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Sidra-tul-Muntaha 2005/FC-CPE-18
Bachelor’s Degree
In
CHEMICAL ENGINEERING
Name:______________
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APPENDIX.................................................................................................................................
Production of Cyclohexane from Benzene
PREFACE
This project is submitted to the Department of Chemical Engineering, University Of
Engineering And Technology Lahore, Pakistan, for the fulfillment of the Bachelors
Degree.
This research report is concerned about the activity of designing a plant for manufacture
of Cyclohexane. The study of said subject offers a way to make Pakistan self supported in
cyclohexane, as all consumer society of it imports this chemical from Saudi Arabia,
China, UAE and Malaysia. The report describes the most economical way to produce
cyclohexane in Pakistan keeping in view all the resources of country.
The survey of demand of cyclohexane in Pakistan has been made with the help of Lahore
Chamber Of Commerce and Trade. Hence the production capacity of our plant is based
on the present needs of it.
Chapter # 2 is Process selection and description of flow-sheet. This chapter gives the
concise listing of commercial processes used for synthesis of cyclohexane. These include
liquid and vapor phase processes, while the one by one description of each process has
been avoided but major strengths of each category has been stated to the level as is the
1
Production of Cyclohexane from Benzene
demand of the work. Contrary to this, process selection is based on the economic analysis
of different methods of production. In the end a detailed description of flow-sheet and
process has been given. The flow-sheet has been taken from Encyclopedia of design and
process for chemical engineers.
Chapter #3 is Material and energy balance of the plant. The lengthy calculations have
been given in tabular form.
Chapter # 5 is the Instrumentation and process control. This is the vast field of
research and makes the job complex. Report states the control of temperature in outer
recirculation cooler. The complete PID has been given. Above it automatic control is the
recommended throught out the plant that results in saving labor expenses along with
improved ease and efficiency of operations.
Plant has not its own power set-up rather it is recommended to purchase on commercial
level.
Although nomographs, simplified equations, and shortcut methods are included, every
effort has been made to indicate the theoretical background and assumptions for these
relations.SI units are emphasized but older fps and cgs systems have not been completely
removed. Conversion factors have been given where ever is needed. The property data
2
Production of Cyclohexane from Benzene
has been collected from various books and simulation software Hysys at the process
conditions.
The Authors
Zaeema Tahir
Sidra-tul-muntaha
Usman Hameed
Waqas Ahmed
Chapter # 1
3
Production of Cyclohexane from Benzene
INTRODUCTION
Cyclohexane is a cycloalkane. Cycloalkanes are types of alkanes which have one or more
rings of carbon atoms in the chemical structure of their molecules. Alkanes are types of
organic hydrocarbon compounds which have only single chemical bonds in their
chemical structure. Cycloalkanes consist of only carbon (C) and hydrogen (H) atoms and
are saturated.
Cyclohexane has following synonyms. Benzenehexahydride,Ciclohexano,
Hexahidrobenceno, Hexahydrobenzene, Hexamethylene, Hexametileno, Hexanaphthene,
Naphthene.
Nylon growth, which is the main driver in the cyclohexane market, has stagnated in many
applications to below GDP levels although there is still some growth in nylon plastics for
automotive and other resin applications. One of the better performing markets for nylon
is engineering thermoplastics. These materials have tough physical properties such as
high tensile strength, excellent abrasion, chemical and heat resistance, which allow them
to replace metals. Automotive applications have been growing strongly where there has
been a drive to replace metals with plastics to reduce the weight of motor vehicles.
FUTURE DEMAND
Future global demand growth for cyclohexane is put at
around 2-3%/year. SRI Consulting estimates global demand
for cyclohexane was just over 5m tonnes in Figure1.1 2005.
With an average growth rate of 3%/year, demand should reach
6m tonnes by 2010.
In Europe, future demand growth is about 2%/year with the
main growth in engineering plastics and some industrial filament uses.
Any new investment in cyclohexane is likely to be focussed in the Middle East and Asia
where demand growth is strongest. Aromatics Thailand started up a 150,000 tonnes/year
4
Production of Cyclohexane from Benzene
NATURAL RESOURCES
Cyclohexane occurs naturally in crude oil and can be released from petroleum
fractions whenever they are refined, stored or used. Another major release is from motor
gases. Naturally is also released from volcanos. It is produed in large quantities for nylon
production and is released in water from plants. However, cyclohexane is resistant to
biodegradation, it degrades only in the presence of other petroleum fractions. Volatization
from water should be the fate process for aquatic life. While bio-concentration in aquatic
organism and adsorbtion to sediments is estimated to occur to a moderate extent.
PROPERTIES
Table 1.1
Cyclohexane
Solvent Properties
CAS 110-82-7
5
Production of Cyclohexane from Benzene
Physical Properties
Molecular weight 84.16
Boiling point 80.72°C
Vapor pressure 77.5 Torr at 20°C
Freezing point 6.54°C
Refractive index 1.4262 at 20°C
Density 0.7785 g/mL (6.497 lb/gal) at 20°C
0.7739 g/mL (6.457 lb/gal) at 25°C
Dielectric constant 2.02 at 20°C
Dipole moment 0 D at 20°C
Polarity index (P') 0.2
Viscosity 1.0 cP at 20°C
Surface tension 24.98 dyn/cm at 20°C
Solubility in water 0.006% at 25°C
Solubility of water in cyclohexane 0.01% at 20°C
Storage Store in an area designed for
flammable storage, or in an approved
metal cabinet, away from direct
sunlight, heat and sources of ignition.
6
Production of Cyclohexane from Benzene
HISTORY
and in the same year E. Haworth and W.H. Perkin Jr. (1860 - 1929) did the same in a
Wurtz reaction of 1,6-dibromohexane.
INDUSTRIAL APPLICATIONS
7
Production of Cyclohexane from Benzene
Cycloalkanes (also called naphthenes , especially if from petroleum sources) are types
of alkanes which have one or more rings of carbon atoms in the chemical structure of
their molecules. Alkanes are types of organic hydrocarbon compounds which have only
single chemical bonds in their chemical structure. Cycloalkanes consist of only carbon
(C) and hydrogen (H) atoms and are saturated because there are no multiple C-C bonds
to hydrogenate (add more hydrogen to). A general chemical formula for cycloalkanes
would be CnH2(n+1-g) where n = number of C atoms and g = number of rings in the
molecule. Cycloalkanes with a single ring are named analogously to their normal
alkane counterpart of the same carbon count: cyclopropane, cyclobutane, cyclopentane,
8
Production of Cyclohexane from Benzene
cyclohexane, etc. The larger cycloalkanes, with greater than 20 carbon atoms are
typically called cycloparaffins.
Cycloalkanes are classified into small, common, medium, and large cycloalkanes,
where cyclopropane and cyclobutane are the small ones, cyclopentane, cyclohexane,
cycloheptane are the common ones, cyclooctane through cyclotridecane are the medium
ones, and the rest are the larger ones.
Chapter # 2
9
Production of Cyclohexane from Benzene
1) OPERATING CONDITIONS
There exist two types of processes one is called liquid phase process and other
is called vapor phase process of cyclohexane manufacture. The phase to be
handled dictates the operating conditions of process. In liquid phase processes the
operating temperature is comparatively low. Hence is less costly process.
Vapor phase processes yield an undesirable low output per unit volume of
reactor zone. This is not only due to low density of treated products but also due
to difficulties encountered in cooling of said reactor zone. It is necessary to use
bulky apparatus comprising critical and costly cooling coils.
2) CATALYST TYPE
3) TEMPERATURE CONTROL
The method used to offset the rise in temperature due to exothermicity of the
reaction. In a fixed bed, this problem can be solved in two ways.
I. By installing several adiabatic reactors in series, and lowering the
temperature between each reactor, by direct quench, or by cooling in heat
exchangers; however, this solution requires considerable equipment.
II. By using a Latitude reactor with1 circulation of a heat transfer fluid on the
shell side; however, the need to fill each catalyst tube uniformly to
guarantee uniform pressure drops, flow rates and unit conversions, as
well as the necessarily large no. of these tubes, makes this solution costly
in terms of capital expenditure and problematic in operation.
If the catalyst is in suspension, the heat can be removed by the circulation of the
medium outside the reactor, through a heat exchanger. Various liquid and vapor
phase processes are tabulated below with their prominent characteristics.
TABLE 2.1
Table 2.2
11
Production of Cyclohexane from Benzene
For this design report, IFP liquid phase process is selected. IFP process is a
mixed phase process; i.e; it is a hybrid of liquid phase and vapor phase process.
This process enjoys the benefits of both process and makes it economical.
Majorly it converts benzene in liquid phase at low temperature after that it
eliminates the inherited drawback of liquid phase process of low purity by
converting rest of the benzene in vapor phase hence also relaxes the need of costly
reactor.
1. It is a liquid phase process that is a stable system with respect to control point of
view.
2. Better heat removal system i.e., by outer-recirculation cooler, so an isothermal
reaction is achieved.
3. Pressure is high which give higher yields at a particular temperature.
4. Lower temperatures can be selected in liquid phase which give higher equilibrium
constant values as the process is exothermic.
PROCESS DETAILS
12
Production of Cyclohexane from Benzene
One mole of benzene reacts with three moles of hydrogen to produce one mole of
cyclohexane. The reaction is highly exothermic, liberating 91500 btu/lb-mol of benzene
converted at 300 oF.
The kinetics are first order in hydrogen partial pressure, zero order of benzene, and
independent of the pressure of cyclohexane.
Fresh benzene from storage tank at 25oC and 1 atm, make-up hydrogen, and
recycle hydrogen are heated to reaction temperature, (benzene in heat exchanger and
hydrogen is heated by compressing adiabatically) and fed to the slurry reactor. Slurry
phase reactor is an isothermal reactor in which benzene in liquid form and hydrogen in
gas phase is introduced and reaction takes place on Raney nickel catalyst. The conversion
in this reactor is 95%. Slurry phase reactor is provided with an outer-recirculation heat
exchange/cooler which removes the heat of reaction and low pressure (70 psi) steam in
generated. Temperatures in the reactor are held below 204 oC to prevent thermal
cracking, side reactions and an unfavorable equilibrium constant that would limit benzene
conversion.
Next to the slurry phase reactor, a catalytic fixed bed pot reactor is provided
which makes-up the conversion almost to 100%. In this reactor the reaction takes place
in vapor phase .Effluent from the fixed bed reactor is condensed and cooled to 160°C and
then this Gas liquid mixture is flashed to 10 atm in a gas liquid flash separator. Excess
hydrogen is recycled to slurry phase reactor and liquid from separator is fed to the
stabilizer column to remove dissolved hydrogen. Liquid product from bottom of
stabilization column at 182oC is cooled in product cooler and send for final storage. The
13
Production of Cyclohexane from Benzene
overheads of low pressure flash are 95% hydrogen which is used as fuel gas or mixed
with sales gas.
14
Production of Cyclohexane from Benzene
HYDROGENATION CATALYSTS
Nickel and noble metals (rhodium, ruthenium and Platinum) are catalysts for benzene
hydrogenation, commonly and for this project Raney Nickel in suspension is used as a
catalyst for liquid phase hydrogenation. Nickel catalysts require generally high
temperatures and pressures.
Raney Nickel is powdered alloy of Nickel with aluminum, activated with caustic soda
solution. Normal percentage of aluminum in the alloy is 10--15%.
Raney Nickel is classified as W1 W2, W3, W5, W6, W7 and W8 due to the activity
difference mainly imparted from the method of preparation. Most active grade is W 6 but
minimum allowed temperature is < 100°C. We select W2 grade because it can be easily
stored under solvent contained sealed container. Nickel catalysts are especially
susceptible to sulfur poisoning. Sulfur compounds in feed are kept below Ippm. Carbon
monoxide is also mentioned as a catalyst poison for Nickel and concentration in the
feeds should be kept below 20 ppm. Catalysts must have high degree of hydrogenation
activity because benzene conversion must be nearly complete to meet product purity.
Activity increases with hydrogen adsorption on the surface.
Instead of Raney Nickel, Nickel oxide (NiO) supported on alumina (Al 2 03) is used for
vapor phase hydrogenation in) fixed bed pot reactor.
The Characteristics of system used are given below:
16
Production of Cyclohexane from Benzene
αµ =29oA
TEMPERATURE SELECTION
Because it is an exothermic reaction, the equilibrium constant decreases as
the temperature is increased. Conversely at very low temperatures, the reaction rate
is impractical. There are two limits for high temperature selection.
In the following, a table T 2.3 is produced which shows the variations in equilibrium
constant values versus temperature.
Table 2.3
TEMPERATURE
EQUILIBRIUM CONSTANT,K.
O
( C)
93 2.29 XlO10
149 2.6x106
204 2.18X103
17
Production of Cyclohexane from Benzene
260 7.10
We selected 204oC at which value of K is appreciable. For pure feed, the yield at
this temperature and system pressure is almost 100%.
PRESSURE SELECTION
K = [C6H12] [E/π]3
[C6H6][H2]3
C6 H12 yield.
According to Le' chattier principle, high pressure will favour more benzene
inversion.
18
Production of Cyclohexane from Benzene
A table is given below which shows the impact of H2/Bz ratio on reaction
conversion at 204 °C.
Table 2.4
S + H2 —> H2S
The H2S in ppm is discarded in purge stream from liquid/gas separator. Although
for purge, concentration of CO is cared about, low ppm H2S is assumed to be
blown - off.
2. Pressure effects on solubility is neglected because total
condensed cyclohexane flashed from separator is recycled back via over-head
condenser.
19
Production of Cyclohexane from Benzene
1. As the capacity selected is claimed for a pilot plant, the design dimensions of all
equipments support the claim, i.e., no commercial scale dimensions are encountered.
2. The dimensions are consistent i.e., design methods/strategies work well and no
unevenness is found.
These features not only confirm the design strategies, but also justify the
assumptions made in the design. Secondly, although it is a pilot plant, there is no need for
special fabrication i.e., all the heat exchangers and rotary machinery is readily
available/fabricated by vendors/fabricators.
20
Production of Cyclohexane from Benzene
Chapter # 3
MATERIAL BALANCE
Basis
Bz : H2
REACTION
From Encyclopedia
M.C.P. = 0.00022
Benzene = 10 ppm
Total = 1.00
Benzene = 0.9978
C.H. = 0.00016
M.C.P. = 0.00012
Impurities = 0.00057
Total = 1.00
22
Production of Cyclohexane from Benzene
H2 = 0.9111 0.98798
CO = 0.00013 0.00001
R-O1
Components In (Kg/hr) Out (Kg/hr)
Benzene 1548.80 78
Cyclohexane 0.3 1583.6
M.C.P. 0195 0.4
Impurities 1.00. 1.7
23
Production of Cyclohexane from Benzene
R-O2
Components In (Kg/hr) Out (Kg/hr)
Benzene 78 0.02
Cyclohexane 1583.6 1667
M.C.P. 0.4 0.4
Impurities 1.7 1.7
Sulfur Trace Trace
Hydrogen 36 30
Carbon dioxide 0.06 0.06
Carbonmonoxide 0.04 0.04
Methane 25 25
Total 1725 1725
24
Production of Cyclohexane from Benzene
V-O1
Components In (Kg/hr) Out (Kg/hr)
Liquid Purge Recycle
Benzene 1.7 0.02 - -
Cyclohexane 1666.545 1666.5 - -
M.C.P. 0.4 0.4 - -
Impurities 1.7 1.7 - -
Sulfur Trace - - -
Hydrogen 30 0.498 16 13.25
6-
Carbon dioxide 0.06 10x6.6 0.03 0.025
6-
Carbonmonoxide 0.04 10x4.2 0.02 0.0167
3-
Methane 26.0 10x3 13.14 11.5
Total 1725 1669 30 25
BALANCE ACROSS STABILIZATION COLUMN (V-O2)
25
Production of Cyclohexane from Benzene
V-O2
Components In (Kg/hr) Out (Kg/hr)
Bottoms Overheads
-3
Benzene 0.02 5.18X10 0.01482
Cyclohexane 1666.5 1666.5 0
-4
M.C.P. 0.4 3.6x10 0.3996
Hydrogen 0.996 0.0258 0.9702
6- 6-
Carbon dioxide 10x6.6 0 10x6.6
6- 6-
Carbonmonoxide 10x4.2 0 10x4.2
3- 3-
Methane 10x3 0 10x3
Total 1669 1666.53 1.3876
26
Production of Cyclohexane from Benzene
27
Production of Cyclohexane from Benzene
ENERGY BALANCE
Watson Equation;
Where;
T= Temperature (OF)
= 996 R.
= 636.36 R
HEAT OF REACITON:-
From537 R to 960 R
28
Production of Cyclohexane from Benzene
c, Cp = (0.6-0.45)/(400-77)
29
Production of Cyclohexane from Benzene
Average Temperature =
= 434K
= -7.701 + 54.543-0.02
30
Production of Cyclohexane from Benzene
Where;
R = 2 Btu/ lb mol - ° F
31
Production of Cyclohexane from Benzene
1. Δ Hr,77
ΔHp = mCpΔT
ΔHR =mCpΔT
= 1013052.4 Btu/hr.
Inserting in (A):
= -3347728.65 + 815762.632-1013052.4
Conversion = 98 % to 100%
= 0.909 lb moles/hr.
33
Production of Cyclohexane from Benzene
(T22– 5002)](33.38)
Hence;
T2 = 522.55 °F
34
Production of Cyclohexane from Benzene
1 2
Fluid Entering Benzene Water
Flow-rate (kg/hr) 26877.3 7978.7
Inlet Temperature 0C 248.88 150.5
Outlet Temperature 0C 204.44 243.3
Change in temperature 0C 44.44 93.3
Heat Capacity (J/kg K) 2590.36 4169.7
Inlet Enthalpy kJ/kg 579 520
Oulet Enthalpy kJ/kg 191.9 907.4
Duty of exchanger (MJ/hr) 3094 3094
35
Production of Cyclohexane from Benzene
1 2
Fluid Entering Cyclohexan Water
PARAMETERS e + Gas
STREAM STREAM
Flow-rate (kg/hr) 1
1725 2
2478.5
Fluid Entering
Inlet Temperature 0
C cyclohexane
272.5 Water
26.7
Flow-rate (kg/hr)
Outlet Temperature 0
C 1669
62 11603.2
149
0
Inlet
ChangeTemperature
in temp. 0
CC 125
202 55.24
122.3
Outlet Temperature(j/kgK)0C
Heat Capacity 125 3
3.6x10 65.6 3
4.19x10
3 3
Heat
Inlet Capacity
Enthalpy (J/kg
kJ/kgK) 3.0x10
891 4.19x10
7.123
Inlet EnthalpykJ/kg 515 126.7
Oulet Enthalpy kJ/kg 378.563 519.56
Outlet Enthalpy kJ/kg 474 167.6
Duty of exchanger 1266 1266
Duty of exchanger (MJ/hr)
(MJ/hr) 600 600
36
Production of Cyclohexane from Benzene
37
Production of Cyclohexane from Benzene
0
Inlet Temperature C 184 25
Outlet Temperature 0C 30 43
Inlet
Duty of exchanger (MJ/hr) 723.85 723.85
Enthalpy= Outlet Enthalpy
275.42=275.42(kJ/kg)
Chapter # 4
38
Production of Cyclohexane from Benzene
DESIGN OF EQUIPMENTS
REACTOR DESIGN
WHAT IS A REACTOR?
39
Production of Cyclohexane from Benzene
a. A container to which reactants are fed and products removed, that provides
for the control of reaction conditions.
b. A device that encloses the reaction space, and which houses the catalyst
and reacting media & is designed to provide residence times for reactants
so that chemical reaction occur among them under proper reaction
conditions.
REACTION
• Main reaction
ΔH = - 214 KJ/mole
• Highly exothermic
• Favored by low T & high ppH2
• Side reactions
• Isomerization
• Favored by high T
1. Fixed-bed Reactors
a. Packed beds of pellet or monoliths
40
Production of Cyclohexane from Benzene
Satterfield has discussed several advantages of slurry reactors relative to other modes of
operation. They include the following.
41
Production of Cyclohexane from Benzene
2. The high heat capacity associated with the large mass of liquid facilitates
control of the reactor and provides a safety factor for exothermic reactions
that might lead to thermal explosions or other "runaway" events.
3. Since liquid phase heat transfer coefficients are large, heat recovery is
practical with these systems.
4. The small particles used in slurry reactors may make it possible to obtain
much higher rates of reaction per unit weight of catalyst than would be
achieved with the larger pellets that would be required in trickle bed
reactors. This situation occurs when the trickle bed pellets are characterized
by low effectiveness factors.
6. Since fine catalyst particles are desired, the costs associated with the
pelleting process are avoided, and it becomes possible to use catalysts that
are difficult or impossible to pelletize.
TYPES
42
Production of Cyclohexane from Benzene
Slurry reactors may take on several physical forms: they may be simple
stirred autoclaves; they may be simple vessels fitted with an external pump
to recirculate the liquid and suspended solids through an external heat
exchanger; or they may resemble a bubble-tray rectifying column with
various stages placed above one another in a single shell. Since a single
slurry reactor has a residence time distribution approximating a CSTR, the
last mode of construction gives an easy means of obtaining stagewise
behavior and more efficient utilization of the reactor volume.
• They have excellent heat and mass transfer characteristics, meaning high
heat and mass transfer coefficients.
• Little maintenance and low operating costs are required due to lack of
moving parts and compactness.
• Wide range of possible operating pressures(5-150bar)
• Absorption of reaction heat is obtain so that isothermal conditions are
approached
• Low pressure drop across reactor
• Little floor space is requried
• High wetting of external catalyst surface to delay catalyst fouling
• Solids can be handled without significant errosion or plugging problems
• The durability of the catalyst or other packing material is high. Moreover,
online catalyst addition and withdrawal ability
INTRODUCTION
A bubble column reactor is basically a cylindrical vessel with a gas distributor at the
bottom. The gas is sparged in the form of bubbles into either a liquid phase or a liquid–
43
Production of Cyclohexane from Benzene
solid suspension. These reactors are generally referred to as slurry bubble column
reactors when a solid phase exists.
44
Production of Cyclohexane from Benzene
45
Production of Cyclohexane from Benzene
DESIGN CALCULATIONS
4. Mass transfer of dissolved gas from the bulk liquid to the outer
47
Production of Cyclohexane from Benzene
= 160.45 cm2/cc
48
Production of Cyclohexane from Benzene
Db = bubble diameter, cm
Db3 = 1.247
Db = 1.076 cm = 10.76 mm
θ = Surface tension.
Estimate the surface tension, θ, using the generalized corresponding state correlation of
Brock and Bird and the Miller relationship. The correlation and the relationship are as
follows:
Where
Tc = critical temperature, K
Tb = 80.1 °C = 353.1 °K
f = 686102 Bubbles/sec.
Solving all diffusion & reaction equations simultaneously gives final equation of the form
Where
50
Production of Cyclohexane from Benzene
Equilibrium exist at bubble-liquid interface, Cig and Cil are related by Henry’s
Law Cig = H Cil
As bubbles are small and in large cone (Large ag), while ac is low and poor agitation so
final expression for ko is
Where,
Hence
kc = 0.0305 cm/sec
H = 1765.4
pp H2 = 35 atm
Xe – Xi = 0.95
F = 5.74 gmol/sec
Vreactor = 2.75 m3
Vessel is cylindrical and in slurry bubble column reactors height to diameter ratio is from
3 to 6. Let height to diameter ratio be 4:1 so
52
Production of Cyclohexane from Benzene
Γ = 1.958 min
SPARGER SELECTION
• Low price
• Easy manufacturing
• Variety of specfications
53
Production of Cyclohexane from Benzene
SPECIFICATION SHEET
Identification
Item Reactor
No. required 1
Position Vertical
54
Production of Cyclohexane from Benzene
Operation Continuous
Type Catalytic
Chemical Reaction
Shape : Spherical
Size : 150 oA
55
Production of Cyclohexane from Benzene
56
Production of Cyclohexane from Benzene
57
Production of Cyclohexane from Benzene
The size a vapor-liquid separator drum (or knock-out pot, or flash drum, or compressor
suction drum) should be dictated by the anticipated flow rate of vapor and liquid from the
drum. The following sizing methodology is based on the assumption that those flow rates
are known.
Use a vertical pressure vessel with a length-to-diameter ratio of about 3 to 4, and size the
vessel to provide about 5 minutes of liquid inventory between the normal liquid level and
the bottom of the vessel (with the normal liquid level being at about the vessel's half-full
level).
Orientation
Type of internals
Type of heads
The selection of the orientation of a gas-liquid separator depends on several factors. Both
vertical and horizontal vessels have their advantages. Depending on the application one
has to decide on the best choice between the alternatives.
58
Production of Cyclohexane from Benzene
liquid removal efficiency does not vary with liquid level because the area in the
vessel available for the vapor flow remains constant
the downward liquid velocity is lower, resulting in improved de-gassing and foam
breakdown;
The preferred orientation for a number of typical vapor / liquid separation applications
are:
59
Production of Cyclohexane from Benzene
Feed Inlet
Inlet Nozzle
The feed nozzle size and the type of feed inlet device (if any) have an impact on the
vapor / liquid separation that can be achieved. The feed nozzle is normally sized to limit
the momentum of the feed. The limitation depends on whether or not a feed inlet device
is installed.
Inlet device
Various inlet devices are available to improve the vapor / liquid separation. Among others
the following inlet devices may be installed:
a deflector baffle
a half-open pipe
a 90 ° elbow
a schoepentoeter
For vertical drums, preferably a deflector baffle or a half open pipe shall be selected. In
case of a slug flow regime in the inlet piping, or if a high liquid separation efficiency is
required, a tangential inlet nozzle with annular ring can be used. However, in case a high
liquid removal efficiency is required, the application of a wire mesh demister is preferred.
60
Production of Cyclohexane from Benzene
For horizontal drums normally a 90° elbow or a slotted diverter is installed. In some
cases a submerged inlet pipe is installed, but this shall not be done in the case of a two-
phase feed.
Normally the selected inlet device for a horizontal drum shall be:
a submerged pipe when the feed is a subcooled liquid and the mixing of liquid and
blanket gas is to be minimized
Internals
After passing through the feed inlet, the vapor stream will still contain liquid in the form
of droplets. The maximum size of these entrained droplets depends on the vapor upflow
velocity. A separation device can reduce this entrainment significantly. Wire mesh
demisters are the most commonly used as separation device. They are used for two
reasons:
To minimize entrainment
Of the drum services having such a requirement, suction drums for reciprocating
compressors are the most notable examples
The allowable vapor velocity in a drum can be increased significantly by using a wire
mesh demister. So, when sizing is governed by vapor-liquid separation criteria, this will
result in a smaller diameter of the vessel
61
Production of Cyclohexane from Benzene
Although the size of the vessel often can be reduced by applying a wire mesh demister,
there are also many services where there is normally no demister installed. Reflux
accumulators, for example, seldom have mist eliminators.
There are several other types of mist eliminators such as vanes, cyclones, and fiber beds.
They are used when conditions are not favorable for wire mesh screens. Selection criteria
for these types of internals are the required efficiency, capacity, turndown ratio,
maximum allowable pressure drop and fouling resistance. These types however will not
be further addressed in this design guide.
Vessel Head
Most vessels have 2:1 elliptical heads, welded to the shell of the vessel. However, in
some cases other types of heads are used. The major alternatives are:
Flat heads
In case of small vertical vessels (diameter less than approximately 30”) often a flanged
top head is used, which also serves to provide access to the vessel. Depending on the
pressure rating, this type of head can either be flat or elliptical, and shall be selected in
consultation with the mechanical engineer
Hemispherical heads
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Production of Cyclohexane from Benzene
INLET STREAM
Impurities= traces
S= traces
INPUTS
VAPORS
H2= 30 kg/hr
CH4=26 kg/hr
LIQUID
Impurities= traces
S= traces
Kg mole of Gases
H2= 15 kg mole
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Production of Cyclohexane from Benzene
CH4=1.625 kg mole
VOLUME OF GASES
= 16.627×0.082×335/10
= m3
V= 45.676 m3/ hr
Density of vapours
= 0.935 kg/min
ρv = 0.935/0.76
= 1.23 kg/ m3
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Production of Cyclohexane from Benzene
Density of liquid
STEPS
Vv=A× Uv
A=πD2/4
LLA=ts× VL
3≥ ts ≤5
L=LL+1.5D+1.5ft
CALCULATIONS
= 0.0579m/s
Vv=A× Uv
A= Vv/ Uv
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Production of Cyclohexane from Benzene
= 0.218 m2
= 2.346 ft2
DIAMETER
D= 1.72 ft
= 1.75 ft
LLA=ts× VL˘
ts= 4 min
VL˘= VL× 5 %
= 0.908× 5 %
= 0.0454 m3 / min
LLA=ts× VL˘
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Production of Cyclohexane from Benzene
LL=ts× VL˘/ A
= 0.0454 ×4 / 0.218 m2
m3 / min×min×1/ m2
=0.633027 m
= 2.73 ft
= 2.75 ft
L= LL+1.5D+1.5 ft
= 6.875 ft
So length is 8.5 ft
L/D= 8.5/1.75
= 4.85
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Production of Cyclohexane from Benzene
69
Production of Cyclohexane from Benzene
STABILIZATION COLUMN
DESIGN
Stabilization column is the last mass transfer Operation in the production of cyclohexane.
Its Objective is to increase the purity of cyclohexane to the level as is demanded in
market and also to stabilize cyclohexane for safe storage, hence is the name stabilization
column.
It removes absorbed light gases( H 2 , CH4 , CO , CO2 ) from cyclohexane by raising its
temperature in column and hence stripping gases in counter current contact of gases and
liquid.
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Production of Cyclohexane from Benzene
Contrary to this there is another design in which the requirement of cold feed may be
relaxed as the need of cold stream is fulfilled with the help of refluxing a part of overhead
vapors. But it is costly due larger number of auxiliary equipments required.
I selected Cold feed without reflux stabilizer column .Saturated liquid feed at 10 atm is
entering at top of the packed column via liquid distributor. As the liquid flows down the
column making a film on packing an intimate contact of liquid and gas phase, which is
coming from bottom reboiler, takes place hence gases desorb from cyclohexane because
temperature of gas phase is higher than liquid: a favorable condition for gases to leave
liquid phase. At the bottom reboiler boils a portion of bottom product and sends back to
column to increase the purity of product to 99.98%. Saturated steam at 10.5 atm is
entering in reboiler’s coils. Overhead products contains majorly hydrogen and trace
amount of other products. This gas is used as a fuel gas and is stored after cooling in
overhead cooler.
MATERIAL BALANCE:
9.9x10-
H2 0.0245 0.498 5.0x10-4 3
0.995 0.4851
2.0x10- 1.07x10 2.1x10-
1.0x10-5 4 -7 6
2.6x10-5 1.9x10-4
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Production of Cyclohexane from Benzene
3.0x10-
CO 1.5x10-7 6
0 0 3.0x10-7 3.0x10-6
3.0x10-
CO2 1.5x10-7 6
0 0 3.0x10-7 3.0x10-6
3.7x10-
CH4 1.8x10-4 3
0 0 3.65x10-4 3.7x10-3
2.19x10 4.3x10-
MCP 2.15x10-3 0.043 -7 6
2.7x10-5 0.0429
Total 1.0 20.385 1.0 19.845 1.0 0.540
DESIGNING OF COLUMN
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Production of Cyclohexane from Benzene
Application of stripping in practical process requires the generation of large contact area
between liquid and gas phase. This is usually done with three basic techniques.
2- Dividing the liquid streams into numerous thin films that flow through continuous
Gas phase ( Packed Column)
3- Dispersing the liquid as multitude of discrete droplets within continuous gas
phase( Spray Contactor)
Above this the fabrication of trays in small diameter column is a difficult job.
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Production of Cyclohexane from Benzene
1. Shell
2. Packings
3. Packing support
4. Liquid distributor
its internals
The distributor and packing are the heart of the performance of this
equipment. Their proper selection entails an understanding
commonly made of expanded metal or woven wire screen that are stacked
in layers or as spiral windings.
1. It should provide large contact area between liquid and gas streams.
2. It should have high flooding limits.
3. It should have high wetting characteristics.
4. There should be less pressure drop in it.
5. It should have open structure so that packing may not plug.
6. It should have good liquid distribution characteristic.
7. It should be mechanically robust.
8. It should be economical and easily available.
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Production of Cyclohexane from Benzene
Literature survey reveals that structured packings have the merits of low
pressure drop, good mass transfer characteristics, high capacity and hence
lower diameter of column but they have the demerits of high cost and
relatively less availability. Also structured packings are employed
particularly in vacuum services where pressure drops must be kept low .
Pall rings have open structure and high flooding and loading limits. Good
liquid / gas distribution and high mass transfer efficiency. Metal rings are
easily wettable. Mechanical Strength of Metal Pall Ring Packing is high.
Other than this it is mechanically robust and can withstand high
temperature of our process hence I selected metal pall rings.
PACKING SIZE:-
In general the largest size of packing that is suitable to the size of packing
should be used; up to 50mm. Smaller sizes are more expensive than larger
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Production of Cyclohexane from Benzene
ones. Above 50mm lower cost per cubic meter does not compensate for
lower mass transfer efficiency. Uses of too large size packings in small
diameter column make liquid distribution poor .
0.3-0.9 25-38mm
>0.9 50-75mm
In high pressure system the capital cost of column is very important. So, it
is generally recommended to reduce the diameter of column and hence
reduce the cost of equipment.
The other choice is to increase the diameter of column and decrease the
height of column, which is not a suitable rule for high pressure systems as
the increase in diameter of column has a very little effect on reduction of
height of tower.
F L v = L/V(√ ρ v / ρ l )
Where;
= 0.46kg/sec
= 0.0143 kg/sec
= 778kg/m 3
=1.5kg/m 3
F LV = 2.3
K 4 = 0.13
K 4 / = 0.23
% flooding = 75%
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Production of Cyclohexane from Benzene
Fp = Packing factor m - 1
Diameter, D = √(4xA)/3.14
D= 0.223m
A= π/4(D 2 )
A= 0.039 m 2
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Production of Cyclohexane from Benzene
Pressure drop per unit height of packing differ from packing to other. It
also depends upon size of packing. Smaller sizes have larger pressure drop
than bigger one.
By graphical Method
X- Coordinate;
G x /G v √ (ρ v /ρ x -ρ v )
Y-Coordinate;
G v 2 F p µ x 0 . 1 /g c (ρ x -ρ v ) ρ v
Pressure drop per unit height of packing has been calculated with the help
of graph given in appendix Figure 4.2.
=0.07414 lb/s-ft 2
=2.419lb/s-ft 2
F p =48.48
X=1.596
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Production of Cyclohexane from Benzene
Y=0.0002
Number of transfer units has been calculated with the help of Kremser’s
Equation given below;
N+ 1 N+1
(S – S) / (S – 1) = Mol fraction of solute gas stripped
N= No Of Transfer Unit
S= Stripping Factor
= KV/L
L= Liquid flow-rate,kg-mol/sec
L= 5.66x10 - 3 kg-mol/sec
V= Vapor flow-rate,kg-mol/sec
V= 1.5x10 - 4 kg-mol/sec
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Production of Cyclohexane from Benzene
K= 76
S= 2.024
N= 8
HETP is a strong function of packing material and its size. Pall rings has
economical HETP. As the size of packing is reduced HETP reduces
because mass transfer efficiency increases, hence we get the benefit of
reduced cost. On the other hand in small size packings pressure drop per
unit height of packing is greater than larger one’s. According to Walas for
a given type of packing material the ratio of HETP to pressure drop
remains constant for all sizes. Hence it is not recommended to decrease
size of packing to have small height of column.
HETP/H O G = ln[mG/L]
[ mG/L-1]
Where
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Production of Cyclohexane from Benzene
[7]
As rule of thumb in when D<0.5m
HETP=D
HETP=0.233m
HOG = 0.54m
Z =N x H O G
Z=8x0.54
Z =4.32m
Z t = Z +H d +H b
= 5.04m
HLw = 0.0004(Lm/Dp)0.6
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Production of Cyclohexane from Benzene
Hlw=0.050m3/m3 of packing
84
1. Item Number V-02 Type:Packed
Production of Cyclohexane from Benzene
2 Service Cyclohexane Stabilizer
3. NO OF EQUIPMENTS 1
4. OPERATION CONTINUOUS
PROCESS CONDITIONS
6. Liquid Flow-rate
20.385
Kg-mol/hr
7. Liquid Quality Slightly corrosive
8. Liquid Viscosity cP 0.12
9. Vapor Handled Cyclohexane
10. Vapor Quality Slightly corrosive
11. Vapor mol.wt 84
12. Temperature K 453
13. Pressure atm 10
OPERATIONAL CONDITIONS
14. Nature of operation Stripping
15. Feed nozzle location Top/Sat. liquid
16. Temperature
442
K
17. Percentage Flooding 75%
COLUMN INTERNALS
85
20. Material of Packing Metallic, Carbon Steel
HEAT EXCHANGER
Heat exchanger is a device that is used to transfer heat between two fluids at different
temperature.
The principle types of heat Exchanger used in Chemical and allied industries are as follows:
SELECTION CRITERIA
Selection process includes a No. of factors all of these are related to the heat transfer
application.
1. Thermal Requirements
2. Material Compatibility
3. Operational Maintains
4. Environmental, Health & Safety Consideration
5. Availability
6. Cost
Shell and tube heat exchangers represent the most widely used vehicle for the transfer of
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Production of Cyclohexane from Benzene
heat in industrial process applications. They are frequently selected for such duties as:
• Process liquid or gas cooling
• Process or refrigerant vapor or steam condensing
• Process liquid, steam or refrigerant evaporation
• Process heat removal and preheating of feed water
• Thermal energy conservation efforts, heat recovery
• Compressor, turbine and engine cooling, oil and jacket water
• Hydraulic and lube oil cooling
• Many other industrial applications
Shell and tube heat exchangers have the ability to transfer large amounts of heat in
relatively low cost, servicable designs. They can provide large amounts of effective tube
surface while minimizing the requirements of floor space, liquid volume and weight.
Shell and tube exchangers are available in a wide range of sizes. They have been used in
industry for over 150 years, so the thermal technologies and manufacturing methods are
well defined and applied by modern competitive manufacturers. Tube surfaces from
standard to exotic metals with plain or enhanced surface characteristics are widely
available. They can help provide the least costly mechanical design for the flows, liquids
and temperatures involved.
Although there exist a wide variety of designs and materials available, there are
components common to all designs. Tubes are mechanically attached to tube sheets,
which are contained inside a shell with ports for inlet and outlet fluid or gas. They are
designed to prevent liquid flowing inside the tubes to mix with the fluid outside the tubes.
Tube sheets can be fixed to the shell or allowed to expand and contract with thermal
stresses by have one tube sheet float inside the shell or by using an expansion bellows in
the shell. This design can also allow pulling the entire tube bundle assembly from the
shell to clean the shell circuit of the exchanger.
Fluid Stream Allocations
There are a number of practical guidelines which can lead to the optimum design of a
given heat exchanger. Remembering that the primary duty is to perform its thermal duty
with the lowest cost yet provide excellent in service reliability, the selection of fluid
stream allocations should be of primary concern to the designer. There are many trade-
offs in fluid allocation in heat transfer coefficients, available pressure drop, fouling
tendencies and operating pressure.
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Production of Cyclohexane from Benzene
1. The higher pressure fluid normally flows through the tube side. With their
small diameter and nominal wall thicknesses, they are easily able to accept
high pressures and avoids more expensive, larger diameter components to be
designed for high pressure. If it is necessary to put the higher pressure stream
in the shell, it should be placed in a smaller diameter and longer shell.
2. Place corrosive fluids in the tubes, other items being equal. Corrosion is
resisted by using special alloys and it is much less expensive than using
special alloy shell materials. Other tube side materials can be clad with
corrosion resistant materials or epoxy coated.
3. Flow the higher fouling fluids through the tubes. Tubes are easier to clean
using common mechanical methods.
4. Because of the wide variety of designs and configurations available for the
shell circuits, such as tube pitch, baffle use and spacing, multiple nozzles, it is
best to place fluids requiring low pressure drops in the shell circuit.
5. The fluid with the lower heat transfer coefficient normally goes in the shell
circuit.This allows the use of low-fin tubing to offset the low transfer rate by
providing increased available surface.
Tubes
Tubing that is generally used in TEMA sizes is made from low carbon steel,
copper,Admiralty, Copper-Nickel, stainless steel, Hastalloy, Inconel, titanium and a few
others. It is common to use tubing from 5/8 to 1-1/2 in these designs. Tubes are either
generally drawn and seamless or welded. High quality ERW (electro-resistancewelded)
tubes exhibit superior grain structure at the weld. Extruded tube with low fins and interior
rifling is specified for certain applications. Surface enhancements are used to increase the
available metal surface or aid in fluid turbulence, thereby increasing the effective heat
transfer rate. Finned tubing is recommended when the shell side fluid has a substantially
lower heat transfer coefficient than the tube side fluid. Finned tubing has an outside
diameter in the finned area slightly under the unfinned, or landing area for the tube
sheets. This is to allow assembly by sliding the tubes through the baffles and tube
supports while minimizing fluid bypass. U-tube designs are specified when the thermal
difference of the fluids and flows would result in excessive thermal expansion of the
88
Production of Cyclohexane from Benzene
tubes. U-tube bundles do not have as much tube surface as straight tube bundles, due to
the bending radius, and the curved ends cannot be easily cleaned. Additionally, interior
tubes are difficult to replace, many times requiring the removal of outer layers, or simply
plugging the tube. Because of the ease in manufacturing and service, it is common to use
a removable tube bundle design when specifying U-tubes.
Tube sheets
Tubesheets are usually made from a round flat piece of metal with holes drilled for the
tube ends in a precise location and pattern relative to one another. Tube sheet materials
range as tube materials. Tubes are attached to the tube sheet by pneumatic or hydraulic
pressure or by roller expansion. Tube holes can be drilled and reamed and can be
machined with one or more grooves. This greatly increases the strength of the tube joint.
The tubesheet is in contact with both fluids and so must have corrosion resistance
allowances and have metalurgical and electrochemical properties appropriate for the
fluids and velocities. Low carbon steel tube sheets can include a layer of a higher alloy
metal bonded to the surface to provide more effective corrosion resistance without the
expense of using the solid alloy.
The tube hole pattern or pitch varies the distance from one tube to the other and angle of
the tubes relative to each other and to the direction of flow. This allows themanipulation
of fluid velocities and pressure drop, and provides the maximum amount of turbulance
and tube surface contact for effective heat transfer. Where the tube and tube sheet
materials are joinable, weldable metals, the tube joint can be further strengthened by
89
Production of Cyclohexane from Benzene
applying a seal weld or strength weld to the joint. A strength weld has a tube slightly
reccessed inside the tube hole or slightly extended beyond the tube sheet. The weld adds
metal to the resulting lip. A seal weld is specified to help prevent the shell and tube
liquids from intermixing. In this treatment, the tube is flush with the tube sheet surface.
The weld does not add metal, but rather fuses the two materials. In cases where it is
critical to avoid fluid intermixing, a double tube sheet can be provided. In this design, the
outer tube sheet is outside the shell circuit, virtually eliminating the chance of fluid
intermixing. The inner tube sheet is vented to atmosphere so any fluid leak is easily
detected.
Shell Assembly
The shell is constructed either from pipe up to 24 or rolled and welded plate metal. For
reasons of economy, low carbon steel is in common use, but other materials suitable for
extreme temperature or corrosion resistance are often specified. Using commonly
available shell pipe to 24 in diameter results in reduced cost and ease of manufacturing,
partly because they are generally more perfectly round than rolled and welded shells.
Roundness and consistent shell ID is neccessary to minimize the space between the baffle
outside edge and the shell as excessive space allows fluid bypass and reduced
performance. Roundness can be increased by expanding the shell around a mandrell or
double rolling after welding the longitudnal seam. In extreme cases the shell can be cast
and then bored to the correct ID.
In applications where the fluid velocitiy for the nozzle diameter is high, an impingement
plate is specified to distribute the fluid evenly to the tubes and prevent fluid induced
erosion, cavitation and vibration. An impingement plate can be installed inside the shell,
which prevents installing a full tube bundle, resulting in less available surface. It can
alternately be installed in a domed area above the shell. The domed area can either be
reducing coupling or a fabricated dome. This style allows a full tube count and therefore
maximizes the utilization of shell space.
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Production of Cyclohexane from Benzene
End channels or bonnets are typically fabricated or cast and control the flow of the tube
side fluid in the tube circuit. They are attached to the tube sheets by bolting with a gasket
between the two metal surfaces. In some cases, effective sealing can be obtained by
installing an O-ring in a machined groove in the tube sheet. The head may have pass ribs
that dictate if the tube fluid makes one or more passes through the tube bundle sections.
Front and rear head pass ribs and gaskets are matched to provide effective fluid velocities
by forcing the flow through various numbers of tubes at a time. Generally, passes are
designed to provide roughly equal tube-number access and to assure even fluid velocity
and pressure drop throughout the bundle. Even fluid velocities also affect the film
coefficients and heat transfer rate so that accurate prediction of performance can be
readily made. Designs for up to six tube passes are common. Pass ribs for cast heads are
intregrally cast and then machined flat. Pass ribs for fabricated heads are welded into
place. The tube sheets and tube layout in multi-pass heat exchangers must have provision
for the pass ribs. This requires either removing tubes to allow a low cost straight pass rib,
or machining the pass rib with curves around the tubes, which is more costly to
manufacture. Where a full bundle tube count is required to satisfy the thermal
requirements, this machined pass rib approach may prevent having to consider the next
larger shell diameter.
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Production of Cyclohexane from Benzene
Cast head materials are typically used in smaller diameters to around 14 and are made
from iron, ductile iron, steel, bronze or stainless steel. They typically have pipe thread
connections. Cast heads and tube side piping must be removed to service tubes.
Fabricated heads can be made in a wide variety of configurations. They can have metal
cover designs that allow servicing the tubes without disturbing the shell or tube piping.
Heads can have axially or tangentially oriented nozzles, which are typically ANSI
flanges.
Baffles
Baffles serve two important functions. They support the tubes during assembly and
operation and help prevent vibration from flow induced eddies and direct the shell side
fluid back and forth across the tube bundle to provide effective velocity and heat transfer
rates. The diameter of the baffle must be slightly less than the shell inside diameter to
allow assembly, but must be close enough to avoid the substantial performance penalty
caused by fluid bypass around the baffles. Shell roundness is important to acheive
effective sealing against excessive bypass. Baffles can be made from a variety of
materials compatible with the shell side fluid. They can be punched or machined. Some
baffles are made by a punch which provides a lip around the tube hole to provide more
surface against the tube and eliminate tube wall cutting from the baffle edge. The tube
holes must be precise enough to allow easy assembly and field tube replacement, yet
92
Production of Cyclohexane from Benzene
minimize the chance of fluid flowing between the tube wall and baffle hole, resulting in
reduced thermal performance and increased potential for tube wall cutting from vibration.
Baffles do not extend edge to edge, but have a cut that allows shell side fluid to flow to
the next baffled chamber. For most liquid applications, the cuts areas represent 20-25% of
the shell diameter. For gases, where a lower pressure drop is desirable, baffle cuts of 40-
45% is common. Baffles must overlap at least one tube row in order to provide adequate
tube support. They are spaced throughout the tube bundle somewhat evenly to provide
even fluid velocity and pressure drop at each baffled tube section.
Single-segmental baffles force the fluid or gas across the entire tube count, where is
changes direction as dictated by the baffle cut and spacing. This can result in excessive
pressure loss in high velocity gases. In order to affect heat transfer, yet reduce the
pressure drop, double-segmental baffles can be used. This approach retains the structural
effectiveness of the tube bundle, yet allows the gas to flow between alternating sections
of tube in a straighter overall direction, thereby reducing the effect of numerous changes
of direction. This approach takes full advantage of the available tube surface but a
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Production of Cyclohexane from Benzene
reduction in performance can be expected due to a reduced heat transfer rate. Because
pressure drop varies with velocity, cutting the velocity in half by using double-segmental
baffles results in roughly 1/4 of the pressure drop as seen in a single-segmental baffle
space over the same tube surface.
STREAM CONDITIONS
HOT FLUID
COLD FLUID
PHYSICAL PROPERTIES
HOT FLUID
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Production of Cyclohexane from Benzene
COLD FLUID
Density � = 995kg/m3
HEAT LOAD
Q = m Cp ∆T
T1 T2
t2 t1
Cold Fluid 43 C 25 C
95
Production of Cyclohexane from Benzene
LMTD = 41.72 K
Ft Factor
R= (T1-T2)/(t2-t1)
= 8.55
S=(t2-t1)/(T1-t1)
=0.113
Ft=0.976
ΔTm=0.967×41.72= 38.684°K
Ud =100 W/m2K
APPROXIMATE AREA
A=Q/Ud× ΔTm
=40.35m2
TUBE SPECIFICATIONS
Thickness = 16 BWG
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Production of Cyclohexane from Benzene
No of Tubes A/a=139
= ( 0.016× 63752)/2.37
= 5425.70
hi = [4200(1.35+0.02t)]/ID0.2
= 4877.57W/m2K
=4107.43W/m2K
FLOW AREA
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Production of Cyclohexane from Benzene
= (0.387×0.004×0.205 )/0.024
= 0.011 m2
MASS VELOCITY
Mass velocity
= 1669/0.011
= 151727kg/hr.m2
(De )= 0.0139 m
Reynold’s Number
= (0.0139×151727)/1.88
= 24434.5
Jh = 90
Prandtl Number
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Production of Cyclohexane from Benzene
Pr = Cpμ/k
= (2.186×1.88 )/0.104
=1.3
= [90×0.104×(1.3)1/3]/0.0139
= 876.23W/m2 K
= 742W/m2K
ACTUAL AREA Ac
=40.70m2
CORRECTED Ud
= (156×103)/(40.70×38.684)
= 99.15 W/m2K
DIRT FACTOR
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Production of Cyclohexane from Benzene
Dirt factor
=0.0087 W/m2K
Gs = 42.27kg/sec .m2
= 741.98N/m2
Length L = 4.88m
n=139
Gt = 177kg/sec.m2
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Production of Cyclohexane from Benzene
=239.45 N/m2
101
Production of Cyclohexane from Benzene
SPECFICATION SHEET
P Position Horizontal
1
N No. of Shell Passes 11
hi 4 4877.57W/m2K
ho 8 876.23W/m2 K
Chapter # 5
MECHANICAL DESIGN
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Production of Cyclohexane from Benzene
SHELL SIDE
SHELL THICKNESS
ts=Shell thickness =?
P=Design Pressure=1.51N/mm2
So ts =3.65
ts =3.65+4
=7.65mm
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Production of Cyclohexane from Benzene
A =m/�v= 0.011m2
Dn = 118mm
NOZZLE THICKNESS
C = Corrosion allowance
=5.11mm
HEAD THICKNESS
W= 1.7706
105
Production of Cyclohexane from Benzene
th = 7.270mm
Db = Ds -4.8
=382.2mm
TUBE SIDE
No. of Passes = 2
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Production of Cyclohexane from Benzene
= 0.0125m2
Dn = 126.18mm
NOZZLE THICKNESS
tn = 0.51
tn = 0.51+4
= 4.51mm
Chapter # 6
INSTRUMENTATION &
PROCESS CONTROL
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Production of Cyclohexane from Benzene
INSTRUMENTS
Instruments are provided to monitor the key process variable during plant operation. They
may be incorporated in automatic control loops or used for manual monitoring of the
process operation. They may also be a part of an automatic computer data logging system
.Instruments monitoring critical process variable will be fitted with automatic alarm to alert
the operator to critical and hazardous situation.
The primary objective of the designer when specifying instrumentation and control schemes
are:
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Production of Cyclohexane from Benzene
These are not separate objectives and must be considered together. The
order in which they are listed is not meant to imply the precedence of any
objective over another, other than that of putting safety first. Product
quality, production rate and the cost of production will be dependent on
sales requirements. For example, it may be a better strategy to produce a
better quality product at a higher cost.
In a typical chemical processing plant these objective are achieved by
combustion of automatic control, manual monitoring and laboratory
analysis.
Process
Any operation or series of operations that produces a desired final result is a process. In this
distillation the process is the cracking of Naphtha.
Measuring Means
Of all the parts of the control system the measuring elements is perhaps the most important.
If measurement is not made properly the remainder of the system cannot operate
satisfactorily. The available is dozen to represent the desired condition in the process.
Variable to be Recorded
Controller
The controller is the mechanism that responds to any error indicated by the error detecting
mechanism. The output of the controller is some predetermined function of the error.
In the controller there is also and error detecting mechanism which compares the measured
variable with desired value of the measured variable, the difference being the error.
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Production of Cyclohexane from Benzene
The final control element receives the signal from the controller and by some predetermined
relationship changes the energy input to the process.
CLASSIFICATION OF CONTROLLER
In general the process controllers can be classified as:
a) Pneumatic controllers
b) Electronic controllers
c) Hydraulic controllers
In the ethylene manufacturing from naphtha the controller and the final control
element may be pneumatically operated due to the following reasons:
i) The pneumatic controller is vary rugged and almost free of maintenance. The
maintenance men have not had sufficient training and background in electronics,
so basically pneumatic equipment is simple.
iii) Transmission distances are short. Pneumatic and electronic transmission system
are generally equal upto about 250 to 300 feet. Above this distance, electronic
systems begin to offer savings.
MODES OF CONTROL
The various type of control are called "modes" and they determine the type of
response obtained. In other words these describe the action of the controller that is the
relationship of output signal to the input or error signal. It must be noted that it is error
that actuates the controller. The four basic modes of control are:
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i) On-off Control
i) A sensor to monitor the control variable and provide an output signal when a
preset valve is exceeded (the instrument).
ii) A link to transfer the signal to the actuator usually consisting of a system of
pneumatic or electric relays.
iii) An actuator to carry out the required action; close or open a valve, switch off a
motor. -
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INTERLOCKS
Where it is necessary to follow the fixed sequence of operations for example, during a
plant start-up and shut-down, or in batch operations-inter-locks are included to prevent
operators departed from the required sequence. They may be incorporated in the control
system design, as pneumatic and electric relays or may be mechanical interlocks.
Temperature Controller
Thermocouples are the most commonly used temperature sensing devices. The two
dissimilar wires produce a millivolt emf that varies with the "hot-junction" temperature.
Iron constrictant thermocouples are commonly used over the 0 to 1300°F temperature
range.
Pressure Controller
Bourdon tubes, bellows, and diaphragms are used to sense pressure and differential
pressure. For example, in a mechanical system the process pressure force is balanced by
the movement of a spring. The spring position can be related to process pressure.
Level Controller
Liquid levels are detected in a variety of ways. The three most common are:
Following the position of a float, that is lighter them the fluid.
Measuring the apparent weight of a heavy cylinder as it buoyed up more or less
by the liquid (these are called displacement meters).
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Measuring the difference in static pressure between two fixed elevations, one in
the vapour above the liquid and the other under the liquid surface. The differential
pressure between the two level taps is directly related to the liquid level in the
vessel.
Transmitter
The transmitter is the interface between the process and its control system. The job of the
transmitter, is to convert the sensor signal (millivolts, mechanical movement, pressure
differential, etc.) into a control signal 3 to 15 psig air-pressure signal, 1 to 5 or 10 to 50
milliampere electrical signal, etc.
Control Valves
The interface with the process at the other end of the control loop is made by the final
control element is an automatic control valve which throttles the flow of a stem that open
or closes an orifice opening as the stem is raised or lowered. The stem is attached to a
diaphragm that is driven by changing air-pressure above the diaphragm. The force of the
air pressure is opposed by a spring.
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Chapter # 7
HAZOP STUDY
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 and 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.
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1) To identify areas of the design that may possess a significant hazard potential.
2) To identify and study features of the design that influence the probability of a
hazardous incident occurring.
6) To provide a mechanism for feedback to the client of the study team's detailed
comments.
Intention
Deviation
Causes
Consequences
Hazards
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These guide words are applied to flow, temperature, pressure, liquid level,
composition and any other variables affecting the process. The consequences of these
deviations on the process are then assessed and the measures needed to detect and correct
deviations are established.
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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.
3) Collect data. Theodore16 has listed the following materials that are usually
needed:
Process description
Process flow sheets
Data 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
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.
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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.
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.
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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 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.
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Chapter # 8
ENVIRONMENTAL IMPACTS
OF CYCLOHEXANE PLANT
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Cyclohexane evaporates when exposed to air. It dissolves 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.
We can, in brief asses the impacts of cyclohexane producing plant in the following
major areas of ecology and sociology.
HUMAN HEALTH
Cyclohexane is not a highly toxic chemical. For 600 to 700 ppm exposure, no chronic
effects have been observed. The recommended threshold limit for cyclohexane is 300
ppm by volume. Exposure time is also important. Usually several days are needed, for
both human and animals, to cause any problem at these ppms.
A. Pharmacokinetics
microscopic changes in the liver and kidneys. Systemic toxicity observed in animals
exposed orally to cyclohexane indicates that gastro- intestinal absorption of the chemical
also occurs. In workers exposed to atmospheric cyclohexane, 22.8% of the total
respiratory intake was absorbed, and a "significant amount" of the absorbed cyclohexane
was either retained or metabolized.
B. Acute Effects
Cyclohexane has low acute toxicity, producing eye irritation in humans and
neurological symptoms , other organ effects, and death in animals at very high doses.
2. Animals - The oral LD50 for cyclohexane in rats ranges from 8.0 to 39 mL/kg
(both greater than 5 g/kg), depending upon the age of the animals. The oral LD50 for
mice is 1.3 g/kg; the minimum lethal oral dose in rabbits is 5.5-6.0 g/kg; and the dermal
LD50 in rabbits is >180 g/kg. Within 1 to 1.5 hours, lethal doses to animals produced
severe diarrhea, vascular damage and collapse, hepatocellular degeneration and toxic
glomerulonephritis. Exposure of rabbits to 3330 ppm (duration not given) produced no
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effect; 18,500 ppm for 8 hours was non-lethal; and 26,600 ppm for 1 hour was lethal.
Application of 1.55 g/day of cyclohexane to the skin for 2 days produced minimal
irritation.
C. Subchronic/Chronic Effects
D. Carcinogenicity
E. Genotoxicity
Cyclohexane was negative for viral enhanced cell transformation in Syrian hamster
embryo (SA7/SHE) cells and for histidine reverse gene mutation in Salmonella
typhimurium.
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F. Developmental/Reproductive Toxicity
G. Neurotoxicity
The central nervous system is a major target organ for the toxicity of cyclohexane.
High concentrations of the chemical produce various effects, ranging from trembling to
death.
2. Animals - Mice exposed to 50 mg/L (14,500 ppm) for 2 hours exhibited minimal
narcotic effects. Exposure to 18,000 ppm produced trembling within 6 minutes,
disturbed equilibrium within 15 minutes, and completes recumbency within 30 minutes.
Cyclohexane caused an excitation of the vestibulo-oculomotor reflex (threshold blood
level, 1.1 mmole/L). Concentrations of ò7445 ppm, 6 to 8 hours/day for 2 to 26 weeks
were lethal to rabbits, producing convulsions, tremors, narcosis, and paresis of the legs.
LAND
In the plant erection and installation stage, extensive damages to the land may
take place. Various concrete and metal dumping and digging etc. are major costs.
In plant operation, chemical leakages and certain solids dumping may impart
effects on land, along with the social activities impacts of plant people.
WATER POLLUTION
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Water is extensively used for cooling and for other purposes in the plant, so water level
of locality and surface concentrations of various salts may disturb.
TLm values for fish range from 32 to 57.7 mg/L, indicating that the chemical is
moderately toxic to aquatic organisms in acute tests. Cyclohexane is expected to be of
low toxicity to terrestrial organisms and has a smog-forming potential.
TLm values for fish (24-96 hr) are 43-32 mg/L (Pimephales promelas, fathead
minnow), 43-34 mg/L (Lepomis macrochirus, bluegill). Mussel larvae (Mytilus edulis)
exposed to 1 to 100 ppm (mg/L) cyclohexane exhibited a 10-20% increase in growth rate.
The threshold concentration of cyclohexane in the cell multiplication inhibition assay,
measured in the protozoa Uronema parduczi Chatton-Lwoff, was >50 mg/L.
Based on the low toxicity of cyclohexane to laboratory animals, the toxicity of the
chemical to terrestrial animals is expected to be low.
C. Abiotic Effects
AIR POLLUTION
Purge from the plant can be burned in boiler furnace but blow-downs and
fugitive emissions (form valve etc.) may pollute air, similarly high temperatures involved
may also warm the atmosphere.
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CULTURAL ACTIVITIES
Extensive cultural activities are involved in erection and production phases of the
project. Also a lot of economical activity is involved. These can affect cultural, social and
morale of the people involved.
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Chapter # 9
MATERIAL OF
CONSTRUCTION
Any engineering design, particularly for a chemical process plant, is only useful when it
can be translated into reality by using available materials of construction combined with
the appropriate techniques of fabrication can play a vital role in the success or failure of a
new chemical plant.
Although many materials have greater corrosion resistance than iron and steel cost
aspects favor the use of iron and steel. As a result they are often used as a material of
construction when it is known that some corrosion will occur. If this is done the
presence of iron salts and discoloration in the product can be expected and periodic
replacement of the equipment should be anticipated. In general, cost of iron and
carbon steel exhibit about the some corrosion resistance. They are not suitable for use
with dilute acids, but can be used with many strong acids; since a protective coating
composed of corrosion products forms on the metal surface.
2) Stainless Steel
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There are more than 100 different types of stainless steels. The main reason for the
existence of stainless steels is their resistance to corrosion. Chromium is the main
alloying element, and the steel should contain at least 11%. Chromium is a reactive
element but it and its alloys passivate and exhibit excellent resistance to many
environments. A large number of steels are available. So stainless steel contains
chromium, nickel, iron, and also containing small amount of other essential properties.
They have excellent corrosion resistance and heat-resistance properties.
Nickel exhibits high corrosion resistance to most alkalies.' Nickel-clad steel is used
extensively for equipment in the production of caustic soda and alkalies. The strength
and hardness of nickel is almost as great as carbon steel. In general, oxidizing
conditions promote the corrosion of nickel, and reducing conditions retard it. Monel,
an alloy of nickel containing 67% nickel and 30% copper is often used in food
industries. This alloy is stronger than nickel and has better corrosion resistance
properties than either copper or nickel.
4) Copper
It has been the traditional metal in breweries for centuries, but with the advent of new
alkaline cleaner, some corrosion problems have occurred. Copper and copper base
alloys are used in the formation of heat exchanger tubing, piping, fittings, etc.
Although the corrosion rates are comparatively high. In the range from room
temperature upto 100°C, the corrosion rate of copper is comparatively small.
However, the corrosion rate of 100°C is about five times that which takes place at
room temperature.
5) Aluminium
The lightness and relative ease of fabrication of aluminum and its alloys are factors
favoring the use of these materials. Aluminium resists attack by acids because a
surface film of inert hydrated aluminium oxide is formed. This film adheres to the
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surface and offers good protection unless materials which can remove the oxide, such
as hydrogen acids or alkalies are present.
6) Lead
Pure lead has low creep fatigue resistance, but. its physical properties can be
improved by the addition of small amounts of silver, copper, antimony or tellurium.
Lead-clad equipment is in common use in many chemical plants. Lead shows good
resistance to sulfuric acid and phosphoric acid but it is susceptible to attack by acetic
acid and nitric acid.
7) Hastelloy
8) Coatings
Breweries are large consumer of quality coatings, not only for tankage but also for
structural steel, flooring and other working areas. The coating used range from high
heat silicones for stacks to special super resistant grouts for floor pavers.
8) Floor Materials
Considerable giazod tile is used in breweries and special expoxies with good
adhesion to very smooth surfaces have employed to coat glazed ceramic tile in order
to prevent crazing (cracking). Bacterial contamination deep in the pores of the
concrete is a common occurrence. If floors are not properly sealed, corrosion of
concrete rebars and structural steel can result, with eventual cracking and spalling of
concrete.
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10) Plastics
For corrosion control point of view, plastics materials are very useful, therefore
they have found application in breweries, water treatment tanks, acid storage, roofing,
and gutters are application for plastics that are common to most industrial activity.
Fiberglass and polyvinyl chloride are among the plastics that have been employed. Small
polypropylene tanks for yeast culture and other specialty service have some record of use.
EQUIPMENT MATERIAL OF
CONSTRUCTION
Storage tank for benzene Carbon steel
Storage tank for cyclohexane Carbon steel
Slurry hydrogenation reactor 316L Stainless Steel
Fixed Bed Cyclohexane Reactor 316L Stainlees Steel
Gas/Liquid Separator Carbon Steel
Stabalization Column Carbon Steel
Chapter # 10
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COST ESTIMATION
An acceptable plant design must present a process that is capable of operating under
conditions which will yield a profit.
It is essential that chemical engineer be aware of the many different types of cost
involved in manufacturing processes. Capital must be allocated for direct plant expenses;
such as those for raw materials, labor, and equipment. Besides direct expenses, many
other indirect expenses are incurred, and these must be included if a complete analysis of
the total cost is to be obtained. Some examples of these indirect expenses are
administrative salaries, product distribution costs and cost for interplant communication.
STORAGE TANK
PUMPS
COMPRESSORS
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HEAT EXCHANGERS
VESSELS
STABALIZER (V-03)
Indirect Cost
Engineering & supervision = 1.514x106 rupees
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REFERENCES
1) Ludwig, E.E, “Applied Process Design”, 3 rd ed, vol. 2, Gulf Professional Publishers,
2002.
2) McKetta, J. J., “Encyclopedia of Chemical Processing and Design”, Executive ed, vol. 1,
Marcel Dekker Inc, New York, 1976.
4) Kuppan, T., “Heat Exchanger Design Hand Book, Marcel Dekker Inc., New York, 2000.
5) Levenspiel, O., “Chemical Reaction Engineering:, 2nd ed, John Wiley and Sons Inc.,
1972.
7) Peters, M.S. and Timmerhaus, K.D., “Plant Design and Economics for Chemical
Engineering”, Fourth ed, McGraw Hill, 1991.
8) Bockhurst, J.F. and Harker, J.H, “Process Plant Design”, Heinemann Educational Books
Ltd, 1973.
10) Coulson, J.m., and Richardson, J.F., “Chemical Engineering”, 4 th ed, Vol.2, Butterworth
Heminann, 1991.
12) Charles G.Hill,JR, “An Introduction to Chemical Engineering kinetics & reactor design”
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13) Peacock, D.G., “Co ulson & Richardson’s Chemical Engineering”, 3rd ed, vol,
Butterworth Heinenann, 1994.
14) Sinnot, R.K., “Coulson and Richardson’s Chemical Engineering”, 2nd ed, vol 6,
Butterword Heinemann, 1993.
15) Kern, D.Q., “Process Heat Transfer”, McGraw Hill Inc., 2000.
16) McCabe, W.L, “Unit Operations of Chemical Engineering”, 5th Ed, McGraw Hill, Inc,
1993.
17) Perry, R.H and D.W. Green (eds): Perry’s Chemical Engineering Handbook, 7th edition,
McGraw Hill New York, 1997.
18) Philip Hall Howard. “Handbook of Environmental Fate and Exposure Data for Organic
Chemicals”.
19) Clement Thomon,Senie-at-Oise,( to Institute of Francaise du
petrol),U.S. Patent 3,202,723, Aug.24 1965.
20) Maurice Stewart, Emulsion and Oil Treating Equipments,vol.5;Gulf
Professional Publishers,1972.
21) Kohl,L. and Richard Nelson, B., Gas Purifications, vol.5; Gulf
Professional Publishers,1997.
22) Walas.S M.,Chemical Process Equipment Selection and Design,Reed
Publishers, 1998.
23) Richardson.J.F & Coluson,J.M., Chemical Engineering,
vol.6;McGraw Hill, New York, 1997.
24) Ernest,L.E., Applied Process Design For Chemical And
Petrochemical Plants,edit.3;vol.2; Gulf Professional Publishers.
25) Richardson.J.F & Coluson,J.M., Chemical Engineering,
vol.6;McGraw Hill, New York, 1997.
26) Ernest,L.E., Applied Process Design For Chemical And
Petrochemical Plants,edit.3;vol.2; Gulf Professional Publishers.
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APPENDIX
Figure 4.1
Figure 4.2
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Figure 4.3
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Figure 4.4
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