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Report of Industrial Training
At
BASF India LTD
Thane site
Submitted by
Kartik Kulkarni
110903014
In partial fulfillment of the requirements for the award of the degree of
BACHELOR OF ENGINEERING
IN
CHEMICAL ENGINEERING
DEPARTMENT OF CHEMICAL ENGINEERING
MANIPAL INSTITUTE OF TECHNOLOGY
(A Constituent College of Manipal University)
MANIPAL – 576104, KARNATAKA, INDIA
June 2014
Index Page
Declaration 3
Acknowledgement 4
Abstract 5
Chapter 1 Introduction
1.1 PU System house 6
1.2 Training objectives 6
Chapter 2 Training Highlights
2.1 Pesol 7-12
2.2 Pre-Polymers 13-19
2.3 Blended polyol 20-24
2.4 Safety 25-27
2.5 Material safety 28-29
2.6 Hazard identification and prevention 30
2.7 Effluent treatment plant 31-32
2.8 Reactor effectiveness 33
2.9 Suggestions 34
Chapter 3 Conclusions
3.1 Conclusions 35
Chapter 4 Company Profile
4.1 History of BASF 36-37
4.2 History in India 38
References
2
DECLARATION
An Engineer is one who converts the theories of the textbooks into practical working models and
processes. We learn many things more perfectly and accurately through observations and
applications.
Learning in classes just gives us the basic idea about any process, while at the same time
industrial training helps us to understand the detailed and thorough working of that particular
process. Hence we can clearly understand the practical application of the theoretical study.
Industrial training is implemented by our college for imparting knowledge about real operations
and processes, and also to learn about working equipment.
This report contains the various unit operations and operational details of the plant. This report
has been prepared on the basis of information collected and provided during the training I
underwent at BASF India Pvt. Ltd., Thane, Navi Mumbai. The information given in the report is
true as per my knowledge and data provided by the industry.
I take immense pleasure in presenting this report and sincerely apologize for any wrong
information printed in it.
3
ACKNOWLEDGEMENT
To begin with, it is my pleasure in showing gratitude to my mentor Mr.Rajesh Shetty, without
whom this project would never have been so informative. In reference to my field work at BASF,
I am thankful to the production manager Mr. Gopinath Ganesan and my H.R. guide Mr. Sunil
Singh for providing me their immense support and precious time. I am grateful to them for
providing me excellent guidance, practical insights and valuable material that have been very
useful in my field work activities. Above all their encouragement and motivation was a driving
force which helped me perform to the best of our potential.
I would like to thank Mr. Viraj Nayak, Mr. M.K. Gupta, Mr. D.S. Sonawane, Mr. B.B. Desai,
Mr. K.D. Bhawalkar, Mr. P.J.Varghese and all other employees of BASF for providing me
opportunity to become a part of their esteemed organization and to learn various skills that will
be useful in shaping my career as a Chemical Engineer.
4
ABSTRACT
Industrial exposure is an integral part of a student’s overall education program. Most employers
rank interpersonal communication and teamwork skills, and practical experience above technical
aptitude. There’s no better way to acquire these skills than to jump into an industrial
environment.
Industrial internships are a proven way to gain relevant knowledge, skills, and experience while
establishing important connections in the field. This term work provides us with valuable
insights into the professional and industrial side of classroom skills.
This report documents all the activities and learning during my four week industrial internship at
BASF India Pvt. Ltd., Thane site. The report shall give an overview of the company’s history
and products produced in the plant assigned to me. It contains various unit operations, process
details and also equipment details of all the equipments needed in the manufacturing. The report
also provides details about the quality assurance tests, safety procedures followed in the industry
along with the different suggestions that I could give to reduce the present batch time of the
products.
CH 1. INTRODUCTION
1. PU SYSTEM HOUSE
BASF is the leading supplier of polyurethanes solutions for systems. The plant setup in
Thane is operational since 2007.
5
BASF offers a comprehensive polyurethanes product portfolio from basic products such as
polyether polyols, polyester polyols, MDI and TDI to polyurethane systems. The major
product manufactured include various grades of polyester polyol and blended polyols. The
blended polyols are further divided into rigid and flexible type.
MDI is used to manufacture both the grades of blended polyols whereas TDI is used to
manufacture only the flexible grade.
All the products are marketed under different names only known to BASF employees and the
customers.
2. TRAINIG OBJECTIVES
- To experience and understand real life situations in industrial organizations.
- To understand the process involved in manufacture of the products.
- To provide suggestions to reduce the current batch time for production process.
- To perceive safety practices and regulations in the industry.
- To understand hazard identification.
- To keep track of trends of reactors for studying asset effectiveness.
CH 2.TRAINING HIGHLIGHTS
1. PESOL
PRODUCTION PROCESS
Raw Materials:
• Adipic Acid: available in powder form in 1000 kg Bags
6
• 1,4-Butanediol: available in liquid state in200L drums
• Catalyst: stored in 50 L drums or jerry cans
• Mono Ethylene Glycol (MEG): stored in storage tank in liquid form
• Diethylene Glycol (DEG): stored in storage tank in liquid form
Process Description:
PESOLs are a result of condensation reaction of carboxylic acids and poly alcohols (glycols).
Water as by-product must be removed in order to shift the equilibrium towards the product.
• Side reactions might occur to small Degree producing Cyclic ester, 1, 4-dioxane,
aldehydes, ether, etc.
Step-wise Procedure:
• Step1: Recipe selection and Batch start phase
-Depending on schedule batch size is decided and recipe is taken from the recipe book.
-The required raw materials are brought from warehouse and kept in plant.
-The liquid raw material is loaded into storage tanks.
• Step 2: Raw material pre-charging phase
The Adipic acid is unloaded into the silo and MEG and DEG is pumped into storage
tanks.
7
MEG Adipic Polyester Polyol
• Step 3: Utility start-up and checking phase
-Cooling water pumps, thermic oil heater unit, chilled water unit, nitrogen supply, steam
supply, instrument air supply are started and checked.
-Vent scrubber pump is switched on and water level is checked.
• Step 4: Raw material charging phase
-Reactor must be empty and bottom valve is closed and vent through scrubber is kept
open.
- The hot oil internal helical coil and external limpet are started. Stirrer is set at 50rpm.
-Reactor and silo both are inertized using nitrogen. Then MEG and DEG are charged into
the reactor. Check the silo weight.
-The jacket temperature is set at 1200
C. When reactor reaches 750
C then adipic acid is
added from silo.
- The jacket temperature is then increased.
• Step 5: Atmospheric distillation phase
-At 1500
C atmospheric distillation phase starts. Vapour temperature and reflux flow must
be checked.
- The level of water collected in water tank is monitored. If distillation column
temperature exceeds 1050
C, the reflux is started. The column temperature must be
maintained at 1000
C to prevent any glycol from coming into the column.
• Step 6: Partial vacuum phase
-At 2000
C when 80% of water generated in reactor is removed, the vacuum pump is
started. The catalyst is charged.
8
- Jacket temperature is increased, the vent valve is closed and bleed valve is opened when
pressure reaches around 1000-100 mbar.
• Step 7: Full vacuum phase
-Reflux to vessel is closed. Pressure reaches 30mbar. The set temperature is reduced
according to steam table.
-After reactor reaches 2450
C wait for 1hr.
• Step 8: Sample checking phase
-sample from reactor is withdrawn and checked for the specifications. It undergoes tests
for viscosity, hydroxyl value and acid value.
- If sample is not within specifications then required adjustments are made.
- Excess glycol is removed.
• Step 9: Cooling and vacuum breaking phase
-The vacuum pump is stopped and vacuum is broken with nitrogen gas.
- The thermic oil which is cooled using a heat exchanger is used for cooling the product.
• Step 10: Transfer, cooling and packing
9
-The product is transferred from one reactor to other where it is allowed to cool down till
800
C using cold thermic oil.
-The cooled product is then packed into drums or tankers.
Utilities:
• Water cooling tower:
Counter flow induced draft water cooling towers are used to cool the hot water from heat
exchanger to a temperature of 270
C. Hot water from the system enters the water cooling
tower and is distributed over the film type fills. Air is induced through the fill causing a
small portion of water to evaporate. This evaporation removes heat from water thus
cooling it. The cooled water is collected in the basin. Make-up water is added to adjust
the evaporated water.
• Water chilling unit:
It is used to bring the water temperature down to 5 to 60
C. It consists of a hot water well,
cold water well, compressor, condenser and a shell and tube heat exchanger for cooling
of water. The refrigerant gas is first compressed and condensed which then flows through
the tube side of heat exchanger. Hot water enters the shell side. Liquid refrigerant absorbs
heat gets converted to gas thus cooling the water. The chilled water is then sent for
cooling the thermic oil and also for condensing water vapour at distillation column.
• Thermic fluid heater:
10
The thermic fluid used for heating and cooling of reaction is Hytherm 600. The thermic
fluid circulates in a coil heated by PNG inside the heater. The automatic control of the
PNG is done using a solenoid valve. Hytherm 600 is heated to 2400
C by keeping the set
point at 2800
C. This heated oil is then used for heating the PESOL reaction.
• Vacuum:
Vacuum is necessary for the distillation and stripping operations. Vacuum is created by
water ring vacuum pump and steam jet ejector. Vacuum as low as 30 mbar is achieved.
• Instrument air and Nitrogen gas:
Instrument air is required for various on/off valves, pneumatic valves etc. It is also used
to control the function of centrifugal pump in charging of raw materials. The nitrogen gas
is used for inertization of the reactors and silo before and during the reaction.
11
EQUIPMENTS DETAILS
• Reaction Vessel: the plant consists of 8 reactors of varing sizes for different batch size
and product.
PESOL: two reactors (one for reaction and mixing and other for cooling)
Its capacity is 12.45 m3
and is made up of stainless steel. It has a half coil jacket and an
internal helical coil and 4 baffles. The first reactor has a pitched blade type agitator and
the second reactor has a paddle type agitator. It can withstand from 3kg/cm2
pressure to
full vacuum and a temperature of 3000
C. The reactor has undergone hydrotest and
radiography test, and has a joint efficiency factor of 0.85. No corrosion allowance is
provided.
12
• Distillation column:
It is a packed column type and has structured packings. The packings are of rasching
ring type. Dimension: 600x7600(mm)
• Silo:
The adipic acid silo consists of unloader with nitrogen aerator. It consists of a lump
breaker having a motor of 1hp and a dust extraction system with a blower having
capacity of 200 m3
/hr.
• Heat Exchanger:
The plant has three heat exchangers. All are shell and tube type heat exchanger made of
stainless steel. Two of them are used as condensers to condense water vapour from
distillation tower and third one is used to cool the thermic fluid for cooling of the
product.
Tests for PESOL quality:
• Viscosity test:
Sample is taken out from the reactor, cooled and some of it is placed in the viscometer.
The viscometer spindle then rotates at 60 rpm and temperature is maintained at 750
C. The
viscometer displays the measured viscosity.
13
• Acid value test:
Equipments required - analytical balance, plastic cup, measuring cylinder, magnetic
stirrer, burette, pipette
Reagents- ethyl alcohol (96%), acetone, distilled water, 0.1 N KOH, phenolphthalein
Procedure- the sample of PESOL is cooled and then mixed with a mixture of ethyl
alcohol and acetone (1:1). This mixture is titrated against 0.1 N KOH solution, in
presence of indicator phenolphthalein. Colour change marks the end point of the titration.
2. PRE-POLYMER
 CHEMISTRY
 Pre-polymer reaction –
Pre-polymers are manufactured by the conversion of a stoichiometric excess of
isocyanate with polyols and possibly further OH components according to the
following reaction equation.
R1-OH + R2-NCO  R1-O-CO-NH- R2
The large scale production of Pre-polymers takes place in discontinuous mixing
vessels , whereby the isocyanate is added followed by a temperature controlled
addition of polyol. To minimize secondary reactions the temperature is kept
below 100 ⁰C.
 During the Pre-polymer reaction, undesired reactions of the isocyanate can occur
under certain conditions.
i. Dimerisation of isocyanate with the formation of uretdions –
14
Isocyanates can interact with dimer formation. This is a balanced reaction
which is almost completely on the side of monomers at high temperatures.
These reactions are only slightly exothermic.
2 R-NCO  Uretdions
ii. Interaction of isocyanates with the formation of carbodiimides –
Isocyanates can also form carbodiimides. The reaction takes place with the
splitting of CO2 and without catalyst only at high temperatures which
leads to the build-up of pressure in the reactor.
R-NCO + OCN-R  R-N=C=N-R + CO2
iii. Reaction of carbodiimides with isocyanates with the formation of
uretoimines –
A further reaction of the carbodiimides with isocyanates gives rise to the
formation of uretonimines, which then causes cross-linkage. As with
dimer formation, uretone formation possesses no safety problems due to
the low reaction enthalpy.
R-N=C=N-R + R-N=C=O  Uretonimines
iv. Trimerisation of isocyanates with the formation of isocyanurates –
Isocyanates are subject to trimerisation to produce isocyanurates. The
reaction takes place at high temperatures. It can occur at low temperatures
if the reaction is catalysed by bases such as KOH or potassium
carboxylate. The trimerisation reaction of multifunctional isocyanates
gives rise to the production of highly branched and insoluble products.
3 R-N=C=O  Isocyanurates
15
v. Allophanate formation through reaction of isocyanates with urethane
groups –
Isocyanates can form allophanates with already formed urethane groups.
This reaction takes place in the absence of catalyst at high temperature.
Allophanate formation is catalysed by the same nucleophiles that also
accelerate the isocyanurate reaction. additionally, allophanates can react
with further isocyanate groups with ring closure whereby an isocyanurate
and an alcohol are produced.
R-NH-COOR’ + R-N=C=O  Allophanate
 PROCESS DESCRIPTION
RAW MATERIAL MODE OF CHARGING REMARKS
Methy Diphenyl Isocynate
(MDI)
Vacuum charging from drums
to reactor
Stored as a solid at -5 ⁰C in
cold storage. Melted at 100 ⁰C
in oven and charged under
vacuum of 500 mbar & 50-55
⁰C
Benzyl Chloride Charged through funnel on top
of the reactor
Charged under atmospheric
pressure
Polyols + Dipropyleneglycol Vacuum charging from drums
to reactor
Premixing of polyols and
dipropyeleneglycol required
before charging material at a
particular flow rate
(undisclosed)
Catalyst Vacuum charging from drums
to reactor
Reactor temperature to be
maintained at 50-55 ⁰C
Triphenyl Phosphate Charged through funnel on top
of the reactor
Material to be charged at a
particular flow rate
16
(undisclosed)
Diiso nonyl phthalate Charged through funnel on top
of the reactor
Material to be charged at a
particular flow rate
(undisclosed)
2,6-di-tert-butyl-p-cresol Charged through funnel on top
of the reactor
Material to be charged at a
particular flow rate
(undisclosed)
 Raw Material testing and making ready for charging –
i. Raw Materials are tested for quality as per the requirements.
ii. Raw Materials are issued from the Warehouse and brought to reactor
using forklift and hand trolley. MDI is issued from cold storage separately.
 Start up check –
i. Reactor must be clean, dry and empty.
ii. Bottom valve must be closed.
iii. Ensure that limpet circulation heating inlet and outlet and cooling inlet and
outlet valves are closed.
iv. Ensure manhole is tightly closed.
v. Isocynate quality is thoroughly checked for various parameters before
charging it since it is very toxic and hazardous.
 Operating Procedure –
17
i. Vessel is purged with 30 mbar Nitrogen for maintaining inert atmosphere
for reaction.
ii. Reactor is preheated to 50 ⁰C.
iii. Reactants are charged as per the table above.
iv. Once charging is completed vacuum is broken by stopping the vacuum
pump.
v. As reaction proceeds temperature of reactor increases due to exothermic
nature of majority of Pre-polymer reactions. Optimum temperature and
pressure for all the Pre-polymer reactions was experimentally estimated as
70 – 75 ⁰C and 30 mbar. This is maintained by operating cooling
water/chilled water supply valves.
vi. Samples are taken at intervals and checked for NCO content. If found
within the specified limit, the pressure of the blender reactor is increased
to 1.5 kg/cm2
and discharging of the product is started.
 Procedure followed in case of failures –
i. In case of runaway reaction – During glycol charging the rate of rise of
temperature of the reactor as well as the current flowing through the motor
of the stirrer are monitored. If the temperature rises by 5 ⁰C/minute or the
current increases rapidly charging of polyol must be stopped. Inhibitor
solution of Benzyl Chloride is added to the reactor. If the temperature or
current continues to increase the material in the reactor must be discharged
immediately while keeping the safety vent open.
ii. In case of failure of ventilation system – Charging of MDI or discharging
of Pre-polymer products must be halted while keeping the stirrer on.
18
iii. In case of failure of cold storage – MDI is highly toxic and its leakage in
the form of vapours can cause deadly damage. Thus, it is instantaneously
shifted to an adjacent cold storage location.
iv. In case of choking of carbon filter – If the differential pressure across the
carbon filter increases to more than 150 mbar, the carbon inside the filter
must be changed and replenished. The exhausted activated carbon is then
disposed as per MPCB regulations.
 PRODUCTS
 COSYPUR – Used for Vehicle Seats, Car Dashboards and Pillows.
19
 ELASTOFOAM – Used for Insulations, Cushions, Car Upholstery and Pillows.
 ELASTOPAN – Used in Footwear (Uses Polyether as raw material).
 LUPRANATE – Used in Footwear (Uses Pesol, that is, Polyester as raw
material).
 QUALITY CONTROL
 Test for NCO Content:
i. 2 grams of sample is added to toluene (acts as a solvent) and a known
quantity of dibutylamine.
ii. The above solution is stirred for 15 to 30 minutes to make it
homogeneous.
iii. sSome dibutylamine is consumed in the above reaction. The quantity
remaining is found by titration with an acid of known concentration.
iv. Potentiometric Titration is performed using an Electronic Auto Titrator
apparatus.
v. End point of Titration is reached when there is a sudden jump in the value
of the potential measured.
vi. The software displays the values of the volume of acid utilized and the
%NCO content in the sample.
 Other Tests performed for Pre-polymers include the OH test and the Amine Test.
However, these tests are performed for very selective grades and hence were not
studied in depth.
 EQUIPMENTS
 Reaction Vessel –
20
It is made up of stainless steel. It has a geometric volume of 13.75 m3
and an
operating capacity of 10 m3
. It has 2 baffles and is designed to withstand from 5
barg pressure to full vacuum and a temperature of 190 0
C. The operating pressure
ranges from 1 barg to 5 barg and the operating temperature ranges from 80 - 90
0
C. The reactor has undergone hydrotest and radiography test. It has a joint
efficiency factor of 1.00. No corrosion allowance is provided.
 Stirrer/Agitator –
Pitched/bolted blade stirrer with variable frequency drive is used in the reactor. It
has 4 impellers at the top and 2 impellers at the bottom. It operates at an RPM of
87.
 Limpet Heating Coils –
They are designed to withstand a pressure of 5 bar(g) while the working pressure
is 3.5 bar(g). They have a pitch of 300 mm. They have a joint efficiency of 0.7
and are not provided with any corrosion allowance. They have a total heat transfer
area of 11.7 m2
.
 Valves –
There are six types of valves used in this process. They are Globe Valve
(example), Gate Valve (example), On-Off Valve (example), Three Way Valve
(example), Pneumatic Valve (example) and the Diaphragm Type Valve
(example).
 Temperature and Pressure indicators –
21
There are various temperature and pressure indicators in the system which
transmits the values of the temperature and pressure at different points via PLC
(programmable logic controller) to the PC in the control room. This permits more
efficient monitoring of the temperature and pressure in the system.
3. BLENDED POLYOL
22
PROCESS
- There are four blenders in the PU plant. The blenders are used to carry out blending for various
polyol systems.
- Raw materials are used in various combinations to obtain various blended products which are
customer specific .
Raw Material Used Mode of Charging Remarks
Polyol Shuttle block pump for tanks/
AODD pump for drums
Requires heating before
charging
Catalysts Through charging funnel at 10
meter level
Pre-weighing is done in
carboys in the room
Additives Through charging funnel at 10
meter level
Pre-weighing is done in
carboys in the room
Blowing Agents From the bottom of the reactor
with AODD pump
Requires low temperature in
the reactor
Flame Retardants From the bottom of the reactor
with AODD pump
Requires low temperature in
the reactor
DM Water From DM water tank N/A
Steps Of Reaction-
1. Raw material is tested and then is made ready for charging.
2. Raw material charging and blending
- Polyol is charged from tanks or drums.
- Flame retardant adition(Product Specific)
- Catalyst additive charging.
- Blowing agent charging.
- DM water addition.
23
3. Sampling and corrections. Quality assurance is done to check if the product is consumer
specific.
4. Filling and packing. The product is packed and transported to the customers.
24
PRODUCTS
Type Application
Elastocool Appliances
Elastoflex Cushions and Insulations
Elastofoam Insulations
Elastopan Footwear
Elastopor Construction
Elastopir Construction
QUALITY CONTROL
* Blended Polyol Rigid Type
1. Moisture Test
- The sample collected is titrated with Karl Fischer reagent and dried methanol.
- The reaction is handled by an automated computer programme..
- Moisture content is showed and is verified for the specific sample.
2. Cup Test
- Sample is cooled and mixed with cyclopentane and is stirred till formation of foam.
Cyclopentane acts as a blowing agent.
- Blend is cooled and methyl diphenyl isocyanite is added. This mixture is agitated.
25
- The foam starts rising and poked with a sharp object to notice thread formation.
- Foam is left to harden and rise time and gel time are noted down.
* Blended Polyol Flexible Type
1. Cup Test
- Blended polyol is cooled and isocyanide is added. The mixture is agitated and foam is formed.
- The foam initially rises and when co2 escapes the foam settles back.
- The rising time/settling time/height are measured using ultrasonic sensors connected to the
computer. The specifications are verified.
2. Cushion Test
- Blended polyol and isocynaide is agitated for 6 sec at 1000-1500 RPM.
- It is immediately transferred into a pneumatic mould which is pre heated to 58o
c.
- The mould is sealed for 5mins. After the cushion is removed it is tested using a compression
machine which gives the compression for a specific force.
EQUIPMENT SPECIFICATIONS
- Reaction is done in a agitated reactor with torispherical head
- Coil jacketed type.
- MOC: Stainless Steel.
26
- No corrosion allowance. Joint efficiency is 0.85
- Can withstand pressure of 3kgf/cm2
and temperature of 100o
c.
- Tests applied are Vacuum test, Radiography and Hydro test.
- Agitator used is (2x3) anchor type. It has 2 turbofoil and 1 pitched blade at the bottom. The
wetted parts are made of stainless steel and the non-wetted parts are made of carbon steel.
- Empty weight is 4000kg.
- Reaction temperature is 70o
c.
4. SAFETY
*SAFETY AND POLLUTION CONTROL
27
Safety cannot be compromised by any of the employees. BASF is having a Full-flegged Saftey
Department with qualified safety officers in a safety committee . Meetings are held regularly and
various problems are discussed. Recommendations are circulated to the concerned departments.
- Adequate safety budgets are made and company has a constant pattern of expenditure on
safety related issues.
- Accidents and incidents are investigated and records are kept. All the employees are
informed about the cause of the accident
- Internal safety inspections and external safety audits are done frequently.
- Safety education and training are given to each employee in detail.
- Awareness of safety is displayed through notice boards and pamphlets and also accident
free days are displayed.
- Hazard identification and control measures are carried out once a month.
- Work permit system exists in the factory. Hot work, confined space entry, digging snd
general permits are available and are followed strictly.
- Waste disposal system of various type of water is also available.
- Mock drills are conducted once in six months
- Fire prevention equipments like hydrant water systems and fire water pumps has been
used to ensure safety of every corner of the plant.
- BASF has set an occupational health center (OHC) in the premises and also houses full
time doctors and an ambulance is always kept on stand by.
28
- As a part of safety program all the pipe lines are color coded as per international norms.
Fluid Color Code
Cooling water Green
Nitrogen Yellow
Instrument Air Sky blue with blue band
Vacuum Sky blue
Fire Hydrant Red
Process Air Sky blue with silver band
Waste Water Green with blue and orange band
Process Water Green with white band
Vent Light brown
- DCC(Disaster Control Centre) is a special program initiated by the chairperson of BASF,
For the safety of its employees at any time and hour of the day. It is a special team spread
confined to only Mumbai currently but aims at every part of the country where BASF has
its mark. Let it be a mass riot or a major accident, the DCC panel would get you out of it
once you inform them about the situation.
29
*PERSONAL PROTECTIVE EQUIPMENT
SR.NO PROTECTION TYPE OF APPLIANCES
1 Head Safety helmets
2 Eye Safety goggles, Welder’s
goggles, Chipper’s goggles
3 Face Face shields, Face masks
4 Hands Specific hand gloves
5 Body Full body aprons, Boiler suit
6 Ear Ear plug
7 Foot and Leg Safety shoes
8 Respiratory Face masks with filter, Gas
masks with canisters.
9 Protection from falling Safety belt
5. MATERIAL SAFETY
Chemical Hazards Protection
30
Diethylene Glycol Acute oral toxicity, acute
dermal toxicity, slightly
flammable in presence of
open flames and sparks
Use adequate PPE, in case of fire use
dry chemical powder or foam but not
water jet.
Monoethylene Glycol Acute toxicity of vapour,
carcinogenic effects,
mutagenic effects, acute oral
toxicity
Adequate PPE required while
handling, must be kept away from
strong acids and bases, water jet
extinguisher must not be used to put
out fire
Adipic Acid May cause eye irritation,
coughing, sneezing. On
ingestion may cause
diarrhoea
Proper PPE must be used
Tetrahydrofurane (by
product of reaction)
Highly flammable,
hazardous if ingested or
comes in direct contact with
skin
It is removed as a distillate during
vacuum phase
1, 4- dioxane Hazardous to aquatic life,
poses problem in water
treatment
Removed as distillate in ambient
pressure phase
Benzoyl Chloride Harmful if inhaled, irritant to
eyes, toxic to aquatic
animals
Adequate PPE must be used, extreme
heat must be avoided
2,6-ditert butyl-p-
cresol
Toxic to aquatic animals Avoid heat and accidental leakage or
spillage into drains
Di-propylene glycol No hazard PPE is necessary
Triphenyl phosphate Toxic to aquatic organisms,
irritant to skin and
Adequate PPE, avoid spillage and
leakage
31
respiratory system
Elastopan/ Elastocool Harmful is inhaled or
ingested
PPE necessary
Elastopor Dangerous for ozone layer Do not let spillage or leakage to enter
drains
Elastoflex Harmful to aquatic
organisms
High spillage precautions must be
taken
Lupraphen No hazard General PPE necessary
6. HAZARD IDENTIFICATION AND PREVENTION:
Hazard Identification is the process of identifying hazards in order to plan for, avoid, or
mitigate their impacts. Hazard identification is an important step in risk assessment and risk
management. BASF with the aim of ensuring and continuing to develop safe working conditions
strictly follows issuing of safety work permit and concept of yellow card.
Certain safeguards that normally protect the worker may have to be removed when repair or
maintenance work is performed. When this occurs, the hazards involved need to be identified
and a safe work system developed to eliminate or control these hazards. A safe work permit is a
written record that authorizes specific work, at a specific work location, for a specific time
period. Permits are used for controlling and co-ordinating work to establish and maintain safe
working conditions. They ensure that all foreseeable hazards have been considered and that the
32
appropriate precautions are defined and carried out in the correct sequence. There are four basic
type of work permit available in the plant: general work permit, confined Space work permit,
height work permit and hot work permit.
During the internship I learnt to fill, document and maintain the safe work permits, thus gaining
knowledge about hazard identification and prevention.
SAFETY MEETING:
Safety meetings are organized every month to discuss the production issues, reported yellow
cards and action taken against the complaint and follow ups, safety trainings conducted, changes
(addition/ deletion) in the plant equipments, etc.
The meeting I attended started with the declaration of remarkable production achieved in the
month of May. The workers were motivated and everyone was thanked for their contribution.
The meeting proceeded to discuss two major issues, lack of man power and space limitation for
storage of materials. Next all the yellow cards reported were discussed along with the
appropriate action taken. Pending issues of previous meeting were addressed and their status was
discussed. The emergency numbers, assembly point details and safety pledge were revised.
7. ETP-EFFULENT TREATMENT PLANT
Effluent generated from the plants is collected in the effluent collection pits placed across the
site and then pumped to the ETP for treatment.
Effluent is treated in three stages
1. Primary treatment (physio- chemical treatment)
2. Secondary treatment ( Biological treatment)
- Anaerobic treatment.
33
- Aerobic treatment.
3. Tertiary treatment.
• Primary Treatment
- Removal of oil and grease is done.
- The suspended solids are removed.
- The equalization and neutralization of effluent is done.
• Secondary Treatment
- Removal of COD and BOD and ammonical nitrogen is done.
- Aeration tanks are provided.
- Microbes decompose organic matter in presence of air.
- Excess sludge is wasted and thickened in the decanter.
• Anaerobic Treatment
- Effluent water of high COD comes here.
- Soda ash is used for neutralization.
- PH is maintained at 11.
- Anaerobic reactor is a fluidized bed of sand.
- Sand is supported by rock at bottom.
- Feed enters from the bottom.
- The filtrate is fed to the aerobic reactor.
34
• Aerobic Treatment
- The treatment takes place due to the activity of bacteria in presence of oxygen.
- PH is maintained at 9-10.
- There are two tanks used for the process. In the first tank batch is made ready by
adding chemicals and in other tank only effluent water is present.
- The effluent is pumped to a first stage clarifier.
- Solid waste will settle down and clear water will pass through.
- Clear liquid is fed to the aeration tank.
- Here the COD decreases from 8000 to 800.
- Following materials are added to the aeration tank for developing bacteria. Food, Di
ammonium Phosphate, Urea and Starch.
- Water is now fed to second stage clarifier.
- In this clarifier there is one agitator present which keeps moving slowly.
- The pure product is fed to the Poly Aluminum Tank.
• Tertiary treatment
- Fenton treatment is given to the effluent from secondary treatment.
- Ferrous sulphate and hydrogen peroxide are added.
35
- Effluent is then treated with lime.
- Clarified effluent is then sent to sand and activated carbon filter.
- Carbon and sand acts as an absorbent and absorb impurities.
- The Treated effluent is finally drained into the MIDC drain through V-notch
chamber.
8. REACTOR EFFECTIVENESS
 ABOUT THE SOFTWARE
 The Software was developed using MS Excel.
 A database of possible reasons for delay in batch time of the reactor was created.
 Each possible reason in the database created above had a rate of loss of tonnage
(of product) associated with it.
 Another database containing all the products manufactured in every reactor and
the theoretically calculated batch time for each of these products was maintained.
 APPLICATION
36
 Weight indicators on each reactor continuously transmitted the measured values
to a PC in the Control Room of the Plant.
 A plot of Weight v/s Time was generated by the PC.
 This plot was carefully monitored and the actual batch time was noted along with
all those time periods wherein the reactor was not utilized (indicated by constant
weight of the reactor).
 By referring to the company logbook, the aforementioned delays were attributed
to the pre-decided reasons from the database.
 Thus, for every product (every new batch) the departure of actual batch time from
the estimated batch time was accounted for and the Reactor Effectiveness was
obtained.
 A bar chart of %Effectiveness v/s Batch Number and %Effectiveness v/s Month
were then simulated for company records.
9. SUGGESTIONS
- Conveyor Belts can be used to transport drums for charging and discharging
thus reducing the time required and increasing the efficiency. Automated filling
37
machines can be used instead of manual charging. Fork lift related accidents will
reduce because of lesser frequency of its usage
- In pesol production, MEG and DEG are first charged into a smaller vessel and
then charged into the reactor. Time is wasted because the amount of DEG and
MEG required for a single batch far exceeds than what the tank can store. Thus
increasing the capacity of the tank or introducing another tank to meet the
requirements of the reaction.
- Pesol required for pre-polymers and blending is imported externally. The pesol
produced in the plant is directly sold. Pesol can be produced in the plant and
directly charged into reactors or stored in the storage tanks. By doing so the time
taken for charging will be lesser than that of charging through drums. Constant
supply of pesol will also be available at all times. Cost and batch effectiveness
increases.
- Delay due to manpower is the biggest issue for blending polyols. So keeping 2-
3 contractors only for charging and discharging of polyols will increase the
effectiveness of the procress. Thus more batches can be produced and the revenue
of the company will increase.
CH 3.CONCLUSION
38
In conclusion, there were many things that I learned and experienced during the
four weeks of my industrial training at BASF India LTD, Thane site. The whole
industrial training was interesting, challenging and application oriented. Through
this training I was able to gain more insight and more comprehensive
understanding about the real industrial working conditions and practices. This
training period has also provided me with opportunities to develop and improve
my soft and functional skills. All of this valuable information and knowledge
were not only acquired through the direct involvements in the tasks given but also
by other aspects of training such as work observation of seniors and also through
logical and instructive interaction with them. It is known for a fact that the
industrial training program is the best way to prepare a student for facing a real
working life and I completely agree with it. As a result of this, I have gained
immense confidence to enter the employment world and build my future career.
39
CH 4.COMPANY PROFILE
1. HISTORY OF BASF
BASF GROUP:AT A GLANCE
We are the world’s leading chemical company: The Chemical Company. Nearly 111,000
employees work at the BASF Group. Our broad portfolio is arranged into six segments:
Chemicals, Plastics , Performance Products, Functional Solutions, Agricultural Solutions
and Oil & Gas.
-Markets and sites
BASF has subsidiaries in almost eighty countries and supplies products to a large number of
business partners in every part of the world. In 2011, we achieved 53% of our sales with
customers in Europe, of which 30% were in oil&gas. In addition 19% sales were generated in
North America and 20% sales in Asia Pacific. Our Verbund site in Ludwigshafen is the largest
integrated chemical complex in the world.
Organization of the BASF Group
- BASF’s six business segments contain 15 divisions which bears the operational
responsibility and manage our 70 global and regional business units. The divisions
develop strategies for the business units and are organized according to products.
40
- The regional divisions contribute to the local development of our business and help to
exploit market potential. They are also responsible for optimization of infrastructure for
our business. For financial reporting purposes, our divisions are grouped into regions.
- Three central division and 5 corporate departments provide group wide services such as
finance, investor relations, communications, human resource, research, engineering and
management.
BASF Group- Strategy and Values.
- BASF aims to strengthen it’s position in the world as the world’s leading chemical
company. We describe this in our” We create chemistry” strategy, which we presented in
November 2011. This strategy is based on our success in recent years and define
ambitious goals for our future.
BASF Purpose- ‘ We create chemistry for a sustainable future’.
BASF- Strategic Principle. -We add value as one company.
41
- We innovate to make our customers more successful.
- We derive sustainable solutions.
- We form the best team
2. HISTORY IN INDIA.
Establishing a strong India presence.
BASF India Ltd was first incorporated as R.A. Cole Private Limited. It was first involved in the
production of Expandable Polystyrene. With this BASF took first step into the manufacturing .
Over the years BASF India’s product portfolio steadily grew. Because of this the first production
site was opened in Thane, India. In 1986 BASF was listed on the Bombay Stock Exchange &
was listed on the National Stock Exchange in 1995.
The Manglore site which was opened in 1996 is currently the largest manufacturing site on India
and South Asia.
• Thane site- Plastic Chemicals.
- BASF India Limited started operations at the Thane site in Navi Mumbai 1967. It is the
first production site of the company in India and currently focuses on the production of
engineering plastics, Polyurethanes , Performance chemicals, care chemicals,
construction chemicals, dispersions, pigments and styropor.
42
- This site houses five plants and technical application centre’s for textile, leather , pharma,
engineering plastics and polyurethanes.
43
REFRENECES
- www.india.basf.com
- Process manuals from the plants
- www.google.com
- Material safety data sheet
44

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BASF FINAL REPORT

  • 1. Report of Industrial Training At BASF India LTD Thane site Submitted by Kartik Kulkarni 110903014 In partial fulfillment of the requirements for the award of the degree of BACHELOR OF ENGINEERING IN CHEMICAL ENGINEERING DEPARTMENT OF CHEMICAL ENGINEERING MANIPAL INSTITUTE OF TECHNOLOGY (A Constituent College of Manipal University) MANIPAL – 576104, KARNATAKA, INDIA
  • 2. June 2014 Index Page Declaration 3 Acknowledgement 4 Abstract 5 Chapter 1 Introduction 1.1 PU System house 6 1.2 Training objectives 6 Chapter 2 Training Highlights 2.1 Pesol 7-12 2.2 Pre-Polymers 13-19 2.3 Blended polyol 20-24 2.4 Safety 25-27 2.5 Material safety 28-29 2.6 Hazard identification and prevention 30 2.7 Effluent treatment plant 31-32 2.8 Reactor effectiveness 33 2.9 Suggestions 34 Chapter 3 Conclusions 3.1 Conclusions 35 Chapter 4 Company Profile 4.1 History of BASF 36-37 4.2 History in India 38 References 2
  • 3. DECLARATION An Engineer is one who converts the theories of the textbooks into practical working models and processes. We learn many things more perfectly and accurately through observations and applications. Learning in classes just gives us the basic idea about any process, while at the same time industrial training helps us to understand the detailed and thorough working of that particular process. Hence we can clearly understand the practical application of the theoretical study. Industrial training is implemented by our college for imparting knowledge about real operations and processes, and also to learn about working equipment. This report contains the various unit operations and operational details of the plant. This report has been prepared on the basis of information collected and provided during the training I underwent at BASF India Pvt. Ltd., Thane, Navi Mumbai. The information given in the report is true as per my knowledge and data provided by the industry. I take immense pleasure in presenting this report and sincerely apologize for any wrong information printed in it. 3
  • 4. ACKNOWLEDGEMENT To begin with, it is my pleasure in showing gratitude to my mentor Mr.Rajesh Shetty, without whom this project would never have been so informative. In reference to my field work at BASF, I am thankful to the production manager Mr. Gopinath Ganesan and my H.R. guide Mr. Sunil Singh for providing me their immense support and precious time. I am grateful to them for providing me excellent guidance, practical insights and valuable material that have been very useful in my field work activities. Above all their encouragement and motivation was a driving force which helped me perform to the best of our potential. I would like to thank Mr. Viraj Nayak, Mr. M.K. Gupta, Mr. D.S. Sonawane, Mr. B.B. Desai, Mr. K.D. Bhawalkar, Mr. P.J.Varghese and all other employees of BASF for providing me opportunity to become a part of their esteemed organization and to learn various skills that will be useful in shaping my career as a Chemical Engineer. 4
  • 5. ABSTRACT Industrial exposure is an integral part of a student’s overall education program. Most employers rank interpersonal communication and teamwork skills, and practical experience above technical aptitude. There’s no better way to acquire these skills than to jump into an industrial environment. Industrial internships are a proven way to gain relevant knowledge, skills, and experience while establishing important connections in the field. This term work provides us with valuable insights into the professional and industrial side of classroom skills. This report documents all the activities and learning during my four week industrial internship at BASF India Pvt. Ltd., Thane site. The report shall give an overview of the company’s history and products produced in the plant assigned to me. It contains various unit operations, process details and also equipment details of all the equipments needed in the manufacturing. The report also provides details about the quality assurance tests, safety procedures followed in the industry along with the different suggestions that I could give to reduce the present batch time of the products. CH 1. INTRODUCTION 1. PU SYSTEM HOUSE BASF is the leading supplier of polyurethanes solutions for systems. The plant setup in Thane is operational since 2007. 5
  • 6. BASF offers a comprehensive polyurethanes product portfolio from basic products such as polyether polyols, polyester polyols, MDI and TDI to polyurethane systems. The major product manufactured include various grades of polyester polyol and blended polyols. The blended polyols are further divided into rigid and flexible type. MDI is used to manufacture both the grades of blended polyols whereas TDI is used to manufacture only the flexible grade. All the products are marketed under different names only known to BASF employees and the customers. 2. TRAINIG OBJECTIVES - To experience and understand real life situations in industrial organizations. - To understand the process involved in manufacture of the products. - To provide suggestions to reduce the current batch time for production process. - To perceive safety practices and regulations in the industry. - To understand hazard identification. - To keep track of trends of reactors for studying asset effectiveness. CH 2.TRAINING HIGHLIGHTS 1. PESOL PRODUCTION PROCESS Raw Materials: • Adipic Acid: available in powder form in 1000 kg Bags 6
  • 7. • 1,4-Butanediol: available in liquid state in200L drums • Catalyst: stored in 50 L drums or jerry cans • Mono Ethylene Glycol (MEG): stored in storage tank in liquid form • Diethylene Glycol (DEG): stored in storage tank in liquid form Process Description: PESOLs are a result of condensation reaction of carboxylic acids and poly alcohols (glycols). Water as by-product must be removed in order to shift the equilibrium towards the product. • Side reactions might occur to small Degree producing Cyclic ester, 1, 4-dioxane, aldehydes, ether, etc. Step-wise Procedure: • Step1: Recipe selection and Batch start phase -Depending on schedule batch size is decided and recipe is taken from the recipe book. -The required raw materials are brought from warehouse and kept in plant. -The liquid raw material is loaded into storage tanks. • Step 2: Raw material pre-charging phase The Adipic acid is unloaded into the silo and MEG and DEG is pumped into storage tanks. 7 MEG Adipic Polyester Polyol
  • 8. • Step 3: Utility start-up and checking phase -Cooling water pumps, thermic oil heater unit, chilled water unit, nitrogen supply, steam supply, instrument air supply are started and checked. -Vent scrubber pump is switched on and water level is checked. • Step 4: Raw material charging phase -Reactor must be empty and bottom valve is closed and vent through scrubber is kept open. - The hot oil internal helical coil and external limpet are started. Stirrer is set at 50rpm. -Reactor and silo both are inertized using nitrogen. Then MEG and DEG are charged into the reactor. Check the silo weight. -The jacket temperature is set at 1200 C. When reactor reaches 750 C then adipic acid is added from silo. - The jacket temperature is then increased. • Step 5: Atmospheric distillation phase -At 1500 C atmospheric distillation phase starts. Vapour temperature and reflux flow must be checked. - The level of water collected in water tank is monitored. If distillation column temperature exceeds 1050 C, the reflux is started. The column temperature must be maintained at 1000 C to prevent any glycol from coming into the column. • Step 6: Partial vacuum phase -At 2000 C when 80% of water generated in reactor is removed, the vacuum pump is started. The catalyst is charged. 8
  • 9. - Jacket temperature is increased, the vent valve is closed and bleed valve is opened when pressure reaches around 1000-100 mbar. • Step 7: Full vacuum phase -Reflux to vessel is closed. Pressure reaches 30mbar. The set temperature is reduced according to steam table. -After reactor reaches 2450 C wait for 1hr. • Step 8: Sample checking phase -sample from reactor is withdrawn and checked for the specifications. It undergoes tests for viscosity, hydroxyl value and acid value. - If sample is not within specifications then required adjustments are made. - Excess glycol is removed. • Step 9: Cooling and vacuum breaking phase -The vacuum pump is stopped and vacuum is broken with nitrogen gas. - The thermic oil which is cooled using a heat exchanger is used for cooling the product. • Step 10: Transfer, cooling and packing 9
  • 10. -The product is transferred from one reactor to other where it is allowed to cool down till 800 C using cold thermic oil. -The cooled product is then packed into drums or tankers. Utilities: • Water cooling tower: Counter flow induced draft water cooling towers are used to cool the hot water from heat exchanger to a temperature of 270 C. Hot water from the system enters the water cooling tower and is distributed over the film type fills. Air is induced through the fill causing a small portion of water to evaporate. This evaporation removes heat from water thus cooling it. The cooled water is collected in the basin. Make-up water is added to adjust the evaporated water. • Water chilling unit: It is used to bring the water temperature down to 5 to 60 C. It consists of a hot water well, cold water well, compressor, condenser and a shell and tube heat exchanger for cooling of water. The refrigerant gas is first compressed and condensed which then flows through the tube side of heat exchanger. Hot water enters the shell side. Liquid refrigerant absorbs heat gets converted to gas thus cooling the water. The chilled water is then sent for cooling the thermic oil and also for condensing water vapour at distillation column. • Thermic fluid heater: 10
  • 11. The thermic fluid used for heating and cooling of reaction is Hytherm 600. The thermic fluid circulates in a coil heated by PNG inside the heater. The automatic control of the PNG is done using a solenoid valve. Hytherm 600 is heated to 2400 C by keeping the set point at 2800 C. This heated oil is then used for heating the PESOL reaction. • Vacuum: Vacuum is necessary for the distillation and stripping operations. Vacuum is created by water ring vacuum pump and steam jet ejector. Vacuum as low as 30 mbar is achieved. • Instrument air and Nitrogen gas: Instrument air is required for various on/off valves, pneumatic valves etc. It is also used to control the function of centrifugal pump in charging of raw materials. The nitrogen gas is used for inertization of the reactors and silo before and during the reaction. 11
  • 12. EQUIPMENTS DETAILS • Reaction Vessel: the plant consists of 8 reactors of varing sizes for different batch size and product. PESOL: two reactors (one for reaction and mixing and other for cooling) Its capacity is 12.45 m3 and is made up of stainless steel. It has a half coil jacket and an internal helical coil and 4 baffles. The first reactor has a pitched blade type agitator and the second reactor has a paddle type agitator. It can withstand from 3kg/cm2 pressure to full vacuum and a temperature of 3000 C. The reactor has undergone hydrotest and radiography test, and has a joint efficiency factor of 0.85. No corrosion allowance is provided. 12
  • 13. • Distillation column: It is a packed column type and has structured packings. The packings are of rasching ring type. Dimension: 600x7600(mm) • Silo: The adipic acid silo consists of unloader with nitrogen aerator. It consists of a lump breaker having a motor of 1hp and a dust extraction system with a blower having capacity of 200 m3 /hr. • Heat Exchanger: The plant has three heat exchangers. All are shell and tube type heat exchanger made of stainless steel. Two of them are used as condensers to condense water vapour from distillation tower and third one is used to cool the thermic fluid for cooling of the product. Tests for PESOL quality: • Viscosity test: Sample is taken out from the reactor, cooled and some of it is placed in the viscometer. The viscometer spindle then rotates at 60 rpm and temperature is maintained at 750 C. The viscometer displays the measured viscosity. 13
  • 14. • Acid value test: Equipments required - analytical balance, plastic cup, measuring cylinder, magnetic stirrer, burette, pipette Reagents- ethyl alcohol (96%), acetone, distilled water, 0.1 N KOH, phenolphthalein Procedure- the sample of PESOL is cooled and then mixed with a mixture of ethyl alcohol and acetone (1:1). This mixture is titrated against 0.1 N KOH solution, in presence of indicator phenolphthalein. Colour change marks the end point of the titration. 2. PRE-POLYMER  CHEMISTRY  Pre-polymer reaction – Pre-polymers are manufactured by the conversion of a stoichiometric excess of isocyanate with polyols and possibly further OH components according to the following reaction equation. R1-OH + R2-NCO  R1-O-CO-NH- R2 The large scale production of Pre-polymers takes place in discontinuous mixing vessels , whereby the isocyanate is added followed by a temperature controlled addition of polyol. To minimize secondary reactions the temperature is kept below 100 ⁰C.  During the Pre-polymer reaction, undesired reactions of the isocyanate can occur under certain conditions. i. Dimerisation of isocyanate with the formation of uretdions – 14
  • 15. Isocyanates can interact with dimer formation. This is a balanced reaction which is almost completely on the side of monomers at high temperatures. These reactions are only slightly exothermic. 2 R-NCO  Uretdions ii. Interaction of isocyanates with the formation of carbodiimides – Isocyanates can also form carbodiimides. The reaction takes place with the splitting of CO2 and without catalyst only at high temperatures which leads to the build-up of pressure in the reactor. R-NCO + OCN-R  R-N=C=N-R + CO2 iii. Reaction of carbodiimides with isocyanates with the formation of uretoimines – A further reaction of the carbodiimides with isocyanates gives rise to the formation of uretonimines, which then causes cross-linkage. As with dimer formation, uretone formation possesses no safety problems due to the low reaction enthalpy. R-N=C=N-R + R-N=C=O  Uretonimines iv. Trimerisation of isocyanates with the formation of isocyanurates – Isocyanates are subject to trimerisation to produce isocyanurates. The reaction takes place at high temperatures. It can occur at low temperatures if the reaction is catalysed by bases such as KOH or potassium carboxylate. The trimerisation reaction of multifunctional isocyanates gives rise to the production of highly branched and insoluble products. 3 R-N=C=O  Isocyanurates 15
  • 16. v. Allophanate formation through reaction of isocyanates with urethane groups – Isocyanates can form allophanates with already formed urethane groups. This reaction takes place in the absence of catalyst at high temperature. Allophanate formation is catalysed by the same nucleophiles that also accelerate the isocyanurate reaction. additionally, allophanates can react with further isocyanate groups with ring closure whereby an isocyanurate and an alcohol are produced. R-NH-COOR’ + R-N=C=O  Allophanate  PROCESS DESCRIPTION RAW MATERIAL MODE OF CHARGING REMARKS Methy Diphenyl Isocynate (MDI) Vacuum charging from drums to reactor Stored as a solid at -5 ⁰C in cold storage. Melted at 100 ⁰C in oven and charged under vacuum of 500 mbar & 50-55 ⁰C Benzyl Chloride Charged through funnel on top of the reactor Charged under atmospheric pressure Polyols + Dipropyleneglycol Vacuum charging from drums to reactor Premixing of polyols and dipropyeleneglycol required before charging material at a particular flow rate (undisclosed) Catalyst Vacuum charging from drums to reactor Reactor temperature to be maintained at 50-55 ⁰C Triphenyl Phosphate Charged through funnel on top of the reactor Material to be charged at a particular flow rate 16
  • 17. (undisclosed) Diiso nonyl phthalate Charged through funnel on top of the reactor Material to be charged at a particular flow rate (undisclosed) 2,6-di-tert-butyl-p-cresol Charged through funnel on top of the reactor Material to be charged at a particular flow rate (undisclosed)  Raw Material testing and making ready for charging – i. Raw Materials are tested for quality as per the requirements. ii. Raw Materials are issued from the Warehouse and brought to reactor using forklift and hand trolley. MDI is issued from cold storage separately.  Start up check – i. Reactor must be clean, dry and empty. ii. Bottom valve must be closed. iii. Ensure that limpet circulation heating inlet and outlet and cooling inlet and outlet valves are closed. iv. Ensure manhole is tightly closed. v. Isocynate quality is thoroughly checked for various parameters before charging it since it is very toxic and hazardous.  Operating Procedure – 17
  • 18. i. Vessel is purged with 30 mbar Nitrogen for maintaining inert atmosphere for reaction. ii. Reactor is preheated to 50 ⁰C. iii. Reactants are charged as per the table above. iv. Once charging is completed vacuum is broken by stopping the vacuum pump. v. As reaction proceeds temperature of reactor increases due to exothermic nature of majority of Pre-polymer reactions. Optimum temperature and pressure for all the Pre-polymer reactions was experimentally estimated as 70 – 75 ⁰C and 30 mbar. This is maintained by operating cooling water/chilled water supply valves. vi. Samples are taken at intervals and checked for NCO content. If found within the specified limit, the pressure of the blender reactor is increased to 1.5 kg/cm2 and discharging of the product is started.  Procedure followed in case of failures – i. In case of runaway reaction – During glycol charging the rate of rise of temperature of the reactor as well as the current flowing through the motor of the stirrer are monitored. If the temperature rises by 5 ⁰C/minute or the current increases rapidly charging of polyol must be stopped. Inhibitor solution of Benzyl Chloride is added to the reactor. If the temperature or current continues to increase the material in the reactor must be discharged immediately while keeping the safety vent open. ii. In case of failure of ventilation system – Charging of MDI or discharging of Pre-polymer products must be halted while keeping the stirrer on. 18
  • 19. iii. In case of failure of cold storage – MDI is highly toxic and its leakage in the form of vapours can cause deadly damage. Thus, it is instantaneously shifted to an adjacent cold storage location. iv. In case of choking of carbon filter – If the differential pressure across the carbon filter increases to more than 150 mbar, the carbon inside the filter must be changed and replenished. The exhausted activated carbon is then disposed as per MPCB regulations.  PRODUCTS  COSYPUR – Used for Vehicle Seats, Car Dashboards and Pillows. 19
  • 20.  ELASTOFOAM – Used for Insulations, Cushions, Car Upholstery and Pillows.  ELASTOPAN – Used in Footwear (Uses Polyether as raw material).  LUPRANATE – Used in Footwear (Uses Pesol, that is, Polyester as raw material).  QUALITY CONTROL  Test for NCO Content: i. 2 grams of sample is added to toluene (acts as a solvent) and a known quantity of dibutylamine. ii. The above solution is stirred for 15 to 30 minutes to make it homogeneous. iii. sSome dibutylamine is consumed in the above reaction. The quantity remaining is found by titration with an acid of known concentration. iv. Potentiometric Titration is performed using an Electronic Auto Titrator apparatus. v. End point of Titration is reached when there is a sudden jump in the value of the potential measured. vi. The software displays the values of the volume of acid utilized and the %NCO content in the sample.  Other Tests performed for Pre-polymers include the OH test and the Amine Test. However, these tests are performed for very selective grades and hence were not studied in depth.  EQUIPMENTS  Reaction Vessel – 20
  • 21. It is made up of stainless steel. It has a geometric volume of 13.75 m3 and an operating capacity of 10 m3 . It has 2 baffles and is designed to withstand from 5 barg pressure to full vacuum and a temperature of 190 0 C. The operating pressure ranges from 1 barg to 5 barg and the operating temperature ranges from 80 - 90 0 C. The reactor has undergone hydrotest and radiography test. It has a joint efficiency factor of 1.00. No corrosion allowance is provided.  Stirrer/Agitator – Pitched/bolted blade stirrer with variable frequency drive is used in the reactor. It has 4 impellers at the top and 2 impellers at the bottom. It operates at an RPM of 87.  Limpet Heating Coils – They are designed to withstand a pressure of 5 bar(g) while the working pressure is 3.5 bar(g). They have a pitch of 300 mm. They have a joint efficiency of 0.7 and are not provided with any corrosion allowance. They have a total heat transfer area of 11.7 m2 .  Valves – There are six types of valves used in this process. They are Globe Valve (example), Gate Valve (example), On-Off Valve (example), Three Way Valve (example), Pneumatic Valve (example) and the Diaphragm Type Valve (example).  Temperature and Pressure indicators – 21
  • 22. There are various temperature and pressure indicators in the system which transmits the values of the temperature and pressure at different points via PLC (programmable logic controller) to the PC in the control room. This permits more efficient monitoring of the temperature and pressure in the system. 3. BLENDED POLYOL 22
  • 23. PROCESS - There are four blenders in the PU plant. The blenders are used to carry out blending for various polyol systems. - Raw materials are used in various combinations to obtain various blended products which are customer specific . Raw Material Used Mode of Charging Remarks Polyol Shuttle block pump for tanks/ AODD pump for drums Requires heating before charging Catalysts Through charging funnel at 10 meter level Pre-weighing is done in carboys in the room Additives Through charging funnel at 10 meter level Pre-weighing is done in carboys in the room Blowing Agents From the bottom of the reactor with AODD pump Requires low temperature in the reactor Flame Retardants From the bottom of the reactor with AODD pump Requires low temperature in the reactor DM Water From DM water tank N/A Steps Of Reaction- 1. Raw material is tested and then is made ready for charging. 2. Raw material charging and blending - Polyol is charged from tanks or drums. - Flame retardant adition(Product Specific) - Catalyst additive charging. - Blowing agent charging. - DM water addition. 23
  • 24. 3. Sampling and corrections. Quality assurance is done to check if the product is consumer specific. 4. Filling and packing. The product is packed and transported to the customers. 24
  • 25. PRODUCTS Type Application Elastocool Appliances Elastoflex Cushions and Insulations Elastofoam Insulations Elastopan Footwear Elastopor Construction Elastopir Construction QUALITY CONTROL * Blended Polyol Rigid Type 1. Moisture Test - The sample collected is titrated with Karl Fischer reagent and dried methanol. - The reaction is handled by an automated computer programme.. - Moisture content is showed and is verified for the specific sample. 2. Cup Test - Sample is cooled and mixed with cyclopentane and is stirred till formation of foam. Cyclopentane acts as a blowing agent. - Blend is cooled and methyl diphenyl isocyanite is added. This mixture is agitated. 25
  • 26. - The foam starts rising and poked with a sharp object to notice thread formation. - Foam is left to harden and rise time and gel time are noted down. * Blended Polyol Flexible Type 1. Cup Test - Blended polyol is cooled and isocyanide is added. The mixture is agitated and foam is formed. - The foam initially rises and when co2 escapes the foam settles back. - The rising time/settling time/height are measured using ultrasonic sensors connected to the computer. The specifications are verified. 2. Cushion Test - Blended polyol and isocynaide is agitated for 6 sec at 1000-1500 RPM. - It is immediately transferred into a pneumatic mould which is pre heated to 58o c. - The mould is sealed for 5mins. After the cushion is removed it is tested using a compression machine which gives the compression for a specific force. EQUIPMENT SPECIFICATIONS - Reaction is done in a agitated reactor with torispherical head - Coil jacketed type. - MOC: Stainless Steel. 26
  • 27. - No corrosion allowance. Joint efficiency is 0.85 - Can withstand pressure of 3kgf/cm2 and temperature of 100o c. - Tests applied are Vacuum test, Radiography and Hydro test. - Agitator used is (2x3) anchor type. It has 2 turbofoil and 1 pitched blade at the bottom. The wetted parts are made of stainless steel and the non-wetted parts are made of carbon steel. - Empty weight is 4000kg. - Reaction temperature is 70o c. 4. SAFETY *SAFETY AND POLLUTION CONTROL 27
  • 28. Safety cannot be compromised by any of the employees. BASF is having a Full-flegged Saftey Department with qualified safety officers in a safety committee . Meetings are held regularly and various problems are discussed. Recommendations are circulated to the concerned departments. - Adequate safety budgets are made and company has a constant pattern of expenditure on safety related issues. - Accidents and incidents are investigated and records are kept. All the employees are informed about the cause of the accident - Internal safety inspections and external safety audits are done frequently. - Safety education and training are given to each employee in detail. - Awareness of safety is displayed through notice boards and pamphlets and also accident free days are displayed. - Hazard identification and control measures are carried out once a month. - Work permit system exists in the factory. Hot work, confined space entry, digging snd general permits are available and are followed strictly. - Waste disposal system of various type of water is also available. - Mock drills are conducted once in six months - Fire prevention equipments like hydrant water systems and fire water pumps has been used to ensure safety of every corner of the plant. - BASF has set an occupational health center (OHC) in the premises and also houses full time doctors and an ambulance is always kept on stand by. 28
  • 29. - As a part of safety program all the pipe lines are color coded as per international norms. Fluid Color Code Cooling water Green Nitrogen Yellow Instrument Air Sky blue with blue band Vacuum Sky blue Fire Hydrant Red Process Air Sky blue with silver band Waste Water Green with blue and orange band Process Water Green with white band Vent Light brown - DCC(Disaster Control Centre) is a special program initiated by the chairperson of BASF, For the safety of its employees at any time and hour of the day. It is a special team spread confined to only Mumbai currently but aims at every part of the country where BASF has its mark. Let it be a mass riot or a major accident, the DCC panel would get you out of it once you inform them about the situation. 29
  • 30. *PERSONAL PROTECTIVE EQUIPMENT SR.NO PROTECTION TYPE OF APPLIANCES 1 Head Safety helmets 2 Eye Safety goggles, Welder’s goggles, Chipper’s goggles 3 Face Face shields, Face masks 4 Hands Specific hand gloves 5 Body Full body aprons, Boiler suit 6 Ear Ear plug 7 Foot and Leg Safety shoes 8 Respiratory Face masks with filter, Gas masks with canisters. 9 Protection from falling Safety belt 5. MATERIAL SAFETY Chemical Hazards Protection 30
  • 31. Diethylene Glycol Acute oral toxicity, acute dermal toxicity, slightly flammable in presence of open flames and sparks Use adequate PPE, in case of fire use dry chemical powder or foam but not water jet. Monoethylene Glycol Acute toxicity of vapour, carcinogenic effects, mutagenic effects, acute oral toxicity Adequate PPE required while handling, must be kept away from strong acids and bases, water jet extinguisher must not be used to put out fire Adipic Acid May cause eye irritation, coughing, sneezing. On ingestion may cause diarrhoea Proper PPE must be used Tetrahydrofurane (by product of reaction) Highly flammable, hazardous if ingested or comes in direct contact with skin It is removed as a distillate during vacuum phase 1, 4- dioxane Hazardous to aquatic life, poses problem in water treatment Removed as distillate in ambient pressure phase Benzoyl Chloride Harmful if inhaled, irritant to eyes, toxic to aquatic animals Adequate PPE must be used, extreme heat must be avoided 2,6-ditert butyl-p- cresol Toxic to aquatic animals Avoid heat and accidental leakage or spillage into drains Di-propylene glycol No hazard PPE is necessary Triphenyl phosphate Toxic to aquatic organisms, irritant to skin and Adequate PPE, avoid spillage and leakage 31
  • 32. respiratory system Elastopan/ Elastocool Harmful is inhaled or ingested PPE necessary Elastopor Dangerous for ozone layer Do not let spillage or leakage to enter drains Elastoflex Harmful to aquatic organisms High spillage precautions must be taken Lupraphen No hazard General PPE necessary 6. HAZARD IDENTIFICATION AND PREVENTION: Hazard Identification is the process of identifying hazards in order to plan for, avoid, or mitigate their impacts. Hazard identification is an important step in risk assessment and risk management. BASF with the aim of ensuring and continuing to develop safe working conditions strictly follows issuing of safety work permit and concept of yellow card. Certain safeguards that normally protect the worker may have to be removed when repair or maintenance work is performed. When this occurs, the hazards involved need to be identified and a safe work system developed to eliminate or control these hazards. A safe work permit is a written record that authorizes specific work, at a specific work location, for a specific time period. Permits are used for controlling and co-ordinating work to establish and maintain safe working conditions. They ensure that all foreseeable hazards have been considered and that the 32
  • 33. appropriate precautions are defined and carried out in the correct sequence. There are four basic type of work permit available in the plant: general work permit, confined Space work permit, height work permit and hot work permit. During the internship I learnt to fill, document and maintain the safe work permits, thus gaining knowledge about hazard identification and prevention. SAFETY MEETING: Safety meetings are organized every month to discuss the production issues, reported yellow cards and action taken against the complaint and follow ups, safety trainings conducted, changes (addition/ deletion) in the plant equipments, etc. The meeting I attended started with the declaration of remarkable production achieved in the month of May. The workers were motivated and everyone was thanked for their contribution. The meeting proceeded to discuss two major issues, lack of man power and space limitation for storage of materials. Next all the yellow cards reported were discussed along with the appropriate action taken. Pending issues of previous meeting were addressed and their status was discussed. The emergency numbers, assembly point details and safety pledge were revised. 7. ETP-EFFULENT TREATMENT PLANT Effluent generated from the plants is collected in the effluent collection pits placed across the site and then pumped to the ETP for treatment. Effluent is treated in three stages 1. Primary treatment (physio- chemical treatment) 2. Secondary treatment ( Biological treatment) - Anaerobic treatment. 33
  • 34. - Aerobic treatment. 3. Tertiary treatment. • Primary Treatment - Removal of oil and grease is done. - The suspended solids are removed. - The equalization and neutralization of effluent is done. • Secondary Treatment - Removal of COD and BOD and ammonical nitrogen is done. - Aeration tanks are provided. - Microbes decompose organic matter in presence of air. - Excess sludge is wasted and thickened in the decanter. • Anaerobic Treatment - Effluent water of high COD comes here. - Soda ash is used for neutralization. - PH is maintained at 11. - Anaerobic reactor is a fluidized bed of sand. - Sand is supported by rock at bottom. - Feed enters from the bottom. - The filtrate is fed to the aerobic reactor. 34
  • 35. • Aerobic Treatment - The treatment takes place due to the activity of bacteria in presence of oxygen. - PH is maintained at 9-10. - There are two tanks used for the process. In the first tank batch is made ready by adding chemicals and in other tank only effluent water is present. - The effluent is pumped to a first stage clarifier. - Solid waste will settle down and clear water will pass through. - Clear liquid is fed to the aeration tank. - Here the COD decreases from 8000 to 800. - Following materials are added to the aeration tank for developing bacteria. Food, Di ammonium Phosphate, Urea and Starch. - Water is now fed to second stage clarifier. - In this clarifier there is one agitator present which keeps moving slowly. - The pure product is fed to the Poly Aluminum Tank. • Tertiary treatment - Fenton treatment is given to the effluent from secondary treatment. - Ferrous sulphate and hydrogen peroxide are added. 35
  • 36. - Effluent is then treated with lime. - Clarified effluent is then sent to sand and activated carbon filter. - Carbon and sand acts as an absorbent and absorb impurities. - The Treated effluent is finally drained into the MIDC drain through V-notch chamber. 8. REACTOR EFFECTIVENESS  ABOUT THE SOFTWARE  The Software was developed using MS Excel.  A database of possible reasons for delay in batch time of the reactor was created.  Each possible reason in the database created above had a rate of loss of tonnage (of product) associated with it.  Another database containing all the products manufactured in every reactor and the theoretically calculated batch time for each of these products was maintained.  APPLICATION 36
  • 37.  Weight indicators on each reactor continuously transmitted the measured values to a PC in the Control Room of the Plant.  A plot of Weight v/s Time was generated by the PC.  This plot was carefully monitored and the actual batch time was noted along with all those time periods wherein the reactor was not utilized (indicated by constant weight of the reactor).  By referring to the company logbook, the aforementioned delays were attributed to the pre-decided reasons from the database.  Thus, for every product (every new batch) the departure of actual batch time from the estimated batch time was accounted for and the Reactor Effectiveness was obtained.  A bar chart of %Effectiveness v/s Batch Number and %Effectiveness v/s Month were then simulated for company records. 9. SUGGESTIONS - Conveyor Belts can be used to transport drums for charging and discharging thus reducing the time required and increasing the efficiency. Automated filling 37
  • 38. machines can be used instead of manual charging. Fork lift related accidents will reduce because of lesser frequency of its usage - In pesol production, MEG and DEG are first charged into a smaller vessel and then charged into the reactor. Time is wasted because the amount of DEG and MEG required for a single batch far exceeds than what the tank can store. Thus increasing the capacity of the tank or introducing another tank to meet the requirements of the reaction. - Pesol required for pre-polymers and blending is imported externally. The pesol produced in the plant is directly sold. Pesol can be produced in the plant and directly charged into reactors or stored in the storage tanks. By doing so the time taken for charging will be lesser than that of charging through drums. Constant supply of pesol will also be available at all times. Cost and batch effectiveness increases. - Delay due to manpower is the biggest issue for blending polyols. So keeping 2- 3 contractors only for charging and discharging of polyols will increase the effectiveness of the procress. Thus more batches can be produced and the revenue of the company will increase. CH 3.CONCLUSION 38
  • 39. In conclusion, there were many things that I learned and experienced during the four weeks of my industrial training at BASF India LTD, Thane site. The whole industrial training was interesting, challenging and application oriented. Through this training I was able to gain more insight and more comprehensive understanding about the real industrial working conditions and practices. This training period has also provided me with opportunities to develop and improve my soft and functional skills. All of this valuable information and knowledge were not only acquired through the direct involvements in the tasks given but also by other aspects of training such as work observation of seniors and also through logical and instructive interaction with them. It is known for a fact that the industrial training program is the best way to prepare a student for facing a real working life and I completely agree with it. As a result of this, I have gained immense confidence to enter the employment world and build my future career. 39
  • 40. CH 4.COMPANY PROFILE 1. HISTORY OF BASF BASF GROUP:AT A GLANCE We are the world’s leading chemical company: The Chemical Company. Nearly 111,000 employees work at the BASF Group. Our broad portfolio is arranged into six segments: Chemicals, Plastics , Performance Products, Functional Solutions, Agricultural Solutions and Oil & Gas. -Markets and sites BASF has subsidiaries in almost eighty countries and supplies products to a large number of business partners in every part of the world. In 2011, we achieved 53% of our sales with customers in Europe, of which 30% were in oil&gas. In addition 19% sales were generated in North America and 20% sales in Asia Pacific. Our Verbund site in Ludwigshafen is the largest integrated chemical complex in the world. Organization of the BASF Group - BASF’s six business segments contain 15 divisions which bears the operational responsibility and manage our 70 global and regional business units. The divisions develop strategies for the business units and are organized according to products. 40
  • 41. - The regional divisions contribute to the local development of our business and help to exploit market potential. They are also responsible for optimization of infrastructure for our business. For financial reporting purposes, our divisions are grouped into regions. - Three central division and 5 corporate departments provide group wide services such as finance, investor relations, communications, human resource, research, engineering and management. BASF Group- Strategy and Values. - BASF aims to strengthen it’s position in the world as the world’s leading chemical company. We describe this in our” We create chemistry” strategy, which we presented in November 2011. This strategy is based on our success in recent years and define ambitious goals for our future. BASF Purpose- ‘ We create chemistry for a sustainable future’. BASF- Strategic Principle. -We add value as one company. 41
  • 42. - We innovate to make our customers more successful. - We derive sustainable solutions. - We form the best team 2. HISTORY IN INDIA. Establishing a strong India presence. BASF India Ltd was first incorporated as R.A. Cole Private Limited. It was first involved in the production of Expandable Polystyrene. With this BASF took first step into the manufacturing . Over the years BASF India’s product portfolio steadily grew. Because of this the first production site was opened in Thane, India. In 1986 BASF was listed on the Bombay Stock Exchange & was listed on the National Stock Exchange in 1995. The Manglore site which was opened in 1996 is currently the largest manufacturing site on India and South Asia. • Thane site- Plastic Chemicals. - BASF India Limited started operations at the Thane site in Navi Mumbai 1967. It is the first production site of the company in India and currently focuses on the production of engineering plastics, Polyurethanes , Performance chemicals, care chemicals, construction chemicals, dispersions, pigments and styropor. 42
  • 43. - This site houses five plants and technical application centre’s for textile, leather , pharma, engineering plastics and polyurethanes. 43
  • 44. REFRENECES - www.india.basf.com - Process manuals from the plants - www.google.com - Material safety data sheet 44