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Contents

1. HEATING TRANSFER MEDIA (HTM)..........................................................................................2


1.1. HTM SYSTEM.....................................................................................................................3
1.1.1. Primary HTM system.................................................................................................3
1.1.2. Secondary HTM system.............................................................................................3
1.2. HTM used..........................................................................................................................3
1.2.1. SANTOTHERM............................................................................................................3
1.2.1.1. Properties...............................................................................................................4
1.2.1.2. Applications............................................................................................................4
1.2.1.3. Process Description................................................................................................5
1.2.1.4. Combustion............................................................................................................5
1.2.1.5. Pilot Flame..............................................................................................................5
1.2.1.6. HFO CYCLE..............................................................................................................5
1.2.1.7. HTM Heating Process.............................................................................................6
1.2.2. DOWTHERM..................................................................................................................6
1.2.2.1. Properties...............................................................................................................6
1.2.2.2. DOWTHERM EVAPORATORS..................................................................................7
1.3. EQUIPMENTS.....................................................................................................................7
1.3.1. Furnace......................................................................................................................7
1.3.2. Conduction.................................................................................................................7
1.3.3. Convection.................................................................................................................7
1.3.4. Radiation....................................................................................................................7
1.3.5. Blower........................................................................................................................7
1.3.6. Economizer................................................................................................................8
1.3.7. Atomizer....................................................................................................................8
1.3.8. Damper......................................................................................................................8
1.3.9. Stack (Chimney).........................................................................................................8
1.3.10. Pre-Heater (HFO)....................................................................................................8
1.3.11. Expansion Vessel....................................................................................................8
2. Paste Preparation....................................................................................................................9
AREA 1817.......................................................................................................................................9
2.1. Description......................................................................................................................10
2.1.1. Day Silo (1817-T01)..................................................................................................10
2.1.2. Paste preparation vessel (1817-v01).......................................................................11
2.1.3. Parameters...............................................................................................................11
3. Esterification..........................................................................................................................12
3.1. DESCRIPTION...................................................................................................................13
3.1.1. ESterification-I (1829-R01).......................................................................................13
3.1.2. ESTERification-II (1829-R02)....................................................................................14
3.1.3. Level TransmittSers..................................................................................................14
4. PROCESS COLUMN.................................................................................................................16
4.1. PROCESS COLUMN Introduction.....................................................................................17
4.2. Difficulties in distillation:.................................................................................................18
4.2.1. Foaming...................................................................................................................18
4.2.2. Entrainment.............................................................................................................18
4.2.3. Weeping/Dumping..................................................................................................18
4.2.4. Flooding...................................................................................................................18
4.3. Types of trays used in tray columns................................................................................19
4.3.1. Bubble Cap Trays.....................................................................................................19
4.3.2. Sieve Trays...............................................................................................................19
4.3.3. Valve Trays...............................................................................................................19
Process Description...............................................................................................................21
5. POLYCONDENSATION............................................................................................................22
5.1. Introduction....................................................................................................................23
5.2. Process Description.........................................................................................................23
5.2.1. ES-2 TO PPR..............................................................................................................23
5.2.2. PPR TO DRR..............................................................................................................23
6. Additives used in the production of PET...............................................................................25
6.1. Antimony Tri-acetate, Catalyst.......................................................................................26
6.1.1. Preparation..............................................................................................................26
6.1.2. Structure..................................................................................................................26
6.1.3. Properties................................................................................................................27
6.2. Titanium Dioxide, Color Dulling Agent........................................................................27
6.2.1. Properties................................................................................................................27
6.2.2. PROCESS DESCRIPTION................................................................................................28
6.2.3. Applications.............................................................................................................29
7. EG CIRCULATION AND VACUUM GENERATION.....................................................................30
7.1. ETHYLENE GLYCOL CIRCULATION:......................................................................................31
7.1.1. Immersion Vessel........................................................................................................31
7.1.2. Spent EG Coolers.........................................................................................................31
7.2. Jet System...........................................................................................................................32
7.2.1. GENERAL APPLICATIONS:.........................................................................................32
7.3. Barometric Leg and its Applications in a vacuum system:.................................................32
7.3.1. INSTALLATION AND CONSIDERATIONS FOR BAROMETRIC LEG:....................................33
7.4. Ejectors:..............................................................................................................................33
7.4.1. Components of an Ejectors.........................................................................................34
7.4.2. Multiple Ejectors Application:.....................................................................................35
7.5. Liquid Ring Vacuum Pump..................................................................................................35
7.5.1. Operation of Liquid Ring Vacuum Pump in Jet System at IFL-III.....................................36
7.6. Knock Out Drum:................................................................................................................37
7.6.1. Design Feature:...........................................................................................................37
PROCESS FLOW DIAGRAM OF PET
1. HEATING TRANSFER MEDIA
(HTM)
AREA 3008
1.1. HTM SYSTEM
There are two HTM systems:

1. Primary HTM System


2. Secondary HTM System

1.1.1. Primary HTM system


The Primary HTM System provides the total heat requirement of the Polycondensation and
spinning plant by liquid heat transfer media.

Inorder to achieve this, the liquid HTM is heated in the HTM furnaces 3008-F11/F12/F13 to a
constant feed temperature of 3250C. The required heat is generated by combustion of fuel oil
or fuel gas.

The primary HTM pumps 3008-P11/P12/P13/P14 are used to circulate the HTM via the primary
heating circuit. There are total three furnace at Polymer Process-III among which two are in
operation and one is at standby. Capacity of each furnace is 11528 kW (41.5GJ/hr).

1.1.2. Secondary HTM system


HTM circulation in the polymer building through HTM Pumps located at 8.0 meters and 16
meters is called the Secondary HTM System.

HTM from the supply header is distributed into several loops including Santotherm and
Dowtherm cycles.

1.2. HTM USED


HTM stands for "heat transfer media". It is used as a source of heating in different units of
plants. As the both esterification / poly-condensation reactions are endothermic so large
amount of heat is required to bring the reactors to the reaction temperature (> 250 C). For this
purpose, two phases of heat transfer are used:

1. Santotherm (Liquid Phase)


2. Dowtherm (Vapor Phase)
1.2.1. SANTOTHERM
Santotherm is partially hydrogenated terphenyl in liquid form. The trade name of Santotherm is
Thermoinal-66. It is used for primary heating. It is heated in coils of furnace by natural gas. Then
at temperature of 325ᵒC is sent to reactors where it is used to heat secondary heating media
after that secondary loops and exhaust return at temperature of 270ᵒC and heated again.

1.2.1.1. Properties
Santotherm is the world’s most popular high temperature, liquid-phase heat transfer fluid. It is
pumpable at low temperatures and offers high-temperature thermal stability.

Average Molecular Weight 240 C


Density at 200o C 1002 kg/m3
Pour Point < -10 C
Flash Point 170 C
Boiling Point 340 C
Auto Ignition Temperature 380 C
Color Clear, Pale yellow liquid
Specific Gravity 1.012
150 m
Maximum Moisture Content

1.2.1.2. Applications
Santotherm is produced by Eastman Chemical Company.

 It is used in a variety of applications, including:


 Hydrocarbon processing (oil and gas, refining, asphalt, gas-to-liquid, etc.).
 Alternative Energy and technologies (concentrated solar power, biofuel, organic Rankine
cycle, desalination, etc.).
 Plastics processing.
 Chemical processing (pharmaceutical, environmental test chambers, etc.).
 Food and beverage processing.
 Heat transfer system maintenance.
1.2.1.3. Process Description
Furnace is used to heat HTM (Santotherm). Currently advanced technology furnace having 5
coils is in operation working on coil system. HTM is in coils of furnace. It has three passes
(primary, secondary and tertiary) for flue gas. Duel nozzles are used for HFO and natural gas
and duel fuel burners are installed vertically at the top of furnace. At plant site, furnace is in
continuous operation it only stops during shutdown.

1.2.1.4. Combustion
To increase temperature of Santotherm in furnace we require combustion. Combustion occurs
by three important elements.

1.2.1.5. Pilot Flame


A pilot light is a small gas flame, usually natural gas or liquefied petroleum gas, which serves as
an ignition source for a more powerful gas burner. Ignition start from electrode sparking and
flame eye detects the pilot flame. Then LPG (liquefied petroleum gas) which is in cylinder is
used to further ignite spark.

1.2.1.6. HFO CYCLE


HFO is pumped towards the furnace with the help of low pressure pumps 3008-P22/P23. It has
a heating system in its shell which pre-heats HFO to ~100oC before being pumped by low
pressure pumps which increase its pressure to ~9 bars. It than goes to the suction of high
pressure pumps 3008-P18/P30 which increase the pressure energy to ~35 bars. The discharge
passes through a pre-heater which uses 25 bar steam as a heating medium. HFO then enters
the furnace and it is atomized with the help of an atomizer.

It is important to pre-heat the HFO, otherwise, cool HFO will disturb the temperature profile of
the furnace. Thus, disturbing the whole process.
1.2.1.7. HTM Heating Process
HFO and natural gas are used as fuel. Force draft fans are used to send air to the top of furnace
by taking air from the atmosphere. Discharge of FD fans goes to economizer having shell and
tube arrangement. Air enters at temperature ~49ᵒC in the economizer at the shell side while
flue gases from furnace enters at temperature ~315-330ᵒC in tube side. Economizer trips when
the temperature rises up to 420ᵒC. The flue gas after circulating through economizer enters in
stack at temperature of 200ᵒC. Flue gases contains maximum amount of CO2 which goes to
vent through stack at height of 35m. The discharged air from economizer went to the furnace
where Santotherm is heated and discharged from the furnace at 325ᵒC. HTM from furnace is
then divided into secondary loops for use in different reactors and evaporators.

1.2.2. DOWTHERM
Diphenyl/Diphenylether is used as dowtherm. It is secondary heating media which is used in
vapor form. It is heated by primary HTM coming from furnaces then It is used to heat reaction
vessels (ES-1, ES-2, PP-1, PP-2 etc.) by staying in the jacket of these vessels.

1.2.2.1. Properties
Dowtherm have low boiling point around 2500C-2600C and hence used as secondary HTM in
vapor form.

Average Molecular Weight 165.7 C

Density at 200 C 1062 kg/m3

Freezing Point 12.3 C

Flash Point 115 C

Boiling Point 258 C

Ignition Temperature in Air 615 C

1.2.2.2. DOWTHERM EVAPORATORS


In Dowtherm evaporators 8181-E01, 8383-E01 HTM (Santotherm) is used in coils as liquid and
in vessel boundaries as vapors. Santotherm is used in the primary cycle where it is heated in the
furnace. This Santotherm then moves in coils to a secondary cycle where it is used to convert
Dowtherm into vapor state in an evaporator. This Dowtherm is used in the linings of the vessel
to maintain the temperature of the mixture and to make sure efficient heat transfer
throughout. All reactors heating through coils (ES-l, ES-ll and PP-l) and jacket (DRR) and product
transfer line heating is done through secondary HTM pumps.

1.3. EQUIPMENTS

1.3.1. Furnace
A furnace is a device used for high-temperature heating. The heat energy to fuel a furnace may
be supplied directly by fuel combustion by electricity such as the electric arc furnace or through
induction heating in induction furnace.

Furnace is there to heat the santotherm which is our HTM to a temperature of 325oC from
270oC. The Furnace is operated with Heavy Furnace Oil (HFO) or another source of fuel for the
Furnace is natural Gas, Natural Gas is being provided by Utility Department at the required
temperature and Pressure. HTM is heated with Conduction, Convection and Radiation mode of
heat transfer.

1.3.2. Conduction
This Mode of heat transfer is effective in those coils which are in direct contact with the burner.

1.3.3. Convection
This mode is effective when the flue gases moves in bulk due to density and momentum
difference.

1.3.4. Radiation
This mode is effective in the whole body of furnace.

1.3.5. Blower
Blower is used to supply air for combustion it converts pressure head to kinetic head and
increases the flow rate for effective combustion. There are three blowers 3008-K11/K12/K13
from which air is taken from atmosphere for the three furnaces separately.

1.3.6. Economizer
Economizer 3008-E11/E12/E13 is also a pre-heater that uses the flue gases and pre-heat the air
coming from blower before providing to the furnace in order to have the maximum utilization
of waste heat.
1.3.7. Atomizer
It is an instrument for reducing a liquid to spray or vapor for disinfecting, cooling, medical use
or perfume spraying. Atomizer works on venturi effect which converts jet of fuel to fine spray in
order to increase effective surface are throughout furnace.

1.3.8. Damper
Natural gas and warm air is added to damper that maintains a specific air to fuel ratio
depending on oxygen contents for maximum oxidizing flame. Until the reducing flame will
cause more toxic emissions that needs to be processed before emitting into the air.

1.3.9. Stack (Chimney)


It is a structure that provides ventilation for hot flue gases or smoke from a boiler, stove,
furnace or fireplace to the outside atmosphere.

Stack has variable area to reduce emission of solid contents and increase kinetic head of gases.
It is used for emission of flue gases after economizer.

1.3.10. Pre-Heater (HFO)


Pre-Heater is used to maximize the efficiency of the process. The purpose of preheater is to
preheat HFO by 6 bar steam followed by 25 bar. It helps to save fuel for maximum heat
economy.

1.3.11. Expansion Vessel


It is used to absorb the pressure fluctuations. Here low boil HTM is recovered. Level of vessel is
maintained at 50%. Stability of expansion vessel is 95% and about 5% annually losses are
calculated. 1 bar nitrogen is given to vessel. It is basically a storage tank to maintain head.
2. Paste Preparation
AREA 1817
2.1. DESCRIPTION
In this stage all the essential components are mixed in specific amounts. A paste is formed
which is then sent to main reaction vessels. Following ingredients are added into this vessel:

 MEG
 PTA
 Catalyst

PTA and MEG are charged in a specific mole ratio:

Moles of EG
Mole Ratio= =1.16
Moles of PTA

Essentially no serious reaction is occurring in the paste preparation chamber that is why the
ratio is set as 1.16. The ratio highly depends on the production rate of plant. In the paste
preparation vessel mostly EGR and SEG are added to run the process economically. However,
fresh MEG is also added to maintain a certain purity level. Fresh MEG is 99.9% pure.
Flowmeters carefully control the flow rates of EG entering the vessel.

1. Increase Effect

If this ratio increases, then acid number starts to decrease.

This increases the formation of DEG due to excess of EG. These high contents of DEG cause the
formation of weak filaments. On the other side IV of the tank decrease which results in the
increase of color B.

2. Decrease Effect

If mole ratio starts coming low it means that the PTA MEG Paste slurry has become thick and its
density has increased. Now the agitator has to stirr thick slurry motor load increases and pump
load also increases. Temperature will also rise. Discharge pressure will also increase as the
amperes of Pumps increases. This decrease in mole ratio also causes the incomplete reaction
due to which, required degree of polymersiation, cannot be achieved. This favors the increase
of carry overs in the tank.

2.1.1. Day Silo (1817-T01)


PTA is added into the paste preparation vessel from the day silo. A rotary feeder directs
PTA to the Shank System, a motor operated assembly. Shank System is an arrangement to
carefully control the flow rate of PTA in order to achieve a specified mole ratio.
2.1.2. Paste preparation vessel (1817-v01)
Agitator (attached to the motor) is continuously mixing catalyst and raw material for a
specific period of time. The PTA, MEG and catalyst are added according to required ratio.
During observation the following flow rates were shown on the DCS.

 PTA = 12740 kg/h


 EG = 5520 kg/h
 Catalyst = 280kg/h

2.1.3. Parameters
 Temperature = 49.70C
 Level = 79.4%
 Set Mole Ratio = 1.167
 Agitator Speed = 80% (23.0 rpm)
3. Esterification
AREA 1829
3.1. DESCRIPTION
A reaction in which an ester is formed is called esterification reaction.

Example: Reaction between an alcohol and carboxylic acid

Alcohol + Acid → Ester + Water

Two reactions are involved in the preparation of polyester from raw materials. The first one is
esterification, which takes place in ES-I and ES-II, and the second is polycondensation which
takes place in PP-I and DRR. In polyester manufacture esterification reaction is carried out
between PTA(Pure terephthalic acid) and MEG(Monoethylene Glycol). From this reaction the
monomer for the polymerization reaction is formed. This process is carried out in two stages.

I. Esterification 1
II. Esterification 2

Reaction

3.1.1. ESterification-I (1829-R01)


In Esterification-I, the PTA and EG react to form monomer/oligomer (Diethylene Glycol
Terephthalate “DGT” / Bishydroxy Ethylene Terephthalate “BHET”) while water is split off and
the polycondensation reaction is initiated while EG is split off.

The degree of Esterification is controlled by maintaining Temperature, Pressure,


Residence Time and Mole Ratio at an appropriate level.

3.1.1.1. Parameters
 Capacity = 196 m3
 Temperature = 257oC
 Pressure = 0.385 bar
 Level = 40.5%
 Agitator Speed = 95% (49.4 rpm)
 Conversion = 91~92%
3.1.1.2. Temperature
The reaction is endothermic in nature and requires sufficient heat to overcome activation
energy. The temperature is provided by Heat Transfer Material (HTM) Santotherm. It is being
circulated in the 13 coils. Santotherm is being pumped by centrifugal pumps. Three centrifugal
pumps are installed, two are in running position and one is in standby.

3.1.1.3. Pressure
The reactor is jacketed and insulated. The reactor must have pressure maintained for the
reaction to move forward. The pressure is being measured by Pressure Recorder Controller
(PRC).

3.1.1.4. Residence Time


The CSTR reactor needs specific amount of time to have the reaction completed. The residence
time of the rector 1829-R01 is 3.2hr.

3.1.1.5. Agitation
The continuous agitation is provided to make sure that heat is uniformly distributed in the
reactor and reactor has homogeneous concentration otherwise non-uniform mixing will occur
which leads to inefficient and incomplete reaction.

3.1.2. ESTERification-II (1829-R02)


The product mixture of ES-I now enters the reactor 2 known as Esterification reactor-II. The
code of reactor is 1829-R02. It has two inlet streams. ES-2 is also a CSTR which has a stirrer at
bottom. Heat is provided by coils and jacket. In coils santotherm is introduced and jackets are
heated by dowtherm. In both of the reactors the water vapors are taken out and some MEG
also comes out with water.

3.1.2.1. Parameters
 Capacity = 73 m3
 Temperature = 266oC
 Pressure = 0.131 bar
 Level = 53.8 %
 Agitator Speed = 90 % (49.5 rpm)
 Conversion = 96~97 %

3.1.3. Level TransmittSers


There are basically three level transmitters for accurate level measurement.
3.1.3.1. Displacer
A displacer consists of a metal rod suspended with help of the spring enclosed in the housing. It
works on the Archimedes Principle which states that if a solid is submerged in a liquid, then a
reduction in the weight of the solid is observed which is equivalent to the volume of the liquid
displaced due to the submerging of solid. This reduction in the weight of the metal rod is
calibrated against the level of the tank. Its zero starts at the top end of the baffles placed in the
reactor and the level is usually maintained at 37%.

3.1.3.2. Radioactive Level Transmitter


Gamma rays are passed through the vessel wall and process fluid and a detector on the other
side measures the radiation intensity and gives information about the level. In this level
transmitter the level is usually around 48%.

3.1.3.3. Diaphragm Level Transmitter


There is a diaphragm connected with wire and spring. It measures the level through calibration
from the pressure head of the fluid. Its zero starts from the bottom of the reactor having
minimum dead volume. It tells the total actual level of the reactor usually having a level of
86.1%.
4. PROCESS COLUMN
4.1. PROCESS COLUMN
INTRODUCTION
The vapors from ES-1 and ES-2 contain a
mixture of ethylene glycol and water
vapors. These vapors are separated in a
distillation column which is called Process
Column at IFL. The purpose of separating
EG and water vapors is to save EG from
waste.

Distillation is a process of separation of two species on the basis of difference in volatility. The
higher volatile specie is collected at top and condensed and the less volatile specie is collected
from bottom as liquid. The distillation operation depends on many parameters. Like nature of
species. If the mixture is azeotropic or there is a very high difference in boiling points then
distillation operation might vary. Distillation is carried out in a vertical column fitted with trays
and also called as tray column.

In tray column the feed is fed to a specific tray and a number of trays are above and below that
tray. The number of trays depends on many parameters like; condition of feed, concentration
of top product, concentration of bottom product, reflux ratio, etc.

Number of trays can be calculated by two methods

 McCabe Thiele Method


 Lewis Method

Parts of Distillation Column:

Parts of distillation column are as follow:

 Tray Column
 Condenser
 Reboiler
 Feed Preheater
 Feed Pump, Bottom Line Product, Top Product Pump, etc .
4.2. DIFFICULTIES IN DISTILLATION:
Adverse vapor flow conditions can cause:

 Foaming
 Entrainment
 Weeping/dumping
 Flooding

4.2.1. Foaming
Foaming refers to the expansion of liquid due to passage of vapor or gas. Although it provides
high interfacial liquid-vapor contact, excessive foaming often leads to liquid buildup on trays. In
some cases, foaming may be so bad that the foam mixes with liquid on the tray above. Whether
foaming will occur depends primarily on physical properties of the liquid mixtures, but is
sometimes due to tray designs and condition. Whatever the cause, separation efficiency is
always reduced.

4.2.2. Entrainment
Entrainment refers to the liquid carried by vapor up to the tray above and is again caused by
high vapor flow rates. It is detrimental because tray efficiency is reduced: lower volatile
material is carried to a plate holding liquid of higher volatility. It could also contaminate high
purity distillate. Excessive entrainment can lead to flooding.

4.2.3. Weeping/Dumping
This phenomenon is caused by low vapor flow. The pressure exerted by the vapor is insufficient
to hold up the liquid on the tray. Therefore, liquid starts to leak through perforations. Excessive
weeping will lead to dumping. That is the liquid on all trays will crash (dump) through to the
base of the column (via a domino effect) and the column will have to be re-started. Weeping is
indicated by a sharp pressure drop in the column and reduced separation efficiency.

4.2.4. Flooding
Flooding is brought about by excessive vapor flow, causing liquid to be entrained in the vapor
up the column. The increased pressure from excessive vapor also backs up the liquid in the
down comer, causing an increase in liquid holdup on the plate above. Depending on the degree
of flooding, the maximum capacity of the column may be severely reduced. Flooding is
detected by sharp increases in column differential pressure and significant decrease in
separation efficiency.
4.3. TYPES OF TRAYS USED IN TRAY COLUMNS
Different types of plates/trays are used in tray columns for gas/liquid contact. Some of them
are as follows:

 Bubble cap tray


 Sieve tray/perforated plates
 Valve trays

4.3.1. Bubble Cap Trays


A bubble cap tray has riser or chimney
fitted over each hole, and a cap that covers
the riser. The cap is mounted so that there
is a space between riser and cap to allow
the passage of vapour. Vapour rises
through the chimney and is directed downward by the cap, finally discharging through slots in
the cap, and finally bubbling through the liquid on the tray.

4.3.2. Sieve Trays


Sieve trays are simply metal plates with holes in
them. Vapour passes straight upward through the
liquid on the plate. The arrangement, number and
size of the holes are design-parameters.

4.3.3. Valve Trays


In valve trays, perforations are covered by liftable
caps. Vapour flow lifts the caps, thus self-creating a
flow area for the passage of vapor. The lifting cap
directs the vapor to flow horizontally into the liquid,
thus providing better mixing than is possible in sieve
trays.
Process Description
Process column is a tray column with 16 trays and feed is introduced on plate at bottom.
Bubble and cap trays are used and feed enters in vapor form at about 250 o C. The average
temperature of plate 5, 7 and 9 is maintained at 150 o C. Reflux ratio is changed depending upon
the temperature of these plates.

Reflux is introduced on the top plate and moves downward. The liquid flows from weirs into
down comers to the lower plates. The vapors rise upward from the bubble and cap
arrangement and come in contact with the liquid. The lower volatile specie condenses and
higher volatile specie vaporizes in result of that. The vapors on a plate and liquid are in
equilibrium. This is how the concentration of higher volatile component increases as we move
from bottom to top.

From top the vapors are collected and taken out of the system. These vapors are condensed in
a condenser and a part of these vapors is introduced back to the column as reflux. The purpose
of introducing reflux is to achieve purity. The liquid which don’t vaporize anywhere flows to
lower plates and finally to the reboiler. Here the reboiler is simply a coil in the bottom of the
column.
5. POLYCONDENSATION
5.1. INTRODUCTION
Polycondensation is the polymerization of DGT(Diethylene Glycol Terephthalate). The
polymerization is of two types:

Addition Polymerization.

Condensation Polymerization.

In addition polymerization the unsaturated hydrocarbons or molecules combine together to


form a polymer.

In condensation polymerization two molecules combine together giving off a small molecule like
water, Amonia etc.

In polyester manufacture the polymerization process taking place is condensation


polymerization water is Ethylene glycol is given off in the process. This is also an endothermic
reaction. EG is taken out from the system to complete the reaction by a vacuum system.

Polycondensation process is also carried out in two stages.

1. Prepolycondensation Reactor
2. Disc Ring Reactor

5.2. PROCESS DESCRIPTION

5.2.1. ES-2 TO PPR


The feed from ES-2 is fed in PPR with help of pressure difference. PPR is a CSTR with agitator at
bottom, it also has baffles in its upper section. The reaction is endothermic and heat is
provided. In coils santotherm is introduced and dowtherm is introduced in jacket. The EG
produced in this stage is taken out by help of vacuum system and taken into a scrapper
condenser. Here EG is condensed and vacuum is developed. This vacuum promotes the forward
reaction by taking the byproduct out of the system.

 Level 35 %
 Temperature 260 oC
 Vacuum 18 mBar

5.2.2. PPR TO DRR


The pre-polymer from PPR is fed to DRR with the help of pre-polymer feed pumps. In DRR PET
introduced has low I.V which is about 0.255. The required degree of polymerization is 105 at
which I.V is 0.62.In DRR the heat is provide by coils which are surrounding the periphery of
reactor and santotherm is used for heating. DRR is a Plug Flow Reactor which has Rings and
Discs which are fitted on an axial shaft and rotating in radial direction. These rings and discs
provide surface for evaporation of EG and hence promotion of reaction and concentration of
the slurry. In DRR the vacuum is developed by jet system and EG taken out is condensed in a
scrapper condenser.

 Level 30.3 %
 Temperature 279 oC
 Vacuum 1.5 mBar
 Agitator Speed 3.35 RPM
6. Additives used in the production of PET
6.1. ANTIMONY TRI-ACETATE, CATALYST
The process of fiber making is an endothermic reaction. It means that the energy required to
start reaction is high. To lower this energy, called as activation energy, catalyst is used. Catalyst
lowers the activation energy by associating itself with the reactants which also helps in reducing
the residence time.

The catalyst used is Antimony Triacetate Sb(CH3COO)3. It helps the reaction in the stage of
polycondensation which will be discussed later. It is imported in the form of bags, each
weighing 15 kg, from USA. It occurs in the form of granules and is fed as two catalyst vessels

 Feed vessel
 Preparation vessel

6.1.1. Preparation
It can be prepared by the reaction of antimony (III) oxide with acetic acid:

Sb2O3 + 6CH3CO2H → 2Sb(CH3CO2)3 + 3H2O

Solution of catalyst is prepared by mixing filtered ethylene glycol and Sb(CH 3COO)3 in a vessel at
a temperature about 75-80oC. The solution is agitated constantly for 4 hours in the vessel, while
1 hour is provided as settling time. At the end, an analysis is done to ensure that the
concentration of the catalyst in the solution is 3%. The preparation of the catalyst solution is
done batch-wise. A number of batches of catalyst solution are prepared to ensure that
continuous process of plant does not stop.

The prepared batch of catalyst solution is filtered and a fixed amount of it is introduced in the
paste preparation unit (170-180ppm of catalyst in product is desired). The amount of catalyst in
the final product is so low that a process for recovery of catalyst is not feasible.

6.1.2. Structure
The crystal structure of antimony (III) acetate has been determined by X-ray
crystallography. It consists of discrete Sb(OAc)3 monomers with monodentate acetate ligands.
The monomers are linked together into chains by weaker C=O···Sb intermolecular interactions.
6.1.3. Properties
Chemical Formula Sb(CH3COO)3

Appearance White powder

Density 1.22 g/cm³ (20 °C)


128.5 °C (263.3 °F; 401.6 K)
Melting Point

6.2. Titanium Dioxide, Color Dulling Agent


Titanium dioxide, also known as titanium (IV) oxide or titania, is the naturally occurring oxide of
titanium, chemical formula TiO2. It is used to make products of different brightness. For making
a semi-dull product, the concentration of TDO in the solution is 10% and 0.3% by weight of PET
in the final product. On the other hand, a bright product must have 3% concentration of TDO in
solution and 0.03% by weight of PET in the final product. It also has following advantages for
the final product

 TDO provides matt finish to the final product.


 It increases the durability of the product.
 TDO Anatase has high refractive index close to diamond, which causes glitter-ness.
 TDO also gives hardness to the product i.e. on a scale of 0-10, where talc has zero
hardness and diamond has maximum of 10, TDO has hardness of 5.5 – 6.5 Mohs.

6.2.1. Properties
Chemical formula TiO2
Molar mass 79.866 g/mol
Appearance White solid
Odor odorless
Density 4.23 g/cm3 (Rutile)
3.78 g/cm3 (Anatase)
Melting point 1,843 °C (3,349 °F; 2,116 K)
Boiling point 2,972 °C (5,382 °F; 3,245 K)
Solubility in water insoluble
6.2.2. PROCESS DESCRIPTION
Sludge containing 2400kg EG and heavy particles of TDO is introduced in 1618-VO1 and
6 bags of TDO are added after agitation the mixture is sent to pearl mill in which grinding occurs
and chilled water is supplied in outer coating of mill to keep the material cool. After the mill
material is filtered and introduced to 1618-V02 in this vessel we have 55% of TDO solution after
this again grinding is done.

After filtration material enters in 1618-V03 in which 1100kg of EG in introduced a concentration


goes to 18%. After that centrifuging phenomenon occurs, the centrifuge undergoes through
three steps during its operation.

 Classifying – Fine and oversized particles are classified and this process lasts for 50
minutes.
 Dispersing – Dispersion of Oversized particles with MEG and this step lasts for ~20
minutes.
 Discharging – Discharging of oversized particles by MEG to Pearl Mill and this step lasts
for ~5 minutes.

After centrifuge we get two streams, one of fine slurry and other of sludge.

Fine slurry

It is sent to two storing vessels 1618-V04 and 1618-V05 in these 1100kg of EG is added
and we get 10% concentration solution. Because two batch at a time are processed so these are
called buffer vessels. From these vessels on the pressure of nitrogen material is transferred to
dosing vessel 1618-V06. After that through two pumps in ES-II for semi dull product to obtain.

Sludge

It goes to 1618-V07 from which is sent to pearl mill and then to 1618-V01 for the
process to start again. Pearl Mill grinds the oversize particles by using a Muller which has fine
particles of Zirconium dioxide of diameter 0.8 micron. Ground particles form pearl mill are again
moved to 1618-V01 vessel.

6.2.3. Applications
The most important application areas are paints and varnishes as well as paper and
plastics, which account for about 80% of the world's titanium dioxide consumption. Other
pigment applications such as printing inks, fibers, rubber, cosmetic products and food account
for another 8%. The rest is used in other applications, for instance the production of technical
pure titanium, glass and glass ceramics, electrical ceramics, catalysts, electric conductors and
chemical intermediates. It is also in most red-colored candy.
7. EG CIRCULATION AND VACUUM
GENERATION
7.1. ETHYLENE GLYCOL CIRCULATION:
The circulation of EG is done through Jet system, Scrapper
condenser and through the distillation of EG vapors. The detail
of which is described below;

The duty of this equipment is to condense the MEG vapors


which are escaping during the Polymerization reaction. These
vapors contain the three following components,

 Ethylene Glycol
 Water
 Oligomer

The Vapors are being condensed by the showering of Cooled SEG. As the EG vapors enters the
condenser, it contact with spent glycol which is sprinkled from the top
periphery. Part of EG condenses and remaining part moves to jet system. In
scrapper part, scrapper deters the carryover to stick with walls of the
condenser and forces it to move to immersion vessel.

7.1.1. IMMERSION VESSEL


Condensate of scrapper condenser is announced in immersion vessel.
Immersion Vessel comprises weir plate. Carryover of the scrapper condenser arrives in the
immersion vessel where is separated with the assistance of weir plate. Weir plate is cleaned
according to the schedule. The oligomer separated there is cleaned after a specific interval of
duration depending on the operation

7.1.2. SPENT EG COOLERS


Spent EG is cooled by means of cooling water in the coolers.
Coolers are of shell and tube type and the coolant medium is
chilled water which is introducing in the production
department through utilities section. Two coolers are installed for this purpose, one is in the
service and other is on standby.

EG from the immersion vessel is pumped with the help of two pumps, usually one is in service
and other on standby, EG passes through cooler where it is cooled to desired temperature. EG
from the cooler is then showered in the scrapper condenser. Summarizing the cooled SEG is
recycled and reused as a cooling agent in the cooler. Head provided by the pumps is sufficient
so that SEG passes through cooler and showers in scrapper condenser. The unusable SEG is
introduced in a separate vessel which could be used according to the requirement or could be
drain if there is no use left.
Hot SEG is used for cleaning of the coolers. When cleaning of the cooler is required, the second
cooler is taken into service while HOT SEG is passed from the former coolers for cleaning.

7.2. Jet System


Jet system comprises of two main following components

1. Booster
2. condenser

Jet system at IFL-III is used to make absolute vacuum of 0.8


mbar. The motive fluid is Ethylene Glycol vapors. It contains
three stages. Each stage is equipped with an ejector and
condenser. Condensate of each stage is collected in an immersion vessel through barometric
leg. A single jet system is used to make vacuum in PP and DRR reactor. Vapors of DRR are
controlled through a control valve while vapors forming in PP reactor are also passed through
jet system.

The principal feature of the Barometric Condenser is that injection water may be discharged
through a tail pipe by gravity, without requiring a pump. The Barometric Condenser is
employed in a variety of industries as an economical means of removing air, exhaust steam, and
other vapors from vacuum equipment

7.2.1. GENERAL APPLICATIONS:


 Filtration; Distillation; Impregnation; Absorption; Drying; Degassing; Dehydration; Evacuating;
Cooking; Evaporating; Vacuum transfer; Chilling
 Removing condensate under vacuum
 Exhausting air from vacuum pans and evaporators
 Priming centrifugal pumps
 Handle air or other gases at suction pressures as low as three microns hg. Abs
 Decarbonating brewery water
 Creating chemical process vacuums
 Water treating by degasifying
 Used in degassing molten steel Perfume concentration;

7.3. Barometric Leg and its Applications in a vacuum system:

 The piping between the condenser and the receiver tank is called the barometric leg.

 To condense the condensable vapors through heat exchangers or condensers in a vacuum


system, the condensate is normally dropped into a receiver tank. This creates a situation where
the condensate is under negative pressure in the condenser and it is tending to move toward a
receiver tank that is under positive pressure. Thereby, the pressure difference is going the
wrong way and producing the backward push. To overcome this backward pushing pressure
differential, the condenser should be located higher than the receiver tank to permit enough
static head pressure of the condensate to surpass the pressure differential.

 A barometric leg is basically a condensate drain. Inappropriate barometric leg design will lessen
the performance of the condenser. Since the condensate drains by gravity, the barometric leg
should have be high enough to make certain the condensate does not enter the condenser and
overflow the lower tubes. If the tubes flood, they will not be able to transfer heat effectually.
 One important thing is kept in account that the barometric leg extends into the receiver and is
submerged enough that atmospheric vent gases cannot be dragged into the piping. This forms
your very necessary seal. If you vent into a system under any pressure, the pressure differential
will increase requiring a taller barometric leg

7.3.1. INSTALLATION AND CONSIDERATIONS FOR BAROMETRIC LEG:


 It is endorsed that the condenser be mounted 34 ft above the Hotwell water level.
Certainly, this is not authoritative for mounting a barometric condenser and the length of
the barometric leg, but considerations should be made as to potential variations in
functioning vacuum to prohibit potential flooding of the barometric condenser.
 There should be no 90 deg turns; should have only ‘straight’ pipe or, if necessary, a 45 deg
‘jog’ as a maximum in the barometric leg assembly.
 The Hotwell receiver itself should have certain criteria of design and offer a liquid level
regulator by setting up a weir baffle and have the barometric leg sealed a minimum of 6”
below the top of the weir.
 The Hotwell would also serve as a sump for condensate removal. The Hotwell receiver sump
could be self-draining if it were elevated above ground level
7.4. Ejectors:
An ejector is a type of vacuum pump or compressor. Since an ejector has no valves, rotors,
pistons or other moving parts, it is a relatively low-cost
component, is easy to operate and requires relatively
little maintenance. Ejectors are simplest, most reliable
and trouble-free vacuum producing equipment. They
provide the largest capacity of all vacuum pumps and are
a static piece of equipment with no moving parts.
Ejectors should be studied accordingly to the following two terms;

 Components of an ejector
 Principle of operation

There are four major components of an ejectors

1. The mode of nozzle


2. Motive chest
3. Suction chamber
4. Diffuser

Principle of Operation:

An ejector works by converting the pressure energy of the motive fluid (potential energy) to
velocity energy (kinetic energy). This is accomplished by adiabatic expansion from the motive
fluid supply pressure to the suction load pressure as motive fluid flows through a converging
diverging nozzle.

7.4.1. COMPONENTS OF AN EJECTORS


Motive chest:

This is the part where the motive fluid enters the ejector. The motive
fluid in most of the cases is steam however it could be any fluid that is
at higher pressure.

Motive nozzle:

When the fluid enters the motive nozzle it expands adiabatically across the converging
diverging motive nozzle, converting pressure to velocity. The differential pressure across the
motive nozzle accelerates the motive fluid as it rushes to the lower pressure region of the
suction chamber. A well-designed converging diverging nozzle efficiently converts high pressure
motive to a high velocity stream leaving the divergent section of the nozzle. The motive gas
expands to a pressure slightly less than the suction load pressure that creates a localized low-
pressure region which draws in the suction load vapor. The design and location of the motive
nozzle is set by manufacturer for our specific operating conditions that plays an important part
in ejector performance.

Suction chamber:

Suction chamber is the mechanical connection between the nozzle and the rest of the ejector.
The high velocity motives stream mixes and entrains the process gases in the suction chamber.
Momentum is transferred from high motive stream to suction load gases accelerating the
suction load gases and consequently decelerating the motive gas to a new mixture velocity.

The last and major component is the diffuser. The mixed gas stream enters the diffuser where
velocity is converted back to pressure and work of the compression occurs, the diffuser consists
of three sections:

1. The inlet converging section


2. Throat section with constant area
3. Outlet diverging section

In the inlet converging section the mixture velocity is decreased and pressure is increased as
the cross-sectional area is reduced.

Diffuser:

The diffuser throat is sized to achieve an optimal transonic shock system. The transition from
supersonic to subsonic flow across the shock system produces a dramatic increase in pressure
slightly more than half of the total compression achieved in an ejector is obtained in this
section. The static pressure temperature and density increase across the shock system whereas
velocity decreases the pressure is increased further in the outlet diverging section of the
diffuser where the subsonic mixture is reduced as cross-sectional area increases from the
throat diameter to the discharge diameter slightly less than half of the total compression
achieved in a lower section through simple deceleration section of the subsonic flow.

7.4.2. MULTIPLE EJECTORS APPLICATION:


Multiple-nozzle ejectors are more efficient. They usually save as much as 10% to 20% in motive steam,
compared with single-nozzle units designed for the same conditions. Multi stage ejectors often promote
economy by including inter condensers between some of the stages to reduce the load. Sometimes, pre-
condensers, booster condensers and after condensers are also used.
7.5. Liquid Ring Vacuum Pump
Working

The liquid ring vacuum pump is named as Liquid ring because of


the presence of Liquid Piston. The liquid ring vacuum pump
uses water or any other suitable liquid. It consisted of chambers
around the periphery that is aligned between the rotor blades.
Furthermore, the chambers are open on the inside as well.
These inner edges of the rotor blades are machined to rotate
around the cone surface with a close non-contact fit.

An internal passage joins the openings from the pump inlet to an inlet port in the cone. There is also a
passage from the cone discharge to the discharge connection on the head. Some pumps have a port
plate configuration rather than conical, but the principle is the same. The spinning of liquid forms a ring
due to centrifugal force. Because the rotor axis and body axis are offset from each other, the liquid ring
is not concentric with the rotor
Inlet

Air or gas entered the pump at the inlet connection. Air or gas traverses the internal passage to the cone
inlet port. The gas is drawn into the rotor chambers by the receding liquid ring, similar to the suction
stroke of a piston in a cylinder. The liquid ring does the job of pistons, while the rotor chambers play the
part of cylinders.
Compression

As each chamber rotates past the inlet port,


the chamber carries a volume of air or gas
around with it. The gas is compressed as the
liquid ring converges with the cone. This
represents the compression of air or gas from
vacuum up to atmospheric pressure or from
atmospheric up to positive pressure in a liquid
ring compressor.
Discharge

When each chamber rotates to the discharge port opening, the compressed air or gas escapes from that
chamber through the discharge port to the internal discharge passage.
Air or gas closely packed to indicate higher pressure, is shown here flowing out of the discharge
connection at right. The flow is continuous without pulsation.
7.5.1. Operation of Liquid Ring Vacuum Pump in Jet System at IFL-III
 Liquid ring vacuum pump is intended to recuperate EG vapors by means of rotating impeller
blades that come in and leave a ring of liquid EG.
 Through the periphery of the pump casing, the impeller forces this sealing liquid where it forms
a moving ring of liquid around a center void.
 Above the centerline of the casing the impeller shaft is mounted; while the blades, although
rotating concentrically, are located eccentrically to the casing and the ring of liquid.
 The axial suction and discharge ports of pumps are exposed to the void but separated apart by
the impeller blades and the ring of liquid.
 As the process gas or vapor is drawn into the pump through the suction port, it is trapped
between the impeller blades and the liquid ring.
 The rotating blades enter deeper into the liquid ring, increasingly reducing the entrapment
space, compressing and then exhausting the gas through the discharge port.
 Ethylene Glycol vapors are vented to harmless place. Nitrogen gas is used to vent EG vapors
because of the explosive nature of EG

7.6. Knock Out Drum:


The Knock out drum is a vessel in the flare header designed to
remove & accumulate condensed & entrained liquids from the
relief gases.

Both the horizontal & vertical design is a common consideration


for the Knock out drum, which is determined based on the
operating parameters as well as other plant conditions. If a large
liquid storage capacity is desired and the vapour flow is high, a
horizontal drum is often more economical. Also, the pressure
drop across horizontal drums is generally the lowest of all the
designs. Vertical knockout drums are typically used if the liquid load is low or limited plot space
is available. They are well suited for incorporating into the base of the flare stack.

7.6.1. DESIGN FEATURE:


Although horizontal and vertical knockout drums are available in many configurations, the
differences are mainly in how the path of the vapour is directed. The various configurations
include the following:

 Horizontal drum with the vapour entering one end of the vessel and exiting at the top of the
opposite end (no internal baffling);
 Vertical drum with the vapour inlet nozzle entering the vessel radially and the outlet nozzle at
the top of the vessel’s vertical axis. The inlet stream should be baffled to direct the flow
downward;
 Vertical vessel with a tangential nozzle. Vertical centrifugal separators differ from vertical
settling drums in that the flow enters tangentially and spins around a center tube, which
extends below the liquid inlet nozzle. The gas and liquid flow radially downward through the
annulus causing liquid droplets to coalesce along the walls and collect in the bottom of the
drum. The vapour changes direction once below the center tube and flows upward to the outlet
nozzle. To avoid liquid re-entrainment, vapour velocity has to be kept low in the turnaround
section of the drum. An additional measure to prevent liquid re-entrainment is a baffle plate
below the turnaround section of the drum. The maximum liquid level is the same as vertical
settling drums;
 Horizontal drum with the vapour entering at each end on the horizontal axis and a center outlet;
 Horizontal drum with the vapour entering in the centre and exiting at each end on the
horizontal axis
 Combination of a vertical drum in the base of the flare stack and a horizontal drum upstream to
remove the bulk of the liquid entrained in the vapour. This combination permits the use of
larger values for the numerical constant in the velocity equation.

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