IN PLANT – TRAINING REPORT

ON

JUBILANT LIFE SCIENCES, NIRA

Submitted To

Chemical department

PADMABHUSHAN VASANTARAODADA PATIL

INSTITUTE OF TECHNOLOGY,
Budhgaon, Tal –Miraj, Dist – Sangli.

As a partial fulfillment on

Degree in Chemical Engineering.

Submitted by

SATHE GANESH BAPURAO

Roll No. 35

OF

Year 2015 – 2016

 Padmabhooshan Vasantraodada Patil

Institute of Technology,

Budhgaon (Sangli)

Certificate

This is certified that Mr.SATHE GANESH BAPURAO

Roll No.35.of B.E. Class has completed satisfactorily a Vocational

Training during the year2015-2016.

Date: 30 /09/2015

Prof. N.V.GHASGHASE Prof. U. S. Patil. Dr. S.V. Joshi.

(Guide) (H.O.D). (Principal)

 INDEX

1. INTRODUCTION
2. CHEMICALS & THEIR PROPERTIES
3. PRODUCTION DISCRIPTION
4. EQUIPMENT DISCRIPTION
5. UTILITIES
6. OPERATIONS USED
7. EQUIPMENTS USED
8. INSTRUMENTS
9. PLANT LAYOUT
10. PLANT START UP
11. CONCLUSION
 ACKNOWLEDGEMENT

I wish to acknowledge my grateful thanks to Mr. Rajesh Doshi

(Vice President), Mr. Ramesh Waza (General Manager) and Mr. Gokhale
(H.R) who has very kindly encouraged me and extended their valuable guidance
to complete this In Plant Training.

I would like to say special thanks to Mr. Vijay Jadhav (Dy.

Manager) and Mr. Mahesh Pawar (Sr. Engg.) for his valuable and dedicated
co-operation to my Training and who kindly advised me and extended all his
help and guidance.

Last but not the least I would like to express my heartiest thanks to
all Plant HOD’s, Operators, Workers and staff members for their valuable and
detail explanation of all the Processes and Operations which improved my
knowledge towards all unit operations and unit processes.
 INTRODUCTION

Founded in 1978, Jubilant Life sciences is one of the largest custom

research and manufacturing (CRAMS) companies & a leading player in Active
Pharmaceutical Ingredients (APIs) in India and a leading formulation
development & supply of finished dosage form player in Europe.

The Company delivers products and services to the global life sciences
industry by leveraging its R&D expertise, knowledge-driven operations and
global scale manufacturing capacities. The company operates in three segments:
Performance Chemicals, Industrial Chemicals, and Life Sciences.

In the area of Industrial Chemicals and Performance Chemicals,

Jubilant Organosys develops, manufactures and sells a wide range of complex
value-added organic chemical intermediates used in pharmaceuticals,
agrochemicals, vitamins, food and feed, dyes, pigments, adhesives and
fragrances, as well as polymers. The Performance Chemicals Division is mainly
engaged in the development and production of Biocides and Oleochemicals.

Globally, Jubilant Organosys is a leading manufacturer in defined

product segments, including certain APIs (e.g. Carbamazepine and Citalopram),
Pyridine based Advance Intermediates and Fine Chemicals, Solid Polyvinyl
Acetate, Vinyl Pyridine Latex and Organic Intermediates (e.g., Ethyl Acetate
and Acetic Anhydride).

Jubilant Organosys has global presence with four manufacturing locations

around the country:

 Gajraula (100 kms from Delhi)

 Samlaya (25 kms from Baroda)
 Nira (75 kms from Pune)
 Nanjangud (25 kms from Mysore)

Recently, it has acquired a formulation and regulatory services company

– Pharmaceutical Services Incorporated (PSI) at Gent, Belgium. Jubilant

Organosys also has representative sales offices in USA and China.

Nira Plant of Jubilant Organosys Ltd is situated 70 km from Pune on the

bank of Nira River. Major Products are Ethyl Acetate, Acetic Acid. Molasses
which is suppose to be considered as waste is converted into wealth. Here they
have implemented efficient effluent treatment which makes the process
environmental friendly. Also they provide liquid fertilizer to near by farmers
free of cost and there by contributing to local development.

ACETIC ANHYRIDE PLANT

INTRODUCTION
Manufacture of acetic anhydride from acetic acid is a two step process:

1. Dehydration of acetic acid/thermal catalytic cracking (pyrolysis) of acetic

acid to ketene & water in presence of Tri Ethyl Phosphate(TEP) catalyst at
about 730-7500c temperature & 150mmHg abs. Pressure.

CH3-COOH → →→ CH2=C=O + H2O 147KJ/mol

ACETIC ACID KETENE

The reaction is endothermic & reversible.

Ammonia is added to the reaction mixture as an inhibitor in order to avoid
reversible reaction (which reacts with TEP catalyst to form ammonium
phosphate).

2. Reactive absorption of ketene in acetic acid to form acetic anhydride

O O
// //
CH2=C=O + CH3-COOH → →→ CH3-C-O-C-CH3 -63KJ/mol
Ketene Acetic Acid Acetic Anhydride

The reaction is exothermic.

PLANT CAPACITY-
Nira Plant 1 --- 50MT/day (existing)
Plant2 --- 125MT/day (existing)

Acetic anhydride has been notified as a ”controlled substance” under “The

Narcotic Drugs & Psychotropic Substances Act, 1985” & therefore falls under
the control of the “ Narcotics Control Bureau” (NCB), controlled by the
Ministry of Finance, Government of India. The object of this Act is tom prevent
the diversion of this “precursor chemical” for any illicit or unlawful purpose.

CHEMICALS & THEIR PROPERTIES

PHYSICAL PROPERTIES
Fl.Pt
0
CHEMICA FORMULA M FOR BP, Sp.g VD LEL/HE ,
0
L W M C r. Kg/m L c
 3
NAME

Acetic (CH3CO)2O 102 L 140 1.08 3.52 2.7/10.3 49

anhydride 2

Acetic acid CH3COOH 60 L 118 1.04 2.07 5.4/16 44

Tri ethyl (C2H5)3PO4 186 L 216 1.06 6.3 NA 115

phosphate 8

ketene CH2CO 42 G -56 GAS 1.45

Ammonia NH3 17 G -33 0.63 0.6

Ethyl CH3COOC2 88 L 77 0.90 3.04 2.2/11

acetate H5 2

CHEMICAL PROPERTIES

1.Contact of acetic anhydride either in crude or pure form with water should be
strictly avoided as it violently reacts with water 7 the reaction is highly
exothermic & instantaneous, to give acetic acid.

2. The reaction of ketene with water is also exothermic & instantaneous to form
acetic acid; therefore ammonia is dosed immediately at the furnace outlet as
inhibitor.
ACETIC ANHYDRIDE DESCRIPTION

Acetic Anhydride is a clear, colorless liquid with a very pungent, penetrating,

vinegar-like odor. It is completely miscible with diethyl ether and can be easily
dissolved in the usual organic solvents; it reacts with alcohols. Acetic
Anhydride is an excellent solvent for numerous organic and inorganic products.
In the presence of water, Acetic Anhydride reacts only slowly at room
temperature to form acetic acid. At elevated temperatures, this reaction can be
extremely violent. It is accelerated by catalytic quantities of sulfuric acid or
other mineral acids and may even be explosive.

ACETIC ANHYDRIDE APPLICATIONS

In the chemical industry, the reactivity of the acetyl group of Acetic Anhydride
is used to synthesize end products and intermediates.

Acetic Anhydride is widely employed industrially for its acetylating and

dehydrating properties.
A major use for it is the acetylation of cellulose to produce acetate fibers,
plastics, coatings and films.
It is especially valuable for the direct esterification of alcohols where acetic acid
cannot be used.

Another large use for Acetic Anhydride is in the manufacture of acetylsalicylic

acid (aspirin), acetylcholine hydrochloride, acetophenacetin, sulfonamides,
aceto-p-aminophenol, cortisone, acetanilide, theophylline, sulfa drugs, certain
vitamins and hormones; and many other pharmaceuticals and pharmaceutical
intermediates.

Acetic Anhydride is also used to produce acetyl ricinoleates, triacetin, acetyl

tributyl citrate, and otherplasticizers. Triacetic glycerol esters are used as
plasticizers in the plastics and paint industry, asfixatives in perfumery and as
solvents for fungicides and basic dyes.

Acetylated fatty acid monoglycerides and acetylated animal and vegetable fats
are used as additivesand auxiliaries in the food industry. In this connection, the
relevant statutory food regulations must beobserved.

Another chemical use is in the manufacture of acetyl peroxide. Acetic

Anhydride is also used as anintermediate in the manufacture of explosives,
weed killers and in the chemical treatment of papersand textiles.
INTRODUCTION OF CHEMICALS USED IN AC2O PLANT

 Acetic anhydride in its crude form i.e. crude anhydride is an intermediate

product & that in pure or finished form i.e. pure anhydride is sale able
product.
 Tri Ethyl Phosphate(TEP) is used as a catalyst in ketene generation.
 Ammonia is used as inhibitor in ketene generation & also as refrigerant in
brine unit.
 Ketene is a gas formed after catalytic cracking of acetic acid in furnace
which after separation from dilute acid is immediately absorbed in &
reacted simultaneously with acetic acid to form acetic anhydride.
 Ethyl Acetate (Ethyl Ester) is used in acid recovery section as solvent in
the liquid extraction process.
 Methanol is used in brine water i.e. brine is a solution of 40% methanol in
water.
Product Description and Handling Guide
Acetic Anhydride

The shelf life of Acetic Anhydride is one year.

The shelf life dates from the day of packaging, for bulk deliveries this is the day
of loading. This period is in general applicable to material stored under
conditions recommended by Celanese Chemicals.
When product exceeds its shelf life or storage deviates from the recommended
conditions, periodic monitoring may be required to verify quality status of the
product.
 Recommended Blanketing ---- Airor Dry Nitrogen
 Recommended Temperature---- Ambient
 Recommended pressure --- Atmospheric
 Bulk Quantities------ Outside, detached tanks
 Small Containers ------Cool, dry, well ventilated area.

Handling

 Thoroughly review Material Safety Data Sheet before handling product.

 Protect small containers from physical damage. Keep containers closed
when not in use. Open containers slowly to allow any excess pressure to
vent.
 Keep away from heat, sparks, flame or other sources of ignition. Use
spark-resistant tools.
  See the National Fire Protection Agency (NFPA) #30 “Flammable and
Combustible Liquids Code” and consult with qualified fire protection
specialists to determine specific storage tank design requirements.
 Use proper electrical grounding and bonding procedures when loading,
unloading and transferring. Refer to the National Fire Protection Agency
(NFPA) #77 “Recommended Practice for Static Electricity” for proper
electrical grounding procedures.
 Electrical equipment and circuits in all storage and handling areas must
conform to requirements of national electrical code (Articles 500 and
501) for hazardous location.
 Blanketing may be used to retain quality in long-term storage conditions.

EQUIPMENTS DESCRIPTION DETAILS

IDENTIFICATION DESCRIPTION IDENTIFICATION DESCRIPTION
NO. NO.

2A&2B Acid vaporizer E-52 Re boiler

3A&3B Super heater E-53A Condenser
8(C,D,E,F,G,H) Separator E-53B Chillers
E-203 A/B/C Ketene D-53 Decanter
condenser
 E-203 A/B/C/D Ketene cooler E-54 Re boiler
D-203 Catch pot E-55 Pre heater
D-204 Catch pot E-56 Vent condenser
V-31A Dilute acid E-57 Vent condenser
vessel
V-31B Dilute acid C-21A/B Ketene
vessel absorption col.
C-42 Column C-24A/B Ketene
absorption col.
E-43A Re boiler C-27A/B Wash column
E-43B Re boiler C-30A/B Wash column
E-47A Feed per heater E-23A/B Intercooler
E-47B Condenser E-26A/B Intercooler
E-48 Condenser E-29A/B Chillers
E-49 Cooler E-32A/B Chillers
C-45A Exhaust column V-51 Acid residue
vessel
E-45A Pure anhydride V-52 Anhydride
cooler residue vessel
E-45B Vent condenser V-28 Crude
Anhydride
Vessel
C-43 Extract column V-33 Vacuum pump
Vessel
E-50A Condenser C-44 Acid distillation
column
E-50B Condenser C-45 Auxiliary
column
E-50C Chillers V-12A/B Dilute acid pot
D-50 Decanter
E-51 Feed condenser

UTILITIES
1. Electricity

2. Steam

3. Cooling water

4. Chilled water
 5. Brine water

6. Bio-gas

7. LDO

8. Producer gas

9. Instrument air

1. PROCESS OF KETENE GENERATION AND SEPARATION

Initially for producing 1 tons of acetic anhydride it requires

ACETIC ACID 1220-1240kg

TRI ETHYL PHOSPHATE 3-4kg
AMMONIA .7-1kg
STEAM 2.7-3 MT
POWER 395KWH
LDO(LOW DENSITY OIL) 100-110lt
BIO-GAS 220-250Nm3

2.Process Description-
FAA GAA

ACID TEP KETENE NH3 KETENE KETENE

VAPORIZER GENERATIO SEPARATION ABSORPTIO
N N & R/C
 CRUDE ANHYD

Initially acetic acid from T-102A/B comes to acid vaporizer, where it is been
mixed with TEP and both will pass through HP steam to generate temperature
of about above 1000c and HP steam of 3-4kg/hr is continuously fed to the
vaporizer.

Super heater is provided to increase the temperature at around 150 to 160 0c

and about 50kg of material is drained in the acid residue vessel V-51 every day
and the pressure will be around 540-640mmHg and this mixture will be fed to
the furnace in which fuel in the form of BIO-GAS, PRODUCER-GAS&LDO is
used. There are 16 burners at the bottom of the furnace and air from air blower
is provided to pass through the top of the furnace for heat recovery. Here the
convection zone temperature is around 850-9000c and radiation zone
temperature is 750-8000c, while the outlet temperature at which ketene is
obtained is about 720-7300c.

Immediately acetic acid is cracked by using TEP as catalyst to ketene+H 2o

and sudden addition of ammonia as inhibitor is done to avoid reversible
reaction. Temperature of chimney is around 240 to 3600c.
CHEMICAL REACTION-

CH3COOH CH2CO + H2O

This reaction is endothermic reaction 144kJ/mol

Now the next step is ketene separation-

The high reaction ketene gas is separated and passes through three ketene
coolers, where gas is separated with un-reacted acid and water and then this gas
is further chilled in a chiller which is used to separate gas and than through
brine water chiller where temperature is -8 to -10 0c and chiller temperature is
around 20 to 250c.
Now from all these separators the dilute acetic acid which is obtained at the
bottom will pass through the V-31(DAA tank). And ketene is moved to
absorption column.

2. KETENE ABSORPTION-
Next step after ketene generation and separation is the absorption of

ketene with glacial acetic acid to form crude anhydride.

CHEMICAL REACTION –

CH2CO + CH3COOH (CH3CO)2 O

This reaction is exothermic reaction -63kJ/mol

In this section ketene gas is absorbed in the four columns C-21, C-24, C-27,
C-30 to get absorbed ketene and thus obtained crude anhydride.

Ketene gas from the last separators V-8 will pass through the absorber C-21

where it gets absorbed which is mixed with 90% anhydride and 10% acid at
a rate of 65000-70000kg/hr. Because this results in the formation of anhydride
and acid with the evaluation of heat. Hot absorbate at the bottom of column is
cooled in a cooler and it is recirculated back to column with the help of pump
and crude anhydride is collected in V-28.

The unabsorbed ketene will move to the next column C-24 were also
anhydride and acetic acid will be recirculated at the rate of 60000-65000kg/hr
with the help of inter cooler and pump back to the column at temperature 42-
45oc. Here GAA from tank T-102C/D is used as a second feed and the bottom
overflows will be connected to the C-21.

The still unabsorbed gas from the top of the C-24 is supplied to the bottom of
the wash column C-27 A&B , crude anhydride from V-28 will be used as feed
to it and the hot absorbate will be recirculated after passing through a chiller and
pump at temperature 5-100c at a rate of 900-1000kg/hr. And the bottom
overflows are again connected to the C-21 col.

The still unabsorbed from the top of the wash column C-27 will pass through
the bottom of the wash column C-30 and act as feed. And acetic acid from V-31
will also act as feed to C-30 and it is recirculated with the help brine chiller and
a pump back to the column, were ketene gas is obtained as the top vapour will
be connected with the vacuum pump while the DAA will move to the col. V-31.

The whole system of ketene generation and absorption is under vacuum and this
in a water ring type centrifugal pump with a pressure of 710 torr and capacity
990ppi. Discharge of the vacuum pump goes to the vacuum vessel V-33. Where
water is circulated with two plate heat exchanger, and the off gas from the
vacuum V-33 which is used in the furnace as off gas burner , thus by
maintaining energy conservation and environmental protection.

3.ACETIC ANHYDRIDE DISTILLATION

Third step in acetic anhydride is the distillation of the crude anhydride.

CRUDE AC2O ANHYDRIDE PURE ANHYDRIDE
DISTILLATION
AA
Crude anhydride from T-103A/B is been pumped as a feed to the C-42 and thus
results in the production of pure acetic anhydride.

The top vapour of the column at a temperature of around 117-120 0c after

passing through a preheater E-47A will pass through the C-42 and then the
vapours are condensed in a condenser E-47B and uncondensed part of it will
move to the next condenser E-48. The condensed liquid after passing through
all three condenser and some part of it is reflux back to the C-42 to maintain
the middle 1 temperature at 130-1320c and middle 2 temperature at around 139-
1420c. And thus obtain acetic acid from it after subcooled in a cooler E-49 ,
which is collected in the T-102A/B.

The bottom vapour of anhydride at a temperature of about 143-144 0c is

removed, by maintaining level in the column about 40-50% & of reboilers about
70-80% & fed to the bottom of the auxiliary(rectifying) column C-45A for
rectification by washing with reflux. The levels of the columns and reboilers are
maintained by regulating the top vapours of the column C-45A, which are then
condensed in a condenser E-45A with CW & an uncondensed part of it in a vent
condenser E-45B with CHW. The condensate is pure acetic anhydride (99%)
and is partly refluxed to the C-45A through rotameter and then removed as a
product and sent to pure anhydride storage tank T-104A/B after cooling in
cooler E-45C. Bottom liquid of column C-45A is returned to the bottom of the
column C-42.

4.ACID RECOVERY SECTION-

ETHYL ACETATE

ACID
LIDUID RECOVERY

EXTRACTION
DIL. AA RECOVERED

ACID

ETHYL ACETATE ETHYL ACETATE

ESTER
RECOVERY
DRAIN TO CETP

Fourth step in the production of acetic anhydride is the recovery of acid from
the whole section.

Here, dilute acid is generated in ketene generation section of the plant. It is

necessary to recover acid from it. But the separation of acetic acid from water is
difficult and requires infinite number of stages in case of ordinary distillation.
So, it requires liquid-liquid extraction followed by distillation.

The dilute acid from DA storage tank T-109B containing 40-50% acidity is
transferred by P-146C to DA preparation tank T-106A. DA lot is prepared in
this tank by adding water to it & the acidity of DA is reduced to 18-20%. Then
this lot is transferred by pump P-146A to DA feed tank T-106B.

This 18-20% DA from tank T-106B is pumped by P-147A/B to the top of the
extraction column C-43. Ethyl acetate from EA tank T-107 is supplied by pump
P-148A/B to the bottom of the extraction column C-43 as a solvent. The column
C-43 is a packed column containing stacked sulzer packing .

The upper phase of the column C-43, the extract phase, containing about 7-10%
acid, 8-10% water & rest ester is continuously removed and collected in extract
tank T-108. The extract from this tank T-108 is pumped by P-149A/B to the
acid distillation column C-44 as feed, after preheating in feed preheater E-50A
with its own top vapour. A reboiler E-52 is provided at the bottom of the
column to which steam is supplied. Top vapour of the column at temperature of
about 73-740c are first passed through feed preheater E-50A & than condensed
& sub cooled in condenser E-50B with CW. EA from T-107 is pumped to the
column top as a reflux. The condensed liquid from both the condenser is
collectively removed & is further chilled in chiller E- 50C with CHW &
supplied to the decanter D-50 for phase separation. The upper phase is EA and
is recycled back to T-107. The lower (aqueous) phase mainly containing acid
and water is supplied to the exhaust column C-45 as (second) feed. The top
temperature of the column is maintained by monitoring middle temperature of
the column 7 regulating the reflux manually. The bottom vapour of the column
is removed at the temperature of 125-1300c, by maintaining column level at 50-
60%, condensed in condenser E-51 with CW & removed as bottom product
which is acetic acid (95-99%) & is sent to recovered acid storage tank T-109A.
The reboiler of column is drained once in a shift and collected in acid residue
vessel V-51.

The lower phase of the column C-43, the raffinate phase, containing about 7-8%
ester, 1-2% acid and rest water is continuously removed & supplied to the
exhaust column C-45 after preheating in feed preheater E-55 with the bottoms
of the same column for the purpose of heat recovery. The column is basically a
stripping column. A reboiler E-54 is provided at the bottom of the column to
which steam is supplied. Top vapor of the column at a temperature of about
960c is first condensed in condenser E-53A with CW having the provision of
sub cooling & then chilled in chiller E-53B with CHW. The chilled liquid is
then supplied to a decanter D-53 for phase separation. The upper phase is EA &
is recycled to EA tank T-107. The lower phase containing mainly water & 1-2%
acidity is again supplied to the column as third feed. The top,middle 7 bottom
temperature of the column are properly monitored. The bottom of the column is
removed at temperature of about 990c, passed through pre heater E-55 & then
sent to CETP by pump P-151A/B by maintaining column level at 50-60%. The
effluent that is sent to chemical effluent treatment plant has about 1% acidity &
BOD about 12000-15000ppm & COD at about 3000-5000ppm.

DOPP KETTLE-
The acid residue from vessel V-10 & that from acid distillation column C-44 in
the form of blowdown collected in acid residue storage tank V-51 & anhydride
storage tank V-52 are supplied, in separate batches, by pump P-143 to dopp
kettle. It is steam jacketed agitated vessel operating under vacuum. The vapors
are taken out from the top of the kettle through a demister pad & are condensed
in a condenser E-57 with CW & respective material is collected in receiver
56A/B & then pumped by pump P-144 to appropriate tanks. Acid feed tank T-
102A/B or crude anhydride tank T-103A/B, as the case may be. The residue is
drained after proper concentration (27-30% solid content).

The dopp kettle system operates under vacuum for the purpose of better
recovery. The rate of vaporization is more at reduced pressures. So the vacuum
is applied to the system. These are also a water ring type centrifugal pump, of
capacity 350PPI and create the vacuum upto 600 torr. Discharge of this vacuum
pump is drained.

STEAM 3kg/hr

vaccum

V-10 C-44
CONDENSER
V-51

DOPP
A-R-V
KETTLE RECIEVE
R
V-52

ANHYDRIDE-R-V

T-102

FROM C-42 T-103

solid material to drain

Operations used
Manufacture of Acetic Anhydride consists mainly of three unit operations :

1. Extraction : Extraction is a liquid – liquid separation operation based on

the use of a different liquid C to extract out one liquid A from a completely
 miscible binary solution of A & B which have relative comparable boiling
points. It makes use of a EXTRACTOR. In this case, the anhydride and
water make a miscible solution which can’t be separated by distillation. So
ethyl acetate is used to extract anhydride from the mixture. Anhydride
solution is fed in the extractor from the top and acetate from bottom. Ethyl
acetate being more soluble in anhydride than in water, mixes up with water
and escapes out form the extractor from the top, while the mixture of acetate
and water settles at the bottom. The acetate can be later recovered using
decantation.

2. Absorption : It is the basic operation which results in the production of

acetic anhydride. A gas is absorbed in other one is called absorption. It takes
place in a unit called ABSORBER. Ketene gas is fed into the absorber from
the bottom and acetic acid is fed from the top. Reactive absorption takes
place between the two gases, to produce acetic anhydride.

3. Distillation : it is the process to separate two liquids on the basis of relative

volatility, in a DISTILLATION COLUMN. The mixture is fed into the
column, and it is heated. So the more volatile component escapes at the top
while the lesser volatile escapes from the bottom. In the plant, a mixture of
acid and anhydride is fed into distillation column. More volatile acetic acid,
escapes off from the top while anhydride vapours are collected from the
bottom.

Equipments used
1. Vaporiser : A “Vaporiser” is a simple cylindrical shell with steam pipes
coiled inside it. It is used to convert the raw acetic acid feed to vapour form to
superheat it to be sent into furnace for heating and ketene generation.
2. Furnace : A furnace is used to provide the necessary high temperatures and
pressures required to generate ketene. It consists of two sections :
CONVECTION and RADIATION Zone. Convection Zone has temperatures
around 500OC while the radiation zone temperature is around 900 OC. In between
these two zones, there exists a connecting CROSS – OVER zone which bears
temperatures around 550 – 750OC. The heat is supplied by burning bio gas,
produce gas or coal in burners.
3. Cooling and Chilling Unit : A Cooling or Chilling Unit is a Shell & Tube
Type Heat Exchanger in which in a liquid (generally the hot one) flows in the
tubes while the cooling medium flows through the shell. If the cooling medium is
cooling water, it is called cooling unit, and if the cooling unit is chilled water or
brine water, it is called chilling unit. It is used to either harness the heat of an
exothermic reaction or to cool down a hot liquid.
4. Absorbers : Absorbers are used to carry out absorption operation. They are
packed bed columns consisting of internal structures to increase the area for
effective mass transfer. Thus the two gases come in contact with each other on
the surface of the internals in the column and undergoes absorption into each
other. In the anhydride generation process, there are two absorbers connected in
series containing pollen rings as internals. Ketene is fed from bottom and acetic
acid is fed from the top of absorbers.The ketene gas is absorbed and converted to
acetic anhydride in these columns.

5. Distillation Column : These are used to carry out distillation, mainly of two
types : Atmospheric and Fractional. The distillation columns are long, cylindrical
shells consisting of plates to increase mass transfer rates. The trays can be of
various types : (i) Bubble Cap (ii) Sieve Tray (iii) Tunnel Tray.
The gas is fed from the bottom of the column while the liquid flows in from the
top. The liquid rests on the trays for a while, where it makes contact with the
upcoming gas. There occurs heat and mass transfer and the volatile gas from the
mixture moves up while the liquid, flows down. Thus it separates the two
components from the mixture. The separated components can be rectified or
stripped if necessary.
6. Extraction Column : These are used to carry out extraction operation in the
plant. The column is a cylindrical shell consisting of internal packing. The
inseparable mixture (acetic anhydride and water ) is fed from the top of the
column, while the extracting media ( ethyl acetate) is fed from the bottom. The
 extracting media is soluble in anhydride and takes it away with itself from top.
This method is very useful in separation of components where distillation is not
useful.
7. Decanter : Decanters are used to separate the liquids on the basis of their
densities. It is a cylindrical shell, less in height than column, which is hollow
from inside. The mixture is slowly fed into the decanters and left to separate by
gravity settling process. The organic phase appears at the top, while the aqueous
phase settles at down. These are then pumped out and used where ever
necessary.
8. Condenser : These are a simple heat exchangers, shell and tube type, designed
only to convert the phase of a vapour to liquid phase. Condenser are specially
designed to remove, only the latent heat of vapour and not to reduce their
temperature. Thus, the inlet and outlet temperature of the hot medium is same in
a condenser.

Instruments
Valves : These are used to restrict, stop and control the flow of liquids through
a pipe. It is sometimes desired to stop the flow through the pipe which is
attained by the valve.
  Gate Valves : It consistsof a gate which sets on seat entirely when the
valve is closed, restricting the flow. It is used when there is no
permissible pressure drop and slow opening and closing action is
permissible.
 Ball Valve : These contain a half spherical ball inside the pipe. The ball
closes the pipe area when the valve is closed and vice versa. It is mainly
used when there is no permissible pressure drop and quick opening and
closing action is needed.
 Butterfly Valve : It is used in non returning valves. It consists of a
circular sheet which is perpendicular to flow when the valve is close and
parallel to the flow when valve is open. It also has a locking mechanism.
 Control Valve : These are pneumatic valves which work on air pressure.
The input to these valves is air of pressure 4 – 20 psi. The flow is
controlled according to the opening which is controlled by the input
pressure. These are always used to electronically control the flow.
 Globe Valve : These valves consists of a upward followed by a
downward stream inside the valve. These valves are used a pressure drop
across the valve is permissible.

Pumps : Pumps are used to pump liquids up to some height above a given
surface. It is basically of two types :
 Centrifugal Pumps : These pumps use the centrifugal action to
increase the pressure of fluid. The suction pipe takes in the liquid and
rotates the fluid through an impeller. This rotational motion increases
the velocity of fluid, thereby increasing the pressure.
 Positive Displacement Pumps : These pumps are based on
reciprocating action of a plunger. The basic principle involves suction of
a small amount of liquid in a cylinder, its max. Compression possible,
and then delivery at higher pressure.
 Vacuum Pumps : These pumps are used to create vacuum in the tubes.
These suck up the air and throw it out from the containers. This in turn
creates vacuum in the container or the pipe.

Transmitters: The Transmitters are used to measure the control variables –

Pressure, Temperature, Flow and Level and transmit them to control room.
TANK FARM AREA

S.N CHEMICAL FOR TANK NUMBE MAX. NORMAL

O / M NO. R STORAG STORAG
UTILITY E E
NAME (MT) (MT)
ACETIC LIQUI T-102A/B 2 100 90
1 ACID D
GLACIAL AA LIQUI T-102C/D 2 100 90
2 D
CRUDE LIQUI T-103A/B 2 150 140
3 ACETIC D
ANHYDRIDE
PURE LIQUI T-104A/B 2 150 140
4 ACETIC D
ANHYDRIDE
DILUTE AA LIQUI T-106A/B 2 80 72
5 D
DILUTE AA LIQUI T-109B 1 15 12
6 D
RECOVERED LIQUI T-109A 1 15 12
7 AA D
ETHYL LIQUI T-107 1 10 5
8 ACETATE D
EXTRACT LIQUI T-108 1 10 5
9 TANK D
CHILLED LIQUI T-201 1
10 WATER D
BRINE LIQUI T-202 1
11 WATER D
LDO LIQUI T-203 1 5 4
12 D
TRI ETHYL LIQUI DRUMS
13 PHOSPHATE D
KETENE GAS _
14
METHANOL LIQUI DRUMS
15 D
AMMONIA GAS CYLINDER
16 S
MAXIMUM CAPACITY 300MT, NORMAL STORAGE 270MT
 DAILY PRACTICE AT ACETIC ANHYDRIDE PLANT

1.Acid – vaporizers 2A & 2B draining

It is done once in shift, about 50kg material is drained from
each vaporizer. However the quantity depends upon the color of the drained
material. More the darkness of the color, more the quantity should be of
draining. Vaporizers 2A &2B operate under vacuum, so the receiver of draining
i.e. the residue collection vessel V-10 is also taken in vacuum temporarily &
once the purpose is over its vacuum is released. The material is transferred to
the Dopp kettle for acid recovery.

2 .Reboiler E-52 draining-

The reboiler E-52 of acid recovery column C-44 is drained
once in a shift in order to remove concentrated liquid in column bottom thereby
maintaining solid material content within limit & avoid reboiler tube side
fouling. This is because column bottom is not continuously removed in the
liquid form but in vapor form.

3.Reboilers E-43A & B draining-

The reboilers E-43A & B are drained once in one or two days
after stopping the distillation temporarily for some time. The vacuum is released
at the time of draining if the column is running under vacuum. About 2500-
2800kg material is removed at one time. This is for the purpose of removal of
solid or concentrated material, if any, present at the bottom of the column &
thereby avoiding reboiler fouling / chocking. The blow down is taken to the
residue collection vessel V-52. The anhydride from it is recovered after
processing it in Dopp kettle K-53.

Presently new procedure is now developed for online draining

of the reboiler. In this case instead of stopping the column for draining, only
vacuum is released temporarily, & reboiler is drained by maintaining both levels
in column & reboiler. Also the column is drained once in two days (48hrs).
 PLANT LAYOUT

DISTILLERY MOLASSES
& CO2 STORAGE
EA 1 EA 3 EA 4

WARE
ALC. HOUSE
COAL
PACKI
STORAGE
NG ADMINISTR STEAM
ATIVE REBOILER
BUILDING

RO-PLANT
EA 2 ACETIC ANHYDRIDE

BIO-GAS
STORAGE
FILLING
AREA
COMMERCIA
L -DEPT.

TIMES
OFFICE

ACCOMO
-DATION
PLANT START-UP
PROCEDURE
Two tests are required
 Pressure test at ketene generation & absorption.
 Vacuum test at 80-90mmHg main vacuum.
 Cooling towers pumps are started and all coolers and condensers are lined
up.
 Brine unit and chilling unit are started.

For Anhydride Generation Section-

 Air blower is started and furnace is fired, only two or three BG burners
are fired and furnace temperature is slowly increased at rate of 50 0c per
hour.
 When furnace box temperature is in between 150-2000c, ketene
absorption pump P-121, P-122, P-123 & P-124 are started and water level
is taken to acid vaporizer 2A& B.
 When furnace box temperature is reached to 200 0c vacuum pump P-
125A/B is started.
 And number of burners are also increased to get a temperature in the
range of 50-700c per hour.
 When furnace outlet temperature is reached to 500-5500c, DM feed to
vaporizer is stopped and acid feed started. Also TEP and NH 3 dosing is
started. Acid vaporizer outlet pressure is maintained to 400-500mmHg.
 Now all burners are started and outlet temperature of the furnace goes to
7000c.
 Furnace outlet temperature are slowly increased and maintained between
720-7300c and when absorbers anhydride composition is 70% BW to
ketene chillers is lined up.
 Once the absorption composition of anhydride is about 85-90%, so GAA
feed to C-24 is started.

For Anhydride Distillation Column-

 After successful completion of pressure and vacuum test at 1kgf/cm 2,

cooling water CW and chilled water CHW are lined up and column C-42
is started.
 Crude AC2O feed to C-42 is started by starting feed pump.
  After getting more than 70% level in re boiler, steam to re boiler is
started.
 Column temperatures start to increase slowly. Steam is slowly increased
by maintaining re boiler level up to 1000-1200kg/hr and maintained till
column temperature starts to rise. Once column top temperature is altered
and starts to come down, this the time were reflux to the column starts
and then steam is slowly increased to attain required bottom pressure and
temperature.
 After getting sufficient temp and pressure in column bottom, 140 0c &
130mmHg, TCV is slowly increased and levels are monitored before
opening LCV, it is confirmed that pure anhydride prodn is diverted to
crude tank T-106A.
 Once required temp and pressure is obtained, pure anhydride is stored in
T-104A/B after is purity (checking). And then column is stabilized and it
is clear

For Acid Recovery Section-

 C-43.C-44 and ester recovery column is started and CW and CHW are
lined up.
 DA and EA feed to C-43 is started in ratio 1:3.
 Extract from T-108 is pumped to C-44 and after getting more than 70%
level at column bottom, steam to re boiler E-52 is slowly started, when
column temp begin to rise, so reflux to column is also started.
 Water or raffinate phase from C-43 taken to C-45 and after getting more
than 50% level at bottom, steam to re boiler E-54 is slowly started and
water is sent to CETP.

EMERGENCY SHUT DOWN

 Vacuum pump suction valve is closed in order to hold the vacuum of the
system.
 Crude AC2O vessel V-28 vent valve is closed in order to avoid its
overflow.
 And after getting the emergency supply, one vacuum pump and one
furnace blower is started.
 Discharge valves of all the pumps are closed.
 Isolation valve of LCV’s, steam PCV’s and Bio-Gas PCV’s, and all Bio-
Gas burners are closed.
 CONCLUSION

Jubilant Life Sciences is very renewed company and working

with such an enterprise was really a great experience. In whole of the
training period I was so admired with management and working of the
system. The company employees and officials helped me a lot during the
training.

Looking ahead, I was able to see closely how a chemical

company works and is thankful to JUBILANT for giving me this
opportunity.