Fyp

Plant Design Project
Production of 100 tons/day

Polyester Chips using
Ethylene Glycol and Terepthalic Acid as
Raw Materials
Supervised By:
Prof. Dr. Rafiullah Khan
Submitted By:
Adeel-ur-Rehman E11-15-CE06
Hamood Ahmad E11-15-CE11
Younis Iqbal E11-15-PG06
Amir Bashir E11-15-PG11
Institute of Chemical Engineering & Technology,
University of the Punjab, Lahore

ACKNOWLEDGEMENT
We reiterate our gratitude to our creator Allah Almighty, for enabling us to complete our work and
without whose help all efforts would have been fruitless.
We wish to acknowledge our debt to our guide Prof. Dr. Rafiullah for helping us with his knowledge
and expertise whenever we felt the need and also for his continued guidance in preparing this report in the
current form.
We wish to express our appreciation for the the library staff at Institute of Chemical Engineering &
Technology, University of the Punjab, Lahore, for co-operating with us to their best abilities during our project
and their help in acquisition of related books and other data.
Those who contributed indirectly in accomplishing this report through their discussions and criticism,
our classmates.
Last but not least, our parents and siblings whose prayers and help were the driving force for our work.
Adeel-ur-Rehman
Amir Bashir
Hamood Ahmad
Younis Iqbal
Contents
Chapter 1: Introduction ....................................................................................................................................... 1
1.1. Polyester .............................................................................................................................................. 1
1.2. Classification of Polyesters .................................................................................................................. 1
1.2.1. Thermoplastic Polyesters ............................................................................................................ 1
1.2.2. Thermosetting Polymers ............................................................................................................. 1
1.3. Types of Polyesters .............................................................................................................................. 1
1.3.1. On Basis of Composition.............................................................................................................. 1
1.3.2. On the Basis of Application.......................................................................................................... 2
1.3.3. On the Basis of Structural Differences/Bonding.......................................................................... 2
1.4. Importance of Polyester ...................................................................................................................... 3
1.5. Consumption of Polyester ................................................................................................................... 3
1.6. Uses of Polyester ................................................................................................................................. 4
1.6.1. Usage of Polyester Films.............................................................................................................. 4
1.6.2. Usage of Polyester in Medical Field............................................................................................. 4
1.6.3. Usage of Polyester Fibers ............................................................................................................ 4
Uses of Polyester Fibers .................................................................................................................................. 4
1.7. Polyester Fiber ..................................................................................................................................... 5
1.7.1. Criteria for Fiber Forming Polymers ............................................................................................ 5
1.8. Economical Prospective ....................................................................................................................... 5
1.9. Uses of PET Polyester .......................................................................................................................... 7
1.9.1. Uses of Polyester for Apparel Purposes ...................................................................................... 7
1.9.2. Industrial Uses ............................................................................................................................. 7
1.9.3. Other Uses ................................................................................................................................... 8
1.10. Conversion of Chips to PET Fiber ..................................................................................................... 9
1.10.1. Spinning ....................................................................................................................................... 9
1.11. Types of Spinning........................................................................................................................... 10
1.11.1. Melt Spinning............................................................................................................................. 10
References: .................................................................................................................................................... 11
Chapter 2: Process Selection ............................................................................................................................. 12
2.1. PET Polymerization ............................................................................................................................ 12
2.1.1. General Description of PET Polymerization............................................................................... 12
2.1.2. Why Two Step Reaction? ........................................................................................................... 12
2.2. Types of PET Polymerization ............................................................................................................. 12
2.2.1. Batch Process............................................................................................................................. 12
2.2.2. Continuous Process ................................................................................................................... 13
2.3. Advantages of Continuous Process over Batch Process .................................................................... 13
2.4. Contrasting the DMT & TPA Processes .............................................................................................. 14
2.5. Difference between DMT & TPA Processes....................................................................................... 14
2.6. Transesterification Process................................................................................................................ 15
2.7. Take Over of DMT Process by TPA Process ....................................................................................... 15
2.8. Basis for the Process Selection .......................................................................................................... 15
2.8.1. Advantages of TPA over DMT .................................................................................................... 15
Chapter 3: Selected Process Description ........................................................................................................... 16
3.1. Direct Esterification ........................................................................................................................... 16
3.2. Reactions ........................................................................................................................................... 16
3.3. Raw Materials .................................................................................................................................... 16
3.3.1. Ethylene Glycol .......................................................................................................................... 16
3.3.2. Terephthalic Acid ....................................................................................................................... 17
3.4. Process Stage ..................................................................................................................................... 18
3.4.1. TPA Unloading and Storage ....................................................................................................... 18
3.4.2. EG Unloading and Storage ......................................................................................................... 18
3.4.3. TDO and Catalyst Preparation ................................................................................................... 18
3.4.4. Slurry Making ............................................................................................................................. 18
3.4.5. Esterification Stage .................................................................................................................... 19
3.4.6. Polycondensation ...................................................................................................................... 20
Chapter 4: Material Balance .............................................................................................................................. 17
4.1. Nomenclature .................................................................................................................................... 17
4.2. Reactions: .......................................................................................................................................... 17
4.3. Molecular Weights of Materials ........................................................................................................ 17
4.4. Overall Material Balance ................................................................................................................... 18
4.4.1. Stoichiometric Calculations ....................................................................................................... 18
4.5. Nomenclature of Streams ................................................................................................................. 19
4.6. Detailed Material Balance ................................................................................................................. 19
4.6.1. Slurry Section (TPA + EG Mixing Tank) ...................................................................................... 19
4.6.2. Esterification Section ................................................................................................................. 21
4.6.3. Polycondensation Reactors ....................................................................................................... 31
Chapter 5: Energy Balance ................................................................................................................................ 44
5.1. Esterification Reactor 1 (ER-1)........................................................................................................... 44
5.1.1. Description................................................................................................................................. 44
5.1.2. Stream Properties ...................................................................................................................... 45
5.1.3. Calculation of Energy Requirements for Stream 1 .................................................................... 46
5.1.4. Total Energy Requirement ......................................................................................................... 47
5.2. Esterification Reactor 2: .................................................................................................................... 48
5.2.1. Description................................................................................................................................. 48
5.2.3. Calculation of Energy Requirements ......................................................................................... 49
5.3. Polymerization Reactor 1 .................................................................................................................. 51
5.3.1. Description................................................................................................................................. 51
5.3.3. Calculations of Energy Requirement ......................................................................................... 52
5.4. Polymerization Reactor-2 .................................................................................................................. 53
5.4.1. Description................................................................................................................................. 53
5.5. Poly-Condensation Reactor ............................................................................................................... 55
5.5.1. Description................................................................................................................................. 55
Chapter 6: Equipment Design ............................................................................................................................ 57
6.1. Storage Units ..................................................................................................................................... 57
6.1.1. Storage Tank of TPA................................................................................................................... 57
6.1.2. Storage Tank of EG .................................................................................................................... 59
6.2. Mixing Tank ....................................................................................................................................... 61
6.2.1. Design of Slurry Mixer ............................................................................................................... 61
6.3. Esterification Reactors....................................................................................................................... 67
6.3.1. Design of Esterification Rector 1 (ES-1) ..................................................................................... 67
6.3.2. Design of Esterification Rector 2 (ES-2) ..................................................................................... 71
Chapter 7: Instrumentation & Process Control ................................................................................................. 75
7.1. Instrumentation................................................................................................................................. 75
7.1.1. Measurement ............................................................................................................................ 75
7.1.2. Control ....................................................................................................................................... 75
7.2. Incentive for Chemical Process Control............................................................................................. 76
7.2.1. Safety ......................................................................................................................................... 76
7.2.2. Product Specification ................................................................................................................. 76
7.2.3. Environmental Regulations ....................................................................................................... 76
7.2.4. Operational Constraints ............................................................................................................ 76
7.2.5. Economics .................................................................................................................................. 76
7.3. Elements of Control System .............................................................................................................. 77
7.3.1. The Chemical Process ................................................................................................................ 77
7.3.2. The Measuring Instrument or the Sensors ................................................................................ 77
7.3.3. Transducers ............................................................................................................................... 78
7.3.4. Transmission lines ..................................................................................................................... 78
7.3.5. Controller ................................................................................................................................... 78
7.3.6. The Final Control Element ......................................................................................................... 78
7.4. Modes of Control............................................................................................................................... 79
7.4.1. Different Types of Control Actions ............................................................................................ 79
7.4.2. Composite Control Modes......................................................................................................... 79
7.5. Selection of Controller ....................................................................................................................... 79
7.5.1. Usage of a Simple Proportional Controller: ............................................................................... 80
7.5.2. Usage of a PI Controller ............................................................................................................. 80
7.5.3. Usage of a PID Controller .......................................................................................................... 80
7.6. Control Loops..................................................................................................................................... 80
7.6.1. Feed Back Control Loop ............................................................................................................. 81
7.6.2. Feed Forward Control Loop ....................................................................................................... 81
7.6.3. Ratio Control Loop ..................................................................................................................... 81
7.6.4. Auctioneering Control Loop ...................................................................................................... 81
7.6.5. Cascade Control Loop ................................................................................................................ 81
7.7. Instrumentation of Slurry Tank ......................................................................................................... 82
7.8. Instrumentation of Esterifier ............................................................................................................. 83
7.9. Instrumentation of Poly-condensation Reactor ................................................................................ 84
Chapter 8: Cost Estimation ................................................................................................................................ 85
8.1. Introduction of Cost Estimation: ....................................................................................................... 85
8.1.1. Accuracy and purpose of capital cost estimates ....................................................................... 85
8.1.2. Classification of Capital Cost Estimations .................................................................................. 85
8.1.3. Capital investment:.................................................................................................................... 85
8.1.4. Fixed Capital: ............................................................................................................................. 86
8.1.5. Working Capital: ........................................................................................................................ 87
8.1.6. Operation Cost........................................................................................................................... 87
8.1.7. Cost Indices ................................................................................................................................ 88
8.1.8. Summary of Production cost: .................................................................................................... 88
8.2. Purchased Cost .................................................................................................................................. 89
8.2.1. Nomenclature: ........................................................................................................................... 89
8.2.2. Purchased cost of TPA Storage tank: ......................................................................................... 89
8.2.3. Purchased Cost of EG: storage tank: ......................................................................................... 89
8.2.4. Purchased Cost of Slurry Tank: .................................................................................................. 90
8.2.5. Purchased cost of esterifier PR-1 .............................................................................................. 90
8.2.6. Purchased cost of Esterifier reactor PR-2 .................................................................................. 90
8.2.7. Total cost of esterifiers: ............................................................................................................. 90
8.2.8. Purchased cost of Polycondensation Reactor RA-21: ............................................................... 91
8.2.11. Purchased cost of condensers: .................................................................................................. 92
8.2.12. Purchased cost of pumps: ......................................................................................................... 92
8.2.13. Purchased cost of coil: ............................................................................................................... 93
8.2.14. Total purchased equipment cost: .............................................................................................. 94
8.3. Total Physical plant Cost (PPC): ......................................................................................................... 94
8.3.1. Fixed Capital: ............................................................................................................................. 95
8.3.2. Working Capital: ........................................................................................................................ 95
8.4. Summary of Production Costs: .......................................................................................................... 95
8.4.1. Variable cost: ............................................................................................................................. 95
Chapter 1
Introduction
Chapter 1 Introduction
Chapter 1: Introduction
1.1. Polyester
Polyester is a category of polymers which contain the ester functional group in their main chain or
Polyester refers to the various polymers in which the backbones are formed by esterification and condensation
of poly functional alcohols and acids. Polyester can also be defined as long-chain polymers chemically
composed of at least 85% by weight of an ester and a dihydric alcohol and a terephthalic acid. Although there
are many polyesters, the term polyester as a specific material most commonly refers to a polyethylene
terephthalate (PET).
1.2. Classification of Polyesters

Depending on the thermal behavior polyester can be a thermoplastic or thermoset, however the most
common polyesters are thermoplastics.
1.2.1. Thermoplastic Polyesters

They can be softened or plasticized repeatedly on the application of thermal energy, without much
change in the properties if treated with certain precautions. They normally remain soluble and fusible after
many cycles of heating and cooling. On the addition of heat, these type of polyesters become soften while the
addition of more heat imparts them a fluid like behavior. However, as they have no cross linking that prevents
thermosetting polyesters from regaining their original shape, they can easily be remolded and recycled
without any adverse effects.
1.2.2. Thermosetting Polymers

As evident from their name, thermosetting polyesters are those which deform from their shape
irreversibly on the addition of heat, through the subjection of a chemical reaction of with the help of radiation.
They can be obtained in soluble and fusible forms in early or intermediate stages of their synthesis, but they
get set or cured and become insoluble and infusible when heated or thermally treated; the curing or setting
process involve chemical reactions leading to further growth and cross linking of polymer chain molecules and
producing giant molecules, e.g. unsaturated polyesters.
Although polyesters can be either thermoplastic or thermosetting, however, the most common
polyesters are thermoplastic.
1.3. Types of Polyesters

1.3.1. On Basis of Composition
1.3.1.1. Aliphatic Polyesters
These polyesters have properties that can be found similar to poly-ethylene and poly-propylene. They
have no odor and can be used for trash bags and cosmetic and average bottles. Examples include poly-lactic
acid and poly-glycolide. They can be formed by the poly-condensation of glycolic acid.
1.3.1.2. Semi-Aromatic Polyesters
These type of polyesters have high chemical decomposition temperatures, good electrical insulation
and excellent chemical resistance. As they have a high glass transition temperature and high melting
temperature, these type of polyesters maintain their shape and strength, even at elevated temperatures. By
the poly-condensation of terepthalic acid with ethylene glycol, semi aromatic polyesters are formed.
1.3.1.3. Aromatic Polyesters

They have excellent thermal stability, high thermal conductivity and are resistant to radiation. In
addition to them, they have high di-electric properties. Examples include vectran. They can be formed by the
condensation of 4-hydroxy-benzoic acid and 6-hydroxy-naphthalene-2-carboxylic acid. Aromatic polyesters
are used in chemical industry, in electronics and instrument industries.
1
1.3.2. On the Basis of Application
1.3.2.1. Polyester Fibers
A synthetic fiber in which the component that forms the fiber is a long chain synthetic polymer which
consists a minimum of 85% by weight of an ester that originated from a di-hydric alcohol and a terepthalic
acid. Their major usage comes along when they are used in a blend with cotton or wool in order to epitomize
the crease retention. It also helps to mitigate the wrinkle formation of garment fabrics.
1.3.2.2. Polyester Plasticizer

As suggested by their name, plasticizers are those substances that increases the elasticity or fluidity
of a material. Polyester plasticizers consists of low molecular weight ranging between 500-5000.
1.3.2.3. Polyester Resin

Manufactured resins which came into being with the reaction of poly-condensation products
of di-carboxylic acids with di-hydroxy alcohols.
1.3.2.4. Polyester Imide
When the ester and imide groups are present in the chain of a polymer, such polymer is known as
polyester imide.
1.3.3. On the Basis of Structural Differences/Bonding

Polyesters can also be classified on the basis of structural differences as saturated and unsaturated
polyesters.
1.3.3.1. Saturated Polyesters

Saturated polyesters refer to that family of polyesters in which the polyester backbones are saturated.
They are thus not as reactive as unsaturated polyesters. They are formed by reacting glycols such as ethylene
glycol. Another method of the production of saturated polyesters incorporates acids or anhydrous acids.
They consist of low molecular weight liquids used as plasticizers and as reactants in forming urethane
polymers, and linear, high molecular weight thermoplastics such as polyethylene terephthalate.
1.3.3.2. Unsaturated Polyesters

Unsaturated polyesters refer to that family of polyesters in which the backbone consists of alkyl thermosetting
resins characterized by vinyl unsaturation. When it comes to formation, unsaturated polyesters can be formed
by the reaction of glycols (mainly ethylene glycol), un-saturated dibasic acids or anhydrides. Since these types
of polyesters are thermosetting, they find their applications in reinforced plastics for making tray containers
and panels. They are mostly used in reinforced plastics.
1.3.3.3. Classification of Unsaturated Polyesters

Unsaturated polyesters are divided into types or classes depending upon the structure of the basic
building block. These are Orthophthalic, Isophthalic, Bisphenol, Fumarate, Chlorendic and Dicyclopentadiene.
The classification of unsaturated is given in Table 01-1.
2
Table 01-1: Classification of Unsaturated Polyesters:
Class Characteristics Uses

Orthophthalics Rigid, Resistant to abrasion, Boats, tub/shower, spas,
Dicyclopentadiene light in colour marble, consumer products,
buttons, corrugated sheet,
building panels, seating,
decorative products
Ophthalics/Terephthalics Tough, good impact and overall Automotive parts, gel coats,
mechanical properties, resistant electrical, bowling balls, trays,
to environmental elements and gasoline tanks, septic tanks,
moderate chemical attack. swimming pools, tooling,
Highly resistant to aromatics aerospace products,
construction products
Chlorendic Rigid, high heat distortion, Corrosion resistant tanks,
highly resistant to oxidizing ducting, stacks, industrial
chemical environments. vessels
Bisphenol-A Rigid, high heat distortion, Corrosion resistant tanks,
highly resistant to most piping, stacks, industrial vessels
chemical environments
particularly caustics
1.4. Importance of Polyester

The relatively easy accessible raw material like PTA or DMT and MEG.
The very well understood and described simple chemical process of polyester synthesis.
The low toxicity level of all raw materials and side products during polyester production and
processing.
The possibility to produce PET in a closed loop at low emissions to the environment.
The outstanding mechanical and chemical properties of polyester.
The recyclability.
The wide variety of intermediate and final products made of polyester.
1.5. Consumption of Polyester

They can be used in nonwoven textiles, cover stock for diapers as filters, fiber balls and felts. According
to a survey that was carried out in 1990, 38.3% of polyesters are used in industrial as well as consumer textiles.
In terms of their usage in industrial as well consumer textiles, seatbelts, fish netting, laundry bags, tents and
paper and fiber reinforcements are some of the uses of polyesters.
Talking about the apparel sector which consumers around 39.4% of the polyester fiber that is
produced every year, top weight fabrics, underwear, night wear and high pile fabrics are made using
polyesters. Now talking about household and interior textiles, 16.9% of the polyesters that are produced every
year are consumed in this sector. Major consumption includes sheets and pillow cases, blankets, bed ticking
and towels. Lastly, carpets and rugs use 5.4% of the polyester fibers and are produced annually.
3
1.6. Uses of Polyester
As polyesters usually offer high tenacity and durability, it is often used in outerwear. The overall
strength of the fiber is so high that it can withstand constant and repetitive movements. In addition to the
tenacity and durability, most polyesters that are in use in todays market have very high hydro-phobic
properties. Thus, they can be used in wet environments without any damage to the outerwear. It is often used
in pants, shirts, suits and bed-sheets either by itself or as a blend because of its wrinkle resistant property and
its ability to retain its shape.
1.6.1. Usage of Polyester Films

Polyester films can be used for packaging, electrical applications, industrial uses, and in imaging as
well as magnetics. In terms of packaging, the polyester films can be used for flexible pouches, snacks, barrier
films and vacuum insulation panels.
In industries, adhesive tapes, plastic cards, labels, lamination films and enhancement films are made
up of polyester films. As far as its usage in electrical equipment is concerned, motor wires and cables as well
as transformer insulation wires can be made from polyester films. In magnetics, video tapes, audio cassettes
while in case of imaging, micro-film printing and X-ray films use the polyester films.
1.6.2. Usage of Polyester in Medical Field

Polyester films can be used for packaging, electrical applications, industrial uses, and in imaging as
well as magnetics. In terms of packaging, the polyester films can be used for flexible pouches, snacks, barrier
films and vacuum insulation panels.
In industries, adhesive tapes, plastic cards, labels, lamination films and enhancement films are made
up of polyester films. As far as its usage in electrical equipment is concerned, motor wires and cables as well
as transformer insulation wires can be made from polyester films. In magnetics, video tapes, audio cassettes
while in case of imaging, micro-film printing and X-ray films use the polyester films.
1.6.3. Usage of Polyester Fibers

Uses of Polyester Fibers
One of the major uses of polyesters comes in the fabric industry. From needle punched fabrics
to geo textiles, from auto-motives to filtration industries, there is not a single corner of industrial or
domestic life where polyester fibers arent used. Needle punched fabrics find their usage in quilts,
sleeping bags, car fabrics and winter cloths.
Talking about geo-textiles and although it is an emerging field, geo-textiles are used to make
roads, pools due to their good strength as well as durability. In the filtration industries, non-woven
fabrics can be used in air filtration, water filtration, and oil filtration sectors. Talking about wadding,
polyester staple fiber is used in the wadding industry. Due to its low cost, high durability and long
life, polyester fibers are used worldwide in cars.
One of the major uses of polyester fibers are in our homes. From sofa sets to pillows and toys
as well as furnitures, there is probably no area of domestic life which the polyester fibers havent
made better. While polyester fibers are good for usage, new techniques have made huge leaps in
making them environment friendly. With the usage of recycled polyester fibers, the burden on
environmental pollution will be quite less.
4
1.7. Polyester Fiber
Polyester fiber is a manufactured fiber in which the fiber forming substance is any long-chain synthetic
polymer composed of at least 85% by weight of an ester of a substituted aromatic carboxylic acid, including
but not restricted to substituted Terephthalic units, p(-R-O-CO-C6H6-CO-O-) and para-substituted hydroxyl-
benzoate units, p(-R-O-CO-C6H6-O-).
By far, the greatest use of polyester is in synthetic fibers, primarily for apparel. Polyester fibers provide
ease of care benefits in apparel and improved mill processing economics on modern, high productivity
machines, its high mechanical properties, good thermal stability, low moisture regain, rot resistance and
abrasion resistance make it useful in a wide range of non-apparel and industrial applications, such as hose
cord, ropes, sailcloth, coated sheeting, conveyor belts, pillows, sleeping bags and carpet.
1.7.1. Criteria for Fiber Forming Polymers

There are different criterions that must be satisfied for a polymer to be fiber forming. These are:
1. A fiber forming polymer should possess sufficiently high molecular weight with preferably narrow
molecular weight distribution. High structural regularity for inherent capacity to crystallize and polar
groups for easy absorption of moisture, dyes, finishes and textile auxiliaries.
2. A fiber making substance should have long molecules so that sufficient length to breadth ratio can be
obtained in fiber produced from it.
3. The polymer should have high degree of inter-molecular cohesion power. Inter-molecular cohesion is
generally expressed in terms of crystallinity of polar characteristics.
4. A fiber forming polymer may also possess rubber-like properties in certain conditions. It will impart
the polymer, a sensitiveness to thermal and mechanical influence. At certain conditions, the polymer
should behave brittle, glass-like amorphous character and sometimes hard crystalline properties. The
fiber making process requires the polymer to traverse the plastic, rubbery and oriented states for the
production of useful properties.
5. At normal working conditions, the polymer should withstand certain treatment in terms of mechanical
properties, thermal properties and chemical properties. So the polymer should have,
i. A high softening point
ii. Adequate tensile strength over a fairly wide temperature range.
iii. A proper modulus or stiffness.
A history of man-made fibers is given in Error! Reference source not found..
1.8. Economical Prospective

Polymers have changed dramatically many aspects of human life since the launch of their commercial
mass production in the beginning of the last century. 235 million tons of synthetic polymers were consumed
worldwide in 2003 by important economic sectors such as electro- and electronic industry, packaging industry,
building and construction, and automobile industry among others. They are replacing metals in different walks
of life because of their distinctive properties.
Polyethylene terephthalate (PET) is one of the widely applied polymers. From annual production
viewpoint, PET is in the second rank among synthetic polymers equally with polypropylene. This is due to its
excellent balance of properties such as impact strength, resistance to creep under pressure, low permeability
to carbon dioxide, high melting point, thermal and hydrolytic stability.
5
Table 1-2: History of Man-Made Fiber
Date Fiber First Commercial Production

1910 Rayon The first man-made fiber.
The first commercial production of rayon fiber in the United States was
in 1910 by the American Viscose Company.
By using two different chemicals and manufacturing techniques, two
basic types of rayon were developed. They were viscose rayon and
cuprammonium rayon.
Today, there are no producers of rayon in the U.S.
1924 Acetate The first commercial production of acetate fiber in the United States was
in 1924 by the Celanese Corporation.
1939 Nylon The first commercial production of acrylic fiber in the United States was
in 1950 by E.I. du Pont de Nemours & Company, Inc.
1950 Acrylic The first commercial production of acrylic fiber in the United States was
in 1950 by E.I. du Pont de Nemours & Company, Inc.
1953 Polyester The first commercial production of polyester fiber in the United States
was in 1953 by E.I. du Pont de Nemours & Company, Inc.
Polyester is the most used man-made fiber in the U.S.
1954 Triacetate The first commercial production of triacetate fiber in the United States
was in 1954 by the Celanese Corporation.
Domestic Triacetate production was discontinued in 1985.
1959 Spandex The first commercial production of spandex fiber in the United States
was in 1959 by E.I. du Pont de Nemours & Company, Inc.
It is an elastomeric man-made fiber (able to stretch at least 100% and
snap back like natural rubber.
Spandex is used in filament form.
1961 Polyolefin / The first commercial production of an olefin fiber manufactured in the
Polypropyle U.S. was by Hercules Incorporated.
ne In 1966, polyolefin was the worlds first and only Nobel-Prize winning
fiber.
1989 Micro The first commercial production of micro-fiber in the U.S. was in 1989
fibers/Micr by E.I. du Pont de Nemours & Company, Inc. Today micro-fibers are
odenier produced in a variety of synthetic fibers (i.e. polyester, nylon, acrylic,
etc.).
The true definition of a micro fiber is a fiber that has less than one denier
per filament. Micro-Fiber is the thinnest, finest of all man-made fibers.
It is finer than the most delicate silk.
To relate it to something more familiara human hair is more than 100
times the size of some micro fibers.
1993 Lyocell The first commercial production of lyocell in the U.S. was in 1993 by
Courtaulds Fibers, under the TencelA trade name.
Environmentally friendly, lyocell is produced from the wood pulp of
trees grown specifically for this purpose. It is specially processed, using
a solvent spinning technique in which the dissolving agent is recycled,
reducing environmental effluents.
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1.9. Uses of PET Polyester
1.9.1. Uses of Polyester for Apparel Purposes
Continuous polyester filament by virtue of its strength and dimensional stability has been widely used
in fine and delicate dress material, nets and tires, but its great success has been in blends with some of the
natural fibers in its staple form. In blends with cotton it has been popular for shirts which need little ironing.
Polyester is frequently claimed for light garments, e.g. blouses and lingerie made from synthetic fibers that
need no ironing. In the staple form polyester has been used for socks, which are fairly comfortable.
1.9.2. Industrial Uses

Polyester fibers are continuously finding new industrial uses such as sewing threads, reinforcement
for V-belts, industrial hoses, tarpaulins, conveyer belts, tent clothes, sail clothes and electrical insulation
material. A very important usage in recent years has been permanent press garments avoids all further ironing.
1.9.2.1. Conveyer belts, V-belts

Polyester fiber endowed with most of the properties required for belts and cords and is best suited among all
fibers for use as belt cloth. That is because of high strength low elongation, resistance to abrasion heat,
corrosion, including resistance of fungi, bacterial, and chemicals.
1.9.2.2. Ropes, Fishing Nets

Polyester fiber ropes are in numerous respects more superior to ropes made from other fibers,
particularly in regard to their use in ships, fishing industry, mining etc., as they possess excellent water
resistant and anti-corrosion properties, the other characteristics which make the fiber popular for ropes for
high tenacity, low elongation, low moisture regains, resistant to weathering, corrosions, chemicals and
abrasions.
Fishing nets of polyester fibers are used for fishing trawlers, due to their extremely low water
absorption and they are extremely high at the high time of haulage from the sea and also allowed to be rapidly
dried.
1.9.2.3. Sewing Threads

Due to the intrinsic properties of the polyester fiber such as outstanding tenacity and elongation, as
well as high resistance to heat. They can be put to wide range of use. Moreover, their initial high modulus of
elasticity, resistance to friction and minimal and shrinkage in boiling water not only facilitates saving, but also
enables the seams to finished beautifully. For these reasons they are expected to replace cotton and silk
sewing threads in future.
1.9.2.4. Filter Cloth

Polyester filament yarn is suitable for filter cloth due to resistance against specially inorganic and
organic acids, high tenacity and low elongation and resistance to bacteria and fungi. All conceivable types of
filter cloth can be made with the use of polyester filament yarn and polyester spun yarn.
7
1.9.2.5. Dryer Canvases
Dryer canvases for paper manufacture are subjected to the most severe conditions found in textile
usage. Polyester fiber exhibits most excellent results because of characteristics such as, considerable wet
strength and resistance to abrasions on wetting, low wet elongation, low absorption of water and rapid drying,
resistance to heat, and high dimensional stability.
1.9.2.6. Hoses
Polyester fiber possesses outstanding qualities for fire and industrial hoses as it is endowed with the
following properties required for fibers in use for hoses:
High strength, especially a high wet strength and low elongation.

Considerable resistance to abrasion in the wet state.
Excellent low water absorption and rapid drying.
Resistance to chemicals and corrosion (fungi and bacteria).
Powerful heat resistance.
1.9.2.7. Woven belts

Polyester fiber has also been used (100%) as a woven belt in paper making to convey the paper web
over heated cylinders in the last stages of drying the requirements for a paper machine belt are that it shall
be resistant to temperature of 120oC and moisture, resistant to acid which arises from the use of aluminium
sulphates a filter for paper, as well as microbial attack when the machine is left standing and shall be resistant
to abrasion caused by the continuous flexing and rubbing of the belt at high speed. In one instance a polyester
belt lasted for 2.5 years, whereas the average life of belts formally used was about 6 months.
1.9.2.8. Electrical Insulators

Most of the synthetic fibers have good dielectric properties, but none of them (apart from the very expensive
Teflon) has good resistance to high temperatures, and since motors and electric gears are inclined to run hot,
this resistance to heat is valuable. Insulators have been mainly required to withstand 105oC but there is a trend
towards higher temperature motors. Polyester is included in the I.E.C. (International Electrical Technical
Commission) classification as a class E insulator. Polyester electrical fabric is heat set at 220 oC to obtain
adequate dimensional stability to the varnishing temperatures. The fabric can be hot slit to form straight or
bias taps, polyester filament yarns are also used for tapping bat wires.
1.9.2.9. Protective Clothing

The chemical resistance of polyesters towards acid makes it useful for protective clothing and it is
used on acid handling plants. A special use for anode is hydrofluoric acid, which no fibers other than Teflon
and polyester has enabled it to use for some water filtration work where cotton and wool had been
unsatisfactory.
1.9.2.10. Photographic Film

PET is treated with gelatin to prepare photographic film. A fine coating of gelatin enhances the
photographic effect.
1.9.3. Other Uses

A fiberfill is made from polyester for filling pillows, it is fluffy, resilient from crushing, non-allergic and
easy to wash and dry. Quilts something like these, but thinner and fatter are made from polyester, as a tie
fabric, polyester is superb.
Curtains in polyester net are popular, and because there resistance behind glass to sunlight is good
and because polyester can be died fast they usually have a long life.
8
It is frequently claimed for light garments e.g. blouse and lingeries made from synthetic fibers that
need no ironing. This may be true if they are washed very carefully, so threat no compression is applied whilst
wet and crumpling, there are no sharp creases but nevertheless, such garments those made from polyester
can be washed almost indefinitely, blouses which drape like heavy silk but can be washed like cotton are made
from polyester, whereas nylon is subjected to disadvantage that after long wear it grey. Polyester does not
suffer from this defect, so that the useful life of polyester garments would not be cut short.
1.10. Conversion of Chips to PET Fiber

In the final stage of the polymer manufacture process, the polymer is quenched and cut into chips
for easy handling, it is then re-melted, filtered and extruded through a pattern of fine holes in a spinneret
plate, quenched in air and wound up in spin bobbin. And then it is further stretched or drawn which give
stability and strength to drawn fibers.
The general methods for the conversion of organic polymers to fibers are known as spinning technology.
1.10.1. Spinning
The term spinning means any process that produces continuous filaments, yarns or threads. Spinning
turns short staple fibers such as cotton or wool and relatively short filaments or fiber strands such as flax,
ramie, jute, sisal etc. into continuous yarns. The mass of fibers or fiber strands is parallelized by carding and
combing processes into silvers and roving from they are appropriately picked up in the spinning frame in well-
designed clusters under controlled speed and then twisted together so that the fibers duly grip one another
to produce what known as spun yarn.
For man-made fibers, the fiber-forming polymer, made randomly flow-able by
1. Melting
2. Dissolution in a suitable solvent medium, is extruded or spun out through the fine holes of a spinneret
as fine continuous filaments.
The extruded melt/solution jets or filaments of any length are suitably hardened by following
processes
1. Cooling and drawing (melt spinning)
2. Solvent evaporation (dry-spinning) in a hot chamber in some cases.
3. Polymer coagulation or regeneration in a non-solvent medium contained in an open trough or vessel
(wet spinning).
A drawing process subsequent or even simultaneous to spinning is commonly followed in each case.
Continuous fine filaments spun and axially oriented in this way, and crimped if desired, may be cut into
fiber clusters of convenient short staple lengths. These may then be further spun into yarns applying
appropriate drawing and twists in much the same way as for cotton and other staple fibers.
The essential step of any spinning technique is the transformation of a solid polymer into a liquid state
so that it may be extruded through fine holes and the emergent jets then returned without loss of form
to a coherent solid state. A practical spinning technology and machine must be sufficiently flexible in
operation to allow the efficient and economic production of a wide range of yarns of high quality and
uniformity. By a wide range of yarns is meant a variety of filament numbers, diameters and physical
properties from one given polymer type.
9
1.11. Types of Spinning
There are two types of spinning processes:
1. Melt spinning
2. Dry spinning
1.11.1. Melt Spinning

Melt spinning and heat advancing are two distinct physical processes. The one being involving a low
tension process at a temperature just above the melting point, the other involving relatively high tension at a
temperature a little above the glass rubber transition point. In an engineering sense, these two processes can
be carried out continuously on a single spin draw unit.
The processing equipment for continuous filament yarn and staple fiber is very similar of converting
chips into fibers.
There are two main processes:
1. The spinning process

2. The drawing process
1.11.1.1. Spinning Process

For a melt spun fiber, the term spinning include melting, filtering, extrusion, quenching and wind up.
In the molten state, polyethylene terephthalate degrade rapidly in the presence of oxygen and moisture,
which must therefore be excluded during spinning. Degradation results in a reduction of the molecular weight
of the polymer, which may be measured in lowering of the melt viscosity or of the intrinsic viscosity, as
measured in some suitable solvent.
In the melt head of spinning units dried polymer chips are gravity fed from a storage hopper and are
melted in an oxygen free atmosphere against a heated plate or grid. A gear type of pump is used to control
the flow of molten polymer and the polymer is filtered before being extruded through a spinneret in to air at
room temperature. In the continuous filament yarn process, the multifilament thread line is converged several
feed below the spinneret and passed over slowly rotating spin finish wheel, which applies oil in water emulsion
in order to lubricate the yarn and reduce static. The yarn is collected finally on a spill bobbin, which is surface
driven at a constant speed of several thousand feet per minute.
Yarns from several spinnerets are converted into one large and wound up at constant speed on
aluminium cans.
During the spinning process, polyethylene terephthalate are quenched rapidly below tile glass rubber
temperature (80oC) and spun yarn is completely amorphous. In the solid state, polyethylene terephthalate can
be amorphous or process various degrees of crystallinity depending on its thermal and mechanical condition
and density of material can be used as a measure of its crystallinity.
Synthetic fiber derive their strength and flexibility largely from the presence of oriented polymer chain
units locked in position chemical cross-links, but no crystallization or orientation processes are possible below
80oC, its glass rubber transition temperature. Below this temperature the amorphous regions are locked by a
glass like structure and unable to yield to applied stress, but above 80oC, certain molecular segments possess
sufficient thermal energy to revolve so that under applied stress the polymer molecules will be able to wriggle
past each other, become oriented and crystallized.
10
1.11.1.2. Drawing Process
Upon extrusion from the spinneret the PET filament does not have all the desired characteristics
because of the random arrangement of the super polymer molecules. The fibers are therefore drawn or
elongated.
The temperature conditions and the extent to which the fibers are drawn depend upon the properties
desired, the pet fibers are usually drawn to 5 times their original length (which results in a fiber diameter that
is one fifth the original size upon extrusion from the spinneret) of higher tenacity fiber is to be produced, the
filaments are drawn to a greater extent, as this increases the linear molecular orientation of the fiber, as they
emerge from the drawing process and meet cold air, the filaments solidify generally, the PET polyester
filaments are drawn hot because this procedure produces more uniform fibers.
Below the glass-rubber transition temperature of 80oC, the tensions required to draw spun filaments
of polyethylene terephthalate are likely to break them or at least produce voids in the filaments. Temperature
well above 80oC the material is rubber like and draws in spinning stretch. A pin is used rather than a plate,
because the drawing zone and ensure that the spin yarn is subjected to low feed tension. Drawing machine
may consist essentially of a feed roll, a hot pin, a draw roll and a standard ring and traveler wound up system.
The drawn yarn is called finally on drawn crystal bobbins and has about one turn per inch of twist in either s
or z series. Staple fiber drawing machine is designed on a similar principle to that used for filament but is of
much heavy construction and capable of dealing yarn tows of the order of several hundred thousand deniers.
After leaving tile staple fiber drawing machine, the drawn tow is feed into a crimping device. The
drawn crimpled tow is then heat set and cut into suitable staple fiber lengths by rotary cutter before passing
through an opening device which separates tile fibers and sprays them with textile dressing or finish. Bailing,
packing and labeling constitute the final stages of the staple fiber manufacturing process.
References:
1. Menachem Lewin and Eli. Pearce, Handbook of Fiber Chemistry, Second Edition, 1998, Marcel
Dekker, Inc.
2. Ludwig Bottenbruch, Engineering Thermoplastics: Polycarbonates, Polyacetals Polyesters, and

Cellulose Esters, 1996, Hanser/Grander Publications, Inc.
3. Arun Pal Aneja, Polyethylene Terephthalate Feedstock Selection and Process Options, Chemical Age
of India, 29(9), 1978.
11
Chapter 2
Process Selection
Chapter 2 Process Selection
Chapter 2: Process Selection

2.1. PET Polymerization
The preparation of the good quality polymer for the production of synthetic fibers is an important
step, since subsequent operation such as spinning, drawing, texturing and dyeing are greatly influenced by the
quality of the polymer. It is therefore essential to give proper attention to the polymerization process so that
smooth running of the subsequent fiber manufacturing operation is achieved and fibers with good properties
are achieved.
2.1.1. General Description of PET Polymerization

PET polymerization consists of two stages:
1. Esterification
2. Polycondensation
In the first step, esterification of acid and alcohol undergoes producing an intermediate (bis-
hydroxyethylene terephthalate, (BHET) as the main monomer for Polycondensation. Regarding a reversible
reaction, the side product is extracted in order to perform reaction up to high conversions. In the second step
that is called as polycondensation oligomers and polymer chains undergo reaction to produce long polymer.
The by-product of polycondensation is removed in order to increase the rate of polycondensation and chain
length.
2.1.2. Why Two Step Reaction?

In order to get a high molecular weight PET essential for fiber formation, it is necessary that the two
raw materials are present during polymerization reaction in equimolar proportion (1:1). To ensure this
stoichiometric ratio of 1:1, a preliminary reaction is carried out between TPA and EG producing a new
intermediate, BHET. This is further polymerized in the second step or polycondensation to get PET. The
intermediate formation leads to a number of advantages compared to a direct mixture of monomers subjected
to polycondensation. These are:
i. Polycondensation process is carried out to a uniform, chemically pure, monomeric starting

material.
ii. Wider choice of catalysts.
iii. Less side reactions.
iv. Higher speed of reaction.
v. Good color of polyester.
vi. Better thermal stability of melt.
vii. Better drawability.
2.2. Types of PET Polymerization

PET polymerization can be carried out in two ways:
1. Batch Process
2. Continuous Process
2.2.1. Batch Process

When a high molecular weight polymer of high purity is needed, batch process is recommended and
mostly used (either using TPA or DMT). The illustration of batch process is given by solid phase polymerization.
12
2.2.1.1. Solid Phase Polymerization (SPP)
Continuous polymerization units of either type are quite satisfactory for fibers, films or cast objects of
relatively modest molecular weight (0.6 intrinsic viscosity) produced on large continuously operating
equipment. When high molecular weight polymer of high purity is required, however, particularly for a
discontinuous operation, solid phase polymerization can be attractive.
In this process, chips, usually from a conventional finisher, are pre-crystallized in a tumble drier at 140-
150oC, the temperature is then raised, and polymerization is carried out under high vacuum or inert gas sweep.
Although solid state diffusion is slower than diffusion through a liquid, the distance involved are much shorter
so the overall effect is to raise molecular weight quickly. Since the reaction temperature is below the molecular
weight quickly. Since the reaction temperature is below the softening point, the chips do not sinter together
and the lower reaction temperature disfavors the degradation reaction.
All melt polymerizations reach an equilibrium stage where the chain-forming and chain breaking
reactions balance each other and no net chain growth occurs. Solid-sate polymerization works because it
allows chain-growth to proceed while minimizing chain-breaking, owing to the different kinetics and activation
energies of the two different sets of reactions. Usually melt-polymerized PET has an intrinsic viscosity (IV) of
about 0.67. It is quite possible by using the SPP process to raise the IV to 0.8-1.10.
2.2.2. Continuous Process

Continuous process for the polymerization of PET can be divided into two types, on the basis of raw
materials:
1. Transesterification Process (DMT Process)

2. Direct Esterification Process (TPA Process)
2.3. Advantages of Continuous Process over Batch Process

We have selected the Continuous Process on the basis of the several advantages that the continuous
process have over the batch process. A comparison of advantages of continuous process over batch process
is given in Table 2-1.
13
Table 2-1: Comparison between Batch and Continuous Process for PET Production
Batch Process Continuous Process

More economical for small scale production than More economical for large scale mass production
continuous process and savings regard to personnel, buildings etc. will
be significant in comparison to batch process. This is
because of higher volumes of output results in a
lower per unit cost.
Product quality may vary from batch to batch. In continuous process a high degree of uniformity is
achieved. This is because, the application of
continuous process permits automation to a wide
extent and the continuous monitoring of the
intermediates allows continuous and constant
process control. This results in a high product
uniformity which is a pre-requisite for trouble-free
spinning and drawing operation.
More production losses as compared to the Less production losses as compared to batch
continuous process. This is because at the start-up process.
and completion, production losses take place.
Polymerization and spinning units operate Polymerization and spinning units operate
independently. continuously.
2.4. Contrasting the DMT & TPA Processes

PET resins are produced commercially from ethylene glycol (EG) and either Dimethyl terephthalate
(DMT) or Terephthalic acid (TPA). DMT and TPA are solids. MDT has a melting point of 240 oC, while TPA
sublimes (goes directly from the solid phase to the gaseous phase). Both processes first produce the
intermediate Bis-hydroxyethyl terephthalate (BHET) monomer and either methanol (DMT Process) or water
(TPA Process). The BHET monomer is then polymerized under reduced pressure with heat and catalyst to
produce PET resins.
2.5. Difference between DMT & TPA Processes

The main difference between DMT and TPA processes is that of the starting material. The older
process used:
i. Dimethyl terephthalate (DMT)

ii. Ethylene Glycol (EG)
As starting materials, it was because of the non-availability of terephthalic acid of sufficient purity in
the early years of the polyester production. This reason behind this was that TPA was a rather intractable
substance and is sparingly soluble in most solvents, and sublimes without melting at about 300oC. It was
therefore difficult to purify and polymerize.
14
2.6. Transesterification Process
This polymerization process was based upon an ester-interchange (EI) reaction between DMT and EG.
In the ester-interchange process, DMT and an excess of glycol are heated together in the presence of various
EI catalysts. Manganese (II) acetate or zinc (II) acetate is typically used for this transesterification step, these
being the best catalysts for this reaction.
The methyl ester group undergoes an exchange reaction with the glycol hydroxyl groups and the much
more volatile methanol distills out, via a fractionating column, thus upsetting the equilibrium, and driving the
reaction to completion. The product is a mixture of BHET and low molecular weight oligomers.
In the second step, the DGT is heated to about 280oC under high vacuum to carry out melt phase
polycondensation. The principle volatile eliminated is EG.
For the second step in the DMT route, the catalyst from the first step (zing or manganese) is
sequestered or deactivated with phosphoric acid and another catalyst for polycondensation, most commonly
antimony triacetate or antimony trioxide is added. This is because zinc and manganese are considered poor
polycondensation catalysts. The literature indicates that the reactivity of metals for the polycondensation
reaction (second step) follows the trend Ti>Sn>Sb>Ge>Mn>Zn. Moreover, for the first step, namely the
transesterification of DMT with EG, the catalytic activity trend follows the reverse order, with zinc being
amongst the most active. For the polycondensation reaction, Sb compounds are commercially established
(compared with Sn and Ti) because the resulting polymer has the most favorable balance of properties. Note,
in a usual operation, it is possible to go from step 1 to step 2 without isolating the DGE. However, if desired,
the DGT and oligomers formed in step 1 can be isolated and used later for melt polycondensation (step 2).
2.7. Take Over of DMT Process by TPA Process

However, the arrival of commercial grade TPA at an economic price made the reaction of EG and TPA
possible and the DMT process then took over. The DMT route is also economically unfavorable because of the
involvement of methanol and the additional step needed to produce DMT from terephthalic acid and
methanol. The production of methanol in the DMT process creates the need for methanol recovery and
purification operations. In addition, this methanol can produce major VOC emissions. To avoid the need to
recover and purify the methanol and to eliminate the potential VOC emissions, newer plants tend to use the
TPA Process.
2.8. Basis for the Process Selection

2.8.1. Advantages of TPA over DMT
We have selected TPA route on the basis of the following advantages that the TPA route has over the
DMT route.
1. When EG is treated with DMT, methanol is produced as by-product. By means of distillation the by-
product is separated but on the other hand, TPA route does not give any by-product which is to be
distilled of. The capacity of the plant increases in TPA route.
2. Because methanol is eliminated from the process system, polymerization rates tend to be higher and
polymer quality is improved.
3. TPA gives about 15% higher yield of polyester as compared with DMT due to difference in molecular
weights.
4. TPA gives higher production due to faster rate of esterification, reduced glycol to be taken off in
polycondensation and reduced raw material weight to produce ratio.
5. The capital investment to construct a polyester fiber plant based on TPA is at least 20% less than one
based on DMT.
6. TPA process needs less EG as compared with DMT. Thus less EG is to be recovered during
polycondensation resulting in lower investment for EG recovery and recycle system. This in turn
promote energy conservation.
15
7. TPA has high bulk density than DMT and hence requires less storage as compared with DMT.
8. TPA process is safe as methanol is not evolved during esterification while in DMT process methanol is
produced as by-product. Methanol is highly inflammable and can cause explosion, so the system must
have explosion proof equipment which add to capital cost in DMT process.
9. Catalyst is used either in very small quantity or not used in TPA esterification. This gives better color
of the polymer, higher spin pack life in spinning and lower breakages in stretching.
10. The time to reach a given molecular weight is less with TPA than with its dimethyl ester.
16
Chapter 3
Process Description
Chapter 3 Selected Process Description
Chapter 3: Selected Process Description
3.1. Direct Esterification

This industrial method uses raw materials
i. Purified Terepthalic Acid (TPA)

ii. Ethylene Glycol (EG)
TPA is used instead of DMT and so it is called the TPA process. Because methanol is eliminated from
the process system, polymerization rates tend to be higher and polymer quality is improved. Also the metal
content of the TPA polymer is less than the DMT polymer, as only one catalyst (for polycondensation) is used
for step 2, and hence the thermal stability of the polymer is higher.
The TPA route to PET is made up of two steps. The first is the esterification of terephthalic acid with
ethylene glycol (EG) to convert to pre-polymer that contains Bis-hydroxyethyl terephthalate (BHET) and short
chain oligomers.
The esterification is not complete, and some acid end-groups remain in the pre-polymer. The
esterification by-product water is removed via a column system.
The second reaction step is polycondensation, in which mainly the following transesterification
reaction, lead to step-growth polymerization in the melt phase.
The reversible nature of the reactions demand that the condensates ethylene glycol (EG) and water
are removed from the melt efficiently by using high vacuum.
3.2. Reactions
In the early stages of the process, esterification reactions are dominant. These reactions are reversible
with equilibrium constants close to unity. Polymerization reactions involve the nucleophilic attack of the
terminal ester group. In one chain by the terminal alcohol group of a second chain. These reactions lead to
rapid molecular growth. The polymerization reactions are also reversible, with the equilibrium constant
slightly below unity.
Rearrangement reactions involve ester groups inside the chain. These reactions are responsible for
randomizing the molecular weight distribution and redistributing segments inside the polymer chain. Since
the number of internal ester group is much higher than the number of terminal ester groups, the molecular
weight distribution approaches the most probable distribution.
3.3. Raw Materials

3.3.1. Ethylene Glycol
Ethanediol is obtained from ethylene which is an abundant supply from the thermal cracking of oil. In
the older industrial process ethene reacts with chlorine and water under pressure to form 1-chloro-2-
hydroxyethane (chlorohydrin)
Which is then hydrolyzed with lime slurry or with sodium hydroxide solution to 1,2-epoxyethane
(ethylene oxide).
A more modern process oxidizes ethane directly to 1,2-epoxyethane using air and a silver catalyst at
250-325oC and 1-3 MPa. Direct oxidation avoids the use of chlorine (which is converted to a by-product
without value, but is complex with an expensive catalyst, and needs careful control-some of ethane is oxidized
through to carbon dioxide.
16
The epoxy-ethane is converted to the diol by reaction with water at about 180oC. A specification sheet
of properties of ethylene glycol (EG) is given in Table 3-1
Table 3-1: Specification Sheet of Mono-Ethylene Glycol
Molecular Formula C2H6O2

Molecular Weight 62 g/mol
Appearance Colorless viscous liquid
Specific gravity 1.115 at 20oC
Specific heat 0.56 kcal/kg (at 20oC)
Boiling Point >197
Melting Point -13oC
Auto ignition temperature 400oC
Flash Point (closed cup) 111oC
Vapor density 2.1 (air = 1)
Solubility in water Miscible in all proportions
Lower flammable limits in air 3.2 approx.
Upper flammable limits in air 15.3 approx.
Explosion limits 3.2-15.3%
Vapor pressure 0.08 mmHg at 20oC
3.3.2. Terephthalic Acid

The principle route to TPA is oxidation of 1,4-dimethlbenzene (p-xylene). P-xylene comes from the
C8-fraction of naphtha that is distilled from petroleum. Distillation of mineral oil produces a fraction which
consists of alkyl-substituted cycloalkane hydrocarbons. Treatment with hydrogen under pressure at about
500oC, in contact with molybdenum oxide and alumina catalysts, dehydrogenates the cycloalkanes to
aromatics.
Fractional distillation of the mixed aromatics gives a xylene fraction which typically, is composed of:
i. 1,3-dimethylbenzene 45% (B.P. 139oC, M.P. 48oC)

ii. 1,2-dimethylbenzene 22% (B.P. 144oC, M.P. 25oC)
iii. 1,4-dimethylbenzene 20% (B.P. 138oC, M.P 13oC)
iv. Ethyl benzene 13% (B.P. 136oC, M.P. 95oC)
The boiling points are too closed together for economic separation by fractional distillation, but the
higher melting 1,4-dimethylbenzene can be separated by crystallization from the cooled liquid. Several stages
are needed to obtain the maximum yield of the isomer at better than 98% purity. The proportion 1,4-
dimethylbenzene in the xylene fraction is improved by isomerizing the ortho and meta isomers over metal
oxide catalysts, and the aromatization and isomerization stages can be combined.
There are several processes for the oxidation of 1,4-dimethylbenzede to acid. This route uses nitric
acid as oxidizing agent about 30% acid at 180oC or so. The product is contaminated with some nitro-substituted
acids.
Liquid phase catalytic air oxidation processes have been devised, and are now widely used. Cobalt
salts, or manganese salts activated by bromine, are employed as catalysts in acetic acid solution. Oxidation of
the first methyl group to carboxylic acid is easier than oxidation of the second, hence 4-methylbenzene
carboxylic acid (p-toluic acid) is the main impurity. Physical properties of terepthalic are given in Table 3-2
17
Table 3-2: Physical Properties of Terepthalic Acid
Molecular formula C8H6O4

Molecular weight 166.13 g/mol
Appearance White crystalline powder
Density 1.522 g/cm3
Specific heat 0.33 kcal/kg (at 30oC) or 1.0 kJ/kg.K
Melting point 425oC
Volatile contents 0.1%
Auto ignition temperature 495oC
Flash point (open cup) 260oC
Vapor density 5.74 (air=1)
Solubility in water 0.0017 g/100 ml at 25oC
3.4. Process Stage

The process consists of the following stages:
TPA unloading and storage

EG unloading and storage
Slurry making or paste preparation
Esterification stage
Polycondensation stage
Conversion of polymer into fiber
3.4.1. TPA Unloading and Storage

TPA is main raw material, which is transported in standard sized bags. Bags are stored in warehouse
and transported by the fork lifters to TPA handling area and lifted up to the charge hoppers. TPA is unpacked,
charged into the hopper (manually) and transported into the TPA silo by means of nitrogen pneumatic
conveyer. About the amount of one day production is stored in the day silo.
3.4.2. EG Unloading and Storage

EG is transported by tank lorry and stored in the storage tank for the consumption of three months. EG is
pumped up to the polymerization building through filter, in which contamination should be removed.
3.4.3. TDO and Catalyst Preparation

TDO is used for making white color and catalyst is used for accelerating the reaction. Both are prepared
one time per day batch wise. TDO is an abbreviation of titanium dioxide which is powder and transported in
bags. TDO powder is dispersed in the EG mixing tank equipped with special high speed rotor, the big particles
are separated in the centrifuge and finally TDO slurry is stored in the storage tank.
Catalyst (Antimony triacetate) which is also in powder form is dissolved in EG in the mixing tank and
big particles are separated by the filter and the catalyst solution is stored in the storage tank.
3.4.4. Slurry Making

TPA is transferred from the silo to the weighing tanks by means of nitrogen pneumatic conveyer. EG
is measured by flow meter and charged into the slurry mixing tank. The mole ration of EG and TPA is
approximately equal to the stoichiometric ratio (2:1) for the reaction and is controlled automatically. The
special type of agitator is applied for the mixing tank, the slurry is then transferred to the esterification stage
by positive displacement type pump.
18
3.4.5. Esterification Stage
A positive displacement pump leads the slurry with additives to the esterification stage, which consist
of two reactors arranged in series. In this esterification stage, TPA and EG react and get converted into BHET.
The reaction is typically un-catalyzed and form low molecular weight oligomers and water. Both the
esterification reactors are single vessels with turbine agitators (paddle type) having four baffles and inner coils.
In each of them reaction pressure is at 2-4 psig. This type of reactor has the advantage that heat transfer can
take place at relatively low temperature of heating surface due to high heat exchanger areas.
Thus the amount of unwanted diethylene glycol (DEG) formed is less and the negative influence of this
product on final product is low. The direct esterification is continued until the required degree of conversion
in the second stage is achieved. One thing which is worth mentioning here is that since esterification is
occurring from the beginning to the end of PET synthesis, it is an equilibrium reaction and thus removal of the
condensed water is necessary to minimize the hydrolysis of the formed ester group. After the required
retention the mixture is transferred from the first esterifier to the 2nd esterifier by the pump.
3.4.5.1. Addition of Stabilizer

Phosphoric acid stabilizer is introduced in the esterification reactor to reduce the degradation and
discoloration of PET polyester and to cool the catalyst, which encourages the degradation of the polymer
formed in the condensation reaction.
3.4.5.2. EG Recovery
Recovery and recycle of EG is important. The efficient recycling is realized by feeding the vapors to a
condenser, which condenses a solid glycol-oligomer solution for recycle. This solution is the introduced in a
distillation column to separate the reaction by produced (H2O) from EG.
3.4.5.3. Reactions
The reaction conditions in the Esterifier are given in Table 3-3.
Table 3-3: Reactor Conditions during Esterification Reaction
Estirifier Temperature Pressure Conversion (%)

(oC) (psig)
1 245 4 95
2 255 2 95
3.4.5.4. Reaction Parameters

Following are the reaction parameters in the esterifiers.
3.4.5.4.1. Temperature
Higher temperatures are needed for esterification, usually in the range of 240-260oC. This is because
at lower temperature the rate of reaction (or reactor performance) is limited by the low solubility of PTA in
EG and also PTA does not melt even at 225oC. Also like most of the other reactions the speed of esterification
approximately doubles with a 10oC rise in temperature.
3.4.5.4.2. Mole Ratio

Esterification is a reversible reaction and the extent of reaction depends on the relative amounts of
each component present. An excess of glycol is an advantage in the ester interchange reaction and it is
therefore generally encouraged so that shift of the reaction equilibrium directed towards the formation of
glycol ester is favorably affected. This is the reason that EG and TPA are used in a mole ratio of 2:1.
However, the use of a large excess also entails disadvantages, e.g. prolonging the total reaction time,
due to the necessity to distill off the excess of glycol and formation of higher amount of EG. Industrially,
19
however, the employment of a small excess has generally given satisfactory results so that the reaction is
performed, e.g. with about one half molar excess of glycol.
3.4.5.4.3. Retention Time

On theoretical basis, it is possible to complete the esterification reaction in less than 30 minutes,
however in actual practice, the corresponding equipment are designed for a reaction time of one to two hours.
In our esterifier retention time is four hours because, selecting that retention time the influences of temporary
disturbances of the process (e.g. power failures etc.) on the uniformity of the final product is minimized due
to the presence of large amounts of product in the apparatus. The influence of harmful side reactions is also
minimized.
3.4.6. Polycondensation
Polycondensation is carried out in three stage continuous polycondensation apparatus. In this step
polycondensation of BHET to PET occurs with the removal of EG as by-product. The reversible nature of the
reaction demands that the condensates ethylene glycol (EG) and water are removed from the melt efficiently
to assure rapid polymerization. This is done by carrying out polymerization under high vacuum. The degree of
vacuum in the reactors increases towards downstream so the vacuum degree of each reactor is moderate for
the degree of polymerization.
The first polycondensation reactor (low polymerizer) and the second polycondensation (intermediate
polymerizer) reactors are a series of stirred tank reactors with turbine type impellers (pitched blade). Because
in these two reactors, the melt viscosity remains relatively low, the EG and water condensation products
formed during the process can evaporate efficiently.
When the molecular weight increases further, the melt viscosity of PET becomes so high that bubble
formation is hindered even under applied vacuum, and EG and water have to diffuse out. Hence it is critical to
reduce the diffusion path at the following reaction stage in order to improve removal of EG and water.
Therefore to provide for the efficient removal of ethylene glycol, the polymerization should be carried out in
a vessel which provides for the maximum area generation and having an agitator that should provide for the
maximum exposure of the reaction mass to the effects of vacuum. These purposes are achieved in the third
polymerizer (high polymerizer) which is a wiped film or a disc reactor. The disc reactor consists of a heated
horizontal cylinder, which contains a number of discs in slanting positions. The discs are arranged in the form
of a cage without a continuous shaft, so that they are immersed in the material being poly-condensed and
transport the material slowly through the apparatus. A part of the material which is retained on the disk is
transported upwards from the sump and slides back again in the form of a thin film. The large surface area so
formed allows a quick removal of mono-ethylene glycol from the poly-condensing material.
The pressure differences and gravity causes the transport of poly-condensation material between the
three polycondensation stages. Polyester from the last polycondensation stage is either directly spun into
fibers, or extruded into 2-4mm thick strands that solidify due to the cooling and are cut into somewhat
cylindrical chips for future processing.
3.4.6.1. Reactions
The reactor conditions in ES-2 are given in Table 3-4
Table 3-4: Reactor Conditions during Esterification Reaction
Stage Temperature Pressure DoP

1 280 120 mbar 30
2 285 120 mbar 90
3 285 18 mbar 120
20
3.4.6.2. Reaction Parameters
3.4.6.2.1. Effect of Temperature
Degree of polymerization increases considerably when the temperature is raised from 265oC to 285oC.
The reaction speed is also increased by increasing the temperature. Raising temperature above 285oC exerts
a slight influence on the reaction speed and in general does not have a favorable effect on the characteristics
of the polycondensate. The thermal degradation of the polymer also increases with increase in temperature
from 285oC to 300oC.
Temperature below 260oC is also not used as the melting point of polyethylene terephthalate is about
260oC and hence some solidification of the polymer may occur at low temperature.
3.4.6.2.2. Effect of Pressure

In order to achieve an adequate degree of polycondensation, a high vacuum is necessary. Application
of high vacuum is useful in removing glycol vapors from the reaction vessel which facilitates in increasing the
reaction speed. Furthermore, according to the law of mass action, the removal of the glycol vapors from the
reaction vessel will shift the equilibrium towards further polycondensation.
3.4.6.2.3. Effect of Stirring

The rate of stirring during polycondensation has an effect on build-up of molecular chains with the
increase in stirring rate from 20 rpm to 80 rpm, the DP increases appreciably. At higher stirring rate, the
removal of the glycol vapors is quicker and hence degree of polymerization increases.
3.4.6.2.4. Catalyst
For better rate of reaction, increase in temperature alone does not help much as at higher temperature the
reactor performance is limited by the solid-liquid mass transfer rate i.e. the upper limit of temperature is
correlated with the boiling point of either alcohol or acid or the ester formed. Thus upper limit of temperature
will be governed by the most volatile component. It is therefore necessary that esterification reaction is carried
out in the presence of some suitable catalyst.
The traditional polymerization catalysts used in the formation of PET is antimony which has the best all-round
properties amongst PET catalysts during melt polymerization, leading to high productivity and polymers with
good thermal stability. The most common of the antimony-containing catalysts are antimony trioxide,
antimony triacetate which are added at the start of the polycondensation.
21
Chapter 4
Material Balance
Chapter 4 Material Balance
Chapter 4: Material Balance
The material balance is a very important stage in the plant design process and is applied in order to
determine the total mass entering and leaving the system (in our case, the polyester plant) as a whole as well
as the mass entering and leaving each component of the system separately. This is done in order to determent
the number as well as size of the equipment to be used and also for determining the energy requirements for
the whole process. Also it is an important need for better control of the process.
4.1. Nomenclature
The nomenclature of the terms used are given below:
ES-1 = Esterification Reactor No. 1

ES-2 = Esterification Reactor No. 2
PR-1 = Polymerization Reactor No. 1
PR-2 = Polymerization Reactor No. 2
PR-3 = Polycondensation Reactor
DP = Degree of Polymerization
Mw = Molecular Weight
TPA = Terephthalic Acid
EG = Ethylene Glycol
BHET = Bis-hydroxyethyl Terephthalate
x= Percentage Conversion
4.2. Reactions:
The reactions involved in the process are mentioned below:
1) TPA + 2EG BHET + H2O

2) n(BHET) (n-1)EG + PET
4.3. Molecular Weights of Materials
Molecular weight of TPA = 166 kg/kmole

Molecular weight of EG = 62 kg/kmole
Molecular weight of BHET = 254 kg/kmol
Molecular weight of repeating unit = 192 kg/kmole
Molecular weight of water = 18 kg/kmole
Molecular weight of PET = 23102.07 kg/kmole
17
4.4. Overall Material Balance
Required Capacity = 100 tons/day
Required Capacity = 4166.667 tons/hr.
4.4.1. Stoichiometric Calculations

4.4.1.1. Inlet Flow Rate of TPA (Basis = 1hr. operation)
23102.07 kg of PET requires TPA = 166.14 120
= 19936.8 kg/
19936.8
1 kg of PET Requires TPA = 23102.07
= 0.8630
4166.667 kg of PET Requires TPA = 0.863 4166.667
= 3595.782 kg.
4.4.1.2. Inlet Flow Rate of EG (Basis = 1hr. operation)
23102.07 kg of PET requires EG = 2 62.07 120
= 14896.8 kg
14896.8
1 kg of PET requires EG = = 0.645 kg
23102.07
4166.667 kg of PET requires EG = 0.645 4166.667 kg
= 2686.772 kg
EG Required = 2686.772 kg
EG Entering (10% excess) = 2686.772 1.1
EG Entering = 2955.45 kg
4.4.1.3. Total Amount of EG Recovered (nth iteration) - (Basis = 1hr.)
EG recovered = 1613.31 kg
Fresh EG required = 2955.45 1613.31
= 1342.1412 kg
4.4.1.4. Mass of Water in the Recycle Stream (Basis = 1 hr.)
Mass of water recycled = 84.91 kg
18
4.5. Nomenclature of Streams
M1 = Mass flow rate of TPA in kg/hr.
M2 = Mass flow rate of EG in kg/hr.
M3 = Mass flow rate of slurry (TPA + EG + Water) in kg/hr.
M4 = Mass flow rate of (EG + H2O) regenerated during reaction in Esterification Reactor-1 (ES-1)
in kg/hr.
M5 = Mass flow rate of BHET (monomer) + unreacted TPA + Unreacted EG + Water
M6 = Mass flow rate of (EG + H2O) regenerated during reaction in Esterification Reacton-2 (ES-2)
in kg/hr.
M7 = Mass flow rate of TPA (unreacted) + BHET in kg/hr. + Unreacted EG + Water
M8 = Mass flow rate of (EG + H2O) regenerated during reaction in Polycondensation Reactor-1
(PR-1) in kg/hr.
M9 = Mass flow rate of polymer formed in PR-1 in kg/hr.
M10 = Mass flow rate of (EG + H2O) regenerated in Polycondensation Reactor 2 (PR-2) in kg/hr.
M11 = Mass flow rate of polymer formed in PR-2 in kg/hr.
M12 = Mass flow rate of (EG + H2O) regenerated during polycondensation reaction in
Polycondensation Reactor-3 (PR-3) in kg/hr.
M13 = Mass flow rate of final product (PET) in kg/hr.
M14 = Mass flow rate of (EG + H2O) from distillation column in kg/hr.
M15 = Mass flow rate of 95% pure EG from distillation tower in kg/hr.
4.6. Detailed Material Balance

4.6.1. Slurry Section (TPA + EG Mixing Tank)
A flow diagram of the slurry section is given in
M1 = Mass flow rate of TPA in kg/hr.
M2 = Mass flow rate of EG in kg/hr.
M3 = Mass flow rate of slurry (TPA + EG) in kg/hr.
wEG = Weight fraction of EG in M3
wTPA = Weight fraction of TPA in M3
wwater = Weight fraction of H2O in M3
M15 = Mass flow rate of 95% EG from distillation tower in kg/hr.
19
15 = Weight fraction of EG in M15
Total Balance
M1 + M2 + M15 = M3
3595.782 + 1342.141 + 1698.22 = M3
M3 = 6636.142 kg/hr.
EG Balance
M2 + M15 = M3 wEG
1342.141 + 1698.22 = 6636.142 WEG
wEG = 0.445
Similarly,
TPA Balance
wTPA = 0.542
Water Balance
wwater = 0.013
Hence,
20
4.6.2. Esterification Section
In the esterification section, EG and TPA react to form BHET and water. The water produced and some
mass of EG is vaporized due to high temperature maintained in the reactor. The vaporized products are taken
out of the reactor separately while the reaction mixture is sent to the next reactor for further conversion
4.6.2.1. Esterification Reactor-2 (ES-2)
Where,
M3 = Mass flow rate of slurry (TPA + EG) in kg/hr.
wEG = Weight fraction of EG in M3
M4 = Mass flow rate of (EG + H2O) generated during reaction in Esterification Reactor (ES-1)
WEG4 = Weight fraction of EG in M4.
wwater4 = Weight fraction of H2O in M4
wBHET = Weight fraction of BHET in M5
5 = Weight fraction of EG in M5
wwater = Weight fraction of water in M5
Total Balance
M3 = M4 + M5
6636.142 kg/hr. = M4 + M5
21
TPA Balance
For 95% Conversion:
Mass of TPA entering the reactor ES-1 = 0.542 6636.142
= 3595.782 kg/hr.
Mass of TPA reacted = 3595.782 0.95
= 3415.99 kg/hr.
3415.99
Moles of TPA reacted = 166.14
= 20.561 kmoles/hr.
Mass of TPA unreacted = 3595.782 3415.99
= 179.79 kg/hr.
Moles of TPA unreacted = 1.082 kmoles/hr.
EG Balance
Mass of EG entering the reactor ES-1 = 0.445 6636.142
= 2955.449 kg/hr.
Moles of EG reacted = 2 Moles of TPA Reacted
= 2 20.561
= 41.122 kmoles/hr.
Mass of EG reacted = 41.122 Mw of EG
= 41.122 62.07
= 2552.434 kg/hr.
Mass of EG unreacted = 2955.449 2552.434
= 403.016 kg/hr.
Moles of EG unreacted = 403.16/62.07
= 6.493 kmoles/hr.
22
BHET Balance
Moles of BHET produced in reactor = Moles of TPA Reacted
= 20.561 kmoles/hr.
Mass of BHET Produced in reactor = 20.561 Mw of BHET
= 20.561 254.24
= 5227.41 kg/hr.
Water Balance
Mass of Water entering the reactor ES-1 = 0.012 6636.142
= 84.91 kg/hr.
Moles of Water generated in reactor = 2 Moles of TPA Reacted
= 2 20.561
= 41.122 kmoles/hr.
Mass of Water generated in reactor = 41.122 Mw of Water
= 41.122 18
= 740.193 kg/hr.
Total mass of water in reactor = 740.193 + 84.91
= 825.104 kg/hr.
Moles of water in reactor = 825.104/18
= 45.84 kmoles/hr.
Composition of Streams
Assuming that 60% of unreacted MEG and 70% of water generated in the esterification reactor is obtained in
the vaporized form. Thus,
Mass of water removed as vapors = 825.104 0.70
= 577.573 kg/hr.
Moles of water removed as vapors = 32.087 kmoles/hr.
Mass of EG removed as vapors = 403.016 0.60
= 241.81 kg/hr.
Moles of EG removed as vapors = 3.896 kmoles/hr.

23
Therefore,
M4 = 577.573 + 241.81
= 819.38 kg/hr.
241.81
wEG4 = 819.38
= 0.295
577.573
wwater4 =
819.38
= 0.705
Also, For M5
Mass of unreacted PTA leaving the reactor = 179.79 kg/hr.
Moles of unreacted TPA leaving the reactor = 1.082 kmoles/hr.
Mass of BHET leaving the reactor = 5227.41 kg/hr.
Moles of BHET leaving the reactor = 20.561 kmoles/hr.
Mass of water leaving with reaction mixture = 825.104 0.30
= 247.531 kg/hr.
Moles of water leaving with reaction mixture = 13.752 kmoles/hr.
Mass of EG leaving with reaction mixture = 403.016 0.40
= 161.206 kg/hr.
Moles of EG leaving with reaction mixture = 2.597 kmoles/hr.
24
Hence,
M5 = Mass of BHET + Mass of PTA + Mass of MEG + Mass of Water
= 179.79 + 5227.41 + 247.531 + 161.206
= 5815.937 kg/hr.
5227.41
wBHET = 5815.937
= 0.90
179.79
wTPA = = 0.030
5815.937
161.206
wEG = 5815.937
= 0.028
247.531
wwater = = 0.042
5815.937
Hence,
25
4.6.2.2. Esterification Reactor 2 (ES-2)
Where,
M5 = Mass flow rate of BHET + Unreacted TPA + Unreacted MEG + Water entering the reactor.
wEG5 = Weight fraction of EG in M5
wTPA5 = Weight fraction of TPA in M5
wBHET5 = Weight fraction of BHET in M5
wwater5 = Weight fraction of water in M5
M6 = Mass flow rate of (EG + H2O) generated during reaction in Esterification Reactor (ES-2)
wEG6 = Weight fraction of EG in M6.
M7 = Mass flow rate of BHET + Unreacted EG + Unreacted EG + Water Leaving the reactor ES-2
wBHET = Weight fraction of BHET in M7
= Weight fraction of EG in M7
Total Balance
M5 = M6 + M7
5815.937 kg/hr. = M4 + M5
26
TPA Balance
For 95% Conversion:
Mass of TPA entering the reactor ES-2 = 0.03 5815.937
= 179.79 kg/hr.
Mass of TPA reacted = 179.79 0.95
= 170.80 kg/hr.
170.80
Moles of TPA reacted =
166.14
= 1.03 kmoles/hr.
Mass of TPA unreacted = 179.79 170.80
= 8.989 kg/hr.
Moles of TPA unreacted = 0.054 kmoles/hr.
EG Balance
Mass of EG entering the reactor ES-1 = 0.028 5815.937
= 161.21 kg/hr.
Moles of EG reacted = 2 Moles of TPA Reacted
= 2 1.03
= 2.06 kmoles/hr.
Mass of EG reacted = 2.06 Mw of EG
= 2.06 62.07
= 127.62 kg/hr.
Mass of EG unreacted = 161.21 127.62
= 33.585 kg/hr.
Moles of EG unreacted = 33.585/62.07
= 0.541 kmoles/hr.
27
BHET Balance
= 5227.41 kg/hr.
Moles of BHET produced in reactor = Moles of TPA Reacted
= 1.03 kmoles/hr.
Mass of BHET Produced in reactor = 1.03 Mw of BHET
= 1.03 254.24
= 261.37 kg/hr.
Total mass of BHET in the reactor = 5227.41 + 261.37
= 5488.781 kg/hr.
Water Balance
= 247.5313 kg/hr.
Moles of Water generated in reactor = 2 Moles of TPA Reacted
= 2 1.03
= 2.06 kmoles/hr.
Mass of Water generated in reactor = 2.06 Mw of Water
= 2.06 18
= 37 kg/hr.
Total mass of water in reactor = 247.5313 + 37
= 284.541 kg/hr.
Moles of water in reactor = 284.541/18
= 15.81 kmoles/hr.
Assuming that 60% of unreacted MEG and 70% of water generated in the esterification reactor is obtained in
the vaporized form. Thus,
= 199.179 kg/hr.
28
= 20.15 kg/hr.
Therefore,
M6 = 199.179 + 20.15
= 219.33 kg/hr.
199.179
wwater6 =
219.33
= 0.908
20.15
wEG6 =
219.33
= 0.092
Also, For M7
Mass of BHET leaving the reactor = 5488.781 kg/hr.
Moles of BHET leaving the reactor = 21.589 kmoles/hr.
= 85.36 kg/hr.
= 13.43 kg/hr.
29
Hence,
M7 = Mass of BHET + Mass of PTA + Mass of MEG + Mass of Water
= 5488.781 + 8.989 + 13.43 + 85.36
= 5596.566 kg/hr.
5488.781
wBHET = 5596.566
= 0.981
8.989
wTPA = = 0.0016
5596.566
13.43
wEG = 5596.566
= 0.0024
85.36
wwater = = 0.015
5596.566
Hence,
30
4.6.3. Polycondensation Reactors
In the polycondensation reactors, polymerization begins. BHET acting as monomer form long chains
by connecting with other monomer molecules. Ethylene glycol (EG) is produced as a by-product and is
removed continuously in order to push the reaction in the forward direction.
4.6.3.1. Polymerization Reactor 1 (PR-1)
Where,
M7 = Mass flow rate of BHET + Unreacted TPA + Unreacted MEG + Water entering the reactor.
M8 = Mass flow rate of (EG + H2O) generated during reaction in Polycondensation Reactor (PR-1)
M9 = Mass flow rate of PET + Unreacted EG + Unreacted EG + Water Leaving the reactor PR-1
wPET = Weight fraction of PET in M7
Total Balance
M7 = M8 + M9
5596.566 kg/hr. = M7 + M9
31
TPA Balance
Mass of TPA entering the reactor PR-1 = 0.0016 5596.566
= 8.989 kg/hr.
Moles of TPA entering the reactor PR-1 = 0.0541 kmoles/hr
Since, no further reaction between TPA and EG takes place
Mass of TPA leaving the reactor PR-1 = 8.989 kg/hr
Moles of TPA leaving the reactor PR-1 = 0.0541 kmoles/hr.
BHET Balance
Mass of BHET entering the reactor PR-1 = 5488.781 kg/hr
Moles of BHET entering the reactor PR-1 = 21.589 kmoles/hr
It is assumed that all of BHET starts converting into polymer hence no BHET is obtained at the outlet of the
reactor.
Mass of BHET leaving reactor PR-1 = 0 kg/hr.
Moles of BHET leaving reactor PR-1 = 0 kg/hr.
PET Balance
Degree of Polymerization achieved in the reactor PR-1 = 30

Moles of PET Produced in the reactor PR-1 =

= 21.589/30
= 0.7196 kmoles/hr.
= ( ) + (-- Mw = Molecular Weight)
Molecular weight of PET = (192.17 30) + 62.07
= 5827.17 kmoles/kg
Mass of PET produced in reactor PR-1 = Moles Molecular Weight
= 0.7196 5827.17
= 4193.421 kg/hr.
EG Balance
Mass of EG entering the reactor PR-1 = 13.434 kg/hr.
32
Moles of EG entering the reactor PR-1 = 0.216 kmoles/hr.
1
Moles of EG produced in the reactor =

301
= 21.589 = 20.8694 kmoles/hr.
30
Mass of EG produced in the reactor = 20.8694 62.07
= 1295.364 kg/hr.
Total EG leaving the reactor = 1295.364 + 13.434
= 1308.798 kg/hr.
Water Balance
Mass of water entering reactor PR-1 = 85.362 kg/hr.
Moles of water entering reactor PR-1 = 4.742 kmoles/hr.
Since, no generation or consumption of water within the reactors take place.
Mass of water leaving reactor PR-1 = 85.362 kg/hr.
Moles of water leaving reactor PR-1 = 4.742 kmoles/hr.
Assuming that 95% of unreacted MEG and 80% of water in the polymerization reactor is obtained in the
vaporized form. Thus,
= 68.290 kg/hr.
= 1243.354 kg/hr.
Therefore,
M8 = 68.290 + 1243.354
= 1311.644 kg/hr.
68.290
wwater8 = 1311.644
= 0.052
1243.354
wEG8 = 1311.644
= 0.948
Also, For M9
33
Mass of BHET leaving the reactor = 0 kg/hr.
Moles of BHET leaving the reactor = 0 kmoles/hr.
= 17.072 kg/hr.
= 65.44 kg/hr.
Mass of PET leaving the reactor = 4193.421 kg/hr.
34
Hence,
M9 = Mass of PET + Mass of PTA + Mass of MEG + Mass of Water
= 4192.421 + 8.989 + 65.44 + 17.072
= 4284.922 kg/hr.
4284.922
wPET = 4284.922
= 0.979
8.989
wTPA = 4284.922
= 0.0021
65.44
wEG = 4284.922
= 0.015
17.072
wwater = 4284.922
= 0.0040
Hence,
35
4.1.1.1. Polymerization Reactor 2 (PR-2)
Where,
M9 = Mass flow rate of PET + Unreacted TPA + Unreacted MEG + Water entering the reactor.
Total Balance
M9 = M10 + M11
4284.922 kg/hr. = M10 + M11
36
TPA Balance
= 8.989 kg/hr.
Water Balance
PET Balance
Mass of PET30 entering the reactor = 4192.421 kg/hr
Moles of PET30 entering the reactor = 0.7196

30
Moles of PET Produced in the reactor PR-2 = 90
30
30
= 90
0.7196
= 0.2399 kmoles/hr.
= 17357.37 kmoles/kg
= 0.2399 17357.37
= 4163.642 kg/hr.
EG Balance
37

Moles of EG produced in the reactor =
entering
9030
= 90
0.7196
= 0.4798 kmoles/hr.
= 29.7784 kg/hr.
Mass of EG leaving reactor PR-2 = 65.4397 + 29.7784
= 95.218 kg/hr.
Moles of EG leaving reactor PR-2 = 1.534 kmoles/hr.
Assuming that 95% of unreacted MEG and 80% of water in the polymerization reactor is obtained in the
= 13.658 kg/hr.
= 90.46 kg/hr.
Therefore,
M10 = 13.658 + 90.46
= 104.12 kg/hr.
13.658
wwater10 = 104.12
= 0.131
90.46
wEG10 =
104.12
= 0.869
Also, For M11

38
= 3.414 kg/hr.
= 4.761 kg/hr.
Hence,
= 4162.642 + 8.989 + 4.761 + 3.414
= 4180.807 kg/hr.
4162.642
wPET = 4180.807
= 0.996
8.989
wTPA = 4180.807
= 0.0022
4.761
wEG = 4180.807
= 0.00114
3.414
wwater = 4180.807
= 0.0008
Here,
39
4.1.1.2. Polycondensation Reactor 3 (PR-3)
Where,
M11 = Mass flow rate of PET + Unreacted TPA + Unreacted MEG + Water entering the reactor.
Total Balance
M11 = M12 + M13
4284.922 kg/hr. = M12 + M13
40
TPA Balance
= 8.989 kg/hr.
Water Balance
EG Balance

Moles of EG produced in the reactor = entering

12090
= 120
0.2399
= 0.05997 kmoles/hr.
= 3.722 kg/hr.
Mass of EG leaving reactor PR-3 = 4.761 + 3.722
= 8.483 kg/hr.
Moles of EG leaving reactor PR-3 = 0.1367 kmoles/hr.
PET Balance
Mass of PET90 entering the reactor = 4163.642 kg/hr
Moles of PET90 entering the reactor = 0.2399

90
Moles of PET Produced in the reactor PR-3 = 30
120
90
= 0.2399
120
= 0.1799 kmoles/hr.
41
= 23122.47 kmoles/kg
= 0.1799 23122.47
= 4159.92 kg/hr.
Assuming that 95% of unreacted MEG and 80% of water in the polycondensation reactor is obtained in the
= 2.732 kg/hr.
= 8.059 kg/hr.
Therefore,
M12 = 2.732 + 8.059
= 10.791 kg/hr.
2.732
wwater12 = 10.791
= 0.253
8.059
wEG12 =
10.791
= 0.747
Also, For M13
= 0.683 kg/hr.
42
= 0.424 kg/hr.
Hence,
= 4159.92 + 8.989 + 0.424 + 0.683
= 4170.017 kg/hr.
4159.92
wPET = 4170.017
= 0.998
8.989
wTPA = = 0.0021
4170.017
0.424
wEG = 4170.017
= 0.0001
0.683
wwater = = 0.0002
4170.017
43
Chapter 5
Energy Balance
Chapter 5 Energy Balance
Chapter 5: Energy Balance
5.1. Esterification Reactor 1 (ER-1)
Q2
(2)
(1)
BHET
PTA Esterification Reactor 1 PTA
Q1 MEG Q4
(245C) MEG
Water
Water
(45C)
(245C)
(3)
Water
MEG
(245C)
Q3
Figure 1: Block Diagram Presenting the Overall Heat Inputs and Outputs in Esterification Reactor-1 (ES-1)
Where,
Q1 = Heat content of the reactants entering the reactor.
Q2 = Heat required to raise the temperature of reactants up to the required conditions and the heat of
reaction.
Q3 = Heat content of water and mono-ethylene glycol mixture leaving the reactor.
Q4 = Heat going out with the product and the unreacted reactants.
5.1.1. Description
An inlet stream comprising of a mixture of mono-ethylene glycol (MEG), purified terepthalic acid
(PTA), and water enters the water at a temperature of 47oC. The temperature of the reactants (MEG & PTA) is
raised to 245oC. At this temperature they react to form Bis-hydroxy ethylene terephthalate. The reaction is
endothermic therefore requires heat input in the reactor.
The heat of reaction can be computed by considering following reaction at 25oC

{ }={ }{ }

44
The heats of formation of reactants and the heat of formation of products are presented in Table 5-1.
Table 5-1: Heat of formation of reactants and products.
Reactants of Formation Heat of Formation Products Heat of Formation

kcal/mole kcal/mole
1 mole of PTA -195.02 1 mole of BHET -261.80
2 moles of MEG -92.07 2 mole of Water -57.79

{ } = {(261.80) + 2(57.79)} {(195.02) + 2(92.97)} = +. /

{ } = + /

5.1.2. Stream Properties

The thermal properties of streams entering and leaving the esterification reactor are given in Table 5-2.
Table 5-2: Thermal properties of streams entering and leaving the esterification reactor.
Stream Temperature Components Weight Specific Heat Specific Heat

Fraction Capacity Capacity of
(Components) (Stream)
o
C kcal/kmol K kcal/kmole K
Average MEG (liq) 0.5418 44.37
Temperature MEG (vap) 0.5418 26.17
1 145 PTA 0.4453 41.31 41.77
Water (liq) 0.0128 18.03
Water (vap) 0.0128 8.18
BHET 0.899 125.94

2 245 MEG 0.277 26.82 115.85
PTA 0.309 50.22
Water 0.425 8.46
MEG 0.295 26.82 13.89

3 245 Water 0.705 8.46
45
5.1.3. Calculation of Energy Requirements for Stream 1

Now, heat required for each component in feed stream is calculated below:
5.1.3.1. Water
The heat required to raise the temperature of water present in feed stream 1 from 45oC to 245oC can be
calculated as follows:
106.9 245
= (45 1 + 106.9 2 ) +
Where,
106.9oC is the saturation temperature of water at reactor pressure of 4 psig.
= Heat required per unit time to raise the temperature of water in the stream from 45oC to 245oC.
= Latent heat of vaporization of water at 4 psig and 106.9oC.
1 , 2 = Specific Heat of water in kcal/kmoles oC.
= kmoles of water entering as feed per unit time.
= A total of mass feed rate of water entering the reactor and the mass of water produced in unit time as
result of chemical reaction.
Taking average specific heat capacities at given temperatures and bringing them out from integration term
as constants.
106.9 245
= (18.0313 45 + 8.18 106.9 ) +
= 4.717(18.0313 (106.9 45) + 8.18 (245 106.9)) + 825.1 (534.65)
= 10593.417 + 441086.25
= . /
5.1.3.2. Terephthalic Acid

245
= 45
Here,
= Heat required per unit time to raise the temperature of PTA in the stream from 45oC to 245oC.
= kmoles of water entering as feed per unit time.
= Specific Heat of water in kcal/kmoles oC.
46
Taking average CP at average temperature i.e. 145oC.

245
= 45
= 21.64 41.31(245 45)

= 178789.68 /
5.1.3.3. Mono-Ethylene Glycol
205.32 245
= (45 1 + 205.32 2 ) +
Where,
205.32oC is the saturation temperature of MEG at reactor pressure of 4 psig.
= Heat required per unit time to raise the temperature of MEG in the stream from 45oC to 245oC.
= Latent heat of vaporization of MEG at 4 psig and 205.32oC estimated to be 12534.52 kcal/kmole.
1 , 2 = Specific Heat of MEG in kcal/kmoles oC.
= kmoles of MEG entering as feed per unit time.
= mass feed rate of MEG as feed.
Taking average specific heat capacities at given temperatures and bringing them out from integration term
as constants.
205.32 245
= (43.02 45 + 26.17 205.32 + )
= 47.615(43.02 (205.32 45) + 26.17 (245 205.32) + 12534.52)
= . /
5.1.3.4. Heat of Reaction

The heat of reaction required in the esterification reactor-1 (ES-1) can be calculated as follows:
= = ( ) ( )
= (3540) (20.561)
= 72785.94 /
5.1.4. Total Energy Requirement

1 = 1 = + + +
1 = 451679.67 + 178789.68 + 974674.86 + 72785.94
= . /
47
5.2. Esterification Reactor 2:
Q2
(2) (5)
BHET BHET
PTA Esterification Reactor 2 PTA
Q1 Q4
MEG (255C) MEG
Water Water
(245C) (255C)
(4)
Water
MEG
(255C)
Q3
Figure 2: Block Diagram Presenting the Overall Heat Inputs and Outputs in Esterification Reactor-2 (ES-2)
5.2.1. Description
The outlet stream from esterification reactor 1 (ES-1) containing Bis-hydroxy ethylene terephthalate
(BHET), mono-ethylene glycol (MEG), purified terephthalic acid (PTA) enters the esterification reactor-2 (ES-2)
where its temperature is increased to 255 and the pressure is reduced to 2 psig. Further conversion of PTA
and MEG into BHET takes place in the reactor. The reaction being endothermic requires heat input. In addition,
heat is also required to raise the temperature of feed from 245oC to 255oC. A simplified block diagram
representing the heats entering and leaving the system (esterification reactor) is shown in Figure 2.
Where,
Q1 = Heat content of the reactants entering the reactor.
Q2 = Heat required to raise the temperature of reactants up to the required conditions and the heat of
reaction.
Q3 = Heat content of water and mono-ethylene glycol mixture leaving the reactor.
Q4 = Heat going out with the product and the unreacted reactants.
48
The thermal properties of streams entering and leaving the esterification reactor are given in Table
5-3.
Table 5-3: Thermal properties of the streams entering and leaving the esterification reactor.

o
C kcal/kmol K kcal/kmol K
Average BHET 0.899 126.94
2 Temperature MEG 0.277 26.986 116.768
250oC PTA 0.309 50.625
Water 0.425 8.4742
BHET 0.9807 127.969

5 255 MEG 0.0024 27.147 125.781
PTA 0.0016 51.0313
Water 0.0153 8.487
MEG 0.0919 27.147

4 255 Water 0.9081 8.487 10.201
5.2.3. Calculation of Energy Requirements

5.2.3.1. Heat Input for Raising Temperature of Stream 2
The heat required to raise the temperature of stream 2 from 245oC to 255oC is calculated as shown
below:
= . ( )
Where,
= Heat rate required to raise the temperature of inlet stream up to desired temperature.
= Mass flow rate of stream
. = Specific heat of the stream at average temperature.
= Final/Desired temperature.
= Temperature at which feed enters the reactor.
Here,
= 5815.937 116.768 (255 245)
= 6791153.316 /
49
5.2.3.2. Heat Input Required to Vaporize the Water Produced
The heat input rate required to raise the water produced in the reactor as vapors can be calculated as
follows:

= =

= 37.01 536.79

= 19866.60
5.2.3.3. Heat of Reaction

The heat required for the reaction to take place can be calculated as follows:
= = ( ) ( )
= (3540) (1.028)
= 3639.12 /

2 = 2 = + +
2 = 6791153.316 + 3639.12 + 19866.80

= . /
50
5.3. Polymerization Reactor 1
Q2
(5) (7)
BHET PET
PTA Polymerization Reactor 1 PTA
Q1 Q4
MEG (280C) MEG
Water Water
(255C) (280C)
(6)
Water
MEG
(280C)
Q3
Figure 3: Block Diagram Presenting the Overall Heat Inputs and Outputs in Polymerization Reactor-1 (PR-1)
5.3.1. Description
In the Polymerization Reactor-1 (PR-1), polymerization of monomer begins. The temperature of the
reactor is maintained at 280oC therefore, energy must be provided to the feed stream of polymerization
reactor to raise its temperature to the suitable conditions. The polymerization reaction is slightly exothermic.
According to the literature, the heat of reaction is about 20 kcal/mol of MEG given out. The heat released as
a result of exothermic reaction is usually ignored because it is almost negligible in heat balance. A simplified
block diagram of the streams carrying energy, entering and leaving the reactor are shown in Figure 3.

Table 5-4: Thermal properties of the streams entering and leaving the Polymerization Reactor 1.

o
Average BHET 0.9807 130.5
5 Temperature MEG 0.0024 27.543 128.266
267.5 PTA 0.0016 52
Water 0.0153 8.52
PET 0.9786 93.03

7 280 MEG 0.0153 27.931 91.615
PTA 0.0021 52.9688
Water 0.004 8.5532
6 280 MEG 0.948 27.931 26.485

Water 0.052 8.5532
51
5.3.3. Calculations of Energy Requirement
5.3.3.1. Heat Input for Raising the Temperature of Stream 5
below:
= . ( )
Where,
Here,
= 5596.566 128.266 (280 255)
= 17946228.36 /
5.3.3.2. Heat Input Required to Vaporize MEG Produced
The heat input rate required to raise the MEG produced in the reactor as vapors can be calculated as
follows:

= =

= 7.65
13945.82

= 106685.523
5.3.3.3. Heat Released during Polymerization Reaction

The heat released during polymerization reaction can be calculated as follows:

= = ( )( )

= (7.65
) (20000
)
= 153000 /

1 = 1 = + +
1 = 17946228.36 + 106685.523 153000

= . /
52
5.4. Polymerization Reactor-2
Q2
(7) (9)
PET (DOP=30) PET (DOP=90)
PTA Polymerization Reactor 2 PTA
Q1 Q4
MEG (285C) MEG
Water Water
(280C) (285C)
(8)
Water
MEG
(285C)
Q3
5.4.1. Description
In the Polymerization Reactor-2 (PR-2), the degree of polymerization of the polymer under process is
increased further. The temperature is increased further to 285oC. MEG is released during the further
polymerization in an exothermic reaction. A simplified block diagram of the streams carrying energy, entering
and leaving the reactor are shown in Error! Reference source not found..

Table 5-5: Thermal properties of the streams entering and leaving the Polymerization Reactor 2

o
Average PET 0.9786 94.08
7 Temperature (DOP=30)
282.5 MEG 0.0153 28 92.644
PTA 0.0021 53.125
Water 0.040 8.56
PET 0.9786 94.25

9 285 (DOP=90) 94.017
MEG 0.0153 28.08
PTA 0.0021 53.34
Water 0.004 8.57
8 285 MEG 0.948 28.08 25.52

Water 0.052 8.57
53
5.4.3.1. Heat Input for Raising the Temperature of Stream 7
below:
= . ( )
Where,
Here,
= 4284.922 92.644 (285 280)
= 1984861.57 /
follows:

= =

= 0.48
13945.82

= 6693.994


= = ( )( )

= (0.48
) (20000
)
= 9600 /

2 = 2 = + +
2 = 1984861.57 + 6693.994 9600

= . /
54
5.5. Poly-Condensation Reactor
Q2
(9) (11)
PET (DOP=90) Poly-Condensation PET (DOP=120)
PTA PTA
Q1
MEG Reaction MEG
Q4
Water (285C) Water
(285C) (285C)
(10)
Water
MEG
(285C)
Q3
Figure 4: Block Diagram Presenting the Overall Heat Inputs and Outputs in Poly-Condensation Reactor
5.5.1. Description
In the Polycondensation reactor, the degree of polymerization of the polymer under process is
increased further and the finally completed and the polymer having a degree of polymerization of 120 is
obtained as product. The temperature and pressure are maintained constant. MEG is released during the
further polymerization in an exothermic reaction. A simplified block diagram of the streams carrying energy,
entering and leaving the reactor are shown in Figure 4.

Table 5-6: Thermal properties of the streams entering and leaving the Polymerization Reactor 2

o
PET 0.9786 94.25
(DOP=90)
7 285 MEG 0.0153 28.08 94.017
PTA 0.0021 53.34
Water 0.004 8.57
PET 0.9786 94.25

9 285 (DOP=90) 94.017
MEG 0.0153 28.08
PTA 0.0021 53.34
Water 0.004 8.57
8 285 MEG 0.948 28.08 25.52

Water 0.052 8.57
55
follows:

= =

= 0.248
13945.82

= 3458.563


= = ( )( )

= (0.248
) (20000
)
= 4960 /

= = +
= 3458.563 4960
= . /
56
Chapter 6
Equipment Design
Chapter 6 Equipment Design
Chapter 6: Equipment Design
6.1. Storage Units

6.1.1. Storage Tank of TPA
Basis = 1 Day
TPA required = 3595.782 kg/hr TPA
TPA required = 3.596 tons/hr
TPA required = 3.596 24
= 86.29 tons/day
Bulk density of TPA = 1.52 tons/m3
Volume of TPA = 56.78 m3/day
Volume of Tank = 62.45 m3/day (10% safety allowance)
6.1.1.1. Calculations
Volume of Silo = Volume of Cylindrical Section + Volume of Conical Section

Volume of cylinder = 4
2 1
Where,
D = Diameter of the cylinder
H1 = Height of the cylinder
So,
H1 = 1.3D
Now,
Volume of cylinder = 1.02 3

1 1
Volume of cone = ( ) = 3 ( 4 2 2 )
3
Where,
H2 = Height of the cone
D = Diameter of the cone
Form right angled triangle ABC

2
= tan()

2
57
Q = 60o (Assumed),

H2 = 2
tan(60)
H2 = 0.866 D
1
Volume of cone = 3
( 4 2 0.866 )
Volume of cone = 0.2266D3
So,
The volume of the Silo = Volume of cylinder + Volume of cone
= 1.02D3 + 0.2266D3
Volume of silo = 1.2466 D3
Thus,
1.2466D3 = 62.45 m3
D3 = 50.096 m3
D = 3.686 m
As,
H1 = 1.3 D
So,
H1 = 1.3 3.686
H1 = 4.792 m
H2 = 0.866 3.686
H2 = 3.192 m
Total height = H1 + H2
= 4.792 + 3.192
Total height = 7.984 m
6.1.1.2. Material of Construction

Material of construction of TPA storage tank is stainless steel type -304. Type 304 (18/8 stainless
steel) is a type of austenite stainless steel, which because of its uniform structure is desired for corrosion
resistance and is the most generally used stainless steel.
It contains the minimum Cr and Ni that gives a suitable austenitic structure. The carbon contents
are low enough, for heat treatment not to be normally needed with thin sections to prevent weld decay.
58
6.1.1.3. Suggested Design
Shape = Conical
No. of units = 1
Volume of the vessel = 62.45 m3
Diameter of vessel = 3.686 m
Height of cylindrical section = 4.792 m
Height of conical section = 3.192 m
Total height of tank = 5.26 m
2
Area of tank = 4
= 10.673 m2
6.1.2. Storage Tank of EG

Basis = 1 day
EG required = 2686.772 kg/hr
EG required = 2.687 tons/hr
EG required = 2.687 24
= 64.482 tons/day
Density of EG = (Specific gravity of EG) (Density of H2O)
= (1.115)(1000)
= 1115 kg/m3
= 1.115 tons/m3
Volume of EG required = 64.482/1.115
= 57.832 m3
Giving 10% safety allowance,
Volume of vessel = 63.615 m3
The vessel is cylindrical so height of the vessel = H
Where,
H = 1.3 D

Volume of vessel = 4
2

= 4
2 1.3
59
Volume of vessel = 1.026 D3.
So,
1.021D3 = 63.615 m3
D3 = 62.307 m3
D = 3.964 m
So,
H = 1.3 D
H = 1.3 3.964
H = 4.121m

Material of construction of TPA storage tank is stainless steel type -304. Type 304 (18/8
stainless steel) is a type of austenite stainless steel, which because of its uniform structure is desired
for corrosion resistance and is the most generally used stainless steel.
It contains the minimum Cr and Ni that gives a suitable austenitic structure. The carbon
contents are low enough, for heat treatment not to be normally needed with thin sections to prevent
weld decay.

Shape = Cylindrical
No. of units = 1
Volume of vessel = 63.615 m3
Diameter of vessel = 3.964 m
Height of cylindrical section = 4.121 m
2
Area of tank = 4
Area of tank = 12.344 m2
60
6.2. Mixing Tank

6.2.1. Design of Slurry Mixer
M1 = Mass Flow rate of TPA
= 3595.782 kg/hr
M2 = Mass Flow rate of EG
= 1353.22 kg/hr
M3 = Mass Flow rate of recycled EG
= 1602.227 kg/hr
M4 = Mass Flow rate of Water
= 84.91 kg/hr
TMix = 70 min (assumed)
Equation Used

=

Vr = ?
Vo = ?
=
Where,
Vr = Volume of the Tank
Vo = Volumetric flow rate
G = Total mass flow rate in the mixing tank
= Density of mixture
6.2.1.1. Calculations
Total mass flow rate in the mixing tank,
G = M1 + M2 + M3 + M4
= 3595.782 + 1353.22 + 1602.227+ 84.91
G = 6636.142 kg/hr
1353.22+1602.227
Weight fraction of EG = 6636.142
XEG = 0.445
61
Similarly,
XTPA = 0.542
XWater = 0.013
As,
pEG = 1115 kg/m3
pTPA = 1520 kg/m3
pmix = (pEG XEG) + (pTPA XTPA) + (pwater Xwater)
pmix = (1115 0.445) + (1520 0.542) + (1000 0.013)
pmix = 1333.015 kg/m3
Volumetric flow rate = G/pmix
= 6636.142/1333.015
Volumetric flow rate = 4.978 m3/hr
So,
Vo = 4.978 m3/hr
Tmix = Vr/Vo
Vr = Tmix Vo
= 1.167 4.978
Vr = 5.809 m3
Giving 10% safety allowance
Vr = 6.39 m3
Where,
H = 1.3 D

Volume of Mixer = 4
2

= 4
2 1.3
1
= 3
(4) 3
Volume of Mixer = 0.2618 D3
D3 = 6.39/0.2618
D3 = 24.408
D = 2.9 m
62
As,
D = 2.9 m
H = 1.3D
H = 3.77 m
6.2.1.2. Wall Thickness

D = 2.9 m
Minimum wall thickness required to ensure that the vessel is sufficiently rigid to withstand its own
weight includes corrosion allowance of 2mm = 5+2 = 7 mm.
Thickness required due to the weight of the fluid slurry is as follows.
6.2.1.3. Thickness of Bottom:

Thickness by (BS-5500) for bottom is given by:

e = 2
F = 135 N/mm2 in temperature range from 0-50oC
Pi = pmix g h
= 1333.015 * 9.8*2
Pi = 26127.09 N/m2
J = 0.85
D = 2.9 m
Putting values in equation 1

26127.09 2.9
e = 20.85135106 26127.09
75768.561
= 229473872.9
e = 3.30184 10-4 m
e = 0.330184 mm
Thickness of bottom = 7 + 0.330184
= 7.33084 mm
Recommended thickness = 7.33084 mm
63
6.2.1.4. Impeller Design Nomenclature
S1 = DT/Da =3
S2 = E/DT = 1/3
S3 = L/DT = 0.25
S4 = W/Da = 1/5
S5 = 1/DT = 1/12
Da = Diameter of impeller, m
DT = Diameter of tank, m
E = Height of impeller from bottom, m
L = Length of blade, m
W = Width of blade, m
J = Width of baffle, m
6.2.1.5. Impeller Design Calculations
1. S1 = DT/Da =3
Da = DT/3
= 2.9/3
Da = 0.967 m
2. E/DT = 1/4
E = DT 1/3
E = 2.9 1/3
E = 0.967 m
3. L/Da = 0.25
L = 0.25 0.967
L = 0.25(0.967)
L = 0.242 m
4. W/Da = 1/5
W = 1/5 Da
W = (1/5) 0.967
W = 0.193
J/DT = 1/12
J = DT/12
= 2.9/12
J = 0.242 m
64
6.2.1.6. Power Requirement to Drive the Agitator
Number of baffles = 4
The power delivered to liquid is computed as,

3 5
P =
N = Number of Revolutions
Da = Diameter of impeller
p.mix = density of mixture
gc = conversion factor
(2 )
Re No. =
Np is obtained from graph between Reynold Number and Np
n = 100 rpm
= 1.66 rps
Da = 0.967
pmix = 1333.015 kg/me
mix = 1100 cp
= 11 poice
= 1.1 kg/ms
As, Re.No. is 1879.67 so Np is 4.5
So,
3 5
P =
4.51.663 0.9675 1333.015

= 1
= 23160.91 Watt
Motor efficiency = 80%
Power required = 23160.91/0.80
= 28951.13 Watt
= 2.895 kW
65
Material of construction of TPA storage tank is stainless steel type -304. Type 304 (18/8 stainless steel)
is a type of austenite stainless steel, which because of its uniform structure is desired for corrosion resistance
and is the most generally used stainless steel.
It contains the minimum Cr and Ni that gives a suitable austenitic structure. The carbon contents are
low enough, for heat treatment not to be normally needed with thin sections to prevent weld decay.

Total volume of vessel = 6.39 m3
Diameter of impeller = 0.967 m
Diameter of tank = 2.9 m
Height of impeller from bottom = 0.967 m
Length of blade = 0.242m
Width of blade = 0.193 m
Width of baffle = 0.242 m
Height of vessel = 3.77 m
Bottom Thickness = 7.4 mm
Wall thickness = 7 mm
Power Requirement = 2.895 kW
66
6.3. Esterification Reactors
6.3.1. Design of Esterification Rector 1 (ES-1)
TPA going to ES-1 = 3595.782 kg/hr
EG going in = 2955.449 kg/hr
Mass flow rate of slurry = 6636.142 kg/hr
Density of slurry = 1333.015 kg/m3
Volumetric flow rate of slurry = Vo
Vo = 4.98 m3/hr
Tres = VR/Vo
VR = Volume of Reactor
Vo = Volumetric flow rate of slurry
As we know that,
Tres = VR/Vo
VR = Tres Vo
= 4 4.98
VR = 19.92 m3
VR = 19.92 m3
VR = 21.912 m3
Now
H = 1.3DT

Volume of reactor = 4
2

= 4
2 1.3
Volume of reactor = 1.021 DT3.
19.92 = 1.021 DT3
DT3 = 21.912/1.0205
DT3 = 21.461 m
DT = 2.779 m
H = 1.3DT
= 1.3(2.779)
H = 3.612 m
Recommended height = 3.62 m
67
weight including corrosion allowance of 2mm = 10 mm
6.3.1.2. Thickness of Bottom

e = 2
------------------(2)
Pi = pmix g h
= 1333.015 9.8 3.62
Pi = 47290.04 N/m2
D = 2.779 m
J = 0.85
F = 95 N/(mm)2 at 245oC.
Putting value in eq. (2)

47290.04 2.779
e = 20.8595106 47290.04
75768.561
=
229473872.9
e = 8.1398 10-4 m
e = 0.81398 mm So,
= 10.81398 mm
6.3.1.3. Impeller Design for Esterification Reactor
S1 = DT/Da =3
S2 = E/DT = 1/3
S3 = L/DT = 0.25
S4 = W/Da = 1/5
S5 = 1/DT = 1/12
J = width of baffle, m
68
S1 = DT/Da =3
Da = DT/3
= 2.779/3
Da = 0.926 m
E/DT = 1/4
E = DT 1/3
E = 2.779 1/3
E = 0.926 m
L/Da = 0.25
L = 0.25 0.926
L = 0.232 m
W/Da = 1/5
W = 1/5 Da
W = (1/5) 0.926
W = 0.185
J/DT = 1/12
J = DT/12
= 2.779/12
J = 0.232 m
69

3 5
P =
pmix = density of mixture
(2 )
Re No. =
n = 100 rpm
= 1.66 rps
Da = 0.926 m
pmix = 1333.015 kg/me
mix = 1100 cp
= 11 poice
= 1.1 kg/ms
(0.9262 1.66 1333.015)

Re = 1.1
So,
3 5
P =
4.51.663 0.9265 1333.015

= 1
= 18682.1454 Watt
= 23352.68 Watt
= 23.895 kW
70
6.3.2. Design of Esterification Rector 2 (ES-2)
TPA going in ES-2 = 179.789 kg/hr
EG going in ES-2 = 161.2063 kg/hr
BHET entering ES-2 = 5227.41
Water entering ES-2 = 247.5313
Mass flow rate of mixture = 5815.937 kg/hr
Density of mixture = X MEG MEG X TPA TPA X BHET BHET
= 1285 kg/m3
Volumetric flow rate of mixture = Vo
Vo = 4.52 m3/hr
Tres = VR/Vo
VR = Volume of Reactor
Vo = Volumetric flow rate of slurry
As we know that,
Tres = VR/Vo
VR = Tres Vo
= 4 4.52
VR = 18.104 m3
VR = 19.914 m3
Now
H = 1.3DT
As,

Volume of reactor = 2
4

= 4
2 1.3
Volume of reactor = 1.021 DT3.
19.92 m3 = 1.021 DT3
DT3 = 19.914/1.0205
DT3 = 19.514 m3
DT = 2.692 m
71
Now,
H = 1.3DT
= 1.3(2.692)
H = 3.499 m
Recommended height = 3.50 m

weight including corrosion allowance of 2mm = 10 mm
6.3.2.2. Thickness of Bottom

e = ------------------(3)
2
Pi = pmix g h
= 1285 9.8 3.5
Pi = 44075.5 N/m2
D = 2.692 m
J = 0.85
F = 95 N/(mm)2 at 255oC.
Putting value in eq. (2)

44075.5 2.692
e =
20.8595106 44075.5
118663.18
= 229473872.9
e = 7.353 10-4 m
e = 0.7353 mm
So,
= 10.7353 mm
72
6.3.2.3. Impeller Design for Esterification Reactor
S1 = DT/Da =3
S2 = E/DT = 1/3
S3 = L/DT = 0.25
S4 = W/Da = 1/5
S5 = 1/DT = 1/12
J = width of baffle, m
S1 = DT/Da =3
Da = DT/3
= 2.692/3
Da = 0.8974 m
E/DT = 1/4
E = DT 1/3
E = 2.779 1/3
E = 0.8974 m
L/Da = 0.25
L = 0.25 0.8974
L = 0.2243 m
W/Da = 1/5
W = 1/5 Da
W = (1/5) 0.8974
W = 0.1795
J/DT = 1/12
J = DT/12
= 2.692/12
73
J = 0.2243 m


3 5
P =
pmix = density of mixture
(2 )
Re No. =
n = 100 rpm
= 1.66 rps
Da = 0.8974 m
pmix = 1333.015 kg/m3
mix = 1100 cp
= 11 poice
= 1.1 kg/ms
(0.89742 1.66 1285)

Re = 1.1
So,
3 5
P =
4.51.663 0.89745 1285

= 1
= 15394.665 Watt
= 19243.33 Watt
= 19.24333 kW
74
Chapter 7
Instrumentation
&
Process Control
Chapter 7 Instrumentation & Process Control
Chapter 7: Instrumentation & Process Control
7.1. Instrumentation
It is carried out to monitor the key process variables during plant operation. Instruments may be
incorporated in automatic control loops or used for the manual monitoring of the process operation. There
may be manual or automatic computer data logging system. Instruments monitoring critical process variables
will be fitted with automatic alarms to alert the operators to critical and hazardous situations.
Industry pursuit of increasingly stringent process control and safety requirements led to an early
adaptation of computational techniques in this field.
Today, a wide range of computing devices, ranging from imbedded microprocessors to dedicated
computers, is commonly employed throughout the industry. The class explores the technical foundations of
process and control instrumentation in use, and covers the practical aspects of its deployment.
7.1.1. Measurement
Instrumentation can be used to measure certain field parameters (physical values). Some of the
variables include:
Pressure
Flow
Temperature
Level
Density
Radiation
Frequency
Current
Voltage
Inductance
Capacitance
Resistivity
Chemical Composition
7.1.2. Control
In addition to measuring field parameters, instrumentation is also responsible for providing the ability
to modify some field parameters to keep the process variables at a desired value.
75
7.2. Incentive for Chemical Process Control
A chemical plant is an arrangement of processing units (reactors, heat exchanger, pumps, distillation
columns, absorbers, evaporators, tanks etc.), integrated with one another in a systematic and rational manner.
The overall objective of plant is to convert certain raw materials into desired products using available sources
of energy, in the most economical way.
In its operation, a chemical plant must satisfy several requirements imposed by its designers and the
general technical, economic and social conditions in the presence of ever-changing external influences
(disturbances). Among such requirements are the following:
7.2.1. Safety
The safe operation of a chemical process is a primary requirement for the well-being of the people in
the plant and for its continued contribution to the economic development.
7.2.2. Product Specification

A plant should produce the desired amounts and quality of the final products. Therefore, a control
system is needed to ensure that the production level and the purity specifications are satisfied.
7.2.3. Environmental Regulations

Various federal and state laws may specify that the temperature, concentrations of chemicals and
flow rates of the effluents from a plant be within certain limits.
7.2.4. Operational Constraints

The Various types of equipment used in a chemical plant have constraints inherited to their operation.
Such constraints should be satisfied throughout the operation of the plant e.g. pumps must maintain a certain
net positive suction head etc.
7.2.5. Economics
The operation of a plant must confirm to the market conditions, that is, the availability of the raw
materials and the demand of the final products. Furthermore, it should be as economical as possible in the
utilization of raw materials, energy, and capacity and human labor. Thus, it is required that the operating
conditions are controlled at given optimum levels of minimum operating cost, maximum profit and so on.
76
7.3. Elements of Control System
In almost every configuration, we can distinguish the following hardware elements.
1) The Chemical Process

2) Measuring elements or sensors
3) Transducers
4) Transmission lines
5) Controllers
6) The final control element
7.3.1. The Chemical Process

It represents the material equipment together with physical or chemical operation that occurs.
7.3.2. The Measuring Instrument or the Sensors

Such instruments are used to measure the disturbances, the controlled output variables, or the
necessary secondary output variables and are the main sources of information about what is going on in the
process.
The measuring means depend upon the types of variable, which is to be measured, and these variables
must be recorded also. Following are some typical sensors, which are used for different variable
measurements.
i) Pressure Sensors
ii) Temperature Sensors
iii) Flow rate Sensors
iv) Level Sensors
Characteristic example of these types of sensors is as follows
i) Thermocouples or resistance thermometers for measuring the temperature, also

used for severe purpose some radiation detectors may also be used.
ii) Venturi meters also flow nozzles for flow measurements
iii) Gas chromatograph for measuring the composition of the stream.
A good device for the measurement depends upon the environment in which it is to be used. Like a
thermometer, it is not a good measuring device, as its signal is not rapidly transmitted. So signal transmission
is very important in selecting the measuring device. So the measuring device must be rugged and reliable for
an industrial environment.
77
7.3.3. Transducers
Many measurements cannot be used for control until they are converted to physical quantities such
as electric voltage and current pneumatic signal. For example, stream gauges are metallic conductors whose
resistance changes when mechanical strain is imposed on it. Thus, they can be used to convert a mechanical
signal to electric one.
7.3.4. Transmission lines

These are used to carry measurements signal from measuring device to the controller. In the past,
mostly transmission lines were pneumatic nature that they are using the compressed air or liquid to transmit
the signal but with the automation of industry and advent of electronic controllers, electric lines have over-
ruled the pneumatic operations.
Many times the measurements coming from a device are very weak and these must be amplified to
get the things right. So it is very often to find amplifiers in the transmission lines to the controller. For example,
the output of a thermocouple is only a few millivolts so they must be amplified to few volts to get the
controller.
7.3.5. Controller
This is the hardware element that has intelligence. It receives the information from the measuring
device and decides what action must be taken out. The older controllers were of limited intelligence, could
perform very limited and simple operations and could implement very simple control laws. The use of digital
computers in this field has increased the use of complicated control laws.
7.3.6. The Final Control Element

This is the hardware element that implements the decision taken by controller. For example, if the
controller decides that the flow rate of the outlet stream should be increased or decreased in order to keep
the level of the liquid in a tank then the final control element which is a control valve in this case implements
the decision by slightly opening or closing the valve.
78
7.4. Modes of Control
There are various modes in which the process can be controlled. The different modes depend upon
the types of controllers and the action it takes to control any process variable. Actually, the controller action
is dependent on the output signal of the transmitter. This signal is compared with the set point to the
controller and the error between these two is used to control the process. Different controllers react in
different manner to control this off-set between the controlled variable and the set point.
7.4.1. Different Types of Control Actions

On the prescribed basis, following are the different types of control actions:
On off control
Proportional control
Integral Control
Rate or derivative control
Composite control
7.4.2. Composite Control Modes

Also there are combined control actions of different types of controllers. Actually in different
operations, it is very rare that only one of the above control actions is found but a composite control action is
more often practiced.
Following are the typical composite control modes which are actually used:
Proportional-Derivate Controller
Proportional-Derivate Controller
Proportional Integral Derivative Controller
In general, the process controllers can be classified as
Pneumatic controllers
Electronic controllers
Hydraulic controllers
7.5. Selection of Controller

Actually in industry, only P, PI and PID control modes are the usual practices. The selection of most
appropriate type of controller for any particular environment is a very systematic procedure. There are many
ways and means that how a particular type of system may be controlled through which type of controller.
Usually, type of controller is selected using only quantitative considerations stemming from the analysis
of the system and ending at the properties of that particular controller and the control objective. Proportional,
Integral, and Derivative control modes also affect the response of the system.
79
Following is the summarized criterion to select the appropriate controller for any process depending
upon the detailed study of the controller and control variable along with the process severity.
7.5.1. Usage of a Simple Proportional Controller:

Simple P-controller can be used if we can achieve acceptable off-set with not too high values of gain.
So far gas pressure and liquid level control, usually a simple proportional controller may be used.
7.5.2. Usage of a PI Controller

A steady state error always remains for a proportional controller so systems where this off-set is to be
minimized, a PI controller incorporated. So in flow control applications, usually PI-controller is found.
7.5.3. Usage of a PID Controller

To increase the speed of the closed loop response and retain robustness. The anticipatory
characteristic of the derivative control enables the use of somewhat higher values of proportional gains so
that off-set minimized with lesser deviations and good response of the system. Also it adds the stability to the
system. So this type of control is used for sluggish multi-capacity process like to control temperature and
composition.
In other words, the following criterion is used for the selection of a best controller
1. Severity of the Process

2. Accuracy required
3. Cost
7.6. Control Loops

For instrumentation and control of different sections and equipment of plants, following control loops
are most often used.
i) Feedback Control Loop

ii) Feed Forward Control Loop
iii) Ratio Control Loop
iv) Auctioneering Control Loop
v) Split range control loop
vi) Cascade Control Loop
80
7.6.1. Feed Back Control Loop
It is a mechanism, process or signal that is looped back to control a system within itself. Such a loop is
called a feedback loop. Intuitively, many systems have an obvious input and output, feed the part of the output
so as to increase the input is positive feed; feedback part of the output in such a way as to partially oppose
the input negative feedback.
In general terms, a control system has input from an external signal source and output to an external
load; this defines a natural sense (or direction) or path of propagation of signal; the feed forward sense or
path describes the signal propagation from input to output feedback describes signal propagation in the
reverse sense. When a sample of the output of the system us fed back, in the reverse sense, by a distinct
feedback path into the interior of the system, to contribute to the input.
7.6.2. Feed Forward Control Loop

It is a loop describing an element within a control system which passes a controlling signal from a
source in its external environment, often a command signal from an external operator, to a load elsewhere in
its external environment.
7.6.3. Ratio Control Loop

The ratio control architecture is used to maintain the flow rate of one stream in a process at a defined
or specified proportion relative to that of another. A common application for ratio control is to combine or
blend two feed streams to produce a mixed flow with a desired composition or physical property. Consistent
with other articles in this e-book, applications of interest are processes with streams comprised of gases,
liquids, powders, slurries or melts.
7.6.4. Auctioneering Control Loop

It is the process of choosing one output signal from a set of multiple input signals. In order to use
auctioneering in your control process, you will first need to have multiple signals all measuring the same
variable. The signals will then be sent to a set of selections aligned in series. For each selector, there will be
two input signals.
For the first selector, the two inputs will be the first two signals from the device being controlled. For
each subsequent selector, one signal will be the output signal from the previous selector, while the other input
signal will be the next signal from the device.
7.6.5. Cascade Control Loop

This is a control in which two or more control loops are arranged so that the output of one controlling
element adjusts the set point of another controlling element. This control loop is used where proper and quick
control is difficult by simple feed forward or feed backward control. Normally, first loop is a feedback control
loop.
81
7.7. Instrumentation of Slurry Tank
In the mixer tank, three feeds are coming which are going out as one. These feeds include recycled
ethylene glycol, fresh ethylene glycol and terepthalic acid. Fresh ethylene glycol and TPA and mixed in a pre-
determined ratio and to maintain the stoichiometric quantities of these different streams.
A ratio control loop is used so that to ensure proper process going on in the slurry tank. Level
measurement is also critical parameter in slurry tank, so level is controlled through placing a valve; transmitter
and level controller on a fail open valve of the level in the vessel increase the given set point, the controller
will control the level by opening the valve.
And if the level in the slurry tank decreases the given set point the controller, control the level by closing
the valve.
82
7.8. Instrumentation of Esterifier
83
7.9. Instrumentation of Poly-condensation Reactor
84
Chapter 8 Cost Estimation
Chapter 8
Cost Estimation
Chapter 8: Cost Estimation
8.1. Introduction of Cost Estimation:

Cost estimation is a specialized subject and a profession in its own right. The design engineer, however,
needs to be able to make quick, rough, cost estimates to decide between alternative design and for project
evaluation. Chemical plants are built to make a profit and an estimate of the investment required and the cost
of the production are needed before the profitability of a project can be assessed.
8.1.1. Accuracy and purpose of capital cost estimates

The accuracy of an estimate on the amount of design detail available and the time spent on preparing
the estimate. In the early stages of a project only an approximate estimate will be required and justified by
the amount of information by then developed.
8.1.2. Classification of Capital Cost Estimations

Capital cost estimated can be broadly classified into three types according to their accuracy and
purpose.
8.1.2.1. Preliminary estimate:

Preliminary estimate accuracy typically 30% which are used in initially feasibility studies and to make
coarse choices between design alternatives. These are based on limited cost data.
8.1.2.2. Authorization estimate:

Authorization estimate accuracy typically 10% to 15%. These are used for authorization of funds to
proceed with the design to the point where an accurate and more detailed estimate can be made.
Authorization may also include funds to cover cancellation charges on any long delivery equipment ordered
at this stage of design to avoid delay. In a contracting organization this type of estimate can be used with a
large contingency factor to obtain a charge for tendering. Normally however an accuracy of about 5% would
be needed and a more detailed estimate would be made, if time permitted. With experience and where a
company has cost data available from similar project. A rough P & I diagram and approximate sizes of the
major sizes of equipment would also be needed.
8.1.2.3. Detailed estimate:

Detailed estimate accuracy typically 5% to 10% which are used for project cost control and estimated
for fixed price contracts. These are based on completed process design firm quotation for equipment and a
detailed breakdown and estimation of the construction cost. The cost of preparing an estimate increases from
0.1 percent of total project cost for 30 accuracy to about 2% for a detailed estimate with an accuracy of
5%.
8.1.3. Capital investment:

Before industrial plant can put into operation, a large sum of money must be supplied to purchase and
install the necessary machinery and equipment. Land and service facilities must be obtained and the plant
must be erected complete with all piping, controls and service. In addition, it is necessary to have money
available for the payment of expenses involved in the plant operation. The total capital required for the
installation and working of a plant is called total capital investment.
Total Capital investment = Fixed Capital + working Capital

85
8.1.4. Fixed Capital:

The capital needed to supply the necessary manufacturing and plant facilities is called fixed capital
investment. It includes the cost of:
I. Design and other engineering and construction supervision.

II. All items of equipment and their installation.
III. All piping, instruction and control system.
IV. Building and structures.
Auxiliary facilities such as utilities, land and civil engineering works. It is once only cost that is not
recovered at the end of the project life, other than scrap value.
The fixed capital is further subdivided into followings:
I. Manufacturing fixed capital investment

II. Non-manufacturing fixed capital investment
The fixed capital investment is classified in to two sub divisions
i. Direct cost
ii. Indirect cost
8.1.4.1. Direct cost:

The direct cost items are incurred in the construction of the plant in addition to the cost of
equipment.
I. Purchased equipment cost

II. Purchased equipment installation
III. Installation cost
IV. Instrumentation and control
V. Piping
VI. Electrical installation
VII. Building include services
VIII. Yield improvement
IX. Services facilities
X. Land
8.1.4.2. Indirect cost:

Indirect cost can be estimated by estimating following cost
Engineering and supervision

Construction expense
Contactor fee
contingencies
Start-up expenses
86
8.1.5. Working Capital:

Working capital is the additional investment needed and above the fixed capital to start the plant up
and operate it to point when income are earned. It includes the cost of
Start-up
initial catalyst charges
raw material and intermediate in the process
finished product inventories
funds to cover outstanding accounts from customer
Most of the working capital is recovered at the end of the project. The total investment needed for a
project is the sum of the fixed and working capital.
Working capital may vary from as low as 5% of the fixed capital for a simple. Single product, process
with little or no finished product storage to as high as 30% for a process producing a diverse range or product
grade for a sophisticated market, such as synthetic fiber. Typical figure for petrochemical plant is 15% of the
fixed capital.
8.1.6. Operation Cost

An estimate of the operating cost, the cost of producing a product is needed to judge the viability of
the product and make choices between possible alternative processing schemes. These cost can be estimated
from the flow sheet which gives the raw material and service requirements and the capital cost estimate.
The cost of producing a chemical product will include items listed below they are divided into two
groups
Fixed Cost
Variable Cost
8.1.6.1. Fixed Cost:

I. Maintenance
II. Operating labour
III. Laboratory costs
IV. Supervision
V. Plants overheads
VI. Capital changes
VII. Rates and other local taxes
VIII. Insurance
IX. License fees and royalty payments
8.1.6.2. Variable Cost:

I. Raw material
II. Miscellaneous
III. Utilities
IV. Shipping and packaging
Certain items can be classified without question but the classification the other items will depend on
the accounting practice of the particular organization. The items may also be classified differently in the cost
sheet and cost standards prepare to monitor the performance of the operating plant. For the purpose of the
fixed cost items for which they be held accountable.
87
8.1.7. Cost Indices

A cost is nearly an index for a given point in time showing the cost at that time relative to certain base
time. So present cost is estimate from cost index as follows
Present cost/Index at present time = Original cost/Index value at time of Original cost.
8.1.7.1. Types of cost indices

Many different types of cost indices are published regularly. Some of these can be used for
estimating equipment cost others apply specially to labor, construction, materials or other specialized fields.
The most common of these indices are:
I. Marshal-and-swift all industry and process equipment index.

II. Engineering news record contraction cost index.
8.1.8. Summary of Production cost:
Variable Cost: Typical Values

1. Miscellaneous material 10% of item (5)
2. Utilities from flow sheet
3. Shipping and packaging
Sub-total A
Fixed Cost
1. Maintenance 5 to 6% of fixed capital
2. Operating labor from manual estimates
3. Laboratory costs 20-23% of (6)
4. Supervision 20% of item (6)
5. Plant overheads 50% of item (6)
6. Capital cost 15% of fixed capital
7. Insurance 1% of Fixed capital
8. Local taxes 2% of Fixed capital
9. Royalties 1% of fixed Capital
Sub-division B
1. Sales Expertise 20 to 30% of

2. General overhead production cost
3. Research and development
Sub-Division C
Annual Production Cost = A+B+C
Production Cost per Kg = Annual Production Cost / Annual production rate
88
8.2. Purchased Cost

8.2.1. Nomenclature:
Ce = Purchased Equipment, $
S = Characteristic Size Parameter
C = Cost constant
N = index for that equipment
8.2.2. Purchased cost of TPA Storage tank:

Purchased cost of TPA Storage tank = Ce = CSn-1
S = 31.28m3/day
C = 4350
N = 0.55
CeTPA = 4350 * (31.28)0.55
= 28899.21 * 2 (for Stainless steel)
= 57797.42 $
Considering 2.50% increase per year
Purchased cost of TPA storage tank = 57798.42 * (1.025)7)
= 6870.16 $
8.2.3. Purchased Cost of EG: storage tank:

Purchased cost of EG = Ce = CSn3
S = 32.68m3/Day
C = 4350
n = 0.55
CeEG = 4350 * (32.68)0.55
= 29603.59 * 2
= 59207.18
CeEG = 5920718 * (1.025)7
= 70378.73
89
8.2.4. Purchased Cost of Slurry Tank:

Height of slurry tank = H
Diameter of slurry tank = D
Material = Stainless Steel
Bare cost from figure = 5.5 * 100
= 5500 * 2 * 1
` = 11000$
Considering 2.5% increase per year3 = 11000 * (1.0257)7
= 12915.10$
8.2.5. Purchased cost of esterifier PR-1

Ce = CSn4
S = 6.7130m
C = 0.45
Ce = 31000(6.71)0.45
Ce = 73010.75
Ce = 73010.75 * 1.0257
Ce = 86786.84 $
8.2.6. Purchased cost of Esterifier reactor PR-2

Ce = CSn2
S = 5.2m3
C = 31000
n = 0.45
Ce = 31000 * (5.2)0.45
= 65097.33
Considering 2.5 % increase per year
Ce = 65097.33 * (1.025)7
= 77380.26$
8.2.7. Total cost of esterifiers:

Total cost of esterifiers = esterifier RA-11 + esterifier RA-12
= 86786.84 $ + 77380.26 $
90
Total cost of both esterifiers = 164167.1088$
8.2.8. Purchased cost of Polycondensation Reactor RA-21:

Ce = CSn4
S = 9.2m3
C = 31000
n = 0.45
Ce = 31000 * (9.2)0.45
= 84152.34$
Ce = 84152.34 * (1.025)7
= 100030.68$

Ce = CSn2
S = 8.4m3
C = 31000
n = 0.45
Ce = 31000 * (8.4)0.45
= 80776.94$
Ce = 80776.94 * (1.025)7
= 96018.39$

Ce = CSn4
S = 8.2m3
C = 31000
n = 0.45
Ce = 31000 * (8.2)0.45
= 79905.73$
Ce = 79905.73 * (1.025)7
= 94982.80$
91
Cost of Polycondensation reactor RA-41 = 94982.80$
8.2.11. Purchased cost of condensers:

Purchased cost of 1 condensers = 1850$2
Considering 2.5% increase for year (based on 2002),
= 1850 * (1.025)9
= 2310.39 $
Total purchased cost of 5 condensers = 5 * 2310.39
= 11551.98 $
8.2.12. Purchased cost of pumps:

No. of pumps = 4
Material of construction = Stainless Steel
8.2.12.1. Pump between EG Storage tank and Slurry Mixing Tank:

Inlet flow rate of the pump = 1345.48 Kg/hr
Density of EG = 1115 Kg/m3
Volumetric flow rate of the pump = Capacity of the pump
= 1345.48 Kg/hr
= 1115 Kg/m3
= 1.21m3/hr
= 3.36 * 10-4m3/sec
Purchased cost of pump = 10808$
= 10808 * 1.0259
= 1348.77$
8.2.12.2. Pump Between slurry tank and esterifier RA-11:

Inlet flow rate to pump = 3813.82 Kg/hr
Density of Slurry = 1304.29 Kg/m3
Volumetric Flow rate to the pump = capacity of the pump
= 3818.82 Kg/hr
= 1304.29 Kg/m3
= 8.11 * 10-4m3/hr
Purchased cost of pump 2020$
92
= 2020 * 1.0259
= 2522.70$
8.2.12.3. Pump Between esterifier RA-11 and RA-12:

= 7.43 * 10-4m3/sec
= 2800 * 1.0259
= 3496.82$
8.2.12.4. Pump Between esterifier RA-12 and Polycondensation reactor RA-21:

= 7.33 * 10-4m3/hr
= 2600 * 1.0259
= 3247.04$
8.2.13. Purchased cost of coil:

8.2.13.1. For esterifier RA-11:
Total surface area of the coil = 7.0306m2
Diameter of the coil = 1.3m
Length of the coil = 2.13m
Tube diameter = 2 in = 0.05m
Purchased cost per unit length = 1500 $
Total purchased cost = 1500 * 2.13
= 3195 $
Total purchased cost of 2 coils used in two esterifiers = 3192 + 3195
Considering 2.5% increase for year (based on 2002), = 6390$
93
8.2.13.2. For Polycondensation Reactor:

For polycondensation reactor = 6390 * 1.0259
= 7980.23$
Total surface area of the coil = 12.1m2
Diameter of the coil = 1.4m
Purchased cost per unit length = 1500 $
Total purchased cost = 1500 * 2.13
= 3195 $
Total purchased cost of 3 such coils used in 3 such polycondensation reactors
= 3192 + 3195 +3195
Considering 2.5% increase for year (based on 2002), = 11970.35$
8.2.14. Total purchased equipment cost:

Total purchased equipment cost = 68704.16 + 70378 + 12915.101 + 86786.84 +100030.68 +77380
96018.39 + 94982.80 + 11551.98 + 10615.33 + 7980.23 + 11970.35
= 649314.851 $where for a predominantly fluids processing plant
8.3. Total Physical plant Cost (PPC):

PPC = PCE (1 +f1 + f2 . + f9)
Where for a predominantly fluids processing plant
F1 = equipment erection = 0.4 * PCE
= 261621.73$
F2 = Piping = 0.70 * PCE
= 457838.03$
F3 = Instrumentation = 0.20 * PCE
= 13081.87$
F4 = Electrical = 0.10 * PCE
= 65405.43$
F5 = Building Process = 0.15 * PCE
= 98108.15$
F6 = Utilities = 0.50 * PCE
94
= 327027.17$
F7 = Storages = 0.15 * PCE
= 981-85.15$
F8 = Site Development = 0.05 * PCE
= 32702.72$
F9 = Ancillary building = 0.15 * PCE
= 98108.15$
PPC = PCE (1 +f1 + f2 . + f9)
= 649314.9 ( 1 + 0.4 + 0.70 + 0.20 + 0.10 + 0.15 + 0.50 +0.15 + 0.05 + 0.15 )
PPC = 2207670.49$
8.3.1. Fixed Capital:

FC = PPC (1+ f10 + f11 + f12)
= 2207670.498 (1 + 0.30 + 0.05 + 0.10)
Fixed capital = 3201122.211$
8.3.2. Working Capital:

Taking 5% of the fixed capital
Working Capital = 0.05 * 3201122.211
= 160056.11$
Total investment required = 3201122.211 + 160056.11
= 3361178.322$
8.4. Summary of Production Costs:

8.4.1. Variable cost:
8.4.1.1. Raw material:
1 Terephthalic Acid
TPA cost per ton = 1470$

Mass of TPA used = 1801.2 Kg/hr
= 1577.8 ton/year
Total cost of TPA per year = 15778.51 *1470
= 23194412.64$/year
2 Ethylene glycol
EG cost per ton = 1050$ / ton
Mass of EG used per year = 1345.48 Kg/hr
95
= 117886.40n * 1050
Total cost of EG per year = 12375725.04$/year
Total cost of raw material:

Total cost of raw material = 23194412.64 + 12375725.04
= 35570137.66$
8.4.1.2. Cost of Miscellaneous Material:
Miscellaneous material = 10% 0f maintenance cost
Maintenance cost = 5% of fixed capital
= 0.05 * 3201122.211
= 160056.11$
Cost of miscellaneous material =0.1 * 160056.11
= 16005.61$
8.4.1.3. Cost of utilities:
Utilities cost is taken as 8% of the fixed capital
Cost of utilities = 0.08 * 3201122.211
= 256089.78$
Shipping and packaging = Not applicable
Total variable cost = Raw material cost + Misalliance materials cost + utilities cost
= 35842233.05$
8.4.1.4. Calculation of fixed cost:
Maintenance cost = 160056.11$
8.4.1.5. Operating labor:

Considering 5 shift crew are in plant to operate the plant in 3 shafts
So total number of opening personal = 15
Now,
Wage rate per hour in US = 8$/ hr
= 64473.6$
Adding 50% of the various allowances and overheads the per year wage of single work
= 64473.6 + 32236.8
= 96710.4$/year
Considering 5 shift crew per 3 shifts,
Total labor cost considering 15 personnel = 15 * 96710.4$
96
= 145065$/year
Laboratory cost = 0.2 * operating labor cost
= 290131.2 $
Supervision cost = 0.2 * operating labor cos
= 290131.2$
Plant overheads = 0.5 * 1450656
= 725328$
Capital charges = 0.1 * fixed capital
Capital charges = 320112.22$
Insurance = 0.01 * FCC
= 32011.2$
Local taxes = 0.02 * FCC
= 64022.44$
Royalties = 0.01 * FCC
= 32011.22$
Total fixed costs = 3364459.61$
Direct Product cost:
Direct product cost = V.C + F.C
= 35842233.05 + 3364450.61
= 39206692.66 $
General operating expenses:
Company general operating experience including sales expenses general overheads and research and
development
= 0.2 * 39206692.66
= 7841338.53 $
Annual Production Cost:
A.P.C = 39206692.66 + 7841338.53
= 47048031.15 $/year
Production cost:

Production cost per Kg =

= 47048031.15$/year
Production cost per Kg = 2.58 $/Kg
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Plant Design Project

Production of 100 tons/day

Institute of Chemical Engineering & Technology,

University of the Punjab, Lahore

1.2. Classification of Polyesters

1.2.1. Thermoplastic Polyesters

1.2.2. Thermosetting Polymers

1.3. Types of Polyesters

1.3.1.3. Aromatic Polyesters

1.3.2.2. Polyester Plasticizer

1.3.2.3. Polyester Resin

1.3.3. On the Basis of Structural Differences/Bonding

1.3.3.1. Saturated Polyesters

1.3.3.2. Unsaturated Polyesters

1.3.3.3. Classification of Unsaturated Polyesters

Class Characteristics Uses

1.4. Importance of Polyester

1.5. Consumption of Polyester

1.6.1. Usage of Polyester Films

1.6.2. Usage of Polyester in Medical Field

1.6.3. Usage of Polyester Fibers

1.7.1. Criteria for Fiber Forming Polymers

A history of man-made fibers is given in Error! Reference source not found..

1.8. Economical Prospective

Table 1-2: History of Man-Made Fiber

Date Fiber First Commercial Production

1.9.2. Industrial Uses

1.9.2.1. Conveyer belts, V-belts

1.9.2.2. Ropes, Fishing Nets

1.9.2.3. Sewing Threads

1.9.2.4. Filter Cloth

High strength, especially a high wet strength and low elongation.

1.9.2.7. Woven belts

1.9.2.8. Electrical Insulators

1.9.2.9. Protective Clothing

1.9.2.10. Photographic Film

1.9.3. Other Uses

1.10. Conversion of Chips to PET Fiber

For man-made fibers, the fiber-forming polymer, made randomly flow-able by

1.11.1. Melt Spinning

There are two main processes:

1. The spinning process

1.11.1.1. Spinning Process

2. Ludwig Bottenbruch, Engineering Thermoplastics: Polycarbonates, Polyacetals Polyesters, and

Chapter 2: Process Selection

2.1.1. General Description of PET Polymerization

2.1.2. Why Two Step Reaction?

i. Polycondensation process is carried out to a uniform, chemically pure, monomeric starting

2.2. Types of PET Polymerization

2.2.1. Batch Process

2.2.2. Continuous Process

1. Transesterification Process (DMT Process)

2.3. Advantages of Continuous Process over Batch Process

Batch Process Continuous Process

2.4. Contrasting the DMT & TPA Processes

2.5. Difference between DMT & TPA Processes

i. Dimethyl terephthalate (DMT)

2.7. Take Over of DMT Process by TPA Process

2.8. Basis for the Process Selection

Chapter 3: Selected Process Description

3.1. Direct Esterification

i. Purified Terepthalic Acid (TPA)

3.3. Raw Materials

Table 3-1: Specification Sheet of Mono-Ethylene Glycol