INTRODUCTION

1.1 INTRODUCTION TO POLYETHYLENE

Polyethylene is basically the polymer of ethylene, and ethylene is the gas

obtained from the petroleum refinery. Ethylene is the member of the alkenes
series. Ethylene has two carbon atoms and four hydrogen atoms. Its structure is

Polyethylene has the simplest structure of all the polymers .other names of
polyethylene are Polymethylene, polyethylene. Polyethylene is the most widely
used plastic material throughout the world, and high density polyethylene is the
most widely used type of polyethylene.

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1.2 WORLDWIDE USAGE OF THE MOST COMMON PLASTIC
TYPES

The chart given below shows the world wide usage of the most common plastic
types in 2000. It is clear from the chart that polyethylene is most widely used
plastic material

5.10% PE
11.60% 40.30% PP
PVC
21.10%
PS
21.90%
ABS/SAN

1.3 GRADES OF POLYETHYLENE

Grades of polyethylene these can be classified as

1): Low density polyethylene
2): Medium density polyethylene
3): High density polyethylene
Density up to .92 g/cm3 will be in the range of Low density polyethylene, if the
density in the range of 0.93-0.94 g/cm3,it will be called as medium density
polyethylene and if the density is above 0.94 g/cm3 ,then it will be called as high
density polyethylene.

2
LDPE has a high degree of branching, which means that the chains do pack into
the crystal structure as well. It has therefore less strong intermolecular forces as
the instantaneous-dipole induced-dipole attraction is less. This results in a lower
tensile strength and increased ductility. LDPE is created by free radical
polymerization
HDPE has a low degree of branching and thus stronger intermolecular forces
and tensile strength. The lack of branching is ensured by an appropriate choice
of catalyst (e.g. Ziegler-Natta catalysts) and reaction conditions. Another
important grade of polyethylene is LDDPE i.e. linear low density polyethylene
LLDPE is a substantially linear polymer, with significant numbers of short
branches, commonly made by copolymerization of ethylene with longer-chain
olefins.
The chart given below showing the worldwide usage of different grades of
polyethylene in 2000

LDPE,
24.5 HDPE
HDPE,
47.4 LLDPE
LDPE
LLDPE,
28.2

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High density polyethylene consumption in Pakistan is 105000 tons in year 2005.
Unfortunately Pakistan has no plant for the production of Polyethylene.

1.4 History of HDPE

The history of HDPE actually began in 1890s with the synthesis of

“Polymethylene” from the decomposition of diazomethane. Between 1897-1938
numerous reports of such polymers have been appeared in the literature.
Another condensation method was investigated by Carothers and coworkers and
reported in 1930.they reacted decamethylene dibromide with sodium in a Wurtz-
type reaction but found it difficult to obtain In(1938-1940) another early approach
described that HDPE can also be prepared by the hydrogenation of carbon
monoxide over ruthenium and cobalt catalysts. The reported melting point of 132-
1340 C and density of 0.980g/cm3 again indicate that linear HDPE have been
obtained.
Today’s low pressure catalytic processes from which the HDPE now comes were
discovered in the early1950s. Patent applications were filed by Standard Oil of
Indiana, in 1951, by Phillips Petroleum Company in early 1953and by Ziegler and
coworkers in late 1953.
The Standard Oil Patent describes a supported reduced molybdenum oxide or
cobalt molybdate on alumina, with the ethylene preferably contacting the catalyst
in an aromatic solvent to affect the polymerization. Operating temperature of 100
to 2700 C were disclosed and the molecular weight could be varied from very
high to low susuch as those of greases..
At about the same time (1951) it was discovered that supported chromium oxide
catalysts would also polymerize ethylene at low pressure to produce high
molecular weight polymers. Reaction temperatures were in the range of 60-190 0
C. Polymer characteristics, particularly, molecular weight and molecular weight
distribution, could be varied by reactor temperature, pressure and the activation
temperature of the “Phillips catalyst”.

4
Shortly, thereafter, yet another transition metal catalyst capable of polymerizing
ethylene at low pressure was discovered in Germany. This approach uses a
transitional metal halide, or other complex activated by an aluminum alkyl co
catalyst .transitions metal compound of group IVa through Via (Ti proffered) was
claimed.
Although the standard oil discovery came first, commercialization was slow.
Three plants were eventually built between 1961 and 1971, but the process had
poor economics and was soon scrapped .In contrast the Phillips and Ziegler
discoveries were commercialized rapidly and still exist today in more advanced
forms. At Phillips the first plants were brought on stream in 1955 and 1956.while
the first Ziegler plant was brought on stream in late 1956 by Hochest .A second
one was built in 1957 by Hercules.
At the end of 1970s considerable interest in what became known as linear low
density polyethylene (LLDPE) which are intermediate in properties and structure
to high pressure and low pressure materials .while strictly speaking these are
copolymers it is more convenient to consider them alongside the homopolymer.
The very low density polyethylene was introduced by Union Carbide in 1985
were closely related.
By the 1990s there was enormous activity in the development of a further type of
polyethylene based on misallocate catalysis methods. Commercial catalyzed
polyethylene production started in 1990s and it is estimated in 2000
Metallocene–catalyzed polyethylene will comprise about 2% of the total
polyethylene market
By the mid 1990s capacity for polyethylene production was about 50,000, 000
t.p.a much greater than any other type of plastic material .of this capacity about
40% was for HDPE ,36% for LDPE and about 24% for LLDPE.

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1.5 Properties of HDPE

Some general properties of polyethylene have been given

Below in the table

Property value

Density(g/cm3) 0.960
Tensile strength(p.s.i) 42000
Elongation (%) 40
Modulus (p.s.i) 140000
Crystalline % 87
Linear thermal expansion coefficient 1.3*10^-4
Water absorption (%) .02
Oxygen index 17
Volume resitivity(log ohm.cm) 17
Molding pressure range Psi 12000-15000
Thermal conductivity(cal.cm/sec.cm2) 0.00011-0.00012

Mould shrinkage (%) 3

Mould temperature range(°C) 30-70
Dissipation factor1kHz .0005
Dielectric constant 1kHz 2.3
Dielectric strength(MV/m) 22
Strain at yield (%) 15

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1.6 Commercial application of HDPE

Its high chemical stability facilitate the processing of HDPE by many conventional
techniques .some of the most common application include injection molding,
blow molding, blown and cast film, pipe and tubing, and wire and table coating.
Injection molding HDPE is injected into a metal mold at 200-260 0C and pressure
will be in the range of (690-1380 atm).the mold is then cold and opened and the
solid article, which is now in the shape of mould, is removed.
Blow molding articles account for the largest single use of HDPE. This technique
is used for rapid processing of large quantities of articles Of relatively simple
configuarations.,such as bottles and simple containers.
The impermeability, stiffness and higher softening temperature of HDPE make it
useful for making its film by blown film extrusion.
Pipes and tubes can also be made by HDPE.HDPE pipe is used in low pressure
applications for transporting potable water, gas, acids, liquid
hydrocarbons,oils,salt water, and others chemicals and solvents.
Excellent electrical properties and moisture resistance make HDPE ideal for
cable and wire coating. Use includes power, communications and control,
applications.
Due to low water absorption HDPE ropes are used in marine applications where
it has a clear advantage over nylon.
Large items such as tote boxes fuel tanks, water storage tanks are often made
by rotational molding operation of HDPE.

7
PROCESS SELECTION

2.1 CURRENTLY USED PROCESSES

All the processes currently in use for the production of HDPE fall into three
categories:
(a) Solution processes
(b) Slurry processes
(c) Gas Phase Polymerization.
These processes, the economics of which are well established, use second and
third generation catalysts, are capable of continuous or discontinuous operation,
and are run as nearly closed loops, causing a minimum of pollution. For the most
efficient HDPE production technology, low investment costs, consistency of
product, low operating costs and the yield of polymer per gram of catalyst are
important considerations.
Each of these polymerization processes has their pros and cons with regard to
these factors.

Solution Processes

The earliest commercial HDPE plants used a solution process in which the
polymer dissolves in a hydrocarbon solvent as it is formed. Cyclohexane was

8
commonly used as a solvent at 120-150 0C. Polymerization ensues giving out
large heat energy. Some processes use water jacketing to remove reaction heat,
while in others cooling is done by monomer refrigeration. Solution processes are
generally run at moderately high pressures
and temperatures and require heavier wall reactors than other processes.
However, because of the beneficial effect of increased temperature on reaction
rates, catalyst efficiencies are usually higher with short residence times. This
allows a higher production rate for a given size reactor. Processes can be highly
automated. For example, product molecular weight can be controlled by
monitoring reaction parameters, and reactor conditions can be changed via
feedback loops. This type of process is inherently limited in the amount of
polymer which can be kept in solution: 35-40% is the absolute maximum. Also,
making high molecular weight polymer gives difficulties by putting high torque on
the stirrer, dropping out of the solution as gel, and fouling the reactor. Thus, it is
more difficult to make extrusion blow molding grades of HDPE with solution
processes, particularly those requiring a very high molecular weight component
for high melt strength and die swell. On the other hand, solution processes
generally excel in producing injection molding grades, where narrow MWDs and
lower MWDs are required.

Slurry Processes

In this type of process, polymerization of ethylene in suspension in a

hydrocarbon diluent is carried out. Diluent is a poorer solvent of polyethylene.
Hence the polymer or copolymer separates out from the diluent as fine particles.
Hence, the viscosity of the diluent does not increase as rapidly as in the solution
process. As result, a higher concentration of polymer can be maintained in the
reactors. Some of the advantages of slurry-type processes include a higher
volume yield of product for a given size reactor, as well as the greater ease of
diluent removal. On the other hand, residence times are usually longer than in
most solution processes. Still another advantage is the potential for making

9
powders, suitable for rotomoulding, directly in the reactor, thus cutting out the
expensive grinding step.
Reactors used for slurry processes may take any of several forms, from kettles to
loop-type designs. The latter have high surface-to volume ratios, which are
advantageous for controlling reactor temperature, so necessary in maintaining
molecular weight and molecular weight distribution as desired. A disadvantage of
the slurry type process is the greater difficulty of automation, since there are
fewer ways to immediately sense any changes in the product itself. Also, slurry
processes tend to make more 'twilight' material in switching from one grade to
another. Also, many processes are susceptible to fouling.
In practice, most slurry processes, unless modified, tend to yield very high
molecular weight materials which are not commercially useful. Thus, a "chain
stopper" or chain transfer agent is often required. For Ziegler-type catalysts,
hydrogen is generally used; it tends to give a "clean" product and is not
extensively expensive.
Because of their tendency to make higher molecular weights, most slurry
processes perform well in making blow molding grades; in some instances,
however, tandem reactors may be required for broad MWDs. Injection moulding
grades are harder to make. Suspension polymerization, like the Hoechst-Ziegler
technology, is still one of the most mature, flexible, versatile and widely used
Processes. It is the only technology capable of producing the wider range of
HDPE polymers - and polymerisation of ultra-high Molecular weight HDPE as
well.

Gas Phase Processes

Unlike solution or slurry processes, the original gas phase processes employed
no hydrocarbon diluent. Union carbide introduced the first gas phase technology
in1968, and other firms soon developed the approach still further, such as
Naphthicime, British Petroleum, BASF, and Amoco. In this technology, solid
catalysts are used for ethylene polymerization or its copolymerization with light

10
comonomeres in the gas phase. the system van be agitated by mechanical
devices, such as horizontal paddles or screws, but more often by a gas stream of
ethylene which fluidizes the polyethylene particles bed.

During the last one decade, vapour phase processes have become a commercial
reality. Initially there were many problems, such as preparation of a suitable
catalyst, excessive catalyst particle size and finding catalyst of sufficiently high
activities along with the desired MW and MWD. Still another problem was in heat
removal and in maintaining constant temperatures. Several companies have
been very active in research, one being Union Carbide, which solved most of
the technical problems listed above about five years back. Since then it has been
the most widely used HDPE process. Reportedly, the process may require two,
or perhaps more, different supported catalysts to make a complete grade slate.
As already described, the process operates on a fluidized bed principle. At start
up, a bed of catalyst-rich polymer is fluidized by an upward stream of ethylene
hydrogen, and possibly a carrier gas. As the particles begin to grow due to build
up of polymer, larger particles tend to fall to the bottom of the reactor, where they
are drawn off through a special valve system.
Reaction temperature is controlled by introducing chilled monomer through the
bottom porous plate. For satisfactory conversions, a number of passes are
required. The product from the reactors is low in ash and can be palletized
without further purification. By its very nature, a fluidized process is expected to
yield broad MWD products. In general this comparatively new technology has
some limitations with respect to flexibility and consistency.
Now the below table will describe the selection of process

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2.2 PROCESS SELECTION

Process Licensor Slurry Gas Phase Solution Phase

Polymerization Polymerization Polymerization

Solvent System n-hexane or -------- cyclohexane

Isobutene
Conversion 98% 2% 95%
Temperature C 70-90 80-100 130-150

Pressure 7-10 atm 50-200 atm 20 atm

ADVANTAGES 1.Very low scale 1.Producing 1. Short residence time

of operation product with very 2. Catalyst activity is
2.Small sized low impurities high
reactors 2. No solvent is 3. High production rate
3.Good for employed for given sized reactor
HMW grades 3. Simplicity 4. Process is highly
4. Higher 4.No solvent cost automatic.
concentration of 5.Small amount of 5. Relatively low cost
polymer catalyst is used 6. Since the process
maintained in operates at high
the reactor. temperature and
pressure, so the reaction
rate will be high.
7. Heat removal is easy
due to large quantity of
solvent.
8. Good for low
molecular weight grades

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Disadvantages 1. Very 1. Difficult method for 1.High pressure is
high residence preparation of required
time suitable catalyst 2.High temperature
2. Difficult 2. Heat removal is required
y of automation problem 3.Due to high
3. low rate 3. Excessive particle temperature and
of reaction size catalyst pressure thick walled
4. low 4. High equipment reactor will be
production rate cost required
5. Very low
conversion
6. Compression cost
is very high
There are various methods for the production of HDPE by solution polymerization
such as DuPont process, Stamicarbon process and Phillips solution
polymerization process, but I have selected the
Phillips solution polymerization process due to the following advantages
1. Conversion is more.
2. Catalyst is more reliable
3. Different grades of HDPE can be produced by using the Phillips catalyst
just by varying the proportion of its components.

PREPARATION OF PHILLIPS CATALYST

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Preparation of the Phillips catalyst requires careful attention to details in order to
obtain the high catalyst activities required. The catalyst contains usually about 2-
5% by weight of by weight of chromic oxide supported on silica- alumina.
The silica alumina support may be used in the form of granules (14/28mesh) or
pellets (5/32 inch).the preferred support has large pore size and a low surface
area to facilitate the dissolution of the coating of the polymer that is sub
sequentially formed. A particular active catalyst is characterized by a surface
area/weight ratio of 400-600m2/gm and a pore diameter of 65-150A0 .
Chromic oxide catalysts are activated, before being used for polymerization by
contacting the finely divided material with air for several hours at temperatures
from 400-9750C.After activation the catalyst is cooled in dry air and stored until
used. the chromium on the surface of the catalyst should be in hexavelent state.
Our catalyst contains about 5 % chromium supported on silica-alumina.

Solvent Properties

In Phillips solution polymerization the solvent used is Cyclohexane. Some

common properties of cyclohexane has been given as

Physical properties

Cyclohexane is a colourless, mobile liquid with mild, sweet odors. It is slightly

soluble in water and soluble in alcohol, acetone, benzene, ethanol, ethyl ether,
olive oil, and carbon tetrachloride.
Melting Point (°C) = 6.47°C
Boiling Point =80.7°C
Specific Gravity = 0.779
formula weight = 84.161 
Viscosity (cp, 20oC) =0.980
Critical temperature =281.0 oC

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Critical pressure =30835mm Hg
Flash point = -18.4oC

Chemical properties

Cyclohexane is a flammable, non-corrosive liquid

Common uses

This compound is used as a solvent to dissolve cellulose ethers, lacquers, resins,

fats, waxes, oils, bitumen and crude rubber. It is also used in perfume
manufacturing, during surface coating operations (lacquers), in synthesis of
adipic acid for production of nylon 66 and engineering plastics, during synthesis
of caprolactam in nylon 6, paint and varnish remover, in the extraction of
essential oils, in analytical chemistry for molecular weight determinations, in the
manufacturing of adipic acid, benzene, cyclohexyl chloride, nitrocyclohexane,
cyclohexanol and cyclohexanone, in the manufacturing of solid fuel for camp
stoves, in fungicidal formulations (possesses slight fungicidal action) in the
industrial recrystallising of steroids, organic synthesis, recrystallising medium
glass substitutes, solid fuels, in analytical chemistry and in manufacturing of
adhesives.

Monomer Properties

Molecular formula
C2-H4

Physical properties

Relative Vapour Density: 0.980

Flash Point: –135.0°C
Percent Volatile by volume: 100

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Boiling point: –104°C
Explosive Limits: 2.7 mol%–36 mol%
Automatic Ignition Temperature: 543°C in air at atmospheric pressure.
Colourless compressed gas with sweet Odour. Slightly soluble in water, soluble
in most organic solvents.

End Uses

Ethylene is the major raw material at the Orica Botany, Botany, New South
Wales Site for the manufacture of polythene, ethylene oxide and its range of
derivatives. Ethylene is also used for the
Manufacture of polyester fibre and film, vinyl acetate and a range of alcohols and
solvents.

Production process

Ethylene is basically obtained from refinery it but it can be prepared form the
dehydrogenation of ethylene that is also a component of petroleum refinary This
is a light fraction of hydrocarbon extracted from underground gas fields in the
Cooper Basin in naphtha, a light fraction produced in the distillation of crude oil
and purchased

Storage and transport

Ethylene is classified as a flammable gas for the purpose of transport. Refer to

State Regulations for storage and transport requirements.
The product must not be loaded with flammable liquids in bulk, flammable solids
(Class 4) or oxidizing agents.

Personal protection

16
Wear impervious gloves, full face shield or chemical goggles, rubber boots and
overalls. Use with adequate ventilation. If inhalation risk exists wear air supplied
mask. Avoid all contact with liquid product to prevent cold burn situations.

2.3 PROCESS FLOW SHEET

2.4 FLOW SHEET DISCRIPTION

First of all the ethylene has been compressed to 20atm and the catalyst has
been slurred with the cyclohexane solvent. Then both of the stream has been
sent to the reactor where the polymerization of ethylene takes place at
1400C.Catalyst contain about 5 % chromium oxide, supported on silica-alumina.
Concentration of ethylene within the reactor may be 10-15% by weight of the
total mixture. Solvent has been used to remove the part of the heat of the
reaction, to dissolve the monomer and polymer, to reduce the viscosity of the
mixture, to promote good polymer growth and to prevent adhesion of HDPE
powder and catalyst with the walls of the reactor. Conversion within the reactor is

17
95%. Heat of reaction will be removed by cooling coil by circulating the cooling
water within the coil.

After the reactor the separation process will be started. Mixture Of solvent,
catalyst, HDPE and unconverted ethylene gas has been sent to horizontal gas-
liquid separator where the ethylene will be recovered from the top by reduction
of pressure and then the remaining mixture will be sent to the first centrifuge
where the catalyst that is in undissolved form will be removed by devolving high
centrifugal force.

Cooling plus centrifugation mechanism to recover the dissolved HDPE from

cyclohexane. In the cooler the temperature has been decreased to 48 0C to make
the HDPE insoluble in the cyclohexane and then the centrifuge will remove the
HDPE from solvent.

HDPE comes from centrifuge contains some cyclohexane contents and we want
to reduce these contents up to .002%. For this purpose we use rotary air dryer.
In rotary air dryer we use air as a heating media to remove cyclohexane contents
up to required extent. The HDPE powder leaving the dryer is about 99.9% pure.

MATERIAL BALANCE

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3.1 BASIS

= 12500 Tons per Annum

= 1578.25 Kg/hr production of HDPE

3.2 OVERALL MATERIAL BALANCE

components Entering, Kg/hr Leaving, Kg/hr

Ethylene gas 1661.25 83.0265
cyclohexane 10668.39249 10668.39249
catalyst 23.5877 23.5877
Water 187491 187491
HDPE ----- 1578.18
air 1469.55 1468.55
Total 201312.73 201312.73

3.3 MATER BALANCE AROUND EACH UNIT

All the units are in Kg/hr

19
Equipmen Ethylen Cyclohexan Catalys HDPE air Water Total
t e e t
Reactor 1661.25 10668.39 23.5877 -------- --------- 18562 197978.22
(in) 5
Reactor 83.0625 10668 23.5877 1578.18 18562 197978.22
(out) 5

Separator 83.0625 10668.39 23.5877 1578.18 ------- 12353.78

(in)
Centrifuge --------- 10668.39 23.5877 1578.18 ------- 12270.71
1 (in)
--------- 10668.39 0.47 1578.18 1866 14113.04
Cooler (in)
Centrifuge --------- 10668.39 0.47 1578.18
2 (in)
Drier (in) --------- 106.68 1578.18 3728.98 5413.84

Drier (out) 106.68 1578.18 3728.98 5413.84

At the end we will get the almost pure HDPE that will contain only .026% solvent
and the remainining solvent will be separated as the side stream by using hot air.

REACTOR

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4.1 GENERAL

Every industrial chemical process is designed to produce economically a desired

product from a variety of starting materials through a succession of treatment
steps. The raw materials undergo a number of physical treatment steps to put
them in the form in which they can be reacted chemically
In the next step they pass through the reactor. The products of the reaction must
then undergo further physical treatment separations, purification, etc. For the
final desired product to be obtained.
Design of equipment for the physical treatment steps is studied in the unit
operations. Economically this may be an inconsequential unit, perhaps a simple
mixing tank. Frequently, however, THE chemical treatment step is the heart of
the process, the thing that makes or breaks the process economically.
Design of the reactor is no routine matter, and many alternatives can be
proposed for a process. In searching for the optimum it is not just the cost of the
reactor that must be minimized. One design may have low reactor cost but the
materials leaving the unit may be such that their treatment requires a much
higher cost than alternative designs. Hence, the economics of the overall process
must be considered.
Reactor design uses information, knowledge and experience from a variety of
areas Thermodynamics, Chemical kinetics, Fluid mechanics, Heat transfer, Mass
transfer, and Economics.
Chemical reaction engineering is the synthesis of all these factors with the aim of
properly designing a chemical reactor. To find what a reactor is able to do we
need to know the Kinetics, the contacting pattern and the performance equations.
In the designing of reactor we want to know that what size and type of reactor
and method of operation are best for a given job. Because this may require that
the conditions in the reactor vary with position as well as time, this question can
only be answered by a proper integration of the rate equation for the operation.
This may pose difficulties because of the temperature and the composition of the

21
reacting fluid may vary point to point within the reactor, depending on the
endothermic or exothermic character of the reaction, the rate of heat addition or
removal from the system, and the flow pattern of the fluid through the vessels. In
effect, then, many factors must be accounted for in predicting the performance of
a reactor.
How best to treat these factors is the main problem of the reactor design.

4.2 CLASSIFICATION OF REACTORS

Classification of chemical reactors can be achieved in two different kinds.

Depending upon the nature of reactants and product
a. Homogeneous Reactors
b. Heterogeneous Reactors
Depending upon the mode of operation
a. Batch Reactors
b. Continuous Reactors ( Stirred tank reactor, Tubular flow Reactor)

Homogeneous Reactors

In Homogeneous Reactors only one phase, usually a gas or a liquid, is present. If

more than one reactant is involved, provision must of course be made for mixing
them together to form a homogeneous whole.
Often mixing the reactants is the way of starting off the reaction, although some
times the reactants are mixed and then brought to the required temperature.

Heterogeneous Reactors

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In Heterogeneous Reactors two or possibly three, phases are involved, common
examples are gas – liquid, liquid – solid, and liquid – liquid systems. In cases
where one of the phases is a solid, it is quite often present as a catalyst; gas –
solid catalytic reactors particularly form an important class of Heterogeneous
catalytic Reactors. In a gas – solid catalytic reactor, the reaction takes place on
the surface of catalyst and hence heterogeneous. However, bubbling a gas
through a liquid may serve just to dissolve the gas in the liquid where it then
reacts homogeneously. The reaction is then homogeneous but the reactor is
heterogeneous itself.
Generally, a heterogeneous reactor exhibits a greater variety of configurations
and contacting pattern than homogeneous reactors.

Batch and Continuous Reactors

Another kind of classification which cuts cross the homogeneous –

heterogeneous division is the mode of operation. Batch wise operation has
carried out small scale preparative reactions in the laboratory. There are many
situations, however, especially in large scale operations, where considerable
advantage occurs by carrying out the chemical reaction continuously in the flow
reactor. In the Tubular Flow Reactors the aim is to pass the reactants along a
tube so that there is as little intermixing as possible between the reactants
entering the tube and the product is leaving at the far end.
In Continuous Stirred Tank Reactor, an agitator is introduced to disperse the
reactants thoroughly into the reaction mixture as they enter the reactor. The
product stream is drawn off continuously and, in an ideal state of perfect mixing,
will have the same composition as the contents of reactor every where in the
reactor.

4.3 COMPARISON OF STIRRED – TANK AND TUBULAR – FLOW

REACTORS

23
The stirred – tank reactor has certain advantages because of the uniform
temperature, pressure, and composition attained as a result of mixing. As
mentioned, it is possible to operate such a reactor under isothermal conditions
even when the heat of reaction is high impossibility is the usual in the tubular
type. Where a small temperature variation is desired, for example, to minimize
side reactions or avoid unfavorable rates, the opportunity for isothermal operation
at the optimum temperature is a distinct advantage. Stirred – tank reactors by
virtue of their large volumes provide a long residence time. This, combined with
the isothermal nature of the reactor, permits operation at the optimum
temperature for a long time. For rate equation of certain type the selectivity in
multiple reactions may be greater in tank reactors than in tubular – flow reactors
for the same residence time.
However, for high – pressure reactions it is usually necessary, because of cost
considerations, to use small – diameter tubular reactors rather than tank types.
Tank reactors that are to be operated at high pressures require a large wall
thickness and complex sealing arrangements for the mixer shaft, factors which
increase both initial and maintenance costs.
The rate of heat transfer per unit mass of the reaction mixture is generally lower
in the tank type than in the tubular reactor.
In Summary stirred – tank reactors can be used when the heat of reaction is high
but only if the temperature level obtained in their isothermal operation is
satisfactory from other stand points. If reactions are endothermic and a high
temperature is required, tubular reactors are usually indicated.

4.4 REACTOR SELECTION

We have to consider the following factors for the reactor selection criteria
1- Conversion
2- Selectivity
3- Productivity

24
 4- Yield
5- Heat exchange
6- Mixing
7- Catalyst Distribution
8- Hold-up Time
9- Availability
10-Compatibility with processing
11-Energy utilization
12-Safety
13-Economics

Advantages of Continuous Stirred Tank Reactor

1. Mixing of Reactants
2. Good Temperature Control
3. High heat and mass transfer efficiencies
4. Useful for slow reactions requiring large hold up time
5. Uniform Composition throughout the reactor
6. Distribution of Catalyst
7. For Liquid-Liquid system
8. Ease of Automatic Control
9. Less Man power requirement

Standard stirred tank reactors

The following table describes the standard stirred tank reactors

Rated capacity Actual capacity Jacket Ft2 Outside diameter (in)

gal gal area ft2

25
500 559 75 54
750 807 97 60
1000 1075 118 66
1200 1253 66
1500 1554 72
135
2000 2083 78
155
25000 2756 84
191
3000 3272 90
230
3500 3827 96
256
4000 4354 102
283
5000 5388 108
304
6000 6601 120
353
8000 8765 132
395
10000 10775 144
466
540

4.5 DESIGNING STEPS

The designing of reactor contain the following steps

1. Collect the physical property data and thermodynamic data required for
the design
2. Find the rate of reaction from the rate equation
3. Volume of the reactor
4. Residence Time
5. Diameter of the reactor
6. Height of the reactor

26
 7. jacket selection
8. Impeller selection
9. Impeller specifications
10. Baffles Dimensions
11. Power calculations
12. Mechanical design

1. Data collection

Given Data

Mass flow rate of ethylene 1661.25kg/hr

entered
Mass flow rate of catalyst 23.5877 kg/hr
entered
Mass flow rate of solvent 10668.39Kg/hr
entered
Density of ethylene 17.36 kg/m3
Density of catalyst 2550kg/m3
Density of solvent 658Kg/m3
Volumetric flow rate of ethylene 95.69m3/hr
Volumetric flow rate of catalyst 0.009250m3/hr
Volumetric flow rate of solvent 16.21m3/hr
Molar flow rate of ethylene 59.33kgmol/hr
Molar flow rate solvent 127.00Kgmol/hr
Molar flow rate of catalyst 0.2382kgmol/hr
Total mass flow rate of the 12353Kg/hr
mixture
Total mol flow rate of the 186.57Kgmol/hr
mixture
Mass fraction of ethylene 0.13447
Mass fraction of catalyst 0.86361
Mass fraction of cyclohexane 0.0019

27
 Wt. average density of the 575.46Kg/m3
mixture
Total vol .flow rate of the 21.466m3/hr
mixture
Temperature of reactor 140co
Pressure inside the reactor 20 atm
Viscosity in the reactor 2.3cp
Conversion 95%

2. Rate Of Reaction
Rate equation
-rp= Kki kp [A][RH][M]2
Kt
Where
K = .023lit/mol/sec
Ki = 26.33lit/mol/sec
Kp = 23.20lit/mol/sec
Kt = .005sec-1

[A] = conc. of catalyst=.0031068/21.433=.00034Kgmol/m 3

[RH] = conc. of co catalyst=.09234/21.433 = .0107Kgmol/m 3
[M] = concentration of monomer
=9.33Kgmol/21.433m3/hr
=.7622Kgmol/m3
By putting the values in above equation
-rp=5.006534mol/dm3/hr
= .08344mol/dm3/min

3. Volume of the reactor

28
 V/Fa0=Xa/-ra
Conversion=95%
Fa0=molar f low rate of the total mixture=186.57Kgmol/hr
Volume of the reaction mixture=35.40m3/hr
Allowances of the reactor =10%
Volume of the reactor =35.40+.1*35.40 = 38.940 m 3
Taking it as standard 40m3

4. Residence time of the reactor

 X A

C Ao r A

CA0=concentration of ethylene = mol. flow rate of ethylene

total vol. flow rate of the mixture
= 59.33/21.46
= 2.7639Kgmol/m3
Residence time = (.95/5.00653)*2.7639 =0.5238hr
Residence Time = 31.43mins

5. Diameter of the reactor

V =volume of the reactor = 3.14*D2*H/4

H=height of the reactor = 1.25*D
V=volume of the reactor = 3.14*D3*1.5/4
D=diameter of the reactor = [40*4/(3.14*1.5)]1/3
D= diameter of the reactor = 3.40m

6. Height Of The Reactor = 1.25*D

29
 =height of the reactor = 1.25*3.40
H = 4.30m

7. Jacket Selection

Dimpled jacket selected (because volume is greater than 1.89m 3)

Heat Load= QRmax, cooling = 2.97*10^6kj/hr
Cooling provided by the jacket = Qj, cooling = Uj Aj (TR – Tj )
ASSUMING JACKET COVERS 90 % OF THE REACTOR
Jacket Area = Aj =πD2 / 4 + π DL
= 53.64m2
Uj = 539.52 W/m2K
Qj, cooling = 624.58* 53.64 * (413 – 323)
= 3.072*10^6KJ/hr
Since Qj, cooling > QRmax, cooling
Hence jacket satisfies our requirement

4.6 IMPELLER SELECTION

Impeller selection depends on

1. Viscosity of Liquid
2. Degree of Mixing
3. Flow Pattern
4. Rpm
5. Power Requirement
6. Economics

Types of Impellers

Factors Propellers Paddles Turbine

Viscosity For Low to For Moderate For Low to High

30
 Moderate Viscous Viscous Liquids Viscous Liquids
Liquids
Flow Pattern For Axial Flow For Radial and For Radial and
Tangential Flow Tangential Flow,
sometimes Axial
Flow also.
Types Square Pitched Flat Paddle, Flat, Vertical,
Marine Propellers Anchor Agitator Curved, and
Pitched Blade
Blades 3-blade,4-Blade 2 and 4 bladed 2-8 Blades But 6-
Toothed Paddles Blade is used as
standard
RPM Ranges 400-800,1150- 20-150 50-250
1750

Why I have selected the flat blade turbine impeller

I have selected the flat blade turbine impeller due to following advantages
1. Turbines are effective over a wide range of viscosity
2. It is generally required slower speed
3. It can circulate the material in the radial direction in a good manner
4. It can operate at slower speed.
5. Cost is low.
Construction of flat blade turbine impeller has been shown below

31
4.7 IMPELLER DESIGN

Diameter of the tank(reactor) Dt = 3.40m

The figure shown describes the dimensions of the impeller

For impeller diameter

Da/Dt = 1/3
Da = 1.13m
Length Of Impeller Blades= L
L / Da = 1 / 4
L= .2825m
W ( impeller blade width )
W / Da = 1 / 5
W = 0.226m

For E ( height of impeller above the tank floor)

E / Dt = 1/3
E = 1.13m

32
For the depth of the liquid in the vessel

H / Dt =1
H = 3.40m
Baffles

Baffles are used to prevent vortexing and rotation of the liquid mass as a whole
Baffle width = Dt/12 = 0.2833m
Baffle offset = Da/2 = 0.565m

Power Calculation
Nq = q/(nDa3)
Nq = flow number
n = revolution per second
Da = dia of impeller
Q = D^2*3.14/4*Vs
Where Vs = superficial velocity=.2439m/sec
q = (Dt 2 *3.14*.2439)/4
= (3.40^2*3.14*.2439)/4
=2.006373m3/sec
Diameter of the impeller = 1.133m
Speed = n = 1.2651rev/sec
rev/min = 75.9066rev/min

Taking it as standard as=84rev/min

Reynolds number=Da2 *n* r /µ
= 1.133^2*1.4*575.46/(2.5*.001))
=413678
As Reynolds number greater than 10,000 so Np=Kt
Np=5.75

33
As power P = Kt*n3*Da5* r
= 5.75*(1.4^3)*1.133^5*575.4
= 16950watt
= 16.950kwatt
Power = 0.47kwatt/m3

4.8 MECHANICAL DESIGN Of CSTR

Shell Thickness
Formula
P * Di
e C
2* f  P

Where
e=thickness of shell
P=internal pressure=20atm=2026kpa
ft=permissible stress=1.65*105 kpa
C=corrosion allowance=3mm
2026 * 3.40
e  3 *10 3
2 * (1.65 *10 )  2026
5

e= .024m

Dome Head

Selected=Ellipsoidal

Thickness calculation

Pi * Di
e
2 * J * f  0.2 * Pi

34
J=joint efficiency=0.85
2026 * 3.40
e
2 * 1.65 * 105 * 0.85  0.2 * 2026

e =0.024m
e =2.2

Weight Of The Shell

Wv =total weight of the shell

Cv =1.085
Dm=mean diameter=(Di+t)=3.424m
Hv=height of the vessel=4.30m
t=thickness=.024m
For s/s vessel Wv  240 * Cv * Dm ( H v  0.8 * Dm ) * e
Wv  240 * 1.085 * 3.424( 4.30  0.8 * 3.424) * .024

Wv = 266.11N

STRESS CALCULATIONS

Longitudinal Stress
Pi * Di
h 
2*t
2026 * 3.40
h 
2 * 0.024
=1.43*105Kpa
Circumferential Stress
Pi * Di
h 
4*t

35
 1013.25 * 5.429
h 
4 * 0.019
 h  7.17*104KPa

Dead Weight Stress

Formula:
Wv
w 
 * ( Di  t ) * t

266.11
w 
 * (3.40  0.024) * 0.024

 w  1031N / m 2

Materials of construction

For Reactor

Stainless steel
Type 302
Cr=17 %, Ni=8 % , C (max) =0.15 %
 Have good corrosion resistance
 Excellent mechanical properties
 Easy to fabricate

For Blades

Stainless steel
Type 316
18% Cr, 8%Ni , 2.5%Mo , 0.08%C
 Mo improves general corrosion and pitting resistance and high

36
  Temperature strength over that of type 302
 Shows good mechanical properties over large flow rates
For Baffles
Stainless steel
Type 405
11.50% Cr , 0.08%C
 Good weld ability and cladding properties
 Have limited harden ability
Mostly use for Baffles, Tower Lining and heat Exchanger Tubing

4.9 SPECIFICATION SHEET

Identification:
Item Reactor
No. required 1
Operation: Continuous
Type: Continuous Stirred Tank Reactor
Temperature: 140 0C Pressure: 2026kPa
Design Data:
Volume: 40 m3
Length: 4.30m Impeller type: Vertical flat blade turbine
Power required: 0.47 kw/m3 No. of blades: Six
Blade material: stainless steel 316 Impeller diameter: 0.937 m
Shell material: stainless steel 302 Baffle width: 0.187 m
Blade width : 0.226 m Diameter: 3.40 m
No. of baffles: Four Impeller speed: 84 rpm

37
Baffles material: stainless steel 405
Jacket type: dimple jacket

PHASE SEPARATOR

5.1 INTRODUCTION

The containers in which the feedstock, intermediate products, and final products
are held are generically known as vessels. Relatively large capacity vessels are
called storage tanks, and small capacity vessels are called drums. In a refinery,

38
drums are widely used not only as procesr, units but also as utility and off-site
facilities.
The types of drums and their internal construction vary, depending upon the kind
of services in which the drums are used; mainly they are used for the following
purposes:

- Vapor-Liquid Separation
- Liquid Surge
- Liquid-Liquid Settling
The typical names of drums used in a refinery are summarized in Table 4-1
together with their functions.

5.2 TYPES OF SEPARATION

There are basically 2 types of separation processes

1) Component separation
2) Phase separation
In component separation the components are separated from a single phase by
mass transfer .e.g. in gas absorption where one or more components are
removed from a gas by dissolving in a solvent.
In phase separation two or more phases can be separated because of a force
acting on one phase differs from a force acting on another phase or one of the
phases impacts on a solid barrier. The forces are usually gravity, centrifugal and
electromotive. Examples are removal of solid from a li quid from a solid by
impaction(filtration),gravity(settling),centrifugal force, and attraction of charged
particles in an electrostatic precipitator. one exception to these mechanisms is
drying by evaporating unbounded water from solids. in this case, separation of
liquid from a solid occurs by mass transfer. For example, the water the water
mixed with sand can be removed by evaporating the water. Many component
separations require contacting two phases like, like liquid-liquid extraction.

39
Component separation is frequently followed by phase separation. Phase
separators can be classified according to phases in contact: liquid-gas, liquid-
liquid, liquid-solid solid-gas, and solid-solid.
Here we have to consider the gas-liquid separator, because we have to remove
the unconverted ethylene gas from the solvent cyclohexane.althoug the mixture
will also contain catalyst and HDPE in solid form, but both substances will be in
dissolved form in cyclohexane. So we consider the basic separation between
ethylene gas and cyclohexane liquid.

5.3 TYPES OF GAS-LIQUID SEPARATORS

There are three commonly types of gas-liquid separators:

1. Vertical gas-liquid separators
2. Horizontal gas-liquid separators
3. Knockout drums

Vertical gas-liquid separators

In vertical gas-liquid separators the gas-liquid mixture is separated by gravity and

impaction. The mixture enters the separator about midway where a splash plate
deflects the stream downward. Most of the liquid flow downward, and the vapor,
containing liquid drops, flow upward. As the vapor rises, large drops settle to the
bottom of the separator by gravity.
Accordingly 95% of separation of liquid from the vapor is normal. If greater than
95% liquid separation is required, then use a wire-mesh mist eliminator, installed
near the vapor outlet. Very small drops are separated by impaction using a wire
mesh pad located at the top of the separator. The mesh usually consists of 0.011
in. (0.279 mm) diameter wires interlocked by a Knitting machine to form a pad
from 4 to 6 in. (0.102 to 0.152 m) thick. Entrained liquid drops in the vapor impact

40
on the wires and coalesce until the drops become heavy enough to break away
from the wire and fall to the bottom of the separator. Because of the large free
volume of the pad (97 to 99%) the pressure drop across the pad is usually less
than 1.0 in. of water. The separation efficiency of a pad is about 99.9% or
greater.
The major objective in sizing a gas-liquid separator is to lower the gas velocity
sufficiently to reduce the number of liquid droplets from being entrained in the
gas. Thus, the separator must be determined. The separator is also designed as
an accumulator for the liquid portion of the stream. Thus, the liquid height is
calculated by allowing sufficient surge time to dampen flow rate variations of the
liquid stream. This liquid height will also be sufficient to allow vapor bubbles to
rise to the top of the liquid before being trapped in the outlet stream at the bottom
of the vessel. This can be achieved by reducing the outlet liquid velocity by
increasing the diameter of the outlet nozzle.
In a separator, there is not a single drop size but a distribution of drop sizes. To
prevent all drops from being carried out by a gas stream would require an
uneconomically large separator. Thus, a maximum gas velocity is specified so
that all but the very small drops are recovered.
Since the vertical and horizontal vapor liquid separators have the same design
equations and have similar design calculations, therefore the only parameter on
which one can be selected for our required separation is for checking the value of
L/D ratio. If L/D<5 value, then vertical gas liquid separators are used and if L/D>5
value, then horizontal gas-liquid separators are used.

Horizontal gas-liquid separators

However, the vertical and horizontal vapor liquid separators have the same
design equations and have similar design calculations; therefore the only
parameter on which one can be selected for our required separation is for
checking the value of L/D ratio. If L/D ratio is greater than 5 values then
horizontal separators are used.

41
Knockout Drums

These are used when the liquid content of the incoming stream is low, is a
special case of gas liquid separators. The drum is placed before the compressor
inlet to prevent liquid drops from entering and damaging the compressors.

5.4 MECHANICAL CONFIGURATION OF SEPARATOR

Nozzles

Normally a horizontal drum is installed on a saddle fixed to a base or foundation.

A vertical drum is installed on a skirt.

Vortex Breaker

When liquid flows into the outlet nozzle at the bottom of a drum, the force of the
liquid flow causes a vortex to form in the liquid above the nozzle. The rotation of
the liquid causes a vacuum to form in the center of the vortex which will lead to
loss of suction at the draw-off pump.
To prevent this, a vortex breaker (anti-vortex baffle) is installed inside the drum at
the top of the nozzle.

Maintenance Procedures

Process equipment requires periodical maintenance to prevent excessive

fouling, wearing, etc., in order to assure safe, continuous and efficient operation.

42
Fire Prevention

As drums usually contain flammable materials, fire prevention procedures must

be strictly observed. For example: before opening a manhole to inspect the
interior of a drum,, the drum must first be thoroughly purged with steam or inert
gas. Operators must also ensure that all drums are properly grounded, to
prevent sparking caused by the discharged of accumulated static electricity.

Lined Drums

Some drums are lined with a special metal or Teflon, or coated with aluminum or
zinc, to protect the drums against corrosion or to prevent deterioration of the
products. Care must be taken to ensure that the lining or coating material is not
damaged during inspection or maintenance work.

Checking Wall Thickness

The wall thickness at predetermined points of the drums must be periodically

measured to check the corrosion status. Usually an ultrasonic thickness gage is
used to measure the wall thickness.

Weld Inspection

Welded joints shall be visually inspected for low pressure vessels. For high
pressure vessels, welded joints shall be subjected to a magnetic particle
examination, to detect fine cracks invisible to the naked eye.
Various parts of horizontal and vertical vapor liquid separator has been shown
below

43
44
5.5 DESIGNING

Total flow rate of mixture entering to reactor= 12353.23022Kg/hr

Unconverted ethylene from the reactor = 83.0265Kg/hr
Mass flow rate of the liquid = 12270.17Kg/hr
Catalyst flow rate in liquid = 23.43Kg/hr
Cyclohexane flow rate in liquid = 10668.39Kg/hr
HDPE flow rate in liquid = 1578.18Kg/hr
Density of HDPE = 960Kg/m3
Density of catalyst = 2550Kg/m3
Density of cyclohexane = 658Kg/m3
Wt fraction of HDPE in liquid = 0.12862Kg/hr
Wt fraction of Cyclohexane in liquid = 0.8694Kg/hr
Wt fraction of catalyst in the liquid = 0.0019Kg/hr
Wt. average density of liquid mixture =
(density of HDPE*wt fraction of HDPE + density of catalyst*wt fraction of
catalyst + density of cyclohexane*wt fraction of cyclohexane)
=0.1268*960+0.8694*658+0.0019*2550
=700.456Kg/m3
Volumetric flow rate of the liquid = (mass flow rate/weighted average density)
= 17.52m3 /hr
Vol. flow rate of the vapor = Vv´ = Mass flow rate of ethylene recovered
Density of ethylene at given conditions.
= 83.0265/13.16
=6.30m3/hr
Vapor velocity = Vv =1.25*Kv* ((ρ liquid –ρ vapors)/ ρ vapors))
½
Where Kv is the velocity constant, its value is .107m/sec with mist eliminator
Vv = 13.72m/hr
Area of the separator = volumetric flow rate of ethylene recovered
Velocity of the vapor

45
 = 0.4594m2
Diameter of the separator = (Area*4/3.14)1/2
=0.765m
Liquid level in the separator is given by the formula,
0.5* Ll * A = VL´ * ts.
Where,
Ll = liquid level in the separator, (m)
ts = residence time in the separator,(sec)= 5min
= 0.083 hr
L1 = 6.33 m
Length of the separator = L1+1.5D+0.4572
=7.93m
L/D ratio for the separator=31.71/2.87m=11.04

5.6 SPECIFICATION SHEET

Identification:
Item Horizontal-Gas Liquid separator
No. required 1
Operation: Continuous
Type: Horizontal Temperature: 140 0C
Pressure 15atm
Diameter of the separator 0.765m L/D Ratio 10.36

46
HEAT EXCHANGER

6.1 INTRODUCTION

A heat exchanger is a heat-transfer devise that is used for transfer of internal

thermal energy between two or more fluids available at different temperatures. In
most heat exchangers, the fluids are separated by a heat-transfer surface, and
ideally they do not mix. Heat exchangers are used in the process, power,
petroleum, transportation, air conditioning, refrigeration, cryogenic, heat
recovery, alternate fuels, and other industries. Common examples of heat
exchangers familiar to us in day-to-day use are automobile radiators,
condensers, evaporators, air pre-heaters, and oil coolers.

In our project a number of heat exchangers are used . Here we will

discuss heat exchanger used as

 Condenser
 Vaporizer
 Cooler

All of these are shell and tube heat exchangers.

47
6.2 SELECTION GUIDE TO HEAT EXCHANGER TYPES

Approxim
ate
relative
Significant Applications cost in
Type Limitations
feature best suited carbon
steel
construct
ion
Condensers; Temperature
liquid-liquid; gas- difference at
Fixed gas; gas-liquid; extremes of
Both tube sheets
tube cooling and about 200 oF 1.0
fixed to shell.
sheet heating, Due to
horizontal or differential
vertical, reboiling. expansion.
One tube sheet
High temperature
Floating “floats” in shell or Internal gaskets
differentials,
head or with shell, tube offer danger of
above about 200
tube bundle may or o leaking.
F extremes; dirty
sheet may not be Corrosiveness of
fluids requiring
(removabl removable from fluids on shell- 1.28
cleaning of inside
e and no shell, but back side floating
as well as outside
removabl cover can be parts. Usually
of shell,
e removed to confined to
horizontal or
bundles) expose tube horizontal units.
vertical.
ends.
Bends must be
carefully made,
High temperature
or mechanical
differentials,
damage and
which might
Only one tube danger of rupture
require provision
sheet required. can result. Tube
U-tube; for expansion in
Tubes bent in U- side velocities 0.9-1.1
U-Bundle fixed tube units.
shape. Bundle is can cause
Easily cleaned
removable. erosion of inside
conditions on
of bends. Fluid
both tube and
should be free of
shell side.
suspended
particles.
Double Each tube has Relatively small Services suitable
0.8-1.4
pipe own shell forming transfer area for finned tube.

48
 service, or in
banks for larger
annular space for
applications. Piping-up a large
shell side fluid.
Especially suited number often
Usually use
for high requires cost and
externally finned
pressures in tube space.
tube.
(greater than 400
psig).
Pipe coil for
Transfer
submersion in
Condensing, or coefficient is low,
coil-box of water
relatively low requires
Pipe coil or sprayed with 0.5-0.7
heat loads on relatively large
water is simplest
sensible transfer. space if heat
type of
load is high.
exchanger.
Not well suited
Composed of for boiling or
metal-formed thin Viscous fluids, condensing; limit
Plate and plates separated corrosive fluids, 350-500 oF by
0.8-1.5
frame by gaskets. slurries, high heat gaskets. Used
Compact, easy to transfer. for liquid-liquid
clean. only; not gas-
gas.
Compact,
Process
concentric plates; Cross-flow,
corrosion,
Spiral no bypassing, condensing, 0.8-1.5
suspended
high turbulence. heating.
materials.

SELECTION CRITERIA

1. Cost – wish to have an exchanger that costs the least.

2. Efficiency – wish to have an exchanger that operates most efficiently, with
minimum loss of energy in the transfer, and minimum drop in pressure of the
fluids.
3. Space – wish to have an exchanger that is small
4. Materials – want an exchanger built from materials that are compatible with
the process streams and don’t cost a lot.
5. Maintenance – want an exchanger that can be easily cleaned.
6. Ease of construction.

49
6.3 SHELL AND TUBE HEAT EXCHANGER

In process industries, shell and tube exchangers are used in great numbers, far
more than any other type of exchanger. More than 90% of heat exchangers used
in industry are of the shell and tube type. The shell and tube heat exchangers are
the “work horses” of industrial process heat transfer. They are the first choice
because of well-established procedures for design and manufacture from a wide
variety of materials, many years of satisfactory service, and availability of codes
and standards for design and fabrication. They are produced in the widest variety
of sizes and styles. There is virtually no limit on the operating temperature and
pressure.

Classification of Shell and Tube heat exchanger.

There are four basic considerations in choosing a mechanical arrangement that

provides for efficient heat transfer between the two fluids while taking care of
such practical matters as preventing leakage from one into the other.
 Consideration for differential thermal expansion of tubes and shell.
 Means of directing fluid through the tubes.
 Means of controlling fluid flow through the shell.
 Consideration for ease of maintenance and servicing.

Heat exchangers have been developed with different approaches to these

four fundamental design factors. Three principal types of heat exchangers

2) Fixed tube-sheet exchangers

3) U-tube exchangers and
4) Floating head exchangers—satisfy these design requirements.

50
Fixed Tube Sheet Design.

Benefits

 Tubes can be cleaned mechanically or chemically from inside. But

outside requires chemical cleaning.
 An expansion joint is provided in the shell to reduce the thermal stress
due to the differential expansion between the tube and shell.
 Tube sheets are fixed at both ends. Simplest & most economical shell &
tube construction.
 Configuration gives a large surface area in a small volume
 Good mechanical lay out :a good shape for pressure operation

DESIGN CALCULATIONS

Composition

Mass flow rate of HDPE = 1578.2 kg / hr

Mass flow rate of Cyclohexane = 106.2 kg / hr

Hot Stream:

Inlet temperature T1 = 423 k

Outlet temperature T2 = 298 k
Δt1 = 102 k

Cold Stream

Inlet temperature t1= 321 k

Outlet temperature t2 = 358 k

51
Δt 2= 60 k

Cp Values

For HDPE = 2.15 kj / kg.k

For Cyclohexane = 2.019 kj / kg.k
For Water = 4.184 kj / kg.k

Heat Load

For HDPE
Q1 = mCpT
= 440095.14 kj / hr
For Cyclohexane
Q2 = mCpT
= 27888.55 kj / hr

Qt = Q1 + Q2
= 467983.7 kj / hr
now
Total heat lost by mixture = Total heat gained by water
So
m = Q / Cp.Δt
= 1864.17 kj / hr

LMTD

LMTD1  (Δt1 – Δt2) / ln ( Δt1/ Δt2)

= 144.065 k
T2  T1
R  2.826
t 2  t1

52
 t 2  t1
S  0.48
T1  t1

Ft = 0.9
△Tm = Ft * LMTD = 129.6584 k

Let
Ud = 850 kg / hr.m2.k

H.T Area:
H.T area = Qt / Ud . △Tm
2
= 4..25 m

6.5 SPECIFICATION SHEET

Tube Specifications

16 BWG
OD = 0.019 m
ID = 0.0148 m
Pt square = 0.0254 m => k1 = 0.156
Length of tube = 4.87 m
Tube Clearance ( C ) = Pt – OD = 0.0235 m
Surface area of one tube = π*OD*L
= 0.306 m2
No. of tubes =N t = H.T Area / area of one tube
= 14
Dia of bundle = Db = OD* ( N t / k1 )
= 0.1356 m
Shell Specifications:

53
 Dia of shell = 0.91 m
Baffle Spacing = B = 0.016 m
Tube Spacing = C = 0.0235 m

Tube Side Calculations: ( Mixture )

Flow area = Af = (0.302 * 0.0254)2

Flow area for total tubes = Af* N t / n => n = #.of
passes
= 0.00291 m2
Mass Velocity = G =m/A
= 5.79*105 kg/m2.hr
NRe = Dt*G / µ
= 1.07*103
Jh = 42
Hi / Фt = Jh*(k / D)*( Cµ / k )1/3
= 30.6
f = 0.82
Shell Side Calculations: ( Water )

 Af = ( ID*C*B) / Pt
= 0.03869 m2
 G = m / Af
= 4.82*104 kg/m2.hr
NRe = 7.21*104
Ho / Фs = Jh*( k / De)*( Cµ / k )1/3

From Graph b/w ( Jh & Res )

= 157.25
f = 0.008

54
 Hio / Фi = ( Hi / Фi)*( ID / OD )
= 23.83
Wall Temperature

Tw = tc + [( Ho /Фs) / {(Ho/Фi) + (Hio/Фi)}]* ( T- tc )

= 416.29 k
At Tw
µ of HDPE = µ w =85.31
µ of Cyclohexane = µ w = 1.51
Hi / Фt = Jh * ( k / De)*( Cµ / k)1/3
Hi = Jh * ( k / De)*( Cµ / k)1/3 * Фt
= Jh * ( k / De)*( Cµ / k)1/3 * ( µ / µw )0.14
=>µ =80
= 28.69
Ho = 157.25 * Фs => Фs = ( 1.323 /
1.513 )
= 137.5

PRESSURE DROP

Tube side
NRe = 1.07 x 103
f = 0.82

specific gravity = 0.779

1 fG t2 L * n
Pt 
2 5.22  10 10 DeS t

= 3001.83 pa
= 0.4355 Psi

55
Shell Side

Re = 7.21 x 104
f = 0.008

No. of crosses = N + 1 =12 Lp/B

 15.28

fG s2  N  1 D5
Ps1 
5.22  1010 DeS

=8340.35 pa

= 1.21 Psi

6.5 SPECIFICATION SHEET

56
SPECIFICATION SHEET FOR 1-2 PASS SHELL FIXED HEAD SHELL AND
TUBE HEAT EXCHANGER

Identification Unit Heat Exchanger

Item No. E-201
Type Fixed Head.
No. of Item Function To Cool The mixture of HDPE in
+cyclohexane.
Operation Continuous
Heat duty 467983.7 kj/hr
Heat transfer area 13.94 ft2
Overall heat transfer coefficient 50.37 Btu / hr.ft2.oF
Dirt factor 0.0019 hr.ft2.oF/Btu.
Shell side Tube side
Fluid circulated Water Mixture of HDPE
+Cyclohexane
Flow rates 1866Kg/hr 1684.7Kg/hr
Temperature Inlet = 298K Inlet = 423K
Outlet = 321K Outlet = 358K
Pressure drop 1.08 psi. .4355psi.
Specifications I.D = 0.91 m
C = 0.0235 m
B = 0.116 m
#.of baffles = 9

57
CENTRIFUGE

7.1 INTRODUCTION

A mechanical device that uses centrifugal or rotational forces to separates

substances of different densities, such as solids from liquids or liquids from other
liquid. Denser material tends to move to the bottom of the tube, displacing lighter
particles to the top. A centrifuge is most often used for the separation of particles
from solutions according to their size; shape, density, viscosity of the medium
and rotor speed. These machines utilize the natural separation realities present
in a high-speed circular G-force environment. Like a high-powered clothes dryer,
these exceedingly fast machines spin in order to separate materials from one
another. The denser materials separate from the less dense during the
centrifugation process. The term “centrifuge” encompasses a wide variety of
process equipment used for many different applications in the chemical process
industries. Although these units may look different and play key roles in very
unrelated processes.
Centrifuges are classified into two main categories that are
1) Filtering Centrifuges
2) Sedimentation centrifuges

7.2 CLASSIFICATION OF CENTRIFUGES

These two categories can be further split into subcategories, depending on

whether the centrifuge runs on a continuous or batch basis.

58
Filtering Centrifuges

Filtering centrifuges effect a separation by using a medium such as

screen or cloth, to separate the solids from liquid. The solids are retained on
the medium, while the liquid passes through both the solids and the medium.

There are following subcategories of filtering centrifuges

 Batch Filtering centrifuges
 Vertical Basket Centrifuges
 Horizontal Peeler
 Inverting Bag Centrifuge

 Continuous Filtering Centrifuges

 Screen Bowl Centrifuge

 Scroll Screen centrifuge
 Pusher Centrifuge
 Vibratory Centrifuge

Sedimentation Centrifuges

These centrifuges effect a separation by having a “heavier” solid, that is a solid

with higher specific gravity than the liquid in which it is suspended, will settle in or
from a lighter liquid, which has lower specific gravity than the solid.
There are following classifications of sedimentation centrifuges
 Batch sedimentation Centrifuges
 Imperforated Basket Centrifuges
 Tubular Centrifuges
 Continuous Sedimentation centrifuges
 Solid Bowl or Decanting Centrifuges

59
  Disc Centrifuges
7.3 SELECTION OF CENTRIFUGES

There are following factors which must be considered in the selection of

centrifuge for a process

Current or past experience

If the application is not new, there is good chance that you can find
documentation of a process that defines the type of centrifuge currently operating
on this application. This does not imply that it is the best centrifuge for the
process, but it may suggest a comfort factor in this technology. There may be a
personal or plant preference for a particular type of centrifuge for the application.

Physical Properties of Materials

The characteristics of the solids and liquids handled in a process will influence
centrifuge selection.

Specific Gravities of the Solids and Liquids

If the solids are lighter than the liquid, a decanting centrifuge is not an option. If
the specific gravities are very close, but the solids are slightly heavier, a
decanting centrifuge may be considered, but only if either the particle size or the
centrifugal force improves the settling of the solids.

Particle Size

Coarse solids with particle size greater than 100 um are generally best suited for
filtering type centrifuges. Finer solids that measures less than 10um are best

60
handled in sedimentation centrifuges. Given that most solids have abroad
particle size distribution, the percentage of solids finer than 100um will influence
the overall expected recovery of solids. It may also dictate the selection of either
batch or continuous equipment.

Performance Criteria

The need to achieve a certain outcome with respect to the recovery of solids,
nature of the recovered solids or liquid and other products characteristics will
dictate the choice of equipment.

Centrate Clarity

Decanting centrifuge provides the best clarity of all centrifuge types. Filtering
centrifuges typically are not used where centrate clarity is the principle process
requirement because they use either a filter medium or a screen.

Solid Recovery

To maximize the percentage of solids captured, decanting centrifuge or batch

basket centrifuges will typically lose 1-5 wt. Percent of solids finer than 100um
through the screen, depending on particle size and feed rate.

Solid Dryness

61
Filtering centrifuges provide the driest solids, while decanting centrifuges provide
the wettest solids. Since the final dryness of the solids will be tied to the particle
size of the solids, the difference in the dryness between a filtering and a
sedimentation centrifuges may be little as only a few percentage points.

Wash Efficiency

A solid washing in a decanting centrifuge is generally ineffective, because the

wash liquid does not have the chance to penetrate the solids and displace the
mother liquor. The batch basket in a filtering centrifuge provides the highest wash
efficiency because of its ability to apply an unlimited wash over an indefinite
period of time.

Process requirements

Continuous centrifuges should be considered when the following criteria are

important.

Logistics

The equipment that is located either immediately before or after the centrifuge
may dictate whether a batch or continuous centrifuge is used. For instance, when
batch reactor or crystallizers feed a centrifuge, which in turn feeds a continuous
dryer, a continuous centrifuge may be more appropriate because it will maintain
a steady flow of solids to dryer.

Pressure and Temperature

62
Continuous centrifuges are used when higher operating pressures are required.
Continuous decanters have been used in operations where pressures were as
high as 90 psig and temperatures as high as 175 C. batch centrifuges are
restricted to lower pressure applications. There does not appear to be a
restriction or preference based on temperature.

Flow Rate (solid loading)

The higher the solid flow rate, the greater the tendency to use continuous
centrifugation. As a rule of thumb, batch centrifuges are applicable for loadings of
up to 1 ton/hr

Solid Concentration

Continuous filtering centrifuges,, with the possible exception of the screen bowl
design, prefer a thick feed slurry (typically 50% by weight). There are two
reasons for this: continuous filtering centrifuges may be limited by the amount of
liquid to be centrifuged.

7.4 DECANTER SOLID BOWL CENTRIFUGE

Description

The Decanter/Solid Bowl Centrifuge operates on the principle of sedimentation.

Often the solids are too fine to be dewatered satisfactorily in the filtering
centrifuges. They can be separated in solid bowl centrifuges provided their
sedimentation speed in the mother liquid is sufficient. The sinking settling speed

63
which is determined by Particle size, Particle shape, difference in density
between solids and liquids as well as their viscosity.
In Decanter centrifuges the cleaning of liquid takes place in cylindrical partwhere
as dewatering of solids by compression of the filter cake takes place inconical
part of the bowl. The geometry of the bowl, relation with length and diameter to
be adapted to suit the application. In most of the cases, good results are
obtained at length to diameter 2 :1 and sometimes depending upon application
2.5/3:1.
The system is continuous, compact and enclosed while offering versatility, high
performance, and low maintenance.

Application

The Decanters / Solid bowl Centrifuges are used for clarification (liquid / solid
separations), dewatering and classification duties in various process
industries.

Typical Products

Inorganic products: Aluminum hydroxide, barium sulphate, lead oxide,

chromium oxide, ferrous hydroxide, magnesium
hydroxide, titanium dioxide, zinc sulphate etc.

Organic products: Carboxymethycellulose, caprolactam,

dimethylterephthalate, terephthalic acid, phthalic acid,
etc.

Plastics: Polyethylene, polypropylene, polystyrene, polyvinyl

chloride, etc.

64
Silicates: Asbestos, clay, etc.
Cellulose: De-inking flotation concentrate.

Foodstuffs: Fishmeal, casein, whey, etc.

Operation
Separation takes place in Horizontal conical / cylindrical bowl with screw
conveyor. The slurry is fed into the bowl through a stationary inlet tube and
accelerated by specially designed inlet distributor. Centrifugal force leads to
instant sedimentation of the solids on the wall of bowl.
The conveyor, rotating in the same direction as bowl with differential speed,
conveys the solids to conical end. The solids are lifted clear of the liquid and
centrifugally dewatered before being discharged into the collecting channel.The

65
clarified liquid flows into the housing through opening in cylindrical end
of the bowl.
The solid bowl decanter centrifuge is a continuous, sedimentation type unit
comprising of three primary components: a cylinder, conical bowl; a conveyer
(e.g. a screw); and a gear unit that provides the differential speed between the
bowl and the conveyer. The centrifuge bowl rotates clockwise at the speed
required to generate the centrifugal force needed to effect the intended
separation. Slurry enters the centrifuge via a stationary pipe that empties into the
hub of the conveyer. In the hub, the feed is accelerated to the speed of the bowl
and is fed through an opening in the hub onto the inside surface of the bowl. The
slurry quickly fills the bowl to a height determined by the weir settings located at
the larger-diameter end of the bowl.

7.5 DESIGN OF SOLID BOWL CENTRIFUGE

66
Diameter of bowl = 36 in = 0.9144 m => rb= 0.4572 , rp = 0.334
RPM of centrifuge = 2000 rev./min = 2000/60 Hz (rev./sec) = 33.33 Hz
Density of HDPE at 48 0C = 960 kg/m3
Density of Cyclohexane at 48 0C = 753 kg/m3
Average density of slurry at 48 0C = 779.67 kg/m3
Viscosity of Cyclohexane at 48 0C = 0.64 cP = 0.0006 Pa.sec
HDPE input to centrifuge = 1578.18 kg/hr
Cyclohexane input to centrifuge = 10668.27 kg/hr
Inlet mass flow rate to centrifuge = 12246.46 kg/hr
HDPE leaving from centrifuge = 1578.18 kg/hr
Hexane leaving from centrifuge =106.68 kg/hr
Temperature = 48 ©
Minimum particle diameter = 100 µm = 0.0001 m

Design Steps

• Volumetric flow rate

• Dia selection
• Length of Centrifuge
• Volume of Bowl
• Residence time of Slurry
• Relative Centrifugal Force
• Settling Velocity of Particles
• Pressure Developed

Calculations
1. Volumetric flow rate entering

67
 Volumetric flow rate = Mass flow rate / Average density
V1 = 12246.46 / 779.67

V1 = 15.707 m3/hr

2. Length of centrifuge

Since capacity of centrifuge is

3.5 LD 2 (  s   L ) d 2 N 2
V 

So
L = V / 3.5D2( S – L )dp2N2
L = 15.707*0.0006/ 3.5*(0.9144)2*207*(0.0001)2(33.33)2
L = 1.5 m
So
L/D = 1.63

4. Volume Of Bowl
Volume of bowl is given below

D 2
VC  L
4
VC = 3.1416*(0.9144)2* 1.5 / 4

V = 0.98 m3
4. Residence Time Of Slurry

Here Residence Time is

t = Volume of the liquid in the bowl / Volumetric Flow rate
Volume of liquid in the bowl is given below

68
 VL  L(r12  r22 )
VL = 3.1416* 1.5* ( 0.45722 - 0.3342 )
VL = 0.458 m3
So
t = 0.458 / 15.707
t = 0.029 hr
t = 1.75 min

5. Relative centrifugal Force

Fc
Here RCF 
Fg

 2r
RCF 
g

Where
 = Angular Velocity of Bowl
  2n
 = 2*3.1416*33.33
 = 209.44 Rad./ sec
So
RCF = (209.44)2* 0.4572 / 9.8
RCF = 2046.44

6. Settling Velocity Of Particles

We suppose laminar flow and consider that fluid is in stokes law range that is
Reynolds number is less than 1. For this situation settling velocity is given below
d p2 (  S   L ) 2 r2
vs 
18

69
 vs = (0.0001)2 *(207)*(209.44)2*(0.9144) / 18* (0.0006)
vs = 2.63 m / sec2

7. Pressure Developed

Here pressure developed is denoted by P and is given as

P  0.5 *  avg * w2 * (r12  r22 )

P = 0.5* 779.67*(209.44)2* ( 0.45722 – 0.3342 )

P = 1666864.638 pa.
P = 16.45 atm.

7.6 SPECIFICATION SHEET

1. Equipment Centrifuge

70
2. Type Solid Bowl 0r Helical Conveyer
centrifuge

3. Method of operation Continuous

4. No. Required 1

5. Function To separate HDPE from the slurry

which contain Cyclo Hexane and
catalyst

6. Bowl Diameter 0.9144 m

7. Speed of bowl 2000 rpm

8. Settling Velocity of Particles 2.63 m / s.

9. Relative Centrifugal Force 2046.44

10. Material of construction of basket Stainless steel 316

11. Pressure Developed 16 atm

71
DRYER

8.1 INTRODUCTION

“Drying is a process of removal of moisture from the solid by using hot gas/air or
steam”
It is the last step in the series of operations.

The factors governing the rates of these two processes determine the drying
rate. The methods of heat transfer in commercial dryers may utilize convection,
conduction, radiation, or a combination of these three mechanisms. Mass
transfer within the solid, however, occurs because of a concentration gradient
that is established in the drying process, which is dependent on the
characteristics of the solid. Removal of the vapor from the surface will be dictated
by the existing flow conditions provided by the dryers.

8.2 SELECTION OF DRYERS

Because of the very wide range of dryer designs available on the3 market at the
present time, classification is a virtually impossible. However, the nature of
material, which is passing through dryer, provides a basis of selection of dryers.
Dryers are classified on basis of following factors:
i. Temperature and pressure in the dryer

72
 ii. The method of heating
iii. The means by which moist material is transported through the dryer
iv. Any mechanical aids aimed at improving drying
v. The method by which the air is circulated
vi. The way in which the moist material is supported
vii. The heating medium, and
viii. The nature of the wet feed and the way it is introduced into the
dryer.
In selecting a dryer for a particular application two steps are of primary
importance
A listing of the dryers which are capable of handling the material to
be dried,
Eliminating the more costly alternatives on the basis of annual costs
(capital charges + operating costs).

8.3 TYPES OF DRYERS

There are various types of dryer available, for example:

i. Fluidized bed dryer
ii. Screen conveyer dryer
iii. Screw conveyor dryer
iv. Tray dryer
v. Rotary dryer
vi. Flash dryer
vii. Spray dryer
viii. Drum dryer
ix. Thin film dryer

73
8.4 DRYERS FOR HDPE

We can use following dryers for removal of n-hexane contents from HDPE
powder,

1 Fluidized bed dryer

2 Rotary dryer
3 Vacuum dryer
8.5 SELECTION CITERIA

1 Reliability of unit
2 Availability of data
3 Quality of product
4 Maintenance cost

All of these factors point towards the selection of co-current direct contact rotary
dryer .
We Prefer to use co-current dryer here because on counter-current contact of
HDPE and air may lead damaging (Degradation) of HDPE.

Advantages of Rotary Dryer

1 Simplest in construction
Most Economical
1 Maximum contact area
2 Higher rate of heat and mass transfer
3 Low operating Cost
4 Low residence time

74
.8.6 DESIGING
Basic Parameters to be Designed

1 Area of Dryer
2 Diameter of Dryer
3 Volume of Dryer
4 Number of Flights
5 Residence Time

Data Needed for Design

DRYER efficiency=99.60%

75
Inl Inlet Flow rate of HDPE=6312.75Kg/Hr

Outlet Flow rate of HDPE=6312.75Kg/Hr

Inlet Flow rate of Cyclohexane=426.7303Kg/Hr

Cyclohexane Removed=425.023379Kg/Hr

Cyclohexane Left in HDPE=1.7069 Kg/hr

Cp of HDPE=2.045Kj/Kg.K

Cyclohexane= 1.9585 Kj/Kg

HDPE+Cyclohexane inlet temperature=48C

HDPEλ+Cyclhexane outlet temperature=90C

Air inlet temperature=150C

Air outlet Temperature =103C

LMTD=43.2034 C

Latent Heat of Solvent=λ= 357.314Kj/Kg

Cpv=0.45
Total Heat needed for Drying

Q=ms[Cps(Tsb-Tsa)+XaCpl(Tv-Tsa)+(Xa-Xb)+(Xa-Xb)y+XbCpl(Tsb-Tvb)+(Xa-
Xb)Cpv(Tva-Tvb)]
=173912.8Kj/hr

76
Amount of air needed (kg/h)

m=Q/[(1+Hb)(Tvb-Tas)Csb]
Csb =0.163
Hb =0.0001

m=3728.986Kg/hr

Area of dryer= A=m/G

=0.746 m2

Diameter of Dryer

D2=4/Π*A
D =0.97471m=3.2 ft

H.T Coefficient

Ua=.5*G/D
=1280.134KJ/m3.C.hr

Volume of Dryer (m3)

V = Q/U.LMTD

77
 = 4.693 m3Length of Dryer

L=V/A
=6.29 m
Number of Flights

N = 3.D
=10
Rotational Speed

N*=4 RPM

Angle=3 degree=0.0698 rad

Slope = 0.0699

Residence Time

Tr=0.13L/N*Dtanθ
=4.001427 min

78
8.7 SPECIFICATION SHEET

Identification:
Item DRYER
No. required 1
Operation: Continuous
Area of dryer=0.746m2
Volume of the dryer=4.693m3
Length of the dryer=6.29m
Diameter of the dryer=0.97471m
Rotational speed =4RPM
Residence time =4min
Amount of air needed =3768Kg/hr

79
INSTRUMENTATION AND CONTROL

9.1 BASIC CONCEPT

Measurement is a fundamental requisite to process control. Either the control can

be affected automatically, semi automatically or manually. The quality of control
obtainable also bears a relationship to accuracy, re product ability and reliability
of measurement methods, which are employed. There fore , selection of the most
affect means of measurements is an important first step in design and
formulation of any process control system.
Common elements of control system are

Measuring elements

The instruments on the process which measure the properties and

important variables such as temperature, pressure, flow rate and level.

Controller

The job of the controller is to compare te process signal from the

transmitter with the set point signal and to send out an appropriate signal to the
control valve. There are three basic types of controllers which are

80
  Proportional action which moves the control valve indirect proportional to
the magnitude of the error.
 Integral action (reset) which moves the control valve based on the time
integral of the error and the purpose of integral action is to drive the
process back to its set point when it has been disturbed.
 Ideal derivative action and its purpose is to anticipate where the process is
heading by looking at the time a rate of change of the error.

Commercial Controllers

The three actions are used individually or combined in three basic controllers.
 Proportional
 Proportional – integral (P.L)
 Proportional – Integral – derivative (P.I.D)

Comparators

A set pont has been given to the comparator. Comparator compares the
measured value with the set point value.

Final Control Elements

Is the mechanism which alters the value of the manipulated

variable in response to the output signal from and automatic controller. In a
majority of systems the final control element is and automatic control valve which
throttles the flow of a manipulative variable.

81
9.2 TEMPERATURE MEASUREMENT AND CONTROL

Temperature measurement is used to control the temperature of outlet and inlet

streams in heat exchangers, reactors, etc.
Most temperature measurements in the industry are made by means of
thermocouple to facilitate bringing the measurements to centralized location. For
local measurements at the equipment bimetallic or filled system thermometers
are used to a lesser extent. usually, for high measurement accuracy, resistance
thermometers are used.
all these measurements are installed with thermo wells when used locally. This
provides protection against atmosphere and other physical elements.

9.3 PRESSURE MEASUREMENT AND CONTROL

Like temperature pressure is a value able indication of material state and

composition.
In fact, these two measurements considered together are the primary evaluating
devices of industrial materials.
Pumps, compressers and other process equipment associated with pressure
changes in the process material are furnished with pressure measuring devices.
Thus pressure measurement becomes an indication of an energy decrease or
increase.
Most pressure in industry are elastic element devices, either directly connected
for local use or transmission type to centralized location. Most extensively used
industrial pressure is the Bourderi Tube or a Diaphram or Bellow gauges.

82
9.4 FLOW MEASUREMENT AND CONTROL

Flow indicator are used to control the amount of liquid. Also all manually
set streams require some flow indication or some easy means for occasional
sample measurement.
For accounting purposes, feed and product streams or metered. In addition
utilities to individual and grouped equipment are also metered.
Most flow measures in the industry are/ by Variable Head devices. To a lesser
extent variable area is used as are many types available as special metering
situation arise.

10.5 CSTR CONTROL CONFIGURATION

83
HAZOP STUDY

10.1 INTRODUCTION

A HAZOP survey is one of the most common and widely accepted methods of
systematic qualitative hazard analysis. It is used for both new or existing facilities
and can be applied to a whole plant, a production unit, or a piece of equipment It
uses as its database the usual sort of plant and process information and relies on
the judgment of engineering and safety experts in the areas with which they are
most familiar. The end result is, therefore reliable in terms of engineering and
operational expectations, but it is not quantitative and may not consider the
consequences of complex sequences of human errors.
The objectives of a HAZOP study can be summarized as follows:

 To identify (areas of the design that may possess a significant hazard

potential.

 To identify and study features of the design that influence the probability of
a hazardous incident occurring.

 To familiarize the study team with the design information available.

 To ensure that a systematic study is made of the areas of significant

hazard potential.

84
  To identify pertinent design information not currently available to the team.

 To provide a mechanism for feedback to the client of the study team’s

detailed comments.

10.2 Steps Conducted in HAZOP Study

A HAZOP study is conducted in the following steps:

1. Specify the purpose, objective, and scope of the study. The

purpose may he the analysis of a yet to be built plant or a review of the
risk of un existing unit. Given the purpose and the circumstances of the
study, the objectives listed above can he made more specific. The
scope of the study is the boundaries of the physical unit, and also the
range of events and variables considered. For example, at one time
HAZOP's were mainly focused on fire and explosion endpoints, while
now the scope usually includes toxic release, offensive odor, and
environmental end-points. The initial establishment of purpose,
objectives, and scope is very important and should be precisely set
down so that it will be clear, now and in the future, what was and was
not included in the study. These decisions need to be made by an
appropriate level of responsible management.

2. Select the HAZOP study team. The team leader should be skilled in
HAZOP and in interpersonal techniques to facilitate successful group
interaction. As many other experts should be included in the team to
cover all aspects of design, operation, process chemistry, and safety.
The team leader should instruct the team in the HAZOP procedure and
should emphasize that the end objective of a HAZOP survey is hazard
identification; solutions to problems are a separate effort.

85
 3. Collect data. Theodore16 has listed the following materials that are
usually needed:

 Process description

on the chemical, physical and toxicological properties of all raw materials,,

intermediates, and products.

 Piping and instrument diagrams (P&IDs)

 Equipment, piping, and instrument specifications

 Process control logic diagrams

 Layout drawings

 Operating procedures

 Maintenance procedures

 Emergency response procedures

 Safety and training manuals

Table-: HAZOP Guide Words and Meanings

Guide Words Meaning
No Negation of design intent
Less Quantitative decrease
More Quantitative increase
Part of Qualitative decrease

86
 As well as Qualitative Increase
Reverse Logical opposite of the intent
Other than Complete substitution

4. Conduct the study. Using the information collected, the unit is divided
into study "nodes" and the sequence diagrammed in Figure , is
followed for each node. Nodes are points in the process where process
parameters (pressure, temperature, composition, etc.) have known and
intended values. These values change between nodes as a result of
the operation of various pieces of equipment' such as distillation
columns, heat exchanges, or pumps. Various forms and work sheets
have been developed to help organize the node process parameters
and control logic information.

When the nodes are identified and the parameters are identified, each node is
studied by applying the specialized guide words to each parameter. These guide
words and their meanings are key elements of the HAZOP procedure. They are
listed in Table.
Repeated cycling through this process, which considers how and why each
parameter might vary from the intended and the consequence, is the substance
of the HAZOP study.

5. Write the report. As much detail about events and their consequence
as is uncovered by the study should be recorded. Obviously, if the
HAZOP identifies a not improbable sequence of events that would
result in a disaster, appropriate follow-up action is needed. Thus,
although risk reduction action is not a part of the HAZOP, the HAZOP
may trigger the need for such action.

The HAZOP studies are time consuming and expensive. Just getting the P
& ID's up to date on an older plant may be a major engineering effort. Still, for

87
processes with significant risk, they are cost effective when balanced against the
potential loss of life, property, business, and even the future of the enterprise that
may result from a major release.

10.3 HAZOP Study of Cyclohexane

In HAZOP Study of cyclohexane we will see its
effects on health, environment

Health effects
In health effect we have to consider the following points.
 What effect might cyclohexane have on my health?
 How might cyclohexane enter my body?
 How might I be exposed to cyclohexane?
 What are the cyclohexane health guidelines?

What effect might cyclohexane have on my health?

Effects of cyclohexane on human health and the environment depend on how

much cyclohexane is present and the length and frequency of exposure. Effects
also depend on the health of a person or the condition of the environment when
exposure occurs. Breathing large amounts of cyclohexane for short periods of
time adversely affects the human nervous system. Effects range from headaches
to anaesthesia, tremors, and convulsions. Contact with cyclohexane liquid or
vapour can damage the eyes. These effects are not likely to occur at levels of
cyclohexane that are normally found in the environment. Human health effects
associated with breathing or otherwise consuming smaller amounts of
cyclohexane over long periods of time are not known. Studies show that repeat
exposure to large amounts of cyclohexane in air causes nervous system effects,
eye damage, and respiratory effects in animals. The cyclohexane industry is now
studying how its chemical affects the reproductive system and the development
of the foetus of animals.

88
How might cyclohexane enter my body?

Cyclohexane enters the body when breathed in with contaminated air or when
consumed with contaminated food or water. It can also be absorbed through skin
contact. Cyclohexane is not likely to remain in the body due to its breakdown and
removal in exhaled air and in urine.

How might I be exposed to cyclohexane?

Exposure to cyclohexane can occur in the workplace or in the environment

following releases to air, water, land, or groundwater. Exposure can also occur
when people use products that contain cyclohexane or when they smoke
cigarettes.

What are the cyclohexane health guidelines?

Work safe (Maximum 8 hour time weighted average (TWA) exposure: 1,030
mg/m³)

Environmental effects
Similarly we again here have the four general questions.
 What effect might cyclohexane have on the environment?
 How might cyclohexane enter the environment?
 Where in the environment does cyclohexane end up?
 What are the cyclohexane environmental guidelines ?

What effect might cyclohexane have on the environment?

Cyclohexane is non-persistent in water, with a half-life of less than 2 days. The

half-life of a pollutant is the amount of time it takes for one-half of the chemical to
be degraded. Virtually 100% of cyclohexane will end up in the air.

89
The concentration of cyclohexane found in fish tissues is expected to be
somewhat higher than the average concentration of cyclohexane in the water
from which the fish was taken.

Cyclohexane has moderate acute toxicity to aquatic life. It has caused membrane
damage in an ornamental crop species. Insufficient data are available to evaluate
or predict the short-term effects of cyclohexane to birds or land animals.

Cyclohexane has moderate chronic toxicity to aquatic life. Insufficient data are
available to evaluate or predict the long-term effects of cyclohexane to plants,
birds, or land animals.

How might cyclohexane enter the environment?

Cyclohexane enters the environment mainly in industrial and municipal

discharges. Cyclohexane evaporates when exposed to air. It dissolves slightly
when mixed with water. Most direct releases of cyclohexane to the environment
are to air. Cyclohexane also evaporates from water and soil exposed to air. Once
in air, it is expected to break down to other chemicals. Because it is a liquid that
does not bind well to soil, cyclohexane that makes its way into the ground can
move through the ground and enter groundwater. Plants and animals living in
environments contaminated with cyclohexane can store small amounts of the
chemical.

Where in the environment does cyclohexane end up?

Cyclohexane by itself is not likely to cause environmental harm at levels normally

found in the environment. Cyclohexane can contribute to the formation of
photochemical smog when it reacts with nitrogen dioxide, ozone, and other
volatile organic carbon substances in air.

90
What are the cyclohexane environmental guidelines?

No national guidelines.

Sources of emissions
 Industry sources
 Natural sources
 Transport sources
 Consumer products that may contain cyclohexane

Industry sources

The primary point sources are petroleum refining, automotive repair shops, and
commercial printing and publishing.

Natural sources

Cyclohexane is a natural constituent of crude petroleum. It also occurs naturally

as a plant volatile and can be released from volcanoes.

Transport sources

Cyclohexane has been detected in motor vehicle exhaust.

Consumer products that may contain cyclohexane

Cyclohexane is used as a solvent, oil extractant, paint and varnish remover, and
in solid fuels.

91
Comparison to other substances

NPI rank (National Pollutant Inventory rank

Approximately 400 substances were considered for inclusion on the NPI

reporting list. A ranking and total hazard score was given based on health and
environmental hazards and human and environmental exposure to the
substance.Cyclohexane was ranked as 64 out of 400. The total hazard score
taking into account both human health and environmental criteria are 2.2.On a
health hazard rating of 0 - 3 cyclohexane registers 0.7. A score of 3 represents a
very high hazard to health, 2 represent a medium hazard and 1 is harmful to
health. On an environmental rating of 0 - 3 cyclohexane registers 1.5. A score of
3 represents a very high hazard to the environment and 0 a negligible hazard.
Factors taken into account to obtain this ranking and these scores include the
extent of the material's toxic or poisonous nature and/or its lack of toxicity, and
the measure of its ability to remain active in the environment and whether it
accumulates in living organisms. It does not take into account exposure to the
substance. Environmental exposure is reflected in the NPI rank for this
substance. A substance that scores highly as an environmental hazard is oxides
of nitrogen at 3.0 and one of the lower scores is carbon monoxide at 0.8. A
substance that scores highly as a health hazard is arsenic at 2.3 and one of the
lowest scores is ammonia at 1.0.

10.4 HAZOP Study of Storage Tank for Cyclohexane solvent:

A HAZOP study is to be conducted on cyclohexane tank, as presented by the

piping and instrumentation diagram show in fig (11.2).
In this scheme, Cyclohexane is unloaded from tank trucks into a storage tank maintained
under a slight positive pressure until it is transferred to the process.

92
10.5 HAZOP STUDY OF ETHYLENE

Health effects

Short term exposure by inhalation is considered to be practically non-harmful.

Skin and eyes

93
Contact with liquid ethylene will produce freezing injury to skin and eye tissue.

Inhalation

Ethylene vapour is an asphyxiant, depriving respired air of oxygen. At moderate

to high concentrations, inhalation of vapour can result in headaches, dizziness
and possible nausea. As with any chemical, ingestion, inhalation and prolonged
or repeated skin contact should be avoided.

First aid

Skin

Immediately wash contaminated skin with plenty of water. Remove contaminated

clothing. Seek immediate medical assistance. In case of 'cold burns' immerse
affected area in warm water for at least 15 minutes.

Eyes

Immediately irrigate with copious quantities of water for at least 15 minutes.

Eyelids to be held open. Remove contaminated clothing and wash contaminated
skin. Urgently seek medical assistance. Transport to hospital or medical centre

Inhalation

94
Remove from exposure—avoid becoming a casualty. Remove contaminated
clothing and loosen remaining clothing. Allow patient to assume most
comfortable position and keep warm. Keep at rest until
fully recovered. If breathing laboured and patient cyanotic (blue), ensure airways
are clear and have qualified person give oxygen through a face mask. If
breathing has stopped apply artificial respiration at once. In the event of cardiac
arrest, apply external cardiac massage. Seek medical advice.

Ventilation

Use with adequate ventilation. DO not enter confined spaces where vapour may
have collected. Maintain concentration below recommended exposure limit.

Environmental effects

The extended period of ethylene release from ethephon (2-

chloroethylphosphonic acid) after application to intact tomato plants has provided
a model system in which the effect of ethylene on photosynthetic metabolism and
release
carbon partitioning has been studied. Ethylene from leaf tissue after
ethephon treatment was 10 times greater than that from untreated control leaves.
The specific activity of 14C2H4 released from [14C] ethephon remained constant
over several days demonstrating that the ethylene was derived from the applied
ethephon. The ethephon-treated plants exhibited extreme epinasty of the leaves
and 24 h after application the flower buds in the first visible cluster had abscised,
leaf expansion at the apex had ceased and developing adventitious roots were
visible on the lower stem.

10.6 HAZOP STUDY OF HDPE

Effects

95
Inhalation : there is no evidence for inhalation. dust may cause irritation
skin contact : generally direct contact doesn’t lead to skin irritation.
Ingestion : the resin itself is inert and harmless, but certain additives could
be harmful.

Ingestion must be avoided

First Aid

Inhalation: in case of excessive inhalation of fumes, remove the affected person

to the
fresh air as soon as possible.
Skin: wash skin with soap and water
Eyes: Flush out with a copious volume of water any material entering the eyes.
Medical assistance is required

The complete MSDS for HDPE has been given in the next chapter.

Material Safety Data Sheet

96
1. Chemical Identity HDPE

Chemical High Density Poly Trade name HDPE

Name ethylene
Synonyms Polyethylene Chemical Synthetic polymer
classification
Formula (C2H4)n CAS Number 25087-34-7/25895-
47-0
UN number DNA UN Hazard class DNA
Hazchem code ( EAC) DNA
REGULATED IDENTIFICATION Hazardous CAS No. 25087-34-
ingredients 7/25895-47-0
Shipping DNA - -
Name
Shipping code/ Label DNA
Hazardous waste Id No. Not pertinent
Uses: Manufacture of pipes, carbuoys, bags, sacks etc.

2. Physical And Chemical Data

Boiling Decomposes Physical Solid Appearanc Spheres,

point/ state e pellets
Range °C
Melting/ 115-130 Vapor DNA Odour Odourless
Freezing Pressure( at
Point °C 20 °C ) mm
Hg
Vapour Not pertinent Solubility in Insoluble Other Information
Density water ( at 30

97
( Air =1) °C)
Specific gravity 0.94-0.958 pH Not pertinent
( at 20 °C ) (water
=1)

3. FIRE AND EXPLOSION HAZARD DATA

Flash point °C DNA Flammability 10 TDG DNA

(CC) LFL % v g/m3 Flammability
(OC) UFL % v Not
appli.
Explosion No Explosion No Auto ignition 390
sensitivity to sensitivity to Temperature °C
impact static electricity
Combustible No Explosive No Hazardous will
Material Material Polymerization not
occur
Flammable No Oxidizer No Corrosive No
Material Material
Prophetic No Organic No Other information :
Material Peroxide
Hazardous Combustion Products

4. Reactivity Data

Chemical stability Stable

Incompatibility with other React violently with F2
Materials
Reactivity
Hazardous Reaction Acrid smoke and fumes. Very low levels of other
Products dec. products as acrolein may develop.

98
5.Health Hazard Data

Route of entry Inhalation, skin contact, ingestion

Effect of Inhalation: there is no evidence for inhalation. Dust may
exposure/ cause irritation
Symptoms Skin contact: generally direct contact doesn’t lead to skin
irritation.
Ingestion : the resin itself is inert and harmless, but certain
additives could be harmful.
Ingestion must be avoided
Emergency Inhalation : in case of excessive inhalation of fumes, remove
treatment the affected person to the
fresh air as soon as possible.
Skin : wash skin with soap and water
Eyes: Flush out with a copious volume of water any material
entering the eyes.
Medical assistance is required
Permissible TLV-TWA DNA STEL(ACGIH) DNA
Exposure Limit ( ACGIH)
TDLo imp-rat: IDLH DNA Odour Not
threshold pertinent
NFPA Hazard Health Flammability Reactivity Special
signals 0 1 0 -

6. Preventive Measures HDPE

PERSONAL Dust mask, gloves, safety goggles or glasses, no slip

PROTECTIVE shoes.
MATERIAL

99
HANDLING AND Keep away from sources of ignition or heat, in dry,
STORAGE well ventilated area. In storage and working rooms
PRECAUTIONS avoid spheres spilling as a possible cause of slipping.

100
6. Preventive Measures HDPE

PERSONAL Dust mask, gloves, safety goggles or glasses, no slip

PROTECTIVE shoes.
MATERIAL
HANDLING AND Keep away from sources of ignition or heat, in dry, well
STORAGE ventilated area. In storage and working rooms avoid
PRECAUTIONS spheres spilling as a possible cause of slipping.

7. Emergency And First Aid Measures

1
FIRE ( Class of fire : A)
Fire extinguish Water spray, foam, dry chemical, carbon dioxide
media
Special cool exposed containers with water
Procedures
Unusual Hazards By direct ignition the product burns with flames developing H 20,
CO2 and in case of oxygen defeciency, also CO
EXPOSURE
First Aid Inhalation: in case of excessive inhalation of fumes, remove the
Measures affected person to the fresh air as soon as possible.
Skin: wash skin with soap and water
Eyes: Flush out with a copious volume of water any material
entering the eyes. Medical assistance is required
Antidotes/ Dosages
SPILLS
Steps to be taken Collect for reuse or disposal
Waste Disposal By disposal at approved landfill tips or incinerator oven. The
Method product is assimilated to urban waste.

8. Toxicological Information

The information provided below can be subject to misinterpretation. Therefore, it is essential

the following

101
Individuals trained in its evaluation interpret information.

9. Chemical Toxicity Data

Polyethylene
No toxicology data available.
All grades of polyethylene are FDA approved and are not considered hazardous
Materials under the OSHA Hazard Communication Standard

10. ECOLOGICAL INFORMATION

No data is available on the adverse effects of this product on the environment. Neither COD
nor BOD data are
Available. Fish or birds may eat pellets, which may obstruct their digestive tracts.

11.OTHER REGULATORY INFORMATION

The following chemicals are specifically listed by individual states; other product-specific
health and safety Data in other sections of the MSDS may also be applicable for state
requirements. For details on your Regulatory requirements, you should contact the
appropriate agency in your state.

102
COST ESTIMATION

Before the plant to be operated, specified money must be supplied to purchase and
install the equipment. The capital needed to supply the necessary plant facilities is
called fixed capital investment while that for the operation of the plant is called the
working principal and sum of two capitals is called total capital investment.

12.1 COST INDEX

Is and index value for a given point in time showing the cost at that time
relative to certain base time. if the cost at any time in past is know , the equivalent
cost at the present time can be determined by multiplying the original cost by the
ratio of present of index value to the index value applicable when the original cost
was obtained. There are many types of cost indexes and the most commune type
are marshall and swift all industry and process industry equipment indexes and
engineering News Record construction index.
Present cost =
Original cost *cost index value at present time/cost index value at past.

12.2 PURCHASE COST OF MAJOR EQUIPMENTS

Compressor 8324 pounds

Reactor 58818

Flash separator 1500

Cetrifurge1 78378

Heat exchanger 10000

Centrifuge 2 78378

Dryer 3050

103
total 238448

Total Purchased cost of Equipments=PCE=₤238448

12.3 FIXED CAPITAL COST

Cost that do not vary with production rate. These are the bills to be paid whatever
the quantity produced is.

Major equipment, total purchased cost

Equipment erection 0.4

Piping 0.70
Instrumentation 0.20
Electrical 0.10
Building process 0.15
Utilities 0.50
Storages 0.15
Site development 0.05
Ancillary building 0.15
Total = 3.40

Physical plant cost = PPC = PCE* (Total

)
PPC = 238448*3.40
=₤810723.2
Design and engineering 0.30
Contractor’s fee 0.05
Contingency 0.10
Total 1.45

104
Fixed Capital = PPC * 1.45
= 810723.2 * 1.45
= ₤1175548.64
Thus Fixed Capital Cost = ₤1175548.64

Fixed Capital Cost =FCC= ₤1175548.64

Fixed Capital Cost =FFC= ₤1175548.64

Cost in year 2006=Cost in year 1998*Cost index in year 2006/Cost index in 1998
Cost index in year 2006=1230
Cost index in year 1998=132

Fixed Capital Cost in year 2006=₤45185150.85

12.4 OPERATING COSTS

Maintenance cost = 0.10 * fixed capital cost

= 0.10 * 45185150..08
= ₤4518515.08
Miscellaneous = 0.10 * maintenance cost
= 0.10 * 1707502.3
=₤451851.50
Operating labor = ₤5*10^5
Laboratory cost = 0.20* labor cost=₤1*10^5
Supervision=0.20* labor cost=₤1*10^5
Plant overheads = 0.50 * labor cost =₤2.5*10^5
Capital charges = 0.15 * fixed capital cost =0.15*45185150.85=6777772.26
Local taxes = 0.02 * fixed capital cost =0.02*45185150.85=903703
Insurance = 0.01 * fixed capital cost=0.01*45185150.85=451851
Regulations and license fees = 2 % of sales price

105
 12.4 PRODUCTION COST
Variable cost
Raw materials = 0.30 * 13371500
= ₤4011450
Miscellaneous = ₤451851.50
Shipping and packing negligible
Sub total = A = ₤4463301.5
Fixed costs
Maintenance cost = ₤4518515.08
Operating labor = ₤5*10^5
Laboratory cost =₤1*10^5
Supervision =₤1*10^5
Plant overheads = ₤2.5*10^5
Capital charges = ₤6777772.26
Local taxes = ₤903703
Insurance = ₤451851
Sub Total B=₤13601841.37
Direct Production Cost = A+B=₤18065142.84
Sales expense, General overheads, R&D=C=0.25* Direct Production Cost
=₤4516285.71
Annual Production Cost =A+B+C=₤321186669.92
Production cost/Kg= 2.569₤/Kg

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106
2) Rase, H.F., “ Chemical Reactor Design for Process Plants” Vol. 1,(wiley) ,
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107
14) .Coulson, J.M., and Richardson,J.F.,”Chemical Engineering”,4 th ed., 2nd Vol.,
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108
28) Mujmader, K.J, “Hand Book of Industrial Drying”.

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109