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Resorcinol
Resorcinol
Resorcinol
RESORCINOL
SUMMER INTERNSHIP AT ATUL; LTD.
From GTU,
TO S.S. AGRAWAL INSTITUTE OF ENGINEERING AND
TECHNOLOGY.
B.E. CHEMICAL ENGINEERING
IN
7th SEM, 4th YEAR
BY
AKASH J. GANGANI
Theory of any subject is important but if learned without practical exposure, the knowledge remains incomplete.
In order to be a good engineer one needs to remain updated with latest developments in his field as well as their
practical applications. Hence this training provided an excellent opportunity for my overall development as an
engineer. This report consists of a detail description of the various unit operations undertaken by us, for study
during training at ATUL LIMITED. The report covers the training period from 27th June 2022 to 16th July
2022 in RESORCINOL PLANT OF BULK AND INTERMEDIATE.
GUJARAT TECHNOLOGYCAL
UNIVERSITY, CHANDKHEDA
RESORCINOL
A SUMMER INTERNSHIP REPORT
BACHELOR OF ENGINEERING
In
CHEMICAL ENGINEERING
7th semester of 4th year, 2022
Projected By:
AKASH J. GANGANI
DECLARATION
I hereby declare that the Internship report submitted along with the Internship
entitled Industrial Training at ATUL LTD. submitted in partial fulfillment
for the degree of Bachelor of Engineering chemical department to Gujarat
Technological University, Ahmadabad, is a confide record of original project
work carried out by me at ATUL LTD. under the supervision of Mr.
Chinmaya Pradhan & theirs staff.
AKASH GANGANI
(201230105523)
Table of Contents
DECLARATION................................................................................................................. 3
1. ABSTRACT .................................................................................................................. 8
2. ACKNOWLEDGEMENT ........................................................................................... 9
3. INTRODUCTION OF INDUSTRY .......................................................................... 10
4. INTRODUCTION OF RESORCINOL ..................................................................... 11
4.1 PROPERTIES OF RESOCINOL......................................................................... 12
4.2 BY PRODUCTS OF RESORCINOL WHILE MANUFACTURING ............... 12
4.3 PROPERTIES OF RAW MATERIAL ................................................................ 13
4.4 APPLICATION OF RESO ................................................................................. 14
4.5 LIST OF UNIT PROCESS & OPERATION IN MANUFACTURE OF
RESORCINOL ............................................................................................................... 14
5. PLANT PROCESS ..................................................................................................... 15
5.1 REACTIONS IN PROCESS: ............................................................................. 16
5.2 BLOCK DIAGRAM OF RESORCINOL PROCESS .......................................... 17
5.3 PLANT DESCRIPTION WITH NEAT FLOW DIAGRAM ............................. 19
5.4 PROCESS DESCRIPTION ................................................................................. 19
BDSA (Benzene Di-Sulphonic Acid) Section: .............................................................. 19
PSR (Plough Stirred Reactor) Section: ......................................................................... 22
SRU (Solvent Recovery Unit) Section:......................................................................... 25
5.5 MAJOR EQUIPMENTS ..................................................................................... 27
VACCUM BELT FILTER: .......................................................................................... 27
TRIPLE EFFECT EVAPORATOR: ............................................................................. 28
DECANTER CENTRIFUGE: ...................................................................................... 28
PEELER CENTRIFUGE: ............................................................................................ 30
1. ABSTRACT
Theory of any subject is important but if learned without practical exposure, the
knowledge remains incomplete. In order to be a good engineer one needs to
remain updated with latest developments in his field as well as their practical
applications. Hence this training provided an excellent opportunity for my
overall development as an engineer. This report consists of a detail description
of the various unit operations undertaken by us, for study during training at
ATUL LIMITED. The report covers the training period from 27th June 2022 to
16th July 2022 in RESORCINOL PLANT OF BULK AND INTERMEDIATE.
2. ACKNOWLEDGEMENT
This training report is prepared not only by a solo effort. A great deal of effort
and time has been involved in preparing this training report. During the course
of our project work I have been guide by many, without whom this project may
not have seen the light of the day. It is my sincere desire to express heart full
thanks for their guidance and support.
I would also like to thank to all the operators and staff members for their
valuable information about the plant and finally thankful to the entire ATUL
LIMITED family for providing us such a warm atmosphere to make our training
period delightful and memorable.
I would also like to thank Mr. Chinmaya Pradhan (Manager) and their
Staff’s for kind advice and guidance during our training period. Theory of any
subject is important but if learned without practical.
3. INTRODUCTION OF INDUSTRY
ATUL LTD is a member of Lalbhai Group, one of the oldest business houses of India, with
interests mainly in textiles and chemical. The group is strongly committed to serve the
society in the fields of education, health as well as culture. Incorporated in 1947, ATUL LTD
(formerly atul products ltd) was founded by Kasturbhai Lalbhai with a dream to make India
self reliant in chemicals, generate employment on a large scale and create wealth for the
society. For the translating his dreams into reality , Kasturbhai Lalbhai brought his
confident, Ballubhai Muzumdar, an economist and his son, Siddharth Kasturbhai Lalbhai, a
chemical engineer to lead ATUL LTD and a large chemical conglomerate .
ATUL LTD. became the first private sector company of India to be inaugurated by
Jawaharlal Nehru, the first PM of the Country; the company thus commenced its business
with just a few dye stuffs, the know-how of which was brought from foreign companies.
Over the years, Atul ltd joined hands with American Cyanamid crop (1952), Empirical
chemical industries plc (1955) and Ciba-Geigy (1960) to from respectively 3 joint venture
companies, namely Cyanamid India Ltd., Attic Industries Ltd. and Cibatul Ltd. respectively.
Atul’s registered office is in Ahmadabad whereas its corporate headquarters are located in
Atul, Gujarat. The company is listed on the NSE in India and has over 35,000 shareholders.
Atul also has officers in the USA, UK, GERMANY, CHINA & VIETNAM that services its
international customers.
4. INTRODUCTION OF RESORCINOL
Resorcinol is the essential component of an adhesive system used in the type
manufacturing process and other fiber-reinforced rubber mechanical goods and also
used as UV stabilizers.
Resorcinol is Dihydroxy benzene. It is the 1, 3-Isomer of benzenediol with the
formula C6H4 (OH) 2.
Benzene-1, 3-diol is the name recommended by the International Union of Pure and
Applied Chemistry (IUPAC) in its 1993, recommendation for the Nomenclature of
Organic Chemistry.
Resorcinol is part of molecule of cat chain, which is natural compound present in tea
and it is having a resorcinol skeleton structure in it. Resorcinol crystallizes from
benzene as color less needles that are readily soluble in water, alcohol and ether, but
insoluble in chloroformed carbon disulphide.
With large amount of application and growing demand of resorcinol in India as well
as international market, there is tough competition among resorcinol producing in
industry.
Some of them are as follows:
INDIA
ATUL LTD, Valsad.
Deepak Nitrate, Maharashtra.
Garuda Chemical, Mumbai.
Zacol India Ltd, Delhi.
Other countries producing resorcinol
China
Switzerland
Mexico
Japan
U.K
Australia
Russia
World’s Top Three Companies Manufacturing Resorcinol is:
Sumitomo Chemicals (Japan)
INDSPEC Chemical Corporation (United states)
Mitsui Chemical (Japan)
Japan’s SUMITOMO CHEMICALS is now the world’s top-ranking resorcinol
producer with an annual capacity of 20K tons per month.
4.1 PROPERTIES OF RESOCINOL
Acid
Sulphonation Filtration
Mono Sulphonation Drying
Di-Sulphonation Decantation
Neutralization Centrifugation
Sodiation Extraction
Fusion Distillation
Quenching Flaking
Acidification
5. PLANT PROCESS
The plant basically divided into three sites, one site consists of the area where the main
reactions and some other operations take place. These reactions include sulfonation of
benzene into the monomass and the dimass, neutralization of the dimass using the limestone
slurry, filtration in VBF, PRN and sparkler filter, concentration in TEE then followed by the
fusion reaction and acidification.
The sulfonation mainly consist of the reaction of benzene with 65% oleum to produce the
monomass for this purpose, there are three reactors which are installed on the second floor of
the plant. The monomass formed is again reacted with excess 65% oleum to produce the
dimass for this purpose, there are three reactors installed on the second floor. This form the
sulfonation section on the second floor of the plant.
For the neutralization of the dimass there are three neutralizing reactors installed on the first
floor. These also include the two sodiation tanks which are used for the removal of the
remaining small amount of the gypsum. These are followed by the two PRN filters. These
formed the neutralizing section of the plant.
For the filtration section which serves for the removal of the gypsum, there are two vacuum
belt filters which are installed on the second floor. The slurry from the neutralizing tank is
used on the VBF then after treatment this slurry goes to the sodiation tank then followed by
the PRN filters. The slurry from the PRN goes to the dil. BDSA storage tank then it goes for
concentration. Concentration section mainly consists of the triple effect evaporator (TEE).
These concentration BDSA then dried to produce dry BDSA powder in the drying section.
This section is in the third site of the plant and it is situated at the top floor of the building.
Fusion section consist several reactors in this section where dry BDSA powder is fused with
the caustic.
This is followed by the quenching which takes place in the quenching section which consists
of the four reactors on the first floor in the plant in the first part. Quench mass goes to the
decanter section which consist of the three decanters situated on the first floor of the reactor.
Reslurry is formed from the solid mass and is fed to the peeler centrifuge on the first floor.
The peeler centrifuge removes the sodium sulfite and the mother liquor obtained is used for
quenching. There are three acidification tank installed on the first floor which are used for the
acidification of the mass obtained as the liquid from the decanter.
Second site of the plant mainly consists of the separation which mainly includes the solvent
extraction, solvent recovery and the distillation operation. It also includes the flacker unit and
the packing unit. Third site includes the PSR unit where the fusion is carried out and at the
top floor there is a drying section.
5.1 REACTIONS IN PROCESS:
5.2 BLOCK DIAGRAM OF RESORCINOL PROCESS
5.3 PLANT DESCRIPTION WITH NEAT FLOW DIAGRAM
Disulphonation
Premix of oleum and glauber salt is prepared in R1-D and maintains it for 3 hrs.
Firstly chill the disulphonation reactor and then add premix solution into R-2A/B/C
as per above after checking the bottom valve.
Transfer the mono mass to premix in R-2A/B/C at 55- 60°Ctemperature.
BDSA is made after the reaction of benzene mono sulphonic acid and premix.
Dropping takes place about 7 hrs. And maintain it for 9 hrs.
Neutralization
Lime slurry (prepared by mixing water, lime and glauber salt) is added from MXT-
2 in R-A/B/C till specific height is attained.
Then dropping of disulphonation mass from reactor R-2A/B/C to R-3A/B/C is
made.
Avoid acidic nature of mixture, if pH decreases (i.e. it becomes acidic) add lime.
Care must be taken in reactor R-3A/B/C for foaming, temperature and pH.
Heat the mixture and maintain the temperature to 70-75oC.
Check pH periodically during addition of disulphonation mass and if pH is below
then give more stirring for 1 hour.
Make final volume by adding raw hot water.
Transfer neutralized mass from R-3A/B/C to R-3D.
Sodiation
Dilute BDSA from HT-9A is transferred to R3E.
Heat to 60°C by direct steam.
After attaining required height 300-350 cm 10 bags of soda is added and then
height of 400-450cm is attained to bring pH 8.5 to 9.
Stir for one hour and then check pH.
Stop stirring and settle the lime stone formed for 3 hours.
Sprinkle some soda ash in sample, if it dissolves completely, it is said that
sodiation is completed.
Pre Acidification
Check R5 vessel empty and bottom valve closed then receive fusion slurry from
R4 vessel.
In quenching section temperature of fusion slurry is brought down very rapidly
from 325°C to 50 - 55°C.
Firstly the fusion mass around 10kl of pH 13 to 14 is brought in R5 and is pre
acidified by adding 40% H2S04 and this brings the pH around 11 – 12 .
Quenching section requires constant stirring.
After pre acidification mass is charged to decanter.
Decanter and Peeler centrifuge
Decanter section contains two major processes of decanter separation and
centrifuging.
The acidified mass from the acidifying section is brought to the decanter for
separating the very important by product, sodium sulphite.
Then the slurry containing sodium sulphite is brought to the peeler centrifuge.
The slurry mass containing the sodium sulphite by product is brought to the
peeler.
Centrifuge for getting sodium sulphite in dry form.
Some mother liquor is extracted from the slurry and used in the PSR section.
The sodium sulphite is dried and collected and packed in 50 Kg bags.
Post Acidification
ML from R7B is fed to R7 - C/D and circulated in order to cool in plate type heat
exchanger than again 40% H2So4 is added and pH here after post acidification is
6.5 – 6.8.
After post acidification it is transfer to ST – 22 for extraction.
SRU (Solvent Recovery Unit) Section:
Extraction
The mother liquor is brought to the overhead storage tank.
In extraction equipment the solvent used is butyl acetate which is stored in the
underground storage tanks.
Packed tower type extractor is used so that the resorcinol is obtained containing
butyl acetate is transferred to the solvent recovery unit.
The raffinate mass contains only sludge and other mud particles which is
transferred to the sludge disposal section.
SOLVENT RECOVERY SECTION
In the solvent recovery unit the solvent is separated from the extract mass from the
extractor.
The extract mass is poured from the short column where it is heated up to a
temperature of 180°C.
Then in the re-boiler it is further heated to 323°C so that the solvent is recovered
from the extract.
This solvent is transferred to the solvent storage underground.
The other mass containing the main product resorcinol is settled down and
transferred to the distillation section.
DISTILLATION
In the distillation section the product is separated along with some by products like
phenol and solvent butyl acetate.
The distillation used here is vacuum distillation.
Firstly, by opening the first ejector vacuum pump to 450 mmHg is obtained.
Then on opening the second ejector vacuum pump 680 mmHg is obtained after
which on opening the third ejector vacuum pump up to 745 mmHg is obtained and
on starting the fourth one vacuum pump up to 758 mmHg is obtained.
Then on starting the process firstly at temperature range such that 120-180°C at top
and 195°C at bottom and vacuum of 650 mmHg solvent butyl acetate are obtained.
After that when at 180-230°C top temperature and 185°C bottom temperature and
vacuum 720 mmHg we get phenol cut which is obtained as a byproduct.
After that at 165-195°C and vacuum up to 758 mmHg we get our main product
resorcinol.
Also resorcinol is obtained in four parts as per their quality as component cut.
The left over is collected in the sludge disposal section.
The obtained resorcinol is dried and flaked into flaker.
The above flow diagram shows the TEE used for the concentration of the dilute BDSA.
The slurry after the removal of the gypsum goes to the dilute BDSA storage tank
installed on the ground floor. The dilute BDSA from the storage tank in then to the
supply tank of the TEE at the rate of the 7m3/hr. In the above steam applied at the
pressure of 0.1 Kg/cm2 in the first evaporator and the condensate is removed. Then we
have the separator which separates the vapors from the liquor then the vapor are fed to
the second effect and the liquor is then recycled. The separator is also under vacuum so
that the vapor gets separated from the liquor. The fed is to the second evaporator i.e. it
is operated in the forward feed and conc. BDSA is obtained from the first evaporator.
The outlet of the second evaporator acts as the fed for the first effect. The advantage of
this type of feed system is that the last concentration will takes place at the maximum
steam pressure. The vapor from the last effect is fed t the barometric condenser to
which vacuum of 600 mm of Hg is applied. In order to maintain the vacuum we need to
maintain the level of water inside the barometric condenser and if the level drops then
will be no maintained. The vapors are condensed with the help of the water from the
cooling tower and then this condensed vapor and the water flows the barometric leg
and then goes to the hot well. The water from the hot well is then fed to the cooling
tower.
DECANTER CENTRIFUGE:
Decanter centrifuges are used to extract solid materials from liquids when they are
mixed together in slurry. Decanter centrifuges are used in many industrial applications
such as:
Chemical slurry
Decanter centrifuge design consists of a solid container, called a bowl, which rotates at
a high speed. Inside the bowl tube, a screen conveyor rotates in the same direction, but
at a slightly different speed. A differential gear is typically used to adjust speed.
Decanter centrifuges are powered by a motor and gearbox combination. The gear box
provided the correct speed and torque to drive the centrifuge. Since this is a mechanical
type of centrifugation, it is subject to frequent preventive maintenance and Mechanical
failures. An AC drive can provide the required torque with greater efficiency and
reliability.
Use at site:
In the process decanter centrifuge area used for the removal of the byproduct sodium
sulphite produced during the fusion step. The quenched mass after the fusion step. The
quenched mass after the fusion step is fed to the decanter at the fed points as shown in
above figure. The separated solids are collected in the tank provided at the bottom and
this solid are again mixed with the water and the slurry is formed which is fed to the
peeler centrifuge. The separated liquid is collected in the tank provided
At the bottom of the decanter and this separated liquid then goes for the acidification
step. Feed rate = 1.5 m3/hr
PEELER CENTRIFUGE:
Peeler centrifuges are successfully used in food stuff, pharmaceutical, plastic, organic
& inorganic chemicals industry for separating solids from solid liquid slurry with 5% to 50%
solids contents and partial size ranging from 2 microns to 10 mm. Products which are
difficult to filter or decent can be easily separated using peeler centrifuge. The unique feature
of peeler centrifuge is the constant basket speed i.e. all operations like feeding, drying
discharging etc. are carried out at full basket speed. The sequence of operations can be
controlled by electro –hydraulic control panel / Pl controller. Typical process cycle
Feeding:
The suspension is fed from the storage tank to the basket rotating at full operational
speed.
Under the influence of the centrifugal force the liquid is drained from the solids,
through filter elements. The solids are collected as ‘cake’ in the basket.
Washing:
If required, in order to remove the traces of mother liquor washing facility can be
provided to the thoroughly was the solids during separation.
Re-drying:
After giving wash or other treatment solids are further allowed to dry.
Discharging:
Solids are “peeled” off by means of full basket width scrapper and is discharged
through cute in front cover of the machine or conveyed by discharge screw.
Use at site:
The reslurry of the solids obtained from the decanter from the decanter is fed to the
peeler centrifuge then the solid obtained collected at the bottom and the mother liquor
obtained is used for quenching of the1 fusion mass. Basically peeler centrifuge are used
so that the dry sodium sulphite is obtained as the solids obtained from the decanter is
wet hence there is need for the user of the peelers.