3.4.3. Pay attention to inspect whether there is interflow between systems and avoid
equipment overpressure strictly. Watch out for gas expansion in the system
and consequent equipment overpressure because of ambient air temperature
change.
3.4.4. During air tightness test, commands should be given uniformly and personnel
in all areas should contact with each other.
3.4.5. During air tightness test of each system, at least two pressure gauges should
be used to observe pressure with required pressure gauge precision of
magnitude 0.4, 1.5-2 times of the highest air tightness pressure.
3.4.6. Handling of leak sources under pressure is not allowed.
3.5.1. Initial leak tests will be performed under KRC or Engineering company
responsibility and the general instructions hereunder shall only be used as a
reminder.
3.5.2. The initial leak tests can be performed using air or nitrogen depending upon
local facilities. The test pressure will be the air or nitrogen system pressure or
the unit (or section of unit) design pressure, whichever is the lower.
3.5.3. The unit is isolated with blinds from adjacent sections containing hydrocarbons
(liquid or gaseous), and from utilities systems where pressure is lower than air
(or nitrogen) pressure.
3.5.4. The pressure rise must be checked on several manometers and possibly
checked on a pressure recorder. Leaks must be carefully located and
tightened. Their location must be recorded.
3.5.5. The leak test is satisfactory when the pressure decrease is lower than
0.005 MPa/hour over a period of 4 consecutive hours.
3.5.6. The air (nitrogen) used for leak tests should be purged out of the unit using low
points drains to remove free water, if any.
3.5.7. For the purpose of leak tests the unit will be divided into sections of
approximatively the same design pressure, as defined hereunder. Air (nitrogen)
will be injected at different locations depending upon check valves.
3.5.8. For the reaction sections the tests can be followed by a vacuum test at
maximum vacuum. Loss of vacuum shall not exceed 25 mm Hg/hour.
In addition, all utilities lines, especially the ones connected to the flare and fuel gas
networks (including safety valves) will be fitted with blind flanges.
The reaction section is isolated as described on the following attached scheme.
The points of isolation are indicative only and must be reviewed on-site, to take into
account actual piping arrangement.
Reaction Section
The airtightness media is N2. Introduce nitrogen from hydrogen recycle
compressor K-71201 outlet to boost pressure. The pressure tapping point
uses pressure at separating drum D-71201 as reference. The highest work
pressure of D-71201 namely 0.4MPa is for reference.
Airtightness steps
1) Use the reforming ejector J-71201 after checking the airtightness flow
(The end lines of all pressure gauge pressure introduction lines should
be isolated before producing vaccuum) to evacuate the reforming
system. If vaccuum can’t reach 600mmHg after evacuuation for 2h, it
means that the system has obvious leak sources and further pressure
boosting is needed for inspection.
2) After vacuum test finishes, install 8-shaped blind plate in D-71201
vacuum line
3) Introduce nitrogen (circulation compressor K-71201 outlet) to break the
vacuum slowly. Pressurize the system to 0.4MPa (boost pressure
according to D-71201 regulations strictly). Make leakage test
inspection to system’s all air tightness points. Air tightness is up-to-
standard if pressure drop is lower than 0.005MPa/h continuously for
4h.
Recontacting Section
The air tightness media is N2. Introduce nitrogen from hydrogen booster
compressor K-71202 outlet to boost pressure. The pressure tapping point
uses pressure at recontacting drum D-71203 as reference. The highest work
pressure of D-71203 namely 2.3MPa is for reference.
Stabilization Section
Air tightness test of steady section uses 2.5MPa nitrogen as media. Introduce
nitrogen from nitrogen line 25-GN-712010 at D-71204 top to pressurize with
pressure tapping point at D-71205 as reference and highest operation
pressure of 1.6MPa. The leakage test is up-to-standard when pressure drop
is smaller than 0.005MPa/h for 4h continuously.
Chronologically, once the initial leak tests are over, the drying out of the unit
takes place, prior to catalyst loading.
4. Unit Drying
4.1. Drying Objective:
Reaction, catalyst circulation and regeneration sections must be dried out prior to
catalyst loading, firstly to avoid damaging the catalyst with water, secondly to
shorten the duration of the low severity operation after first oil in.
K-71201→E-71201→F-71201→R-71201→F-71202→R-71202→F-
71203→R-71203→E-71201→A-71201→D-71201→K-71201
4.4.5.2. Light small fires in the preheater F-71201 and heaters F-71202 & F-71203
according to ignition instructions in KRCIM 71200.07 and increase reactor
inlet temperature at a rate of 40°C per hour up to 200°C.
4.4.5.3. The following steps must now take place to circulate nitrogen in the
recontacting section and nitrogen section:
Line up the H2 rich gas circuit to reductor D-71311 and to 1st and
2nd reactors lift pots D-71331 & D-71332. Note that hydrogen
purification unit M-71301 is isolated and by passed.
Start the H2 rich gas compressor K-71202A/B at 25% capacity, all
the compressed gas being recycled to H2 rich gas compressor KO
drum D-71207, the spill back PV2068C is full open in manual. KO
drums PIC2079 & PIC2080 are set in auto mode.
Establish flow of gas (up to normal flow taking into account you
are handling nitrogen) to the 1st and 2nd reactors lift pots and to
the reduction chamber.
Line up the N2 lift gas circuit to the regenerator and last lift pot,
upper surge drum and first upper hopper, fines filters. Set
PIC3014 on N2 lift gas compressor discharge at 0.3 MPa g.
Start up K-71303 to establish flow to first upper hopper D-71310.
This will assure the smooth operability of elutriation system.
Start N2 lift gas compressor K-71302 and load the valves to
circulate the gas at 100% capacity.
Establish flow of gas to the regenerator and last lift pot up to the
normal flow.
4.4.5.4. When the above steps are completed, the nitrogen circulation for drying
purpose is fully established, as shown on the attached drawings (DWGS.
ReactionDRY, RecontactDRY & NitrogenDRY).
4.4.6. The reduction electrical heater H-71304 is then switched on and reduction
chamber inlet temperature is progressively increased at a rate of 20°C per hour
up to 200°C. H-71304 flow is 1900Nm3/h.
4.5. Notes
4.5.1. During the temperature rise, watch the skin temperatures of the heater tubes
and flue-gas temperature to avoid any overheating of the tubes. Check also the
temperature of each equipment in order not to exceed the design figures.
4.5.2. Welded plates heat exchanger (feed/effluent) E-71201
The following precautions must be carefully observed:
Owing to the narrow space (2.5 mm) between plates, the upstream
piping must be thoroughly flushed prior to flow through the exchanger.
During shell or bundle flushing (to remove air or process fluids) the
differential temperature between the feed stream and the effluent stream
must not exceed 50°C.
The plate are stainless steel. Presence of chloride and liquid water for
an extended period must be avoided.
Ensure that the feed side pressure always exceeds the effluent side
pressure. Consequently:
o the exchanger must be pressurized only from the feed inlet
(recycle compressor discharge).
o the exchanger must be depressurized only from the effluent outlet
(separator drum).
When introducing the naphtha feed (Oil-in stage) at a linear rate in order
to reach 60% of the design within ten minutes. Ensure that both inlet
flows are balanced.
5. Catalyst Loading
5.1. Preliminary
5.1.1. When the reaction section drying out is complete and nitrogen has been
replaced by air, the CCR reactors and the regenerator can be opened for
inspection of the internals, cover plates and grids, to make sure that thermal
expansion has not caused any damage.
5.1.2. If needed, the reactors and regenerator will be brushed and vacuum cleaned
before catalyst loading starts.
5.1.3. The catalyst loading period must be as short as possible to minimize the risk of
moisture entering the reaction system. If necessary, the job will be done in
shifts.
5.1.4. Catalyst loading will preferably be interrupted in case of rain or snow, or
efficient protection must be in place.
5.1.5. The catalyst must be handled with care to avoid breakage of the catalyst
spheres. During the loading, the loading sleeves will be adjusted to allow a free
fall no higher than 2 meters above the catalyst level.
5.1.6. A representative of the Gamma Ray Level manufacturer is required for level
calibration.
Note:This personnel shall be permanently present during the loading operation. The
total number of personnel will be obtained by multiplying by the number of shifts.
Reactor 1 : drums *
Reactor 2 : drums *
Reactor 3 : drums *
First upper hopper : drums
2d upper hopper : drums
3d upper hopper : drums
Regenerator manhole 5 : drums *
Regenerator manhole 1 : drums
Lock hopper : drums
Upper surge drum elutriator : drums
*: Check of the outlet catalyst pipes
m3 DRUMS
2nd Reactor Upper hopper 0.32
Upper hopper legs 0.17
Other legs 0.13
Reactor 12.15
2nd Reactor lower hopper and lift pot 0.13
TOTAL 2nd REACTOR SECTION 12.90 80
m3 DRUMS
3rd Reactor Upper hopper 0.32
Upper hopper legs 0.17
Other legs 0.13
Reactor 20.31
3rd Reactor lower hopper and lift pot 0.13
TOTAL 3rd REACTOR SECTION 21.06 130
m3 DRUMS
Legs 0.07
Lock hopper 0.63
Regenerator 4.07
First lower hopper and first lift pot 0.13
TOTAL REGENERATOR SECTION 4.90 30
TOTAL CATALYST TO BE LOADED
Reactors 44.64
: m3
Regenerator 4.90: m3
TOTAL 49.54
: m3 (307 Drums)
Note: Four additional drums to be stored nearby the catalyst loading device for
future loading and to be protected against rain.
5.6.2.3. Knock on the pipe wall to check whether catalyst pipes are full.
5.6.2.4. Open the special tight manual valves under each lower hopper and unload
the catalyst in a clean drum installed under the lift pot.
5.6.2.5. When catalyst flow stops, check again by knocking that the catalyst pipes
are empty.
5.6.2.6. Close special tight manual valves under the lower hoppers and reinstall
the primary hydrogen gas nozzle on the lift pots.
5.6.2.7. When the test is completed, catalyst loading can start.
CATALYST LOADING
5.6.2.8. When the catalyst level reaches the upper part of the reactor centerpipe,
the catalyst loading is stopped.
5.6.2.9. Reinstall the sectors pieces and the removed cover plates, except 4 of
them located at 90° kept dismantled to control the end of catalyst
loading.
5.6.2.10. Fill up the conical parts of the catalyst bed.
5.6.2.11. Fit in the last 4 cover plates.
5.6.2.12. Install the reactor inlet distributors.
5.6.2.13. Install the reactor inlet elbows.
5.6.2.14. Install the four upper inlet catalyst pipes.
Note: For the end of catalyst loading, the procedure for the first reactor is different
from the other reactors (go to first reactor end of loading).
5.6.4.7. Open the special tight manual valve under the 1st upper hopper, the
reduction chamber will be filled up partially.
5.6.4.8. Fill the 1st upper hopper, with 1 additional drum.
5.6.4.9. Close the special tight manual valve under the 1st upper hopper.
5.6.4.10. Fill up the 1st upper hopper, calibrate its level, in coordination with the
level manufacturer:
xx drums and xx liters are loaded, this is 0% of the LI
xx drums are loaded, to fill completely the cone: xx% of the LI
xx drums are loaded: xx% of the LI per drum.
A total of xx drums will be loaded.
Note that the low level alarm LALL of the 1st upper hopper should be
switched off before reaching 20% at the LI.
5.6.4.11. Open the special tight manual valve under the 1st upper hopper and
finish filling the reduction chamber. Check the deviation of the 1st upper
hopper level LI on the DCS.
5.6.4.12. Check that the primary hydrogen nozzle of the first lift pot is reinstalled
and open the special tight manual valves under the 1st reactor lower
hopper. The lift pot will be filled up. Check again the deviation of the 1st
upper hopper level LI indication on the DCS.
5.6.4.13. Install the 1st upper hopper elutriator pipe and connect the piping. This
finishes the initial loading of the reactors.
Operation schedule
5.6.1. Open manholes MH1, MH2, MH3, MH4 and MH5 of the regenerator and the
MH of the upper surge drum.
5.6.2. Check if the atmosphere in the regenerator is breathable, for entry.
5.6.3. After inspection, and tack welding of the bolt pins, close the top manhole MH1
and reinstall the catalyst line from the lock hopper bottom to the regenerator.
After setting the internal plug, close the MH of the upper surge drum.
5.6.4. A good house keeping around the regenerator top manhole MH1 must be
maintained.
5.6.5. Remove the primary gas injection nozzle from the bottom of the lift pot.
5.6.6. The lift pot under the regenerator must be checked again (primary injection
nozzle location).
5.6.7. Remove the upper surge drum elutriator to permit lift pipe checking.
5.6.8. After lift pipe checking close the special tight manual valve on the lift pipe.
5.6.9. The catalyst pipes of the first lower hopper must be checked to make sure
that no foreign material remains inside.
5.6.10. Air flush from the regenerator each of the 6 catalyst pipes one by one.
5.6.11. Then, when the flow from the lift pot bottom is dust free, close the special tight
manual valve under the first lower hopper.
5.6.12. The catalyst flow test can now be carried out.
5.6.13. One drum of catalyst will be loaded into the calcination zone of the
regenerator through the lower manhole MH5, in order to fill the first lower
hopper and the catalyst outlet pipes.
5.6.14. Check that the hopper pipes are full of catalyst (knock on the pipe wall).
5.6.15. Open the special tight manual valve under the first lower hopper and unload
the catalyst into a clean drum installed under the lift pot.
5.6.16. When catalyst flow stops, check that the first lower hopper pipes are empty.
5.6.17. Close the special tight manual valve under the first lower hopper and reinstall
the primary gas nozzle on the lift pot.
5.6.18. When the test is complete close the lower manholes MH4 and MH5 after
having set the internal plug.
5.6.19. Catalyst loading can now start.
5.6.20. At the beginning of the operation catalyst will be loaded from the upper surge
drum using the elutriator nozzle.
5.6.21. Open the automatic special catalyst tight valve UV between the upper surge
drum and the lock hopper.
5.6.22. Open the automatic special gas tight valve UV between the lock hopper and
the regenerator.
5.6.23. Open the automatic special gas tight valve UV between the upper surge drum
and the lock hopper.
5.6.24. Close the automatic special catalyst tight valve UV between the lock hopper
and the regenerator.
5.6.25. Check the lock hopper catalyst sampling device.
The level indicator LI of the regenerator can now be calibrated. This must
be done, in coordination with the level manufacturer.
5.6.45. Catalyst will be loaded drum by drum from the top of the upper surge drum.
5.6.46. All the automatic special catalyst tight valves are opened. The low low level
alarm LALL is switched OFF while the level indicator LI shows 0%.
5.6.47. Load xxx drum. The level indicator LI must show 10%.
5.6.48. Load drum after drum to perform level calibration including DCS low level and
high level alarms of this vessel.
5.6.49. Total number of drums added: xxx).
5.6.50. Check that the primary gas nozzle of the lift pot is reinstalled and open the
special tight manual valve between the first lower hopper and the regenerator
lift pot.
5.6.51. The lift pot will be filled. Check in parallel the deviation of the upper surge
drum level indicator LI on the DCS.
5.6.52. Close the automatic special catalyst tight valve UV between the upper surge
drum and the regenerator, and load the lock hopper with xxx drums, from the
top of the upper surge drum.
5.6.53. Reinstall then the elutriator and the related piping on top of the upper surge
drum.
5.6.54. Close manholes MH2, MH3 of the regenerator. This finishes the initial
loading of the regeneration section.
7. Supplements
StartupScheme
DWG.ReactionLEAK
DWG.RecontactLEAK1
DWG.RecontactLEAK2
DWG.StabilizationLEAK
DWG.NitrogenLEAK
DWG.RegenerationLEAK
Dryingcurve1
DWG.ReactionDRY
DWG.RecontactDRY
DWG.NitrogenDRY
Appendix 1
Appendix 2
Appendix 3
Appendix 4
Appendix 5
Appendix 6
Appendix 7
Appendix 8
Appendix 9
Appendix 10
Appendix 11
Appendix 12
Appendix 13
Contents: This instruction outlines the procedure for the start-up of the CCR reforming
Unit from the stage where the catalyst is being loaded. The text includes:
1.2. Status
The status of the unit prior to its initial startup is a follows:
1.2.1. Each section as defined in chapter (3.6/ KRCIM 71200.05) “Recommended
sections for leak tests" has been leak tested (initial leak tests).
1.2.2. All the sections (except the stabilization section) have been dried.
1.2.3. Catalyst has been loaded in the reactors and the regenerator and the relevant
sections leak tested again and partially inerted (residual content of 0 2
between 2 and 5% volume).
1.2.4. The stabilization section has not been inerted
1.2.5. The unit is isolated with blinds at the battery limits:
on the feed and products lines.
on the flare and fuel gas headers.
1.2.6. Pressure relief valves in the reaction and HP absorber sections are blanked
off, except those to atmosphere.
1.2.7. The PCV on the separator drum discharges to atmosphere.
1.2.8. Pressure relief valves in the regeneration and nitrogen sections are directed
to atmosphere (normal status).
1.3. Chronology
The sequence of first startup is as follows:
1.3.1. Circulation of catalyst and drying of catalyst under an atmosphere with a
residual O2 content.
1.3.2. Complete inerting of the sections involved in the circulation (i.e. all sections
except stabilization) O2 content is reduced to less than 0.2% volume.
1.3.3. Complete inerting of the stabilization section.
1.3.4. Stabilization section startup on total reflux.
1.3.5. Pressurization with hydrogen of the reaction section and the HP absorber
section.
1.3.6. Heating up and reduction of catalyst.
1.3.7. Oil in.
1.3.8. Operation of the unit at low capacity and low severity.
1.3.9. Operation of the unit at low capacity and high severity.
1.3.10. Operation of the unit at nominal capacity and high severity.
1.3.11. Start of the catalyst circulation.
1.3.12. Start of catalyst regeneration.
Note: When pre-reduced catalyst is used heating and drying of the catalyst cannot
be performed. After recycle gas compressor startup reaction section heaters pilots
are lighted-on and the temperature of the circulating gas shall not be higher than
100°C.
Always start by the FCV to set the primary flow to empty the small catalyst
quantity which is already engaged on the lift area and, then have a smooth
action on the DPCV lift valve to get catalyst lift smooth start-up.
2.2.6. As the catalyst circulation may not be stable due to low pressure drop across
the reactors, it may not be easy to keep running the catalyst circulation
continuously.
the upper surge drum and from the regenerator lift pot to the 1st upper hopper use
nitrogen. Moreover an independent source of nitrogen referred to as " N 2 seal gas" is
used (refer Fig. 12):
to maintain a controlled nitrogen over pressure between the first
reactor upper hopper and the reduction chamber.
to maintain an overpressure in the last reactor lower hopper against
the lift pot pressure on one side and the reactor pressure on the other
side (refer to Fig. 13).
to maintain an overpressure in the first lower hopper against the lift pot
pressure and the regenerator pressure (refer to Fig. 13).
Note: Seal gas using hydrogen is also injected in the lower hoppers of reactors 1
and 2 to prevent hydrocarbons from entering into the lift pipes.
In normal operation (hydrocarbons in the reaction section) nitrogen seals and
hydrogen seals must always be established prior to starting catalyst
circulation.
The details of the catalyst circulation and drying procedure are covered in the
following paragraphs.
2.4. Preparation
2.5.1.3.5. Put in service PDIC3005 between regenerator top and first burning
zone.
2.5.1.3.6. Put in service PDT3003 (Differential Pressure between second
burning zone and oxychlorination/calcination zone in regenerator) but
keep corresponding control valves PDV3003A and PDV3003 B in
manual.
2.5.2.1. Establish N2 seal gas to the first reactor upper hopper D-71310
2.5.2.1.1. Override interlocks IS3019 and IS3025 to allow proceeding with next
steps.
2.5.2.1.2. Open ON /OFF valve UV3012 (N2 seal gas to upper hopper).
2.5.2.1.3. Open FIC3011 (before UV3012) manually: adjust flow to the design
figure. Switch into auto. Set corresponding FSLL 3114 at design
value.
2.5.2.1.4. Put PDIC3019 and PDALL3122 in service (Differential Pressure First
upper hopper / reduction chamber).
2.5.2.1.5. Open ON/OFF valve UV3011 manually between D-71310 and D-
71311.
2.5.2.1.6. Wait a few minutes to allow pressure and flow to stabilize.
2.5.2.1.7. Reset interlock IS3019. UV3012 and UV3011 must remain open
2.5.2.1.8. Correct flow coefficient of orifice for use of nitrogen
Since the first upper hopper is now sealed from the reduction chamber,
reduction gas circulation can be established to the reduction heater, reduction
chamber and coolers (refer to Fig 14). Line up the equipment involved and put
in service PDIC3012 at tube side outlet of reduction exchanger, FIC3017 at
shell side inlet of reduction exchanger and PIC3004 at shell side inlet of
hydrogen lift gas exchanger
2.5.3.2. Operators must now open the other valves on catalyst (manual local
catalyst tight valves): on seal legs between lower hoppers and lift pots of
1st and 2nd reactors.
2.5.3.3. For each of the four lift pots, first adjust total gas flow manually through
the four corresponding FICs to the recommended figure as indicated in
"Lift gas flow". For the FICs through second and third lift pots, correct
coefficient for nitrogen. Then switch to auto mode
2.5.3.4. Open slowly PDV3011 (last reactor lift pot) in order to lift catalyst to the
upper surge drum until the level in the 3 rd upper hopper decreases to
40%.
2.5.3.5. Then open slowly PDV3009 (second reactor lift pot) in order to lift
catalyst to the 3rd upper hopper until the level in the 3rd upper hopper
decreases to 40%.
2.5.3.6. Then open slowly PDV3008 (second reactor lift pot) in order to lift
catalyst to 3rd upper hopper until the level in the second upper hopper
decreases to 40%.
2.5.3.7. Then open slowly PDV3006 (first reactor lift pot) in order to lift catalyst to
the 2nd upper hopper until the level in the 1st upper hopper has been
decreased by about 30%.
2.5.3.8. Make Adjustments to keep the levels constant
2.5.3.9. The PDIs of the lift pipes will be set at a value between 0.010 and 0.020
MPa as to obtain equal catalyst flows
2.5.3.10. Stabilize the circulation, in manual mode, until the levels in the upper
hoppers are steady. Set the catalyst circulation at about 25% of the
design flow. Then set the control in auto-cascade from level controllers
to differential pressure controllers
2.5.4.1. Catalyst handling from surge drum D-71301 to lock hopper D-71302:
2.5.4.1.1. The level of catalyst increases in the upper surge drum while it
decreases in the regenerator. When these levels reach the transfer
conditions, open the pressure equalizing valve UV3006 between the
lock hopper and the surge drum: the pressures will equalize.
2.5.4.1.2. Open then the two ON/OFF valves UV3001 & UV3002 below the
upper surge drum, allowing the catalyst transfer into the lock hopper.
2.5.4.1.3. Then close the pressure equalizing valve UV3006 and the two
ON/OFF valves UV3001 & UV3002.
2.6.1.2. If required, inject air in reaction section at the recycle compressor K-71201
suction and in regeneration section at suction of loop compressor K-
71301.
2.6.1.3. To test the make up air compressor K-71304, if possible, operate this
machine to introduce air in the regeneration section.
Note: During trial run, (according to the pressure of lift pot), recalculate N2 flow rate.
3. Final Inerting
The purpose is to reduce the O2 content in all the sections below 0.2% volume prior
to hydrocarbons introduction. All the sections (with the exception of the stabilization
section) have been partially inerted (2 to 5% volume of residual O2). The stabilization
section has not been inerted at all.
3.1. All sections except stabilization
3.1.1. The catalyst beds have been left at approximately 300°C at the end of the
catalyst circulation .
3.1.2. Electrical and fired heaters are off. But fired heaters pilot burners are on.
3.1.3. All compressors are stopped. They must be isolated and purged with N 2 and
left under an atmosphere of pure N2.
3.1.4. Remove blinds on all process lines between the sections (if any remain) - with
the exception of the stabilization section - remove also blinds to/from the
battery limits (with the exception of the liquid feed).
3.1.5. Remove blinds on the safety valves to flare.
3.1.6. Install blinds on the safety valves which were previously routed to atmosphere.
(Reaction, Recontacting and stabilization sections only). Install also a blind on
PV2068 previously directed to atmosphere (suction of recycle compressor).
3.1.7. Close double block valves on start-up lines:
Between recycle compressor suction and nitrogen lift gas compressor
suction 100-GN-712003
Between hydrogen rich gas product and nitrogen lift gas compressor
discharge: 80-GN-713050
3.1.8. Depressurize the reaction section to 0.010 MPa gauge then introduce N 2 to
recycle compressor discharge and raise the pressure to 0.400 MPa g.
Depressurize again to 0.010 MPa gauge, through all the low points dead legs,
etc. Vent and drain the special heat exchanger (reactor feed/effluent) last.
Renew the operation until the O2 content is below 0.2% volume. Leave a
residual N2 pressure of 0.005 to 0.010 MPa gauge.
ISSUE DATE: 20/03/06 - 138 -
KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (2)
CCR UNIT KRCIM 71200.06 REV.0
3.1.9. Repeat same steps for the recontacting section. Residual pressure 0.005 to
0.010 MPa gauge.
3.1.10. Do the same for the regeneration section. Residual pressure 0.350 MPa
gauge.
Note: After reforming feed oil is cut, lift tower pressure to 1.56MPa according to
normal process conditions, control operating temperature at 57°C / 224°C ( top/
bottom).
4.2.2. Preparation
4.2.2.1. Nitrogen lift gas circuit is pressurized with nitrogen up to 0.350 MPa at
nitrogen lift gas compressor KO drum D-71307.
4.2.2.2. Regeneration circuit is pressurized with N2 up to 0.450 MPa at the suction
of the regeneration loop compressors K-71301.
4.2.2.3. N2 seal gas lines are commissioned
4.2.2.4. Pressurize the reaction and recontacting sections with pure hydrogen
(electrolytic H2). The resulting nitrogen in these sections is about 25 vol. %
which is favorable for a steadier catalyst circulation.
4.2.2.5. Set pressure controller of the separator drum D-71201 at 0.030 MPag
above the start-up pressure (0.35MPa), Increase the pressure of the
separator drum via the recycle compressor discharge.
4.2.2.6. Commission the split range pressure control PV2068C on the H 2 rich gas
compressor K-71202A/B suction
4.2.2.7. Check again all the flanges for leaks using an explosimeter, and all
interlocks related to catalyst circulation are made operational
4.2.3. Operation
4.2.3.1. Start one nitrogen lift gas compressor at 100% capacity, PIC3014 at
nitrogen compressor discharge set at design pressure, send N 2 to the inlet
of regeneration loop compressor K-71301A/B.
4.2.3.2. Start one regeneration loop compressor and increase capacity to 100%
(BIAS not in service). FIC3004 of the Burning gas is set at 80% of design
capacity (944 m3/h)
4.2.3.3. FIC3019 and 3009 of calcinations and oxychlorination gases are set in
auto mode at 80% of design capacity (87 m3/h)
4.2.3.4. Commission all oxygen analyzers. Remember that certain ranges have
been changed during catalyst drying and information to DCS inhibited.
4.2.3.5. Commission the regeneration dryer DR-71301
4.2.3.6. Start the H2 recycle compressor K-71201. Increase the capacity up to the
maximum allowed by manufacturer.
4.2.3.7. Commission the hydrogen purity on line analyzer AI2001
4.2.3.8. Start K-71202A/B at 50% capacity and bring the recontacting drum D-
71203 pressure to about 0.120 MPa g, recycling all the gas to the H 2 rich
gas KO Drum D-71207
4.2.3.9. All H2 users and lines to fuel gas are isolated, only FV3017 on reduction
gas, PDV3012 at the tube side outlet of E-71304 and the HV3003 at the
tube side outlet of E-71305 are closed but block valves are open.
4.3.2. Procedure
4.3.2.1. The pressure must be maintained by make-up of hydrogen or nitrogen.
Nitrogen content in the circulating gas must not exceed 30% vol.
4.3.2.2. Some water will be released from the catalyst. This water will be
collected in D-71201.
4.3.2.3. Light the burners of F-71201/202/203 and increase the temperatures at
the inlet of reactors up to 300°C at the rate of 25°C/h.
4.3.2.4. Switch-on H-71301/302/303, then increase the temperature at the heater
outlet TIC3001/3005/3006, up to 300°C at the rate of 40°C/h.
4.3.2.5. Set the flow H2 FIC3017 to reduction chamber at 80% of design capacity
(294m3/h) and PDIC3012 between reduction chamber outlet and first
reactor at 0.010 MPa.
4.3.2.6. Switch on H-71304 and increase its TIC3007 outlet temperature to
400°C at the rate of 40°C/h
4.3.2.7. When the temperature of 400°C is reached in the reactors, start catalyst
circulation first from the 3rd reactor lift pot D-71333 to the upper surge
drum D-71301, etc. Note however that either nitrogen or hydrogen will
be used depending on the lift pot (nitrogen for the third reactor lift pot
and regenerator lift pot).
4.3.2.8. Set the catalyst circulation flow at the maximum compatible with the P
in the reaction section.
4.3.2.9. Increase the temperature to 480°C at the reactors inlets and at the
reduction chamber D-71311 inlet at a rate of 25°C/h.
4.3.2.10. Maintain this temperature for a minimum of 12 hours until the total water
drained at the low points is lower than 0.2L/h.
4.3.2.11. Owing to the difficulty of sustaining a steady catalyst circulation when the
reaction section is under hydrogen (low DP in reactors), this step shall
be maintained long enough to ensure that the catalyst contained in the
upper and lower hoppers has been reduced.
4.3.2.12. After reduction of the total inventory of catalyst contained in the
regeneration system, the catalyst circulation rate is increased to fill the
lock hopper in about 3 hours.
4.3.2.13. Whenever possible it is recommended to stop the catalyst circulation
after a transfer from the upper surge drum to the lock hopper. The
reason for leaving an empty surge drum is explained in regeneration
start up
4.3.2.14. Decrease then temperatures at reactors and reduction chamber inlets
down to 360°C at the rate of 40°C/hour.
4.3.2.15. Stop catalyst circulation: isolate the manual catalyst tight valves under
the lower hoppers.
4.3.2.16. Close the remote operated ON/OFF valves on the catalyst pipes:
4.3.2.17. Between first lower hopper and lift pot UV3005
4.3.2.18. Between third reactor lower hopper and lift pot UV3013
4.3.2.19. Reduce gas flow of reducing chamber to 40% of design flow (147m 3/h)
4.3.2.20. Keep in service the N2 lift loop and the regeneration loop compressor at
75% capacity to burning oxychlorination and calcination beds with the 3
electrical heaters in service (300°C outlet temperature).
5. Oil in
5.1. Integrated Start-up Scenarios
The aim of this paragraph is to give an overview of a combined pretreatment plus
reforming startup.
The ideal situation to start a reforming is when a source of hydrogen of adequate
purity, independent from the unit is available. In this case the pretreatment unit will
be started with this hydrogen gas, and once the pretreatment effluent is on
specifications (with respect to sulphur nitrogen and water mainly) it will be fed to
the reforming unit.
Generally, however, this is not the case. A batch of desulfurized naphtha will then
be used as start up feed for the reforming unit.
One possible way of starting a reforming unit when no external H 2 is available is as
shown in Fig. 16 at the end of chapter 6.5 “First startup of the unit”. The
desulfurized naphtha batch from the storage is used to start the reforming unit. As
soon as a steady and reliable amount of hydrogen is produced, the pretreater can
be started with raw naphtha. The off-specifications product is sent back to the raw
naphtha tank, until the hydrotreater splitter effluent is on specifications. Then it is
switched to the reforming unit. All possible precautions must be taken to ensure
this naphtha batch is free of water. It is recommended to store it in a fixed roof
blanketed tank and to thoroughly drain the tank bottom and the feed line.
An alternate hydrotreatment plus reforming startup sequence is sometimes used
when dryness of the desulfurized naphtha is questionable.It consists of feeding the
desulfurized naphtha from storage to the hydrotreater stripper - through the
hydrotreater startup by pass in order to remove the water, if any, at the stripper
reflux drum. The stripper bottom effluent is sent back to the desulfurized naphtha
tank. When operators are satisfied with the water content (10 ppm wt) then the
stripper bottom can be switched to the reforming unit and the reforming unit started
with desulfurized dry naphtha to produce hydrogen.
During the whole period of pretreatment startup (approximately 12 hours) it is
strongly recommended to operate the unit at low severity (see later on) in order to
minimize the impact, of possible upsets (sulphur, water content) on the catalyst
The specifications of the feed acceptable for the reformer start-up are:
Feed with similar ASTM distillation as design feed. Impurities are according to
the following:
Note: During the oil in, when the water content of the recycle is within the range of
the analyzer and until the reaction section operating conditions are stabilized, the
water content in the recycle gas must be recorded every hour.
The low severity operation allows lowering the water and hydrogen sulfide content in
the recycle gas, without damage to the catalyst. It also enables a check of the
operation of the catalyst circulation and to carry out the reduction of any fraction of
the catalyst which was at the very beginning in the regenerator, and has not been
contacted by H2 gas.
The low severity operation is characterized by:
A higher than design H2/HC ratio (feed at 60% and recycle compressor at full
capacity).
A pressure higher than normal.
Temperatures which will be increased step by step as the water content in the
recycle drops.
The low severity operation yields a gasoline with a relatively low RON. This
product can be routed to the gasoline pool when found suitable.
During the different steps the water content of the recycle will be determined
by lab analysis until it falls within the range of the on line moisture analyzer
400˚C(752˚F) stage
1. Raise temperature at reactor inlet to 400°C at a rate of 20°C/h.
2. Check water content in the recycle by lab analysis. Whenever possible put
the moisture analyzer on. Cross-check results of both measurements.
3. Drain water at low points and D-71201
4. Initiate chlorination agent injection: starting rate 5 ppm wt of pure
component related to feed rate
5. Stabilize the unit conditions at 400°C
Caution:
From the moment when feed is introduced do not stop K-71201 since this
would favor a quick build up of coke on the catalyst. In an emergency shut
down of the recycle compressor, shut-off heaters and feed immediately (refer to
“Emergency shutdown”).
Start the catalyst circulation in order to perform the coking of the catalyst
contained in the regeneration system (See paragraph 2.5.3 above).
At the end of the catalyst reduction phase, the upper surge drum has been left
empty. Hence the catalyst we will recover in the upper surge drum is representative
of the catalyst from the bottom of the 3rd reactor. Take sample of catalyst every day
in order to analyze carbon and chlorine contents. The regeneration will be started
when the coke level of the circulating catalyst reaches 3%.
6. Regeneration Start-up
Regeneration is started when the coke content of catalyst is higher than 3% wt. For the
first startup, the catalyst circulation only is already on stream. During routine operation,
situations may occur when the regeneration (and the catalyst circulation subsequently)
have been stopped. The sequence below describes the catalyst circulation and
regeneration startup.
6.1.6. Resume catalyst circulation in black burning mode as soon as excess O 2 at the
2nd bed outlet is satisfactory
6.1.7. Change to normal burning mode as soon as Oxychlorination/Calcination zone
is free of coke
The detailed procedure is given below.
6.2.2.9. Adjust the trim cooler E-71303 outlet temperature as near as possible to
design conditions (42°C).
6.2.2.10. Both air injection FV3007/3002 (oxychlorination/calcination and burning
air) are closed, including the block valves, start-up the air compressor K-
71304 and set the discharge pressure at design value (0.88 MPa).
6.2.2.11. Put in service the air dryer DR-71302
6.2.2.12. Line up piping to be ready for air injection to the burning zone only.
When the coke content of the circulated catalyst reaches 3.0% wt the coke
burning can be started.
6.2.4.1. UV3016 air to 1st bed is open while UV3017 air to oxychlorination /
calcination is closed.
6.2.4.2. The air is slowly introduced through FV3007 (before UV3016) in order to
reach 0.4 vol.% of O2 in the flow to the burning zone (check analyzer
AIC3001 at the shell side inlet of E-71301).
6.2.4.3. At 410/415°C in the burning zone the combustion will start immediately
and all the oxygen will be consumed. Check the first burning bed
TDI3122A/B/C read by difference of TI indication at inlet and outlet of the
bed, which must not exceed 40°C. Then begin to inject air through
FV3002 in the second burning bed in order to reach ~ 0.2% vol. O2 at
the outlet (check relevant analyzer AIC3002 on line to the second
burning bed ).
6.2.4.4. Stabilize the conditions and then set in auto cascade these AIC3001 and
FIC3007 through HS3124 selector and the AIC3002 to FIC3002.
6.2.4.5. Resume catalyst circulation with 50–75 % design flow rate
6.2.4.6. Air can be switched from the 1st burning zone to the
oxychlorination/calcination zone only when the catalyst contained in the
oxychlorination/calcination zone has been replaced by regenerated
catalyst. The safe way is to change the air injection only when the
catalyst sampled in the first upper hopper has a coke level lower than
0,2% wt. For such a purpose the catalyst circulation can be increased up
to 75% (310 kg/h). Air switch is made by opening UV3017 to
oxychlorination/calcination and closing UV3016 to 1 st burning bed. After
stabilization of FIC3017 air injection will be cascaded to analyzer
AIC3004 on oxychlorination/calcination gas which will receive its set
point from analyzer AIC3001 on first burning bed inlet.
Notes:
This period of replacement of the coked catalyst with regenerated
catalyst will take place after 8 to 10 hours of burning. In case of
temperature increase after the switch of the air injection to the
oxychlorination/calcination zone, return immediately to the previous
situation and wait another couple of hours before switching again air to
the oxychlorination/calcination zone.
Check carefully the operation of the regeneration loop trim cooler E-
71303
Check the operation of D-71306, caustic solution circulation, caustic
soda and water make-up, water injection. The gas effluent temperature
shall be maintained as low as possible.
ISSUE DATE: 20/03/06 - 151 -
KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (2)
CCR UNIT KRCIM 71200.06 REV.0
The circulating caustic solution shall be analyzed, twice a day, for total
sodium concentration (to be kept higher than 3%) and the pH analyzer
AI3101 at caustic recycle pump suction, it shall remain higher than 8.5
(9.5 max.).
Check the operation of the regeneration gas dryer and air dryer DR-
71301/302 (once per shift during startup period).
Check that O2 content to the calcination zone stays between 4 to 6
vol.%. When the temperature in oxychlorination zone reaches 470°C,
the chlorination agent injection can be started. The amount to be injected
is calculated as follows:
6.2.5.1. By raising PDIC3006 of the master lift (from regenerator to first reactor),
increase slowly the catalyst circulation. Check that the lift flows are set at
the recommended value.
Adjust TIC3001 between 470-480°C.
Adjust TIC3003 between 470-480°C.
Adjust TIC3006 between 510-520°C.
Adjust TIC3005 between 500-510°C.
6.2.5.2. Then the catalyst circulation shall be increased until the following values
are obtained:
Oxychlorination zone:
500 °C outlet
< T° 510°C
<
Calcination zone:
510°C outlet
< T° 520°C
<
6.2.5.4. Take catalyst samples from the 1st upper hopper D-71310 to control coke
and chlorine content on the regenerated catalyst.
The chlorination agent injection is adjusted in proportion to the catalyst
circulation and to the chlorine level of the spent catalyst contained in the
upper surge drum D-71301 (refer to injection rate formula).
6.2.5.5. Check regularly the satisfactory operation of the dryers as well as all
washing drum parameters.
6.2.5.6. The field operators shall regularly perform the following operations:
Drain the analyzer upstream KO pots. Check and if necessary correct the
sampling flow rates.
Drain the dryers upstream KO pot.
Drain the loop compressor K-71301 suction bottles.
Check NaOH injection rate (pump strokes and tank level).
Check chlorination agent injection rate (pump strokes and tank level).
They must report to the shift foreman for any deviation.
During the increase of temperature, the thermal expansion of the reactor internals will
tend to increase the quantity of catalyst contained in the reactors and consequently
will tend to decrease the quantity of catalyst in the circulation loop. The level of the 1st
upper hopper D-71310 will have to be set at a lower value to compensate for this
"loss". Conversely when temperatures are reduced the upper hoppers will operate at a
higher catalyst level.
7. Unit Restart
7.1. Restart Of The Entire Unit
(including regeneration section)
7.1.1. Any unit restart procedure derives from the first startup procedure. The only
difference results from the unit status after the shutdown which dictates the
point where the general startup procedure can be resumed.
7.1.2. For instance, assume a shutdown of the feed pump P-71102A/B of a short
duration: the unit will be kept on stand-by with the recycle compressor K-71201
running, the heater still on, the reactor temperature lowered, Recontacting
section blocked, the H2 rich gas compressor K-71202A/B stopped and possibly
(depending upon the expected duration) the regeneration loop and catalyst
circulation stopped. In this specific case operator will have to resume the first startup at
paragraph " Preparation and feed introduction ", including, if required, the restart of the
regeneration section.
Then, the restart procedure will be resumed at stabilizer total reflux (“Stabilizer
startup on total reflux”) or catalyst heating up and reduction (“Catalyst heating
up and reduction”). However the reduction step of 12 hours at 480°C for water
removal is not required.
Also the feed can be introduced again at a temperature of 425°C, no need for
steps at 360°C and 400°C (no or very little water is expected).
7.1.4. Note also that the unit shutdown results (in the general case where no
independent H2 supply is available) in the shutdown of pretreatment unit 71100.
The unit will be restarted with desulfurized dry naphtha.
7.1.5. An extreme case of unit restart is when the catalyst has been regenerated, or
the reaction section was aerated (for inspection), in this case the restart
procedure will start all over again from the beginning i.e. leak test and partial
inerting (“Second leak test and partial inerting”), catalyst circulation heating and
drying (“Catalyst circulation procedure and principle of catalyst transportation”)
until oil in (“Preparation and feed introduction”).
IMPORTANT:
Under normal steady conditions and design feeds the unit typically operates with a
coke content on the catalyst between 4 to 6% wt (Refer to “Regeneration”).
However, the reforming unit can be maintained on stream without the
regeneration section for some period of time.
In this case, the limiting factor being the coke deposit, the lower the severity, the
longer this period. It is then recommended to reduce reactors inlet temperatures to
approximately 480°C and flow to approximately 60% with maximum recycle rate, in
order not to significantly exceed the 6% wt coke deposit. The period without
regeneration might then last up to two weeks.
However, regeneration with coke deposit higher than 6% wt. have been carried out. In
this case, operators must bear in mind that the coke burning capacity (Kg/h) of the
unit is limited.
Consequently upon restart of the regeneration they must adjust the catalyst circulation
rate taking account of:
a) the maximum coke burning capacity
b) the actual wt% coke deposit
Moreover, they must carefully watch the temperature increase in the burning zones.
It is recommended to start with a lower circulation rate (say 80% of the maximum rate)
and increase progressively, according to the temperature increase in burning beds.
8. Supplements
DWG.InitialStatus
DWG.ReductionCurve
DWG.LoopControl
Oil In Scheme
Contents: This instruction outlines the operation of the CCR heating furnaces. The text
includes:
readiness of a furnace for operation is the shell temperature. When the fires
are started in a new furnace the moisture of the outer surface of the refractory
evaporates into gases but much of the moisture held deeper in the refractory
is driven back into the insulation next to the shell. During this period the
furnace shell remains cold. Then, as heat density in the combustion chamber
is increased the lining heats through and the moisture from the insulation
begins to evaporate. This causes the furnace shell to heat up by the
generation of steam on the adjacent insulation. However when this moisture
has been throughly evaporated, the shell temperature will gall again. If the
operator keeps some progressive account of the shell temperature, he will
note this rise and fall during the drying out process and when the shell
temperature has decreased to the rated casing temperature the furnace can
be considered ready for operation.
2. Start-up Procedure
2.1. System Purge, Pressure Test, Hearth Sweeping
2.1.1. Fuel system purge pressure test
After checking, conduct steam blowing downstream PV4303. Before purging,
disconnect flanges on every main and pilot burner gas line. Remove flame
arrester. Meanwhile, gas knock-out drum D-71401 pressure shall not exceed
0.4MPa controlled by PV4303. After purging is over, connect nitrogen at main
gas drain point to evacuate water in the system.
2.1.2. Hearth sweeping
F-71101.71102.71205 Use air blower to purge, open all main burner throttles.
Purge for 15 minutes above.
2.1.3. Flue gas duct test
Contact instrument to regulate and test F-71101, 71102, 71205, 71201, 71202,
71203 flue dampers and solenoid valves and ensure good condition (flexible
and not jamed).
2.3.8. Ensure that a stable pilot flame has been established before removing the
torch burner.
2.3.9. Check pilot gas pressure downstream of the pressure regulator
2.3.10. If the burner fails to light within 10 seconds, promptly close the gas valve and
repeat the operation starting from steam purging
2.3.11. When checking flame through flame window, operator must stand beside
flame window. Looking to fire flame, must wear special fire glass.
2.3.12. Before lighting main fuel gas burners it is necessary to circulate a cooling
medium through the heater tubes to prevent local and general overheating.
2.3.13. With the primary and secondary air registers half open, slowly open (1/3) the
first fuel gas gate valve to the first main gas burner
2.3.14. Check main burner is ignited through fire window; regulate the flame through
the globe valve. Fully open manual valve and regulate burner air register.
2.3.15. If the gas burner fails to ignite with in 10 seconds, promptly close the gas
valve and repeat the operation starting from steam purging.
2.3.16. Symmetrically ignite another burner.
2.3.17. Main burner must be ignited by light pilot burner
2.3.18. After igniting all burners as above, conduct overall check on furnace.
2.3.19. Ensure heating furnace under normal burning, turn furnace solenoid valve to
automatic position and conduct stability test of pilot burner and main burner.
2.3.20. After ignition and heat up of heating furnace, when furnace outlet temperature
reaches and stabilize at normal operation value, can switch from manual
control to cascade control.
2.4.13. Ensure heating furnace under normal burning, turn furnace solenoid valve to
automatic position and conduct stability test of pilot burner and main burner.
2.4.14. After ignition and heat up of heating furnace, when furnace outlet temperature
reaches and stabilize at normal operation value, can switch from manual
control to cascade control.
4. Troubleshooting
7 Flame Excess furnace load, flue damper Reduce fuel gas quantity & Regulate air door or flue
pulsation opening small, suction small damper.
Fuel gas pressure unsteady or containCheck pipe network or unit generated gas, and
liquid conduct pressure stabilization regulation
accordingly.
8 Unstable Fuel gas pressure change or fuel gas Stabilize fuel gas pressure
furnace with oil According to furnace load, burning status,
outlet Burning influencing factors change determine the number of burners to be ignited, the
temperature (Ex: Climate, load etc..) height of whole flame shall not exceed two-third of
Instrument auto control failure hearth height, every part of hearth shall be heated
Hearth temperature change uniformly
Inspect and adjust auto control of furnace
Make adjustments according to feed flow rate when
feed temperature changes. In case of larger
change, can regulate outlet temperature as above-
mentioned 1-2 minute in advance
9 Tube coking Flame uneven, making temperature Retain uniform hearth temperature
inside hearth uneven, causing local Retain stable feed, timely burnout in case of feed
overheating interrupt and insure uniform feed rate in every loop
Feed rate changed too large or Regulate flame, ensure more burners, uniform
stopped suddenly flame, short burning flame, hearth bright, flame
Flame deflects to furnace tube, cause vertical, not burn furnace tube, not generate local
local overheating overheating area
5. Shutdown
5.1. Normal Shut-Down Of Heating Furnace
5.1.1. General Precautions
During controlled shutdown or in an emergency, the following dangerous
conditions must be avoided:
Fuel gas entering the combustion chamber when all fires are off as,
explosions may occur.
The presence of heavy hydrocarbons at low velocity in the coils. This can
lead to coke deposition.
Thermal shock due to a rapid cool-down.
Either a positive pressure in the combustion chamber or too high a vacuum.
Either condition can cause refractory cracking.
Contents: This instruction outlines the operating conditions and control of the reforming
section. The text includes:
1. Operation Influencing Parameters
2. Principles Of Key Parameters Control
3. Adjustment Of Operating Conditions
4. Troubleshooting
5. Operation Conventional Control
6. Analysis Control
7. Supplements
An increase of temperature (i.e. WAIT) have the following effects, assuming the
space velocity (i.e. the feed rate) and feed characteristics stay unchanged:
Increases octane.
Decreases the yield (of C5+ fraction).
Decreases the H2 purity.
Increases the coke deposit.
The set of curves given in (Figures 20 to 24) allows an estimate of the increment in
the WAIT which would result from increment in the selected parameter:
ISSUE DATE: 20/03/06 - 178 -
KRC REFORMING SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0
Not regulated normally, working control pressure is product separator pressure (i.e.
D-71201 pressure) instead of reactor pressure, reaction changes along with the
change of system pressure. D-71201 pressure normally controlled at 0.243MPa, D-
71201 pressure controller PIC-2068 output adopts two split-range control, normal
pressure regulation controlled by valve PV-2068A and valve PV- 2068C . Open PV-
2068 / B only in case of system overpressure.
The low pressure which favors high yields, favors also coke build up. During
transient conditions (startup, shutdown, upsets) it is recommended to increase the
pressure to 0.34MPa.
Knowing the liquid flow rate (or the space velocity), plus the recycle flow and the
reactors operating conditions enables to calculate the actual flow in the reactor,
hence the contact time.
The lower the space velocity (i.e. the higher the contact time), the higher the
severity, assuming all other conditions unchanged.
Lowering the space velocity has, then, the same effects as increasing the
temperature i.e., it:
ISSUE DATE: 20/03/06 - 179 -
KRC REFORMING SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0
If temperature increase is limited (by heater design duty or anything else) lowering
space velocity (i.e. decreasing flow rate) can give an additional boost to octane.
Operators must bear in mind that each time liquid feed rate is changed, a
temperature correction must be applied if octane is to be maintained. When feed is
increased, temperature must be raised and conversely, when feed is reduced
temperature must be lowered.
Original Increased
conditions feed
bbl/h 800 1000
Feed vol.
m3/h 127.19 158.99
(API) lb/bbl (55) 265.3 no change
Sp gr
Kg/m3 756.9 no change
lb/h 212,240. 265,300.
Feed wt
t/h 96.270 120.340
wt (lb) 117,910. no change
Catalyst
(t) 53.480 no change
WHSV 1.8 2.25
WAIT reading (°C) -2 + 2.5
WAIT change (°C) Base + 4.5
CONCLUSION: For an increase of WHSV from 1.8 to 2.25 the WAIT must be
increased by 4.5°C.
The unit's space velocity is 1.6, usually not less than half of design value.
Fig. 23 gives an estimate of the relationship between PNA and severity. As with
the other figures it is used by determining increments related to an existing
base case (see example).
(°C) (°F)
IBP (Initial Boiling Point) 70-100 158-212
EP (End Boiling Point) 150-180 302-356
One must also consider the distillation end boiling point (EP). High EP means
heavier fractions which are richer in aromatics and naphthenes and thus are
easier to process. However the high boiling point fractions are potential sources
of polynuclear aromatics which are coke precursors. EP higher than 180°C
(356°F) are generally not recommended.
Note that some water analyzers drift, with time, towards lower readings. It is
wise to check the analyzer prior to start water injection.
3.2.3. A higher H2S content in the recycle indicates a malfunction of the hydrotreater,
either a too low temperature in the reaction, a sudden increase of total sulfur in
the hydrotreater feedstock, or simply a poor operation of the stripper. The
cause must be found and corrected as to reduce the total sulfur of the feed
down to the design value.
3.2.4. If the H2S content of the recycle gas tends to increase, do not compensate with
a temperature increase. The reason for the sulfur content in the feed must be
found and corrected.
3.2.5. Anyway if this value reaches 5 ppm vol. the feed flowrate and severity must be
decreased to 480°C until the problem is solved and the H 2S content of the
recycle gas restored to its normal value.
4. Troubleshooting
4.1. General
The main causes of concern, related to process, are a possible:
Unexpected decrease of octane number.
Loss of reformate yield.
Unexpected T reduction in the first catalytic bed.
Note that critical equipment or system failures (recycle compressor, H2 rich gas
compressor, instrument air, cooling water ...) which lead to an automatic emergency
shutdown are covered in “Emergency instructions manual”.
Prevention
4.6.1.6. The best prevention is to record, on a periodic basis, the lift conditions
and the reactor pressure drop. The lift gas velocity must be adjusted to
the recommended velocity as calculated above in 4.3 "Lift gas flow". One
must keep in mind that when an excessive pressure drop occurs it is
already too late to correct the cause. This is why maintaining the
recommended catalyst velocity in the pipe is so important.
Reactor cleaning
4.6.1.7. The only way to reduce the pressure drop when it becomes
unacceptable is to shut down the unit, unload the affected reactor and
screen the catalyst with a 1.7 mm x 1.7 mm mesh with a screening
machine. The catalyst must be stored in drums under an atmosphere of
nitrogen.
4.6.1.8. Depending upon the time available for this unplanned shutdown and also
of the time to run until the next planned shutdown, the reactor may be
inspected and cleaned. Special attention must be then given to the
cleaning of the center pipe.
4.6.1.9. Then the screened catalyst will be loaded again. Generally a catalyst
make-up of 3 to 4% is required.
5.1.1. Reactor inlet temperature and furnace gas pressure cascade control
Influencing factor Remedies
Fuel gas composition and Properly regulate gas flow
pressure change
Recycle compressor Troubleshoot compressor failure
malfunction causes H2 flow
fluctuation
Feed fluctuation Stabilize feed
5.1.2. C-71201 tower bottom temperature and F-71205 gas pressure cascade control
Influencing factor Remedies
Furnace operation fluctuation Regulate furnace operation
Tower pressure fluctuation Stablize pressure
Reflux rate fluctuation Stabilize reflux
5.2. Pressure
6. Analysis Control
6.1. Recommended Methods And Frequency
The frequencies given here below are related to routine operation.
Stream Test Item Test Method Frequency
SN
Name IFP SEI IFP SEI IFP SEI
Relative Density ASTM D4052 1/D 1/W
Distillation °C ASTM D86 2/W 1/W
ASTM ASTM
Sulfur,ppm 1/D 1/W
D4045 D5453
Nitrogen,ppm ASTM D4629 Occas
ASTM SH/T063
Bromine Index Occas 1/W
D2710 0
SH/T023
Hydrotreated Naphtha -Feed
LPG
ASTM
sampling Occas
1265
method
Relative ASTM
1/W
Density D4052
ASTM
Distillation °c 1/D
D86
Vapor ASTM
2/W
SN- Pressure D323
Reformate
71210 Octane # ASTM
Occas
(RON) D2699
ASTM
Gum Occas
D381
SH/T023
Composition 2/W
9
7. Supplements
DWG.PresureControl
Contents: This instruction outlines the shut-down procedure of the CCR reforming
Unit.The text includes:
1.1. Description
1.1.1. The normal shutdown applies to a shutdown planned long in advance
(preventive maintenance) or to unexpected events which are not of an
emergency nature. The shutdown shall then be performed in planned stages.
The operators of the upstream or downstream units shall be informed of the
shutdown to enable them to make the necessary adjustments and/or to plan
their own shutdown.
1.1.2. The general procedure to be followed for a total shutdown is:
To lower the severity and the capacity of the unit.
To shut down the reaction section.
To shut down the catalyst circulation and the regeneration sections.
1.1.3. Note: If no external source of hydrogen is available the hydrotreater unit will
also have its capacity reduced first, then be shut down. Special care will be
taken during this period as to keep the hydrotreated product on specifications.
1.1.4. Several shutdown cases are considered:
Short duration normal shutdown (less than 24 hours).
Long duration normal shutdown.
Shutdown with catalyst unloading.
Normal shutdown of the catalyst circulation and regeneration only
Step 1
Start lowering reactors R-71201/202/203 inlet temperature to 470°C, by
increments of 5°C.
Step 2
One hour after the start of step 1, start reducing the feed flowrate, by
increment of 3t/h, to 60% of the design capacity (30 t/h), which must be
reached at 470°C. Adjust flow increments in order to maintain the product
quality within acceptable limit. At the same time the feed to the pretreatment
unit (71100) is proportionally reduced and its reaction temperature adjusted.
Step 3
Simultaneously with the preceding step, increase the reaction section
pressure to approximately 0.350 MPa g (at separator drum D-71201). During
this pressure increase, watch carefully the catalyst circulation, the N 2 lift
PDV's opening and adjust the bias if required to maintain catalyst circulation
Step 4
Stop the catalyst circulation and the regeneration loop as described in
“Catalyst regeneration section” (Partial shutdown) 8.1 of KRCIM 71300.05
Step 5
Stop the feed to the pretreatment unit 71100 and when the level in the bottom
of the C-71101 stripper starts to decrease, stop the feed to the reforming unit
71200. Close FV2006. Line-up the product to the slop tank. Shut-off the
reduction heater K-71304 and close the H2 valve FV3017 to reduction
chamber and PDV3012 as well as HV3003 at reduction gas outlet
Step 6
Immediately after the feed cut off, shut down the H2 rich gas compressor K-
71202. Close in manual mode the spill back PIC2068C of the H 2 rich gas
compressor to avoid the quick depressurization of the recontacting section
into the reaction section and the release of the separator drum PSV. Shut
block valves at compressor K-71302 suction and discharge. Start lowering
reactor inlet temperatures at a rate of 25°C/h to 400°C. K-71201 remains
in operation, in the meantime, retain D-71201 pressure not less than 0.3MPa,
D-71201 liquid level retains 30%, if liquid level is higher, use P-71201 to
transfer oil to C-71201 through start-up line.
Step 7
When the level starts to decrease in D-71201, stop the pump P-71201 to the
recontacting section and isolate the block valves of LV2002.
Step 8
When the level starts to decrease in D-71203, isolate the block valves of
LV2008 to the LPG absorber drum D-71205
Step 9
When the level starts to decrease in D-71205, stop pump P-71204 to the
stabilizer and close the block valves of the FV2015
Step 10
Then isolate the bottom of the stabilizer C-71201, by closing reformate
FV2026 & LPG LV2019 block valves. Keep the column at total reflux
conditions.
3.2. Status
Before shutdown, all subunits and utilities are operating normally. During shutdown,
these parts will be stopped successively.
3.4.6. Before shutdown, organize staff members and workers to study shutdown
scheme.
Step 1
Start lowering reactors inlet temperature to 470°C, by increments of 5°C.
Step 2
One hour after the start of step 1, start reducing the feed flowrate, by increment
of 3t/h, to 60% of the design capacity (30 t/h), which must be reached at 470°C.
Adjust flow increments in order to maintain the product quality within acceptable
limit. At the same time the feed to the pretreatment unit (71100) is
proportionally reduced and its reaction temperature adjusted.
Step 3
Simultaneously with the preceding step, increase the reaction section pressure
to approximately 0.350MPag (at separator drum D-71201). During this pressure
increase, watch carefully the catalyst circulation, the N2 lift PDV's opening and
adjust the bias if required to maintain catalyst circulation
Step 4
Stop the catalyst circulation and the regeneration loop as described in “Catalyst
regeneration section” (Total shutdown) 8.2. of KRCIM 71300.05
Step 5
Stop the feed to the pretreatment unit 71100 and when the level in the bottom
of the stripper C-71101 starts to decrease, stop the feed to the reforming unit
71200. Close FV2006 and install a blind in the line. Line-up the product to the
slop tank. Shut-off the reduction heater H-71304 and close the H2 flow control
valve FV3017 to reduction chamber and PDV3012 as well as HV3003 at
reduction gas outlet
Step 6
Immediately after the feed cut off, shut down the H 2 rich gas compressor K-
71202. Close in manual mode the spill back PIC2068C of the H 2 rich gas
compressor to avoid the quick depressurization of the recontacting section into
the reaction section and the release of the separator drum PSV. Shut block
valves at compressor suction and discharge. Isolate with blinds all H2 outlet /
inlet lines to the unit. Start lowering reactor inlet temperatures at a rate of
25°C/h to 400°C. K-71201 remains in operation, in the meantime, retain D-
71201 pressure not less than 0.3MPa, D-71201 liquid level retains 30%, if liquid
level is higher, use P-71201 to transfer oil to C-71201 through start-up line 100-
P-2099
Step 7
After 6 hours of hydrogen sweeping, allow the catalyst beds to further cool
down while decreasing reactor outlet temperatures progressively to 200°C,
then cut off the fired heaters F-71201/202/203. Continue circulating hydrogen
with the recycle compressor until the temperature in the reactor beds is 50°C.
Step 8
Depressurize D-71201 to the flare to 0.05MPa, fill D-71201 with nitrogen from
K-71201 outlet to 0.3MPa. Depressurize again to flare. Fill again to 0.3MPa,
ensure that the speed of pressure rise and fall per hour shall not exceed
0.1MPa. Drain at every low point and dead angle position of hydrogen system.
Lead-in instrument pressure line, nitrogen purging replacement at sampling
opening. D-71201 pressure is maintained at 0.3MPa, continue nitrogen
replacement from K-71201 outlet, control pressure and depressurize to flare.
When hydrogen and hydrocarbon content in sampling analysis is less than
0.5%, depressurize to 0.1MPa. Close PIC2068 manual valve, stop K-71201
and close block valves at inlet and outlet.
Step 9
When reforming system uses nitrogen for inerting, use K-71302 outlet to
replace hydrogen gas in lift lines with N2 from start-up line. If replacement is
qualified, stop K-71302 The (H2 + HC) content of the gas in the reaction section
shall drop to approximately 0.2 vol. %.
Step 10
M-71301 depressurize to flare system, feed nitrogen to inlet until hydrogen
hydrocarbon content of sampling analysis less than 1%.
Step 1
Before reforming feed cut, decrease D-71203, D-71204 & D-71205 liquid level
to 20-30%. Keep C-71201 level at 60% on total reflux and change gasoline to
offspec tank .
Step 2
Close reformate and LPG out valves
Step 3
Maintain liquid level of tower bottom at 60% and perform a single tower
circulation. Reduce F-71205 outlet temperature to 150˚C at the speed of 25-
30˚C/h, and stop F-71205. P-71202 continues circulation till tower bottom
temperature is less than 80˚C
Step 4
Connect nitrogen to K-71202 outlet and fill pressure to 0.8MPa, flush oil in D-
71203 and pipeline to D-71205. Isolate with blind D-71203 bottom. Then use
nitrogen to purge D-71204 overhead pipe to D-71205. Use P-71204 to transfer
oil to C-71201. If D-71205 is emptied then stop P-71204.
Step 5
After pump P-71204 is stopped, close FIC2015 valve and close gate valve from
D-71204 to D-71205. Depressurize from PIC2085 to flare, and conduct nitrogen
replacement of system.The (H2 + HC) content of the gas in the reaction and
recontacting sections shall drop to approximately 0.2 vol. %.
Step 6
Stop P-71202 and connect N2 to outlet and purge oil in furnace tubes into C-
71201. Send oil in D-71204 into C-71201, stop P-71203 and reduce C-71201
bottom oil to offspec tank.
Step 7
Drain all lines until you observe gas then close drains.
Note: Close all gate valves to isolate the control valve which you close
Alternate procedure
4.2. The alternate to the above procedure, is the coarse decoking of the catalyst in the
regenerator, prior to unloading. Of course the oxychlorination will not be in service.
Note 1: During these operations, the regeneration section is kept under nitrogen
atmosphere. Care should be taken to avoid stress corrosion by chlorine for the
stainless steel equipment
Note 2: Another alternate to the dumping of coked catalyst from the reactor and
regenerator bottom is possible. It applies when the catalyst is to be replaced by a
fresh one, but when no reactor(s) or regenerator inspection is planned. It consists
in dumping the catalyst at the bottom of the lock hopper, while the reaction
section is in service at low severity, and in replacing it, in the same vessel, by
fresh catalyst, by means of the catalyst loading deveice, plugged atop the lock
hopper. In such a case, the regenerator is used only to dry the new.
Table of Contents
1. Unit Introduction
2. Manual Structure
1. Unit Introduction
1.1. General
Continuous Catalytic Reforming Unit (CCR) of Khartoum Refinery Company is built
under the expansion project of the refinery, phase II. The unit is designed by
Sinopec Engineering Incorporation. The process utilizes Axens's "State of the art"
moving catalyst bed with continuous catalyst regeneration.
The unit is designed to process 400,000 metrics tons per year and to operate at a
severity of RON 98 with an on-stream factor of 8000 hours/year.
2. Manual Structure
The design information and operating instructions of the Continuous Catalytic Reforming
Unit (unit71) are covered by six different volumes as follow:
1. Basis of design
2. Unit Description
3. Catalyst
4. Chemistry
1. Basis Of Design
1.2.1. Air
Plant air
(oil-free for catalyst regeneration)
Pressure Temperature
Minimum: 0.6MPa(G)
Normal: 0.8MPa(G)
Instrument air
Minimum: 0.6MPa(G)
Normal: 0.8MPa(G)
1.2.2. Water
1.2.3. Nitrogen
1.2.4. Fuel
Minimum: 0.30MPa(G)
Normal: 0.35MPa(G)
Maximum: 0.40MPa(G)
Quality : Thermal value:7000kcal/kg
These data are required for reference only to indicate if a need exists for tracing or
winterizing.
Relative humidity
o Average: 27%
o Maximum: 44%
Barometric pressure
o Minimum: 96.3kPa
o Maximum: 96.9kPa
o Average: 96.56kPa
2. Unit Description
Coke burning.
Catalyst oxychlorination.
Catalyst calcination.
Catalyst cooling.
Catalyst reduction.
The first three steps are performed in the regenerator, the fourth step in the first lower
hopper and the last step in the reduction chamber.
2.1.1. Regenerator
Spent catalyst coming from the lock hopper D-71302 is stored in the
top of the regenerator during the equivalent of 1 to 2 hours of catalyst
circulation, where it is smoothly preheated by a part of the heat
released by the combustion zone.
Then the spent catalyst flows from this zone to the burning zone by 6
descending pipes.
The burning zone is composed of two radial beds. The two beds are
physically linked by 6 descending pipes.
Temperature : 510 °C
Temperature : 520 °C
If the entire amount of coke is not burnt off at the end of the second
bed, the regenerator will be operated in black burning mode : the
catalyst, though not free of coke, flows through the oxychlorination
and the calcination zones, in which the air injection as well as the
chlorination agent and water injections have been previously totally
stopped.
The 8 pipes are not insulated in order to allow a natural cooling of catalyst
by convection.
Catalyst flows from there down to the first lift pot D-71305, where it is lifted
by a flow of nitrogen gas into the first upper hopper D-71310, before being
introduced into the reduction chamber D-71311.
The latter is sent to the purification unit M-71301 to upgrade its purity up to
99 % mol minimum of H2. Residue of hydrogen purification unit is sent to
fuel gas. Permeate is preheated in the reduction exchanger E-71304. Then
an electrical heater (reduction heater H-71304) allows a precise adjustment
of the reduction inlet temperature.
The first stream preheats the inlet reduction gas in the reduction exchanger
E-71304, the second stream preheats the hydrogen-rich gas going to the lift
system in hydrogen lift gas exchanger E-71305. Both streams are then
mixed before being sent back to the reaction section.
The reduced catalyst is then introduced into the first reactor R-71201.
This gas is mixed with the gas leaving the first burning bed. It is used to
adjust the inlet temperature of the second bed.
Water is injected in this oxychlorination gas. Then the gas is heated through
an electrical heater H-71303 which allows to control the oxychlorination gas
inlet temperature and some chloriding agent is added just before entering
into the regenerator. Contacting is performed into M-71307 static mixer,
right downstream the injection point.
The oxychlorination gas and the calcination gas are mixed in the
oxychlorination bed. The oxychlorination effluent is sent to the calcination
feed/effluent exchanger E-71302 and then mixed with the combustion
effluent going to washing section in order to eliminate chlorine compounds.
The air injected in the regeneration loop is taken from air instrument
network, compressed by means of a double stage air compressor (K-71304
A/B), cooled down by air trim cooler E-71308, passed through air dryer
drum D-71342 and then dried by air dryer DR-71302 (up to less than 50
ppm vol. of water).
The gas coming from the washing drum flows through a dryer DR-71301,
then through a filter M-71304 where possible particles, in particular
dessicant alumina particles, are trapped and finally to the regeneration loop
compressor K-71301 A/B.
At the compressor discharge, the gas is split into the three streams
described above:
o Burning gas
o Quench gas
o Lift 2, between the first reactor R-71201 and the second reactor R-
71202.
o Lift 3, between the second reactor R-71202 and the third reactor R-
71203.
The catalyst flow is adjusted as follows: the total flowrate of the lift gas
must remain as steady as possible because any change in this flow
will affect the velocity of the catalyst in the lift line. This flowrate must
be checked carefully because a too high velocity may lead to a higher
rate of catalyst attrition.
This gas going to the lift pots D-71305 / D-71331 / D-71332 / D-71333
is divided into two streams:
The pressure drop measured between the lift pot and the next upper
hopper indicates the catalyst flow: nearly null when there is no
catalyst flow, this pressure drop will increase to about 0.010 MPa
when there is catalyst flow. Therefore this measure is used as an
indication of catalyst flow in the control used for the follow-up of the
operation of the lifts.
Nitrogen gas from lift 4 is separated from the catalyst in upper surge
drum D-71301 and flows through a fines filter M-71303 where catalyst
dust is recovered.
In this filter, the gas circulates in upflow: it enters at the middle of the
drum and flows through several cartridges of filtering elements where
catalyst dust is trapped. These cartridges are automatically cleaned,
when the pressure drop increases, by a counter current flow of
nitrogen.
Nitrogen gas from lift 1 is separated from the catalyst in the first upper
hopper D-71310 with an elutriation system, and cleaned in a second
fines filter M-71302.
The other part of the gas is mixed with the nitrogen lift gas coming
from the upper surge drum D-71301.
The total nitrogen gas flow is cooled through the nitrogen loop trim
cooler E-71306 and circulated by means of a compressor K-71302
A/B to the lift 1 and to the lift 4. A spillback line of nitrogen loop allows
pressure control of N2 circuit.
This hydrogen-rich gas is recovered in the 2nd and 3rd upper hoppers
and mixed with the reactors feed. For instance, for lift 2, hydrogen-rich
gas is separated from the catalyst in the second upper hopper D-
71312 and mixed with the feed of the second reactor R-71202.
Using nitrogen gas as lift gas between the regeneration and the
reaction section allows to isolate the regeneration section from the
reaction section which are connected by the catalyst circulation lines.
o Safety valves : if the nitrogen sealing fails for any reason, the
valve between the first upper hopper D-71310 and the
reduction chamber D-71311 and the valve between the fourth
lower hopper D-71323 and the fourth lift pot D-71333 will close
automatically, isolating the two sections.
o A safety valve between the first lower hopper D-71304 and the
first lift pot D-71305 is also provided to isolate the regenerator
R-71301 from the nitrogen gas system.
To avoid the reactors and regenerator basket screens plugging, two catalyst
elutriation systems are installed on the catalyst loop.
The first one, using the up-flow design (which requires less elutriation gas), is
installed at the inlet of the regeneration section (at the top of the upper surge drum)
to remove catalyst fines.
The second one, using the down flow design, installed before the reaction section (at
the top of the first upper hopper) to remove catalyst fines and ships
Oxygen atmosphere, including the whole regenerator, except for the top part used
for a temporary storage of the spent catalyst. An entering nitrogen stream ensures
the seal function.
Nitrogen atmosphere, including the upper surge drum, the lock hopper, the top of the
regenerator, the first upper hopper, the first and last lower hoppers, and the first and
last lift pots. The seal function is ensured by a nitrogen gas stream leaving this zone.
Hydrogen rich gas atmosphere, including the upper hoppers (except for the first), the
reduction chamber, the reactors, the second, third, and fourth lower hoppers and lift
pots. In this zone, reactors are special areas allowing, in addition to hydrogen, the
presence of hydrocarbon molecules.
3. Catalyst
The CCR reforming catalyst consists of metals impregnated on an alumina base. A wide
variety of metals can be used, but platinum is the chief metal. The alumina base acts as a
support for the metal. the alumina is also a support for chloride.
In reforming reactors, both the metal and the chlorided base help catalyze desirable
reactions. The chlorided alumina acid function catalyzes isomerization and cracking
reactions.
Optimum catalyst performance requires a proper balance of these two catalytic functions.
too much or little of one or the other will upset the selectivity and activity of the catalyst.
As a result, the performance of the catalyst will suffer.
The operation of the Catalyst regeneration section has a great effect on the proper
balance of the metal and chloride functions. Each of the four main steps of catalyst
regeneration must be done well to insure the proper balance is maintained. Proper
operation of the Catalyst regeneration section will help insure optimum performance of
the catalyst and long catalyst life.
In addition to its optimum catalytic properties, the catalyst also has strong physical
properties. It is specially made to resistant to attrition. Proper construction and operation
of the Catalyst regeneration section will help preserve the good mechanical strength of
the catalyst and minimize attrition.
4. Chemistry
The Catalyst regeneration process is a four-step (excluding cooling here) process where
the desirable regeneration reactionsare completed on the catalyst. The operating
conditions for each are designed to favor certain chemical reactions. Each step is
important in its own right, and all four steps must be performed correctly. The goal is to
restore the catalyst to a condition that is close as possible to that of fresh catalyst. the
basic regeneration chemistry is the same for all regeneration sections.
Spent Catalyst
O2 Combustion
O O
O O
Pt Pt
Cl OH
Pt Pt Pt
Al2O3
Chloride
Compound Oxychlorination
+ O2 + H2O
Reactors
Cl Cl
Pt
OH Cl
O O
Al2O3
O2 Calcination
Cl Cl
Pt
OH Cl
O O
Al2O3
+ H2 Reduction
H H
Pt Pt OH Cl
Regenerated Catalyst
This reaction is necessary and desirable to remove coke, but it can easily damage
the catalyst. It results in a temperature rise on the catalyst, and high temperatures
greatly increase the risk of permanent damage to the catalyst. So the burning must
be controlled. This is done by controlling the oxygen content during the burn. High
oxygen makes the burn temperatures high. But low oxygen makes the burning too
slow.
4.2. Oxychlorination
The second step adjusts the chloride content and oxidizes and disperse the metals
(i.e., platinum) on the catalyst. These reactions take place by complex reactions with
oxygen and an organic chloride compound. These reactions need both oxygen and
chloride. The chloride adjustment reactions can be summarized as follows:
Chloride is needed on the catalyst to keep the proper activity of the acid function.
But too much or too little chloride will have undesirable effects in the reforming
reactors. So the amount of chloride on the catalyst must be controlled. This is done
by controlling the injection rate of the chloride compound.
More evenly distributed metal on the catalyst surface results in better metal function
of the catalyst. The conditions that promote proper oxidation and re-dispersion of the
metal are high oxygen concentration, adequate residence time, correct temperature,
and correct chloride concentrations.
4.3. Calcination
The third step dries excess moisture from the catalyst. Excess moisture is present
from the coke burning step. Drying occurs when a hot, dry gas flows cross the
catalyst, removing water from the catalyst base:
The drier the catalyst is before it re-enters the reforming reactors, the better its
overall performance will be. This drying step is favored by high temperature,
adequate drying time, and adequate drying gas flow rates.
4.4. Reduction
The fourth step converts the metals from the oxidized state to a reduced state. This
must be done after the oxychlorination step to return the metals to a state that is
optimum before returning the reforming reactors. The reduction reaction takes place
with hydrogen by the following reaction:
The more complete the reduction, the better the metal will perform in the reforming
reactors. The conditions that favor this reaction are high hydrogen purity, sufficient
reduction chamber temperature and reduction gas flow rates adequate to ensure
good gas distribution.
1. Plant Inspection
2. Cleaning of Piping and Equipment
1. Plant Inspection
In addition to all points mentioned under same heading in KRCIM 71200.04, catalyst
regeneration section should be specifically inspected for the following:
1.1. Reactors
The status prior to inspection is supposed to be as follows: reactor is erected
with all its internals installed. Piping is connected.
Enough clearance must have been provided around the top of each reactor to
allow for the removal of the inlet elbow.
Four catalyst pipes from the upper hoppers will be dismantled to ease the
removal of the inlet elbow. The inlet distributor is removed then and checked
for size and positioning.
Air must be circulated through the reactor to allow for entry.
1.2. Regenerator
If the removable parts of the regenerator are not installed yet, they will be
cleaned, checked on ground and preassembled before being fitted in. If they
are already installed, they will be inspected from inside.
Before closing the manholes of the equipment, a last inspection is carried out. The
aim is to check the presence of foreign bodies inside the equipment and to see
whether internals such as wire mesh, compartments, trays, vortex breakers, length
and position of the thermocouples, reflux and feed distributors, etc.. have the right
size and are properly fitted.
Contents: This instruction outlines the procedure for the start-up of the CCR
regeneration Unit. The text includes:
1. Start-Up Requirement
2. Unit Purging
3. Initial Leak Test
4. Unit Dryout
5. Catalyst Loading
6. Second Leak Test And Partial Inerting
7. Unit Start-up
8. Catalyst Regeneration Section Shutdown
1. Start-Up Requirement
1.1. All overhaul activities and technical modifications influencing Start-up are completed.
All units, removal of equipment and pipeline blinds conform to process requirements.
1.2. Pressure gauges and safety valves are checked. Replacement work and installation
is completed.
1.3. All chemical raw materials are ready and sufficient.
1.4. All process lines and equipment has been purged, qualified in pressure test and
undergone final inspection according to the following procedures.
1.5. Disassembled or replaced equipment flanges are padded and screwed uniformly.
1.6. Safety valves in good condition and its set pressure meet the requirement.
1.7. Close all atmospheric relief valves and drain.
1.8. Verify all instruments are in good condition.
1.9. Utilities services are working normal.
1.10.Ensure complete fire appliances, place inflammables and explosives in fixed area,
clean sundries on site.
1.11.Contact dispatch, maintenance department, fitters, electrical maintenance and lab.
Complete corresponding support work.
1.12.Complete and examine all Start-up schemes, planning diagrams, all related
procedures sheet and work permits.
1.13.All maintained and revamped equipment has acceptance qualification sheet.
1.14.Inspection of the unit is done according to “Plant Inspection” procedure in (KRCIM
71300.04)
2. Unit Purging
2.1. Purging objective
2.1.1. Eliminate welds rods and slags, abrasive dusts, oxides and in general other
substances which might impede the normal unit operation or damage the
equipment (valves, pumps, compressors, turbines, etc.)
2.1.2. Timely find existing problems through process line. Ensure system operability.
2.1.3. Make operators further understand field flow path.
2.4.8. Flushing of P-71301A/B and P-71302A/B outlet and inlet pipelines and D-71306 outside pipeline
Inject soft water into D-71306; when liquid level reaches a certain height, discharge it through upper and bottom liquid
level glasses simultaneously, and flush middle and bottom outlet pipelines.
After D-71306 establishes liquid level, flush P-71301A/B inlet pipelines to clean, then, start up P-71301A/B to flush the
water in pump outlet pipeline, disconnect it at alkali-injection nozzle for discharging.
Inject water into T-71301 to a certain liquid level, flush P-71302A/B inlet pipelines to clean, then, start up pump to flush
pump outlet pipeline, disconnect it at alkali-injection nozzle for discharging
3.4.1. Pressure boosting speed should be slow and air tightness test pressure should
comply with the regulations strictly without overpressure.
3.4.2. Any leak source found should be marked in time and the maintenance
personnel should be contacted for handling.
3.4.3. Pay attention to inspect whether there is interflow between systems and avoid
equipment overpressure strictly. Watch out for gas expansion in the system
and consequent equipment overpressure because of ambient air temperature
change.
3.4.4. During air tightness test, commands should be given uniformly and personnel
in all areas should contact with each other.
3.4.5. During air tightness test of each system, at least two pressure gauges should
be used to observe pressure with required pressure gauge precision of
magnitude 0.4, 1.5-2 times of the highest air tightness pressure.
3.4.6. Handling of leak sources under pressure is not allowed.
3.5.1. Initial leak tests will be performed under KRC or Engineering company
responsibility and the general instructions hereunder shall only be used as a
reminder.
3.5.2. The initial leak tests can be performed using air or nitrogen depending upon
local facilities. The test pressure will be the air or nitrogen system pressure or
the unit (or section of unit) design pressure, whichever is the lower.
3.5.3. The unit is isolated with blinds from adjacent sections containing hydrocarbons
(liquid or gaseous), and from utilities systems where pressure is lower than air
(or nitrogen) pressure.
3.5.4. The pressure rise must be checked on several manometers and possibly
checked on a pressure recorder. Leaks must be carefully located and
tightened. Their location must be recorded.
3.5.5. The leak test is satisfactory when the pressure decrease is lower than
0.005 MPa/hour over a period of 4 consecutive hours.
3.5.6. The air (nitrogen) used for leak tests should be purged out of the unit using low
points drains to remove free water, if any.
3.5.7. For the purpose of leak tests the unit will be divided into sections of
approximatively the same design pressure, as defined hereunder. Air (nitrogen)
will be injected at different locations depending upon check valves.
In addition, all utilities lines, especially the ones connected to the flare and fuel gas
networks (including safety valves) will be fitted with blind flanges.
The reaction section is isolated as described on the following attached scheme.
The points of isolation are indicative only and must be reviewed on-site, to take into
account actual piping arrangement.
Nitrogen Section
Airtightness requirements and standard
The airtightness media is nitrogen. The pressure tapping point for
airtightness of this part uses pressure of N2 compressor knockout drum
D-71307 as reference, namely, the highest operation pressure in D-
71307 of 0.225MPag.
Airtightness standard
Static
Pressure Constant
Airtightness Airtightness allowed
boosting pressure
part phase pressure
MPa(G) speed time
MPa/5min h
drop
MPa/h
Nitrogen 0.225 0.1 8 0.005
Regeneration Section
Airtightness requirements and standard
The airtightness media is nitrogen. The pressure tapping point for
airtightness of this part uses pressure of washing drum D-71306 as
reference, namely, the highest work pressure of 0.445MPa.
Airtightness standard
Chronologically, once the initial leak tests are over, the drying out of the
unit takes place, prior to catalyst loading.
4. Unit Drying
4.1. Drying Objective:
Reaction, catalyst circulation and regeneration sections must be dried out prior to
catalyst loading, firstly to avoid damaging the catalyst with water, secondly to
shorten the duration of the low severity operation after first oil in.
4.2.3. The first loop uses the recycle compressor, the hydrogen rich gas compressor
and the nitrogen lift gas compressor and includes the reaction section,
absorber section and nitrogen section as defined above in chapter 3.6
"Recommended sections for leak tests". The fired heaters are used for warming
up.
4.2.4. The second loop is the regeneration section (regeneration section as defined in
3.6 "Recommended sections for leak tests") and uses the regeneration loop
compressor to circulate nitrogen which is heated in the electrical heaters
(burning, oxychlorination and calcination heaters). The regeneration drying loop
is isolated from the previous one by the special gas tight valves between the
lock hopper and the upper surge drum and the valve on the seal leg between
the first lower hopper and its lift pot.
5. Catalyst Loading
Please refer to chapter 5 of KRCIM 71200.05
8.2.4. Decrease both electrical heaters outlet temperature to about 350°C. Then keep
the regeneration loop compressor K-71301 running to maintain about 300°C in
burning, oxychlorination and calcination beds.
8.2.5. Maintain the pressure in regeneration loop.
8.2.6. When burning and oxychlorination/calcination beds temperature are about
300°C, then:
Stop the caustic make-up.
Stop the caustic soda circulation.
Stop the H2O make-up to caustic circulation.
Stop the washing water injection.
Stop regeneration loop compressor K-71301
Close block valves on LV's 3001 and 3002 (washing drum bottom
outlet).
Keep the regeneration loop under N2 pressure.
Isolate the caustic recycle pumps P-71302, drain and wash them with
BFW.
8.2.7. Cool catalyst to below 50°C, by this time, regenerating section completely
shutdown.
Contents: This instruction outlines the operating conditions and control of the catalyst
regeneration and circulation section. The text includes:
1.1.2. The first combustion step operates with a limited inlet O2 content (0.6 to 0.8%
vol.) controlled through analyzer AIC3001 on first burning bed inlet resetting
analyzer AIC3004 on oxychlorination and calcination gas , which then resets
FIC3007 air flow. This limits the temperature increase. The 2 nd combustion step
operates with an excess of O2 (0.2 % vol. at outlet) to ensure a complete
combustion: the analyzer AIC3004 resets FIC3007 air flow.
The regeneration is designed to burn a given amount of coke per hour.
Trying to exceed this limit results in excessive regeneration temperature and
possible catalyst damage.
During the various steps of the regeneration, the catalyst must not be
overheated (max. temperature in calcination shall not exceed 520°C.).
1.1.3. The operators must then monitor the catalyst regeneration and set the catalyst
circulation with the following guidelines.
A circulation rate (say between 60 - 90% of design rate) will be selected -
based on the trend in coke deposit (higher circulation when increased coke
deposit).
Burning and oxychlorination/calcination gas flows are set to design values.
Temperatures at burning beds inlets are adjusted through the electrical
heaters.
Air injections are adjusted to 0.6 - 0.8% vol. at first burning bed inlet and
0.2% vol. at second burning bed outlet.
Then operators must watch the first burning bed outlet temperature.
If this temperature is too high, the following options are possible:
Decrease the TI at inlet temperature (not below 470°C ).
Decrease catalyst circulation rate.
Note that if high regeneration temperature is due to an increased coke deposit
content, decreasing the catalyst circulation is only a short term solution, because
coke keeps building up, if the conditions which caused the increased coke are still
prevailing. In this case, sooner or later the severity must be lowered
IMPORTANT: Catalyst inlet pipes must always be full of catalyst otherwise the
sealing system between nitrogen section and reaction section would not work. For
that purpose very low level (LALL) in regenerator upper section or in any of the
reactor upper hopper actuates the relevant "sequences" IS3014, or IS3018 or IS
3020 managing closure of the relevant lifts, i.e. stops withdrawal from the respective
reactor - through the closure of the relevant PDV on the secondary lift gas injection.
Example:
The LALL3112 in the first reactor upper hopper actuates sequence IS3018
which closes the secondary gas injection and the relevant PDV3008 to the
first reactor lift pot and thus stops catalyst flow from this reactor.
A high level in the upper surge drum LAHH3106 actuates sequence IS3021
which closes the secondary gas injection and the relevant PDV3011 to the
third reactor lift pot and stop catalyst flow from this reactor to upper surge
drum.
Catalyst circulation will be automatically shut down through any one of the following
interlocks:
IS3019 related to N2 seal gas default to first reactor upper hopper. It closes
ON/OFF valve UV3011 between upper hopper and reduction chamber.
IS3022 related to N2 seal gas default on the last reactor lower hopper. It
closes the ON/OFF valve UV3013 between last reactor lower hopper and lift
pot.
IS3016 related to N2 seal gas default to first lower hopper. It closes ON/OFF
valve UV3005 between first lower hopper and lift pot.
The recommended figure for PDC3008 set point of lift A is between 0.012 to 0.020
MPa.
The PDC set points for the other lift pots are adjusted in order for the catalyst level in
the upper hoppers to stay constant. Operator must keep in mind that too high figures
for these set points may affect adversely the flow of catalyst into the lift pot, and end
up in a complete stop of the catalyst circulation.
Pressure
(barg)
N2 system Reaction
9.0
8.0
loop compressor
recycle compressor
7.0 top
bias 1 bottom
lift pot 1 +0.6 barg
6.0
N2 compressor
RX1
PDIC
4.0
Pressure
(barg)
7.0
recycle compressor
top
lift pot 1
+0.6 barg
RX1
PDIC
5.0
lift pot 5
RX4
washing
drum
4.0
ko drum separator
3.0 bias 2
-0.2 barg
A hardwired interlock logic (i.e. separated from the DCS) performs automatic emergency
shutdown actions upon the occurrence of potentially harmful situations.
In the DCS, four control sequences called UC (multiple variable control) have been
programmed to execute the following tasks:
UC 1 Regeneration loop pressure control.
UC 2 Catalyst transfer.
UC 3 Hydrogen system pressure control.
UC 4 Nitrogen loop pressure control (introduces automatically fresh nitrogen in the
nitrogen lift section, should the latter have been polluted with hydrogen or oxygen).
Also programmed in the DCS are sequences, related to catalyst lift pipes and their
associated lower and upper hoppers.
Upon the occurrence of undesirable event(s) such as (but not limited to) low level in upper
hoppers and high level in upper surge drum, the four relevant secondary lift gas PDV
valves would close.
Sequences result in catalyst circulation shutdown or regeneration stand by. When the
original conditions are restored the different systems affected go back on stream.
Sequences are the result and the way of correcting minor incidents but do not affect,
normally, the running of the unit.
o reduction chamber
o first lower hopper and lift pot
High temperature in the regenerator
Interlocks operate automatically upon the occurrence of the undesirable event(s) but
can also be activated by operators.
Circulation Loop
4.1. Lift Gas Flow
4.1.2. The lift gas flow needs to be adjusted each time the specific gravity of the H 2 lift
gas varies due to a change in the operating conditions.
4.1.3. This adjustment must be made to maintain a constant speed of catalyst in the
lift pipe and to prevent an excessive attrition of the catalyst.
4.1.4. The lift gas flow rate is modified as follows, in order to keep the actual lift gas
velocity constant:
Flow c = Flow r x MW
MW d x Pop Td
op Pd Top
Where: (Flow)c :corrected flow (vol.) for Pop, Top, MWop
(Flow)r :flow (vol.) reading for Pd, Td, MWd
Pop, Top, MWop :operating P, T and MW
Pd, Td, MWd :design P, T and MW for which the flow meter is calibrated
Temperature :must be expressed in R or K
4.1.5. For each change of feed quality and / or severity which can lead to a change of
the H2 rich gas composition, a lift gas flowrate check shall be made, using the
formula above to calculate the actual flow, at conditions, and the calculation
example hereunder to calculate the recommended flow.
4.1.6. When the unit operates at steady conditions a check is made once a week.
Calculation examples
N2 Gas = T = 100 + 250 = 175 C
P(MPa abs) = 0.680 2
28.0 x 0.680 x 273.15
= = 5.11 Kg/m 3
22.414 x 0.1013 (273.15 + 175)
7.67
FF = = 3.39 m/s
5.11
Gas lift velocity = 3.39 + 2.5 = 5.89 m/s
Flow (volume) = 3.5 10-3 x 3600 x 5.89 = 74.2 m3/h (P and T)
Flow (weight) = 74.2 x 5.11 = 379 Kg/h
H2 Gas lift = P (MPa abs) = 0.610
T( C) = 200 + 250 = 225
2
MW = 3.9
3.9 x 0.610 x 273.15
= = 0.58 Kg/m 3
22.414 x 0.1013 (273.15 + 225)
7.67
FF = = 10.07 m/s
0.58
Gas lift velocity = 10.07 + 2.5 = 12.57 m/s
Flow (volume) = 3.5 10-3 x 3600 x 12.57 = 158.8 m3/h (P and T)
Flow (weight) = 158.8 x 0.58 = 92 Kg/h
A simple control can be done. It consists in checking the gas lift FV's and PDV's
opening. For a given catalyst flow a decrease of the lift pipe P is the consequence of
an increase of the actual lift gas flow, if all other conditions are unchanged.
ISSUE DATE: 20/03/06 - 48 -
KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0
The graph below gives the recommended lift gas flow to maintain a catalyst velocity between
2.5 and 3 m/s, at various gas density. This graph is valid for 3" schedule 160 pipes.
Lift gas flowrate to minimise catalyst attrition
(lift pipe 3" sch.160)
500
vg=2.5m/s
vg=3 m/s
400
300
gas flowrate (kg/h)
200
100
0
0.0 1.0 2.0 3.0 4.0 5.0 6.0
Regeneration Loop
4.2. General
4.2.1. The operating conditions of the regeneration loop are linked to the amount of
coke deposited on the catalyst and to the quantity of circulated catalyst.
4.2.2. In order to know the trends of carbon and chlorine contents, AXENS
recommends to analyze on a daily basis the carbon and chlorine on the spent
and on the regenerated catalyst and to plot on a chart the results versus time.
4.2.3. When the operating conditions are steady the coke level of the spent catalyst
shall be preferably maintained between 4 to 6% wt, depending upon the unit
capacity, the required severity and the feed quality. This is obtained through
adjustment of the catalyst circulation rate.
4.2.4. However, when operating at high severity, high flow rate and relatively poor
feedstock (paraffinic feeds), the percent of coke deposit may momentarily
exceed the above value. In this case, operators must remember that the
burning capacity of the unit is limited and that the catalyst circulation must
match the burning capacity.
4.2.5. Then catalyst circulation must not exceed the design capacity of the
circulation. The design coke burning capacity is 32 kg/h and catalyst flowrate
is 410 kg/h. Moreover regeneration temperature must be carefully watched.
4.2.6. It is obvious that, if the severity is such that the actual amount of coke build-
up is, on average, higher than the design coke burning capacity, the severity
must be lowered - or the feed rate reduced.
4.2.8. Also care shall be taken in keeping an O2>0.2 vol. % at the 2nd burning zone
outlet, to be sure that full coke combustion takes place in the second burning
zone. Otherwise residual combustion will occur in the oxychlorination zone
inducing undesired T° and a possible shutdown by TAHH3132 and 3134
trips.
4.2.9. The quantity of air sent to the calcination zone should be higher (or equal)
than the quantity sent to the second burning zone. If necessary, analyzer
AIC3004 on the oxychlorination inlet shall be set higher to increase the air
flow to the oxychlorination (therefore to the 1st burning bed).
4.3. Temperatures
(Refer to DWG. “LoopControl” in KRCIM 71200.06)
Temperatures must be adjusted as follows :
4.3.1. The 1st bed inlet temperature is monitored at 480°C through the burning
heater.
4.3.2. The 2nd bed inlet temperature is adjusted at 480°C with the quench gas
recovered from the regeneration loop compressor.
4.3.3. However, the first burning zone outlet must be controlled between 535°C
to 545°C by action on inlet temperature and on inlet O 2 analyzer. Use
following rule of thumb: 0.1% O2 leads to 10°C temperature rise.
4.3.4. The temperature at the second burning zone outlet (TI3118) must not
exceed 510°C and simultaneously the outlet O2 content must be kept
above 0.2%. If the temperature exceeds 520°C one must:
Either increase regeneration gas flow with a decrease in O2 set point.
or increase slightly 1st bed O2 analyzers set point. It will result in a lower
T across second bed and a higher T across first bed.(This solution
only used if outlet temp of 1st bed is not already high)
Or decrease inlet temperature into second bed(not less than 470°C)
or decrease catalyst circulation to get the same temperature decrease.
Note: If the differential pressure between the 2nd burning bed and the calcination
zone is set too low, some gas may flow back through the catalyst pipes to the
burning zone and the oxychlorination, calcination feed effluent / exchanger efficiency
will be reduced.
4.5. Pressure
The pressure at the regenerator bottom (i.e. calcination gas inlet) is controlled
through PDV’s3002 A and B located on top of the washing drum. This pressure set
point is equal to the first reactor top pressure plus a selected increment (or bias).
The recommended value for the bias is 0.060 MPa.
5. Troubleshooting
5.1. General
Mechanical troubles or failures which, hopefully do not result in immediate
shutdown, must also be considered. The most frequent are covered in this chapter:
Failure of regeneration.
Failure of nitrogen lift system.
Failure of chlorine injection.
Failure of catalyst circulation.
Washing section default.
Difficulties in controlling the regeneration temperatures.
5.2.1. Regenerator
An excessive pressure drop may also develop in the regenerator by the same
process as for the reactor(s).
5.2.1.1. As soon as the pressure drop reaches 0.100 MPa instead of the normal
figure of 0.002 MPa a catalyst unloading of the regenerator is
recommended. Fortunately this operation can be conducted without
shutting down the feed to the reforming unit.
stop catalyst circulation,
isolate the regenerator from the reaction section,
let the regeneration loop cool down : shut down electrical heaters
and continue nitrogen circulation if applicable,
depressurize the regenerator,
unload the catalyst under the lower hopper,
screen the catalyst.
Depending upon the downtime available and the time to run until
the next planned shutdown, will decide to inspect the regenerator
or not, prior to reloading the catalyst.
5.3.2.4. Stop air injection to the 1st and 2nd burning beds.
5.3.2.5. Switch off electrical heaters.
5.3.2.6. Stop caustic circulation pump, caustic injection pump, water to washing
drum.
5.3.2.7. Whenever possible, keep the regeneration section under pressure.
Note that the modifications of the set point of FV3007 on air injection is
automatically placed under the direct control of analyzer AIC3001 at the inlet of
first burning bed.
6. Analysis Control
6.1. Recommended Methods And Frequency
The frequencies given here below are related to routine operation.
Hardnes
******
s
Iron Titration 1/D
Copper Titration 1/D
Silicon
Titration 1/D
Oxide
Sodium Titration 1/D
Boiler Feed Dissolve
****
Water d Titration 1/D
Oxygen
PH Titration 1/D
Oil UV
1/D
Content Method
Phosphat
Titration 1/D
e
Alkalinity Titration 1/D
7. Supplements
1. Control Functions
2. Catalyst Transfer Sequence Description (UC2)
3. Catalyst Circulation Control
4. Hydrogen System Pressure Control (UC 3)
5. Special Loops Description
6. Temperature Control Optimization
7. Appendix
1. Control Functions
The following control functions are necessary for the sequence and must be implemented
in the system.
1.1. Function : ON/OFF VALVE MONITORING
This function is used when one of the On/Off valves involved in the catalyst transfer
from the upper surge drum D-71301 to the regenerator R-71301 (refer to figure 1 in
appendix) is commanded.
The function executes sequentially 3 actions described hereafter.
The sequence waits until the pressure in the lock hopper (PI 3116) becomes nearly
equal to the pressure in the upper surge drum (PI 3136). If after 5 minutes, the
pressures are not equalized, a message is displayed and the sequence continues to
wait.
LOAD phase
1. Check that the conditions are good to start the LOAD :
The valves UV 3001, UV 3002, UV 3003, UV 3004, UV 3006, UV 3008, UV 3009,
and UV 3010 must be closed and there must be a low level (LAL 3109) in the
lock hopper
2. Open valve UV 3008 to depressurize the lock hopper
3. Wait until PI 3116 = PI 3136 +/- 0.005 MPa (adjustable value)
4. Close valve UV 3008
5. Open valve UV 3006 to equalize pressures between upper surge drum and
lock hopper.
6. Wait for enough catalyst in the upper surge drum : LI 3107 > 65 % (adjustable
value).
8. Open the valve UV 3001: the catalyst will fill up into the lock hopper.
9. Wait for high level in the lock hopper (LAH 3108). The lock hopper is now full of
catalyst.
10. Close the catalyst valve UV 3001.
11. Wait 10 seconds (adjustable value). The tight gas valve UV 3002 must not be
actuated in presence of catalyst
12. Close the valves UV 3002 and UV 3006.
UNLOAD phase
1. Wait for the good conditions to start the UNLOAD :
The valves UV 3001, UV 3002, UV 3003, UV 3004, UV 3006, UV 3008, UV 3009
and UV 3010 must be closed
2. Open valve UV 3010 to increase the pressure in the lock hopper by nitrogen
injection.
3. Wait until PI 3116= PI 3106 +/- 0.005 MPa (adjustable value)
4. Close valve UV 3010
5. Open valve UV 3009 to equalize pressures between lock hopper and regenerator.
6. Wait for low level in the regenerator storage : LI 3103 < 30 % (adjustable value).
7. Open valve UV 3004
8. Open UV 3003 : the catalyst is unloaded from lock hopper into the top of the
regenerator.
9. Wait for low level in the lock hopper : LAL 3109. The batch of catalyst has been
transferred in the regenerator.
10. Close the valve UV 3003.
11. Wait 10 seconds (adjustable value). The tight gas valve UV 3004 must not be
actuated in presence of catalyst
12. Close the valves UV 3004 and UV 3009.
Note : The operator must be able to change the adjustable parameters without
stopping the sequence.
2.3. Calculations
After each UNLOAD phase, the following statistics must be calculated and displayed
on the DCS console.
the number of catalyst transfers since the last statistics reset
the quantity of catalyst transferred during the last transfer
the quantity of catalyst transferred averaged over the the 10 last transfers
(adjustable value)
OPERATOR REQUEST NO
=
STOP (HS 3115)
YES
Close UV 3001
Close UV 3002
Close UV 3003
Close UV 3004
Close UV 3006
Close UV 3008
Close UV 3009
Close UV 3010
AUTHORIZE RESTART IN
PHASE LOAD OR UNLOAD
- STOP sequence -
The START, LOAD RESTART and UNLOAD RESTART must be configured on the
DCS console.
1) Normal start
OPERATOR REQUEST NO
=
START
YES
NORMAL SEQUENCE :
PHASE LOAD
NORMAL SEQUENCE :
PHASE UNLOAD
OPERATOR REQUEST NO
=
RESTART IN LOAD PHASE
YES
Close UV 3001
Close UV 3002
Close UV 3003
Close UV 3004
Close UV 3006
Close UV 3008
Close UV 3009
Close UV 3010
OPERATOR REQUEST NO
=
RESTART IN UNLOAD PHASE
YES
Close UV 3001
Close UV 3002
Close UV 3003
Close UV 3004
Close UV 3006
Close UV 3008
Close UV 3009
Close UV 3010
Interlock 1 :
When at least one of the valves UV 3003, UV 3004, UV 3008, UV 3009, or UV 3010
is open, the software interlock forbids to open the valve UV 3001 or the valve UV
3002 or the valve UV 3006.
Interlock 2 :
When at least one of the valve UV 3001, UV 3002, UV 3006, UV 3008 or UV 3010 is
open, the software interlock forbids to open the valve UV 3003 or the valve UV 3004
or the valve UV 3009.
Interlock 3 :
When at least one of the valves UV 3001, UV 3002, UV 3003, UV 3004, UV 3006,
UV 3008 or UV 3009 is open, the software interlock forbids to open the valve UV
3010.
Interlock 4 :
When at least one of the valves UV 3001, UV 3002, UV 3003, UV 3004, UV 3006,
UV 3009 or UV 3010 is open, the software interlock forbids to open the valve UV
3008.
Interlock bypass :
A bypass for each interlock to allow valve operation during start-up or test periods
should be configured. These bypasses must be under restricted access.
If an interlock is bypassed, the commands on the corresponding valves are no more
filtered. In this case, when these valves are commanded, a message must be
displayed (Example: "INTERLOCK ON VALVE UV 002 BYPASSED ").
Operating parameters
lift gas molecular weight : MW (g/mol) entered by operator
lift pot absolute pressure : P (kg/cm²) measured by DCS
lift pot temperature : T (°C) measured by DCS
MW d (g/mol) is the gas molecular weight for which the flowmeter is calibrated
The lift gas corrected mass flowrate FLOWRATEC (kg/h) is calculated :
FLOWRATE c FLOWRATE K
<0
On detection of the shutdown of the hydrogen purification unit (M-71301), the following
actions must be done :
FIC 3017 is set in MANUAL mode with 0% output value.
Control valve HV 3003 on reduction effluent is closed by action on its solenoid
HIC 3003 is set in MANUAL mode at 0% output
a signal is transmitted to ESD to trigger the second lift shutdown logic
a signal is transmitted to the ESD to trigger the third lift shutdown logic
Note : There is also an oxygen content control at the second burning bed inlet : the
setpoint of FIC 3002 is modified by AIC 3002 so that the second burning bed inlet
contains 0.8 % vol. oxygen. This control does not depends on the operation mode.
0%
0% 50% 100%
dead PDIC 3017
band output (%)
foreseen. This dead band is usually 10% (no action between 45% and 55% output).
0%
0% 50% 100%
dead PDIC 3002
band output (%)
5.5. Pressure Difference Control Between Burning Zone And Oxychlorination Zone
To prevent oxychlorination gas with high content in oxygen from flowing upward in
the burning section, a pressure difference (typically 0.002 MPa) must be maintained
between the burning zone and the oxychlorination zone. However this pressure
difference must not be too high to avoid damaging the baffle between the two zones
in the regenerator.
For this purpose, the pressure difference between the burning zone and the
oxychlorination zone is controlled by PDIC 3003 which is acting in split range on the
valves PDV 3003A (burning section outlet) and the valve PDV 3003B
(oxychlorination outlet).
The PDIC 3003 is acting as follows :
In steady state conditions, the pressure difference between the burning zone and the
oxychlorination zone is equal to the setpoint (about 0.002 MPa). The controller PDIC
3003 is at 50 % output value and the control valves are both closed.
If the pressure difference exceeds the setpoint, the oxychlorination outlet valve will
close to increase the pressure in the oxychlorination zone. The pressure difference
will decrease.
In the opposite case, the burning outlet valve will close to increase the pressure in
the burning zone. The pressure difference will increase.
To avoid continuous pressure fluctuations, a dead band in the split range is
foreseen. This dead band is usually 10% (no action between 45% and 55% output).
valve
opening (%)
PDV 3003A PDV 3003B
(burning outlet) (oxychlor. outlet)
100%
0%
0% 50% 100%
dead PDIC 3003
band output (%)
TI 3116 > 495°C + dead band/2 (TIC 3001) setpoint will ramp from 490 to 470°C
TI 3116 < 495°C - dead band/2 (TIC 3001) setpoint will ramp from 470 to 490°C
The dead band (10°C for example) around 495°C is used to avoid permanent
change of the setpoint.
TI 3118 < 523°C - dead band/2 (TIC 3003) setpoint will ramp from 460 to 480°C
TI 3118 > 523°C + dead band/2 (TIC 3003) setpoint will ramp from 480 to 460°C
The dead band (10°C for example) around 550°C is used to avoid permanent
change of the setpoint.
7. Appendix
Figure 1
CATALYST TRANSFER
TO FINES
FILTER
PI 3136
EQUILIBRIUM LINE
LI 3107
2. UPPER
UV 3006
SURGE
4. D-
DRUM LIFT 4
71301
UV 3001
ATM
UV 3008 UV 3002
3002
PI 3116
LAH 3108
EQUILIBRIUM LINE
N2
UV 3010 LAL 3109
3. LOCK
5. D-
HOPP
UV 3003
UV 3009
71302
ER
UV 3004
EQUILIBRIUM LINE
PI 3106
LI 3103
1.1 Regenerat
or
6. R-
71301
TO FINE
FILTERS
FROM
LOCK HOPPER
Figure 2 LSHH 3110
LIFT 1 CONTROL 1st upper
hopper
D-71310
LSLL 3103
Regenerator
R-71301
LIFT 1
Reductor
D-71311
N2
HEADER
D-71304
R-71201
Catalyst
First flow-rate UV 3005 PDSLL 3114
lift stop
adjustmen
PDIC 3006 t LIFT 1 STOP
Causes :
D-71305 LSLL 3103
TI LSHH 3110
Lift 1 gas ZSC 3005
FIC 3010 flow-rate 3153 REGENERATOR SEAL (IS 3016)
N2 PI 3153 (PDSLL 3114 or HS 3114)
LIFT adjustmen CATALYST CIRCULATION STOP (IS 3015)
t (regenerator shutdown or HS 3116)
Second
reactor
R-71202
UV 3011 PDSLL 3122
Reductor
LSLL 3113 D-71311
LIFT 2
First
reactor R-
71201
LIFT 2 STOP
Second Causes :
D-71321 LSLL 3112
lift stop
LSLL 3113
ZSC 3011
PDIC 3008 FIRST REACTOR SEAL (IS 3019)
(PDSLL 3122 or FSLL 3114 or AAHH 3104B or
AAHH 3105B or HS 3118)
D-71331
REDUCTION HEATER SHUTDOWN (IS 3017)
H2 pressure TI 3147 Lift 2 gas H2 PRESSURE CONTROL (UC 3)
FIC 3012
control flow-rate CATALYST CIRCULATION STOP (IS 3015)
(regenerator shutdown or HS 3116)
PI 3124 adjustment
H2 LIFT
H2 H2
NETWORK NETWORK
LIC 3117
D-71312 D-71313
LSLL 3119
Third
Second
reactor
reactor
R-71203
R-71202
LIFT 2 LIFT 3
Figure 4
LIFT 3 CONTROL
D-71322
Third
lift stop
PDIC 3009
D-71332
TI 3149 Lift 3 gas
LIFT 3 STOP
flow-rate Causes :
H2 pressure adjustment LSLL 3119
control FIC 3013 PI 3129 H2 PRESSURE CONTROL
CATALYST CIRCULATION STOP (IS 3015)
(regenerator shutdown or HS 3116)
H2 LIFT
LSHH 3106
LIC 3120
LSLL 3122
9. D-
8. D-
713
713
LIFT 4 LIFT 3 13
01
7. T
PDSLL 3137
H
IR
D N2
HEADER
R UV 3014
E FSLL 3117
D-71323
A
C
T
UV
O 3013
LIFT 4 STOP Fourth lift PDIC 3011
Causes : stop R
LSLL 3122
LSHH 3106
R-
D-71333 TI 3153 Lift 4 gas
ZSC 3013 71 flow-rate
THIRD REACTOR SEAL (IS 3022) FIC 3015 20 adjustment
(PDSLL 3137 or FSLL 3117 or ASHH 3104B PI 3153
or ASHH 3105B or HS 3114) 3
CATALYST CIRCULATION STOP (IS 3015) N2 LIFT
(regenerator shutdown or HS 3116)
Figure 6
LIFT GAS RETURN LIFT GAS RETURN
1 1
LAH 3108 AH AH
3 3 LIC 3117 LIC 3120
LAL
LAL 031
3109 LALL 3113
0 1 LALL 3119 LALL 3122
9.2 D
1 LIFT 4 0
-
13. D 12. D- 11. D-
7
- 71 713
LI 3103 1
7 13
LSLL 3104 3
31
1 2
1
3
1
0
16. R-2
10. R- 15. R 14. R- FIC 3016
PDIC 3007 713
712 - 712
01
01 7 03 UV 3014 15.1.1
16.1.2UVN3007
2 D-71304
LIFT 1
D-71322
LIFT
D-71321
1 16.1.1 L 2 3 D-71323
I 0
UV 3005 F 2 UV 3013
T
PDIC 3006 D-71305 PDIC 3008 D-71331 D-71332 D-71333
PDIC 3009 PDIC 3011
2
FIC 3012 FIC 3013 FIC 3015
FIC 3010
16.1.3 N
16.1.4 H
ISSUE DATE: 20/03/06 - 82 -
2
2
L
L
KRC CATALYST REGENERTION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0
Figure 7
OXYGEN CONTENT CONTROL
REGENERATOR
FIRST BED INLET
AIC 3001
QUENCH GAS
HS 3124
SELECTOR
FIC 3007
Normal
AIR mode OXYCHLORINATION OUTLET
UV 3016
CALCINATION INLET
Contents: This instruction outlines the special equipment technology used in catalyst
regeneration section. The text includes:
1.1. Objective
To boost the reduction hydrogen purity
1.2. Technology
Membrane separation technology realizes gas separation by taking advantage of
gas molecules passing through membrane at different speeds. Gases permeating
faster concentrate richly on permeation side while gases permeating slower on feed
side. Membrane separation is mainly characterized by low energy consumption,
simple equipment, easy operation, few moving parts, and high operating reliability.
The operations of hollow fiber membrane separator can be generalized into three
aspects, i.e. startup procedure, shutdown procedure, and normal operational
requirements.
The startup procedure consists of feed gas purifying, feed gas heating and pre-
emptying, and changeover from pre-emptying to membrane separator. Pre-emptying
during startup is mainly to inspect the oil content in feed gas and temperature
conforming to related requirements after being treated with purification and heating.
It is required that the oil content in feed gas after purifying should be less than
0.01mg/m3 with the temperature of feed gas reaching 45 °C after being heated.
Qualified feed gas must be then changed over slowly from emptying to membrane
separator under the condition of continuous purifying and heating. The whole
equipment will go into normal operation after feed gas being emptied is changed
over to membrane separator. In the circumstances that no fault occurs to auto
control instruments, the operation is simple with the process and operation
parameters able to be adjusted from time to time on different points.
No matter what shutdown it will be, i.e. normal shutdown, emergency shutdown or
fault shutdown, a shutdown instruction has to be input through the safety interlock
control system to realize shutdown after such instruction is received. Meanwhile, the
equipment will go into enclosed protection state automatically. Except HV3451 that
is kept open, all regulating valves in other positions will be closed. After shutdown,
the feed gas in the equipment will be in static pressure state, however, at this point
the pressure of feed gas is still higher than that of permeating gas, so the
permeation process is still going on, which is demonstrated by the pressure of feed
gas in separator decreasing gradually and the pressure of permeating gas
increasing gradually.
The safety interlock system of the equipment can have an auto shutdown control
over super high and low limits of cyclone separator liquid level, feed gas over-
temperature, etc.
Operational requirements will be described below for each process in the equipment:
1.5.1.3.1. Feed gas heating.The feed gas exiting from cyclone separator and
high efficient filter will be heated to 45̊C by heater (E-71344A) and
then is sent into membrane separator for separation. In addition to
mentioned reason for heating, increasing temperature is also an
important factor to improve the permeable performance of a
membrane separator. Permeability of a membrane increases as
temperature rises, resulting in a higher hydrogen recovery rate.
However, too high temperature will have an unfavorable influence on
the strength and lifespan of a membrane. The temperature is under
control of membrane regulating valve TV-3413A.
1.5.1.3.2. Instrument functions and parameters:
TIC3413A- Heating temperature indication control, 45 ̊C;
TIA3415A- Heating temperature indication, alarm and
interlock. Upper heating temperature value for alarm 55 ̊C,
interlock value 60 ̊C.
TG3463- Temperature as indicated on field after heating, 45
̊C.
1.5.1.3.3. Pre-emptying. The feed gas being purified, heated should not come
into membrane separators immediately, which must experience pre-
emptying treatment through valve HV-3455. The purpose of pre-
emptying is to inspect that feed gas purification and heating
temperature conform to requirements of indicators. A71343 is a
sample-analyzing valve. Valve FZ06 will be opened during startup.
1.5.1.4.1. Feed gas input. The feed gas being purified and heated to related
requirements is gradually changed over from pre-emptying to
membrane separators. Feed gas changeover is an important part of
operations that should be grasped skillfully.
1.5.1.4.2. Before changeover, keep the two groups of membrane inlet master
valves FZ05 and bypass valve FL04 in close state, close pneumatic
ball valve HV3457 in the main permeating gas line, close the tail gas
regulating valve FV3442 and FZ07, FZ08, open permeating gas and
tail gas emptying valves FZ09, FZ13, with the regulating valve
HV3456 for permeating gas emptying being 30% opened, the inlet
valves for membrane separators, open the outlet valves for tail gas,
permeating gas.
1.5.1.4.3. Check that the states of the mentioned valves are correct. Open
slowly inlet sub-line valve FL04 to feed air to membrane separators,
at this point permeating gas and tail gas are emptied.
1.5.1.4.4. In 3-5 minutes, close emptying valves FZ13, FZ09, HV3456. When
the pressure in membrane separator rises to 2.08MPa, first open
pneumatic ball valve HV3457, fully open regulating valve HV3454
and then open sequentially valves FZ08, FZ05, FZ07 and close FL04
again and set tail gas regulating valve FV3442 to auto. Until now, the
process for feed gas to change over from pre-emptying to membrane
separators is completed.
1.5.1.4.5. Open valve FZ10, set regulating valve TV3414A to auto and control
the permeating gas heating temperature. In this operating process,
the above procedure must be strictly followed to prevent counter-
pressure buildup in membrane separators, which refers to
permeating gas pressure being higher than that of membrane inlet.
1.5.1.4.6. Instrument functions and parameters:
PI3403- Indicate membrane penetrating feed gas pressure,
(0.695 MPa)
FI3441- Indicate membrane penetrating feed gas flow,
(2762Nm3/h)
HIC3454- Regulating valve, which is fully opened during
normal operation and closes automatically during shutdown.
TIC3414A- Permeating gas temperature controller, (90°C)
1.5.1.4.7. Discharge of permeating gas. The permeating gas separated from
six membrane separators concentrates in the header with a pressure
0.695MPa for going to subsequent procss. During normal operation,
pneumatic ball valve HV3457 will open and close during shutdown,
playing a role of enclosed protection to membrane separators.
Regulating valve HV3456 is used for replacement and emptying
during startup and for permeating gas emptying during shutdown,
which is closed during normal operation. Valves FH1, FH3 are check
valves to prevent counter-pressure. A71346 is sample-analyzing
valve.
1.5.1.4.8. Instrument functions and parameters:
PI3404- Indicate permeating gas pressure, (0.695MPa)
FIC3442- Permeating gas flow controller, (2762Nm3/h)
1.5.1.4.9. Tail gas discharge. 85% H2 in feed gas will be separated in six
membrane separators with the remaining tail gas to be discharged
after the flow being stabilized by membrane regulating valve. The tail
gas regulating valve shall be mainly used for flow control and
1.5.2.2.1. In case of receiving any request for other posts or any failure to the
equipment requiring emergency shutdown, operate to normal
shutdown procedure.
1.5.2.2.2. When any operating parameter of the equipment exceeds that as
required, the equipment will shut down under automatic control of the
safety interlock system and enter into enclosed protection state. At
this point, operators should deal with it by following step 1.5.2.1.3 to
1.5.2.1.7 for normal shutdown.
1.6.1. Operations must be kept slowly for increasing and decreasing pressure during
the process of startup, shutdown.
1.6.2. The difference in pressure between feed gas and permeating gas must be put
under strict control below 2.5MPa. Excessive pressure difference can result in
damage to separator.
1.6.3. No counter-pressure shall be allowed regardless of which state a membrane
separator is it, startup, shutdown, or operation, i.e. the pressure of PI3404
should never be greater than that of PI3403.
1.6.4. Keep the temperature under strictly control at 45 °C during temperature rise for
heating feed gas.
1.6.5. Forward and back difference in pressure must be within the permissible range
for filter. When the pressure difference is too high, it is necessary to change
over to another filter group to ensure efficient filter working normally.
1.6.6. Maintain frequent inspections, maintenance to control instruments to keep them
under normal working state.
TI3413 45 °c
TI3414 90 °c
TI3415 45 55 60 °c
TI3416 <30 °c
LIA3421 <30 30 50 %
PdIA3431 <0.15 0.18 . MPa(g)
FI3441 2652-2762 Nm3/h
FI3442 2072-2158 Nm3/h
Field indications:
Instrument number Operation value unit
PG3481 2.08 MPa
PG3482 2.08 MPa
PG3483 2.05 MPa
PG3484 2.0 MPa
PG3485 2.0 MPa
PG3486 1.8 MPa
PG3487 1.8 MPa
PG3488 0.695 MPa
PG3489 0.695 MPa
PG3490 >0.8 MPa
PG3491 1.0 MPa
PG3492 >0.4 MPa
PG3493 0.3 MPa
TG3461 40 °C
TG3462 35 °C
TG3463 45 °C
TG3464 45 °C
TG3465 90 °C
TG3466 180 °C
TG3467 <30 °C
LG3422 <30 %
PdG0l-06 Green zone
2.5. Efficiency
H2O content at outlet is less than 50ppm(v)