Understanding & Study of the Resin Production Process

Vocational Industrial Training Project Presentation

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Under the guidance of:E r. A b h i s h e k S h a r ma P r e s e n t e d b y: Jayant Kushwaha P a w a n k r. F u l f a k i r F i n a l y e a r, c h e mi c a l E n g g . D r. B . R . A mb e d k a r n i t , J a l a n d h a r ( P u n j a b )

ABOUT SRF
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SRF is a multi business entity engaged in the manufacture of Chemical based industrial intermediates. Today its business portfolio covers Technical Textiles, Chemicals, Packaging films and Engineering Plastics. SRF Limited is a USD 760M Industrial group. From its inception in 1974, SRF today operates from eight plant locations in India and abroad. Packaging Film Business (PFB) involves the production of Bi-axially Oriented Poly Ethylene Terephthalat (BOPET) or Polyester Film.

INTRODUCTION TO RESIN PLANT

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In Resin Plant, PET Resins (Chips of PET Polymer) are made from

which the packaging films are made. In Resin Plant, Batch Polymerization (BP) & Continuous Polymerization (CP) both are running simultaneously. At full capacity CP runs at 150 tons/day and BP runs at 20 tons/day. Polyester or Poly Ethylene Terephthalat (short PES or PET), is produced in two chemical steps. The raw material, 1 mol of Pure Terephthalic Acid (PTA) reacts with 2 mol of Mono Ethylene Glycol (MEG or simply EG) at raised temperature (240C 260C) to form Bis (2-Hydroxyethyl) Terephthalat (BHET) also named Di-glycol Terephthalat (DGT).

INTRODUCTION (continued)
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This first step of reaction is called esterification and can be

carried out at different pressures. In this plant MEG or EG (monomer) is fed at lower molecular ratio than 2. Due to which the product obtained, the monomer is a mixture of monomer, pre-polymer & nonreacted PTA and EG. In the second step the monomer is poly-condensed by the use of a catalyst (Sb2O3) & heat stabilizer at Vacuum and temperature between 270C - 285C.

RAW MATERIAL FOR RESIN PLANT

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Pure Terephthalic Acid (PTA) PTA is a white crystalline free flowing powder. It is delivered in tank trucks, container or 1 ton flexible big bags which are kept at discharge station. These big bags are lifted to the top of the PTA feeding tank by an elevator. These bags are then emptied directly into the PTA feeding tank.

RAW MATERIAL FOR RESIN PLANT

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Mono-Ethylene Glycol (MEG

or EG)

MEG is a clear liquid, mixable with water. It is delivered in tank trucks or railway tank wagons. After laboratory check, the MEG is pumped into the storage tank. From there the MEG is automatically pumped to the consumers in the poly-building.

OTHER CHEMICALS USED IN RESIN PLANT

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Di-Ethylene Glycol (DEG)

Catalyst:- Antimony Tri-Oxide (Sb2O3)

Poly-Phosphoric Acid Colour Additive RED (RG)

Colour Additive BLUE (RH)

Silica Magnesium Acetate

Heat Transfer Fluids (HTF): Therminol 66 Therminol VP-1

Chemistry of Polyesters (PET)

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Polyesters are highly polymeric substances, the individual units of macromolecules are connected by the ester groups.
O CO

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Esterification Reaction:

n HOOC COOH + (n+1) HOCH2CH2OH

n HOCH2CH2OOC OOC-CH2CH2OH + 2n H2O Condensation Reaction: HOCH2CH2OOC -[-COOCH2CH2OOC -]-(n)COOCH2OH + HOCH2CH2OOC OOC-CH2OH HOCH2CH2OH + HOCH2CH2OOC -[-COOCH2CH2OOC -]-(n+1)COOCH2OH

PROCESS DESCRIPTION
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Polyester or Poly Ethylene Terephthalat (short PES or PET), is produced in two chemical steps. The raw material, 1 mol of Pure Terephthalic Acid (PTA) reacts with 2 mol of Mono Ethylene Glycol (MEG or simply EG) at raised temperature (240C - 260C) to form Di-glycol Terephthalat (DGT). The production plant consists of the following main process steps:1) Paste Making 2) Esterification with Pre-polymerization 3) Polycondensation 4) Chips Production

PASTE MAKING
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o The paste making system for both CP & BP are located

o
o

below the PTA feeding tank. This tank has double cone and serves both paste mixing system for CP & BP. All raw material PTA, MEG, DEG are mixed to form a paste which is feed to the esterification. The paste is white slurry. Its viscosity is depending on mole ratio, form and size distribution of PTA crystal. Mixing of all raw material including colorful additives is done in the paste mixer at atmospheric pressure, but with nitrogen purge. The mole ratio of EG/PTA, is determined according to the source and type of PTA and other operating factors.

CATALYST PREPARATION SYSTEM

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EG moistured Antimony Trioxide is used as poly-

condensation catalyst. The catalyst is dissolved in virgin Ethylene Glycol at a temperature of 130 to 140C. The conc. of catalyst in the solution should be 1 to max 1.5%. The catalyst is poured into the dissolving vessel. The catalyst solution is dosed into the paste mixer according to the PTA feed. Normal feed is 270ppm Sb on polymer.

ESTERIFICATION
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Esterification and pre-polymerization takes place in UPR (Universal Polymerization Reactor). UPR have 3 zones: 1. The ester 1 zone 2. The ester 2 zone 3. The prepoly zone In the esterification zones the raw materials are reacting and forming the monomer DGT. The esterification reaction is carried out in two reaction zones, one at the top of the other and at a product temperature of approx. 255C to 262C and overpressure.

ESTERIFICATION (continued)
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The first reaction zone is equipped with an inbuilt heat exchanger and an agitator that works as a circulation pump. That agitator circulates the product through the heat exchanger coils and mix the new PTA/EG slurry with the reacted monomer. The second reaction zone serves for further reaction. In both zones reaction water and EG are Evaporated. In the first zone, which is operated at approx 2 to 2.5 bars overpressure, the large amount of heat, which is required to heat the raw materials and to evaporate water and EG is transferred to the product.

ESTERIFICATION (continued)
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The monomer of first esterification zone is feed to the second zone by pressure difference. The second zone is operated at a lower pressure, preferably at 0.4 to 0.7 bar overpressure. The product operating temperature is about 260C to 262C. The product transfer from 2nd ester zone to the Prepoly zone, which is the lower part of the UPR reactor is achieved by the difference in operating pressure. The ester 2 operates at 0.4 to 0.7 bar & the Prepoly zone at a vacuum of 25 to 40 mbar. In this plant a monomer connection from ester 2 to the batch plant is foreseen. By a mass flow meter and control valve a certain quantity of monomer can be continuously taken out and fed to the esterification reactor of the batch plant.

PROCESS COLUMN & STRIPPING COLUMN

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o The Process vapor of esterification is led to a Process

Column to separate water from EG. o The column top is operated at atmospheric pressure and has a re-boiler at its lower end. o At the top of the column, the low boilers like water & aldehydes are bleed off. Whereas the high boilers, EG & some water leave the column at the bottom. o The condensed reaction water is led to a stripping column in order to reduce the BOD & COD values. The water is flowing from top to bottom whereas air is passed in counter current.

POLYCONDENSATION
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In Polycondensation, the remaining excess EG is evaporated, which results in the formation of long molecular chains of polymer with the required properties of the Polyester. The reaction takes place in two steps at raised temperatures, 270C to 285C and vacuum between 40 and 0.5 mbar. The first step of Polycondensation is made in the Prepoly reactor that is installed in the lower part of the UPR reactor. This part of the reactor is a combination of flasher and pre-polymerizer in which up to 95% of the excess EG is evaporated. From the outlet of Prepoly the polymer flows to a polymer gear pump that transports the pre-polymer to the Finisher. A viscometer is installed in the polymer line that measures continuously the viscosity of the polymer that is fed to the Finisher. In the Finisher the pre-polymer is brought to its final viscosity and properties.

FINISHER
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o The FINISHER is a horizontal jacketed heated vessel with a o o

o o

horizontal, ex-centric shaft less cage agitator with disks. The speed of the shaft can be varied between from 0.5 to 5 rpm. A standard speed is 2 to 3 rpm. In the product inlet zone, where the viscosity is relatively low, the pre-polymer is moved upwards by cups mounted to the disk rings. While rotating to the top, the cups are emptied and the polymer flows down, forming films & strings. The internals of the reactor are designed to work as a cascade to avoid remixing of the polymer.

CHIPS PRODUCTION
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Behind the polymer filter, the polymer flows to the two die (casting) heads of the underwater (Reiter Supply). The polymer is pressed through the holes of the die plate, forming wires of approx. 2mm to 3mm diameter. Below the spinnerets the polymer wires are cooled down on the special stainless steel cooling board, they solidify and are led to the cutter. In the cutter the wires are cut to length. Solidification and cutting is done under water to cool the polymer and to avoid sticking.

CHIPS PRODUCTION (continued)

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The mixture of cooling water and chips, coming from the cutter is pre-separated in special screen. A part of the water flows back to the water tank of the cutting system. The chips and remaining water is passing a pre-dryer, centrifuge in the centrifuge the remaining water is separated from the chips and also flows to the water tank. The chips are falling on a screen that separates uncut or long parts.

STABILIZER PREPARATION SYSTEM

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Poly Phosphoric acid is used as heat stabilizer.

The stabilizer is a viscous liquid that is dissolved in virgin

EG at a temperature of 30 to 40C. The conc. of stabilizer in the solution should be 1 to 1.5%. Normally the concentration of active stabilizer in the paste is around 82 to 84%. The stabilizer solution is dosed into the monomer after esterification. Normal feed is 10 to 15ppm phosphorous on polymer.

SILICA PREPARATION SYSTEM

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Silica slurry is prepared using silica and virgin glycol.

The final conc. (ppm) of silica slurry to be prepared is first

decided, then measured quantity of virgin EG is taken in preparation vessel. Measured quantity of silica powder is then added to preparation vessel over a period of 2-3 hrs. The slurry is then passed through a pearl mill which crushes the agglomerates. Then this slurry is transferred to an adjustment vessel where the conc. is measured & glycol is added to adjust the concentration.

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