Production of Cyclohexane From Benzene

Production of Cyclohexane from Benzene
Session 2005-2009
Project Advisor
Prof. Dr. Shahid Naveed
Authors:
Zaeema Tahir
2005/FC-CPE-10
Sidra-tul-Muntaha
2005/FC-CPE-18
Ahmad Waqas
2005/FC-CPE-16
Usman Hameed
2005/FC-CPE-03
DEPARTMENT OF CHEMICAL ENGINEERING

U.E.T - LAHORE -PAKISTAN
This report is submitted to department of Chemical

Engineering, University of Engineering & Technology
Lahore- Pakistan for the partial fulfillment of the
requirements for the
Bachelors Degree
In
CHEMICAL ENGINEERING
Internal Examiner:
Sign:_____________
Name:______________
External Examiner
Sign:_______________
Name:_______________
DEPARTMENT OF CHEMICAL ENGINEERING

UNIVERISITY OF ENGINEERING AND TECHNOLOGY
LAHORE-PAKISTAN
DEDICATED TO
Our
Beloved Parents,
Respected Teachers
And
Sincere Friends
ACKNOWLEDGEMENT
We express gratitude and praise to ALMIGHTY
ALLAH, the creator of universe, who is beneficent and merciful,
guided us in difficult and congeal circumstance, who endowed
us with the will to undertake this design project. Great respect
our Holy Prophet Hazrat Muhammad (PBUH), who taught us to
learn till lap of grave.
At this point, the end of a purposeful learning period,
our emotions are very strong, feelings are deep, and we are still
remembering the time when our dreams came true and we
came at U.E.T, a dynamic institution with professionals loving
and professional making setup.
The time which was spend over here, the practical
and conceptual knowledge which we gained made this golden
time, of course, a milestone in our professional career with the
name of department of chemical engineering a long list of polite
cooperative and affectionate professional teachers came across
our mind. For whom we confess our negligence of vocabulary to
say thanks for their assistance.
We pay special homage to our respective teachers; Dr.

Saleemi (Chairman of Department) and our lenient and
cooperative project advisor Prof. Dr.Shahid Naveed, who really
paid their special attention in the completion of our project.
TABLE OF CONTENTS
PREFACE.......................................................................................................................................
CHAPTER 1......................................................................................................................................
Introduction................................................................................................................................
CHAPTER 2......................................................................................................................................
Process selection and description of flow sheet.....................................................................
CHAPTER 3......................................................................................................................................
Material balance & Energy balance.......................................................................................
CHAPTER 4......................................................................................................................................
Design of Equipments..............................................................................................................
Reactor design ..................................................................................................................
Vapor/liquid separator design............................................................................................
Stabilization column design..........................................................................
Heat Exchanger design.................................................................................
CHAPTER 5......................................................................................................................................
Mechanical Design of Heat Exchanger................................................................................
CHAPTER 6......................................................................................................................................
Instrumentation and Process control...................................................................................
Control scheme of Outer-recirculation Cooler.................................................................
CHAPTER 7......................................................................................................................................
HAZOP Study ........................................................................................................................
HAZOP Study of Gas/Liquid Separator..............................................................
CHAPTER 8......................................................................................................................................
Environmental impacts of Cyclohexane Plant.....................................................................
CHAPTER 9.....................................................................................................................................
Material of Construction.......................................................................................................
CHAPTER 10....................................................................................................................................
Cost Estimation .....................................................................................................................
REFERENCES..........................................................................................................................
APPENDIX.................................................................................................................................
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.
Cyclohexane is the major pre-cursor for the production of Nylon. Automotive
applications of nylon have been growing strongly where there has been a drive to replace
metals with plastics to reduce the weight of motor. Hence it will a cost effective solution
in this sector also.
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.
The basic structure of report is given below.
Chapter # 1 is the introduction of cyclohexane that covers the areas of demand of it in
present days and as well as in future. A brief view of natural resources and physical
properties has been given. The properties of benzene and hydrogen have been given
where ever their need is. Important Industrial applications and discovery of this chemical
has also been given.
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
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 # 4 is the Design of Equipments in which operating conditions, process
conditions and Design of equipments has been given in details. The conventional design
of each equipment has been preferred on the complex designing procedures. Authors
have made efforts to their level best to make all the equipments economical and easy to
handle for plant personnels.
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.
Chapter # 6,7,8.9 and 10 covers Mechanical design, Hazop study, Environmental
impacts of cyclohexane, Material of construction and Cost estimation respectively.
The contents of these chapters give an over view of the respected subject. There is no
such detail demanded in this report.
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
has been collected from various books and simulation software Hysys at the process
conditions.
Finally, as is customary, the errors that remain are our.
The Authors
Zaeema Tahir
Sidra-tul-muntaha
Usman Hameed
Waqas Ahmed
Chapter # 1
3
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
plant in May 2006 although production could be increased to180,000 tonnes/year

depending on feedstock availability.
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
Cyclohexane, C6H12, formula weight 84 is a colorless, water-insoluble, noncorrosive liquid. It is an excellent solvent for cellulose ethers, resins, fats, waxes, oils,
bitumen and crude rubber. The main use is as an intermediate in the manufacture of
nylon.
Table 1.1
Cyclohexane
Solvent Properties
CAS 110-82-7
Physical Properties
Molecular weight
84.16
Boiling point
80.72C
Vapor pressure
77.5 Torr at 20C
Freezing point
6.54C
Refractive index
1.4262 at 20C
Density
0.7785 g/mL (6.497 lb/gal) at 20C

0.7739 g/mL (6.457 lb/gal) at 25C
Dielectric constant
2.02 at 20C
Dipole moment
0 D at 20C
Polarity index (P')
0.2
Viscosity
1.0 cP at 20C
Surface tension
24.98 dyn/cm at 20C
Solubility in water
0.006% at 25C
Solubility of water in cyclohexane
0.01% at 20C
Storage
Store in an area designed for

flammable storage, or in an approved
metal cabinet, away from direct
sunlight, heat and sources of ignition.
Flash point
-4F (-20C) by closed cup
Lower explosive limit
1.3%
Upper explosive limit
8.0%
HISTORY
In 1867 Marcellin Berthelot reduced benzene with hydroiodic acid at elevated
temperatures. He incorrectly identified the reaction product as n-hexane not only because
of the convenient match in boiling point (69C) but also because he did not believe
benzene was a cyclic molecule (like his contemporary August Kekule) but rather some
sort of association of acetylene. In 1870 one of his sceptics Adolf von Baeyer repeated
the reaction and pronounced the same reaction product hexahydrobenzene and in 1890
Vladimir Markovnikov believed he was able to distill the same compound from Caucasus
petroleum calling his concoction hexanaphtene
In 1894 Baeyer synthesized cyclohexane starting with a Dieckmann condensation of
pimelic acid followed by multiple reductions:
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.
Surprisingly their cyclohexanes boiled higher by 10C than either hexahydrobenzene or

hexanaphtene but this riddle was solved in 1895 by Markovnikov, N.M. Kishner and
Nikolay Zelinsky when they re-diagnosed hexahydrobenzene and hexanaphtene as
methylcyclopentane, the result of an unexpected rearrangement reaction.
INDUSTRIAL APPLICATIONS
7
1-Commercially most of cyclohexane produced is converted into cyclohexanone.

Cyclohexanone is the organic compound with the formula 5CO. The molecule consists of
six-carbon cyclic molecule with a ketone functional group. This colorless oil has an
odour reminiscent of pear drop sweets as well as acetone.
2-Cyclohexanol (or "KA oil") is the organic compound and is formed by
catalytic oxidation. KA oil is then used as a raw material for adipic acid. Adipic acid is
the organic compound with the formula 4(CO2H) 2. From the industrial perspective, it is
the most important dicarboxylic acid: About 2.5 billion kilograms of this white
crystalline powder are produced annually, mainly as a precursor for the production of
nylon.
3-Cyclohexane is also an important organic solvent.
Also it is used in Electroplating , Electroplating - Vapor Degreasing Solvents, Laboratory
Chemicals, Solvents Extraction, Machinery Mfg and Repair , Rubber Manufacture,
Solvents - Rubber Manufacture, Wood Stains and Varnishes
STRUCTURE
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
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
PROCESS SELECTION &

DESCRIPTION OF FLOW
SHEET
Commercially cyclohexane is synthesized by various processes. Each process has its
own merits and demerits. Categorizing various processes we can differentiate among
them on following characteristics;
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
Liquid phase or vapor phase
Type of metal used
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
II.
exchangers; however, this solution requires considerable equipment.

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.
LIQUID PHASE PROCESSES

10
TABLE 2.1
Process Name
Operating cond.
Catalyst
Heat Removal
UPO (Universal oil
Temp: 200 - 300C
Fixed bed of of
Quenching shots from
Press: 3xl0 Pa abs
pt
Pt based catalyst
cooled reactor effluent
Temp: 160 - 235C
Pt-based catalyst
Three reactors in
Press: several atms
in fixed beds.
series; 1st treats bulk of
products) Hydrar
process
Houdry Process
feed and recycle, ,

2nd treats effluent from
1st, remainder feed and
recycles. Adiabatic
operation.
Sinclair/engelhard
Temp; 250C
process
Noble
metal
fixed bed.
Heat is removed in
Situ by means of a tube
bundle with the
production of steam
IFP (Institut
Temp: 200 - 240C
Raney 'Nickel in
Outer- recirculation
Francais du Petrole)
Press: 35 atm
Suspension
Heat removal.
VAPOR PHASE PROCESSES

Table 2.2
Process Name
Operating cond. Catalyst
Heat Removal
Bexane DSM:
Temp. 370C
By a coolant
Pt-based catalyst
11
Nederlandse
Pressure 3xl06pa
abs
Hytoray Process
Temp. 370C
Pressure 3xl06pa abs
Pt-based
By a coolant
catalyst
SELECTED PROCESS FOR CYCLOHEXANE

MANUFACTURE
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.
The main features of this process are given below;
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
(I)
BASIC CHEMISTRY
The hydrogenation of benzene proceeds according to:

12
C6H6 +3H2
C6H12
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.
(II)
REACTION KINETICS
The kinetics are first order in hydrogen partial pressure, zero order of benzene, and
independent of the pressure of cyclohexane.
PROCESS DESCRIPTION & PROCESS FLOW DIAGRAM

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 160C 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
overheads of low pressure flash are 95% hydrogen which is used as fuel gas or mixed
with sales gas.
14
HYDROGENATION CATALYSTS
1.
FOR LIQUID PHASE

15
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 < 100C. 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.
SLURRY CATALYST SYSTEM

Particle size
Density of cat.
Conc.in solution
150 A
8:9 g/cc.
0.07%.
2. VAPOR PHASE CATALYST

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:
Diameter of pellet, Dp =60m
16
Specific surface, Sg
=278m2/g
Specific Volume, Vg
=0.44cm3/g
Density of catalyst, pg =2.63g/cm3

Density of pellet, pp
=2.24g/cm3
=29oA
REACTION CONDITIONS SELECTION

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.
At 260oC, thermal cracking of benzene begins.

At 248oC, isomerization of cyclohexane to methyl cyclopentane begins.
So upper temperature range is 248.88oC

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
260
7.10
315
7.03 x 10-2.
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
High pressure i.e., 35 atmosphere" is chosen due to following reasons.
(i)
At 204C, the vapor pressure of benzene is very high, so to get

a liquid phase reaction, high pressure must be specified.
(ii)
The expression for equilibrium constant for this reaction is

K =
[C6H12]
[E/]3
[C6H6][H2]3
Where = pressure in atmospheres absolute.

The expression shows clearly that higher Pressure favours higher
C6 H12 yield.
(iii)
The stoichiometric equation for reaction is
C6H6 + 3H2
C6H12
According to Le' chattier principle, high pressure will favour more benzene
inversion.
SELECTION OF HYDROGEN TO BENZENE RATIO
18
A table is given below which shows the impact of H2/Bz ratio on reaction
conversion at 204 C.
Table 2.4
Temperature
H2/Bz
% Excess
Benzene Concentration
(OC)
(Mol/Mol)
Hydrogen
204
11700 ppm.
204
3.03
1.0
5350 ppm.
204
3.15
5.0
205 ppm.
204
3.75
25.0
6 ppm.
204
6.00
100.0
1ppm.
204
0.5 ppm.
Our choosen conversion is 99.998% equivalent to 510 ppm equilibrium benzene so 25% excess benzene
is used.
ASSUMPTIONS AND THEIR JUSTIFICATION

1.
All the sulfur in benzene feed is converted to H2S.

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
3.
Steady state equimolar flow of cyclohexane (vapor and liquid) is assumed in

stabilizer because both streams are fed when they are saturated.
4.
For some heat exchangers, average transfer coefficients are used which are
justified for preliminary design.
RECOMMENDED DESIGN CAPACITY

Data taken from Lahore Chamber Of Commerce for the import of cyclohexane in
Pakistan is in the range of batch operation to make it in continuous operation range the
minimum capacity is 40 tons/day so we have selected it. Continuous processes are less
expensive and product cost per unit of time is less than batch operations.
The final purity of product is 99.98% that is suitable to market.
GENERAL DISCUSSION ON DESIGN

When
one
sees
the
design
results,
two
prominent
features
are
highlighted.
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
Chapter # 3
MATERIAL BALANCE &

ENERGY BALANCE
MATERIAL BALANCE
Basis
40 tons (19.84 Kg mole/ hr or 1668.56 kg / hr) per day of cyclohexane
21
Bz
1
:
:
H2
3.75
(in mol fraction )
REACTION
C6H6 + 3H2
C6H12
From Encyclopedia
Product composition: (wt. basis)
C.H.
0.9988
M.C.P.
0.00022
Benzene
10 ppm
Impurities (CH4 + C2H6 etc) =

Total
0.001
1.00
Benzene Feed Composition (Wt. basis)

Benzene
0.9978
C.H.
0.00016
M.C.P.
0.00012
Impurities
0.00057
Sulfur
0.5 ppm
Total
1.00
Hydrogen Feed Composition

22
(Wt. basis)
(Mol basis)
H2
0.9111
0.98798
C02
0.0002
0.00001
CO
CH4
0.08853
0.012
TOTAL
1.00
1.00
0.00013
0.00001
BALANCE ACROSS REACTOR (R-O1)
R-O1
Components
Benzene
Cyclohexane
M.C.P.
Impurities
In (Kg/hr)
1548.80
0.3
0195
1.00.
Out (Kg/hr)
78
1583.6
0.4
1.7
23
Sulfur
Hydrogen
Carbon dioxide
Carbonmonoxide
Methane
Total
Temp (C)
Trace.
150
0.06
0.04
25
1725
204.4
Trace
36
0.06
0.04
25
1725
204.4
Press (atm)
35
34.625
BALANCE ACROSS REACTOR (R-O2)
R-O2
Components
Benzene
Cyclohexane
M.C.P.
Impurities
Sulfur
Hydrogen
Carbon dioxide
Carbonmonoxide
Methane
Total
In (Kg/hr)
78
1583.6
0.4
1.7
Trace
36
0.06
0.04
25
1725
Out (Kg/hr)
0.02
1667
0.4
1.7
Trace
30
0.06
0.04
25
1725
24
Temp (C)
204.4
273
Press (atm)
34.625
33.6
BALANCE ACROSS FLASH DRUM (V-O1)
V-O1
Components
In (Kg/hr)
Benzene
Cyclohexane
M.C.P.
Impurities
Sulfur
Hydrogen
Carbon dioxide
1.7
1666.545
0.4
1.7
Trace
30
0.06
Carbonmonoxide
0.04
Methane
26.0
Liquid
0.02
1666.5
0.4
1.7
0.498
610x6.6
6-
10x4.2
3-
10x3
Out (Kg/hr)
Purge
16
0.03
Recycle
13.25
0.025
0.02
0.0167
13.14
11.5
Total
1725
1669
30
BALANCE ACROSS STABILIZATION COLUMN (V-O2)
25
25
V-O2
Components
In (Kg/hr)
Benzene
Cyclohexane
M.C.P.
Hydrogen
Carbon dioxide
0.02
1666.5
0.4
0.996
610x6.6
Carbonmonoxide
Methane
Total
6-
Out (Kg/hr)
Bottoms
Overheads
-3
5.18X10
0.01482
1666.5
0
-4
3.6x10
0.3996
0.0258
0.9702
60
10x6.6
10x4.2
3-
10x3
1669
1666.53
6-
10x4.2
3-
10x3
1.3876
OVERALL MATERIAL BALANCE
26
27
ENERGY BALANCE
LATENT HEAT OF VAPORATION:Watson Equation;
Lv = Lvib [ (Tc T)/(Tc Tb) ]0.38
Where;
T=
Temperature (OF)
Tc =
Critical temperature for cyclohexane
996 R.
Tb =
=
Boiling point, for cyclohexane

636.36 R
HEAT OF REACITON:C6H6 + 3H2

(1)
C6H12
(g)
(g)
[Sum of products Heat of formation] [Sum of products Heat of formation] =Heat of

reaction
[- 29430] - [11720 + 0] = -74135.32 btu/lb-mol
SPECIFIC HEAT OF CYCLOHEXANE VAPORS:From537 R to 960 R
C0p = (1.8)
(-7.701 +125.675xl0-3 T- 41.58x10-6 T-2) dt (1.8)
dt
Cp =
37.15 Btu/lb mol. F

28
Cp = 154.43 kJ/ kg-mol. K

Critical pressure
= 588 psia
Critical temperature
= 996 R
Reduced Pressure,Pr
= 0.87
Reduced temperature,Tr = 0.96.

Cp - Cp
= 9.6 x 10-6
Specific Heat,Cp
= 37.15 Btu/lb mol. F
Specific Heat,Cp
=155.5 kJ/ kg-mol.K
SPECIFIC HEAT OF HYDROGEN:Cpo =
(6.52+0.78xl0-3T+0.l2xl05 T-2)dt
= [(6.52 T +0.78x10-/23T2 -0.12x105 /T ) ]
dt
[960-537]
Cp = (1532.2 + 76.16 + 17.754)/235

= 6.92 Btu / lb-mol-oF
=28.96 kJ/ kg-mol.K
SPECIFIC HEAT OF LIQUID BENZENE:a, Cp at 77 F =
0.45 Btu / lb-mol-oF
b, Cp at 400 F=
0.6 Btu / lb-mol-oF
c, Cp
(0.6-0.45)/(400-77)
29
4.644xl0-4 Btu / lb-mol-oF
Specific heat, Cp =
(a + ct)dt
Specific heat, Cp = [
0.45dt +
dt
4.644/2x10-4 Tdt] [400-77]
43.74 Btu/lb mol F
183.09 kJ/ kg-mol. K
SPECIFIC HEAT OF LIQUID CYCLOHEXANE:Average Temperature =
Reduced Temp.,Tr
Accentric factor ,
434K
0.784
0.214
Cp, vapor heat capacity = -7.701 + 125.675 x 10-3 (434)

- 41.584 x 10-6 (434)2
=
-7.701 + 54.543-0.02
46.824 Btu/lb mol. F

=
195 KJ/ kg-mol.K
Using Sternling and Brown relation:-
30
(Cp l - Cpo )/2 = (0.5 + 2.2 )[3.67 + 11.64(1-Tr)4 + 0.634(1-Tr)-1]

Where;
R = 2 Btu/ lb mol - F
(Cp l - Cpo )/2 = (0.971) [3.67 + 0.0253 + 2.935]
(Cp l - Cpo )/2 = 6.44
CpL = 59.7 Btu/ lb- mol F
= 248.17 KJ/ kg-mol. K
31
ENERGY BALANCE AROUND REACTORS:-
HR,77F + H PRODUCTS,500F - HREACTANTS,400F

1.
(A)
Hr,77
= 74135.32 Btu/lb mol (C.H.) F x 45.157 moles/hr = 337728.65 Btu/hr.
2.
HPRODUCT FROM 400 TO 500 F
Hp
= mCpT
= 45.157x37.15 Btu/lb mol - F (500-77) +36.21(500-77) (6.93)
= 709617 + 106145.632 = 815762.632 Btu/hr.
3.
H reactants from 77 to 400 F

32
HR =mCpT
= 45.45 moles/hr x 43.74 Btu/lb mol - F x (400 - 77) +
166.26 x 6.91 x (400-77)
= 1013052.4 Btu/hr.
Inserting in (A):
= -3347728.65 + 815762.632-1013052.4
= - 3.5 xlO6 Btu/hr.
So,
= 3.5 x 106 Btu/hr or 5.9 x 104 Btu/min.

5.9 x 10 Btu/min. has to be removed by outer circulation.
FIXED BED REACTOR OUT-LET TEMPERATURE:Conversion
98 % to 100%
Moles converted= 45.45 (0.02)

= 0.909 lb moles/hr.
Heat generated at 77 F = 67389 Btu/hr.
Inlet temperature
500 F
Assume adiabatic operation:
45.45 (-7.701+125.675x10-3 T)dt +
33.383(6.52+ 0.78x10-3T)dt
33
37438.33 = [-7.701(T2-533) +
(T22 5002)] (45.45) + [6.52(T2 500) +
(T22 5002)](33.38)
37438.33 = [-350T2 + 186555.57+2.856T22 811348l]
+ [217.66T2 - 116011.3 + 0.013 7/
-3698.66]
37438.33 = -132.34 T2 + 2.87 T22 - 744502.5
Hence;
2.87 T22 - 1 3 2 . 3 4 T 2 - 781940.82 = 37438.33
On solving the above quadratic equation, we get temperature in oF
T2 = 522.55 F
34
ENERGY BALANCE OF HEAT EXCHANGERS

ENERGY BALANCE OF OUTER RECIRCULATION COOLER:Item NO. E-01
PARAMETERS
STREAM STREAM
1
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
Inlet Enthalpy
kJ/kg
Oulet Enthalpy
kJ/kg
579
4169.7
520
191.9
907.4
Duty of exchanger (MJ/hr) 3094
3094
Inlet enthalpy = outlet Enthalpy

579+520=191.9+907
1099kJ/kg=1099KJ/kg
ENERGY BALANCE OF CONDENSER FOR CYCLOHEXANE

VAPORS:Item No. E-02
35
PARAMETERS
STREAM
STREAM
Cyclohexan
Water
PARAMETERS
e + Gas
STREAM
STREAM
Flow-rate (kg/hr)
1
1725
2
2478.5
cyclohexane
272.5
Water
26.7
1669
62
11603.2
149
CC
125
202
55.24
122.3
Outlet
Temperature(j/kgK)0C
Heat Capacity
125 3
3.6x10
65.6 3
4.19x10
Heat
(J/kg
Inlet Capacity
Enthalpy
kJ/kgK)
Inlet EnthalpykJ/kg
Oulet Enthalpy
kJ/kg
Outlet Enthalpy kJ/kg
Duty of exchanger
Duty
of exchanger (MJ/hr)
(MJ/hr)
3
3.0x10
891
515
378.563
474
1266
600
3
4.19x10
7.123
126.7
519.56
167.6
1266
600
Fluid Entering
Fluid
Entering
Inlet Temperature
Flow-rate
(kg/hr)
Outlet Temperature
Inlet
Temperature
Change
in temp.
Inlet Enthalpy = Outlet Enthalpy

891+7.123
= 519.56+378.563
898.123kJ/kg = 898.123 kJ/Kg
ENERGY BALANCE OF OVERHEAD CONDENSER:Item No. E-03
36
Inlet Enthalpy = Outlet Enthalpy

503+9.23
= 419.56+84.03
512.23kJ/kg = 512.59 kJ/Kg
ENERGY BALANCE OF PRODUCT COOLER:Item No. E-05
37
PARAMETERS
STREAM
STREAM
cyclohexane
Water
1669
8042.22
184
25
Outlet Temperature 0C
30
43
Fluid Entering
Flow-rate (kg/hr)
Inlet Temperature
Heat Capacity
(J/kg K)
3.0x103
4.19x103
Inlet Enthalpy
kJ/kg
233.52
41.9
200
75.42
723.85
723.85
Outlet Enthalpy
Inlet
kJ/kg
Duty of exchanger
(MJ/hr)
Enthalpy= Outlet Enthalpy

275.42=275.42(kJ/kg)
Chapter # 4
38
DESIGN OF EQUIPMENTS
REACTOR DESIGN
WHAT IS A REACTOR?
39
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
H = - 214 KJ/mole
Highly exothermic
Favored by low T & high ppH2
Side reactions
Isomerization
Impacts final product quality
Ring opening
Favored by high T
COMMON TYPES OF MULTIPHASE CATALYTIC

REACTORS
1. Fixed-bed Reactors
a. Packed beds of pellet or monoliths
40
b. Multi-tubular reactors with cooling

c. Slow-moving pellet beds
d. Three-phase trickle bed reactors
2. Fluid-bed and Slurry Reactors

a. Stationary gas-phase
b. Gas-phase
c. Liquid-phase
i.
Slurry
ii.
Bubble Column
iii.
Ebulating bed
SELECTION OF REACTOR TYPE

Slurry reactors are commonly used in situations where it is necessary to
contact a liquid reactant or a solution containing the reactant with a solid
catalyst. To facilitate mass transfer and effective catalyst utilization, the
catalyst is usually suspended in powdered or in granular form. This type of
reactor has been used where one of the reactants is normally a gas at the
reaction conditions and the second reactant is a liquid, e.g., in the
hydrogenation of various oils. The reactant gas is bubbled through the
liquid, dissolves, and then diffuses to the catalyst surface. Obviously mass
transfer limitations can be quite significant in those instances where three
phases (the solid catalyst and the liquid and gaseous reactants) are present
and necessary to proceed rapidly from reactants to products.
Satterfield has discussed several advantages of slurry reactors relative to other modes of
operation. They include the following.
1. Well-agitated slurry may be kept at a uniform temperature throughout,
eliminating "hot" spots that have adverse effects on catalyst selectivity.
41
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.
5. Continuous regeneration of the catalyst can be obtained by continuously
removing a fraction of the slurry from which the catalyst is then separated,
regenerated and returned to the reactor.
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.
A major deterrent to the adoption of continuous slurry reactors is the fact
that published data are often inadequate for design purposes. Solubilization
and mass transfer processes may influence observed conversion rates and
these factors may introduce design uncertainties. One also has the problems
of developing mechanical designs that will not plug up, and of selecting
carrier liquids in which the reactants are soluble yet which remain stable at
elevated temperatures in contact with reactants, products, and the catalyst.
A further disadvantage of the slurry reactor is that the ratio of liquid to
catalyst is much greater than in a trickle bed reactor. Hence, the relative
rates of undesirable homogeneous liquid phase reactions will be greater in
the slurry reactor, with a potential adverse effect on the process selectivity.
TYPES
42
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.
WHY BUBBLE SLURRY COLUMN REACTOR
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
SLURRY BUBBLE COLUMN REACTOR

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
solid suspension. These reactors are generally referred to as slurry bubble column
reactors when a solid phase exists.
Bubble columns are intensively utilized as multiphase contactors and reactors in

chemical, petrochemical, biochemical and metallurgical industries. They are used
especially in chemical processes involving reactions such as oxidation, chlorination,
alkylation, polymerization and hydrogenation, in the manufacture of synthetic fuels by
gas conversion processes and in biochemical processes such as fermentation and
biological wastewater treatment. Some very well known chemical applications are the
famous FischerTropsch process which is the indirect coal liquefaction process to
produce transportation fuels, methanol synthesis, and manufacture of other synthetic fuels
which are environmentally much more advantageous over petroleum-derived fuels.
44
REACTOR SKETCH & MATERIAL AND ENERGY

BALANCE
45
DESIGN CALCULATIONS
STEPS AFFECTING THE GLOBAL RATE
1. Mass transfer of gas from bubble to bubble/liquid interface.
46
kg = mass transfer coefficient for gas diffusion

ag = gas bubble-liquid interfacial area per unit volume of
bubble free slurry
Cg = concentration of hydrogen in gas
Cig = H2 concentration at benzene-hydrogen
bubble interface (at gas side)
2. Mass transfer from the stagnant liquid film of bubble to bulk of

liquid.
kl = mass transfer coefficient for gas absorption
ag = gas bubble-liquid interfacial area per unit
volume of bubble free slurry
Cil = H2 concentration at benzene-hydrogen
bubble interface (at liquid side)
Cl = bulk concentration of H2 in solution
3. Mixing & diffusion in bulk liquid.

The rise of bubbles through liquid is sufficient to achieve uniform conditions in
bulk liquid. Hence the resistance of step 3 can be neglected.
4. Mass transfer of dissolved gas from the bulk liquid to the outer
47
surface of solid catalyst.

kc = mass transfer coefficient for particles
ac = external surface area of paticles
Cl = bulk concentration of H2 in solution
Cs = concentration of H2at the external surface area of catalyst
pellet
5. Reaction on the catalyst and diffusion of products to liquid phase.

k = specific reaction rate constant
ac = external surface area of paticles
Cs = concentration of H2at the external surface area of catalyst
pellet
CATALYST SYSTEM CHARACTERISTICS

Particle size
150 A (spherical)
Catalyst density
8.9 g/cc
Cone, in solution =
mcat =
0.07%
Conc. in solution x liq. density

=
(0.0007) (0.51) = 3.57 xlO-4 g/cc
= 160.45 cm2/cc
48
BUBBLE DIAMETER CALCULATIONS

Kumar and Kuloor Correlation
Db = bubble diameter, cm
= kinematic viscosity, cm2/sec = 1.9 x 10-3
Q = Vol. flow rate of gas, cc/sec = 23419.34
g = gravitational constant, cm/sec2 = 980
Db3 = 1.247
Db = 1.076 cm = 10.76 mm
ag = 4r2 = 3.637 cm2
BUBBLE FREQUENCY CALCULATION
= Vol. flow rate of gas = 23419.34 cc/sec
= Orifice diameter = 8mm = 0.8 cm
= Surface tension.
Estimate the surface tension, , using the generalized corresponding state correlation of
Brock and Bird and the Miller relationship. The correlation and the relationship are as
follows:
where K is defined as follows:

49
Where
= surface tension in dynes/cm
Pc = critical pressure, bar
Tc = critical temperature, K
Tb = normal boiling point, K
Tb = 80.1 C = 353.1 K
Tbr = 0.63 Tr = 0.85
Pc = 48.3 atm,
=
=
Tc = 562.1 K,
K = 0.6366
6.857 dynes/cm
686102 Bubbles/sec.
FINDING OVERALL RATE EQUATION

Solving all diffusion & reaction equations simultaneously gives final equation of the form
Where
Under the assumptions:

Gas is pure so Cg = Cig
Catalyst is highly active so k is very large
50
Equilibrium exist at bubble-liquid interface, Cig and Cil are related by Henrys
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
And overall reaction rate is
LIQUID FILM DIFFUSION COEFFICIENT CALCULATION

Mass transfer correlations from Bulk liquid to catalyst particle
Where,
D = diffusivity of hydrogen = 3.8 x 10-5
l = viscosity of benzene = 0.001 poise
l = density of benzene = 0.51 g/cc
Hence
kc = 0.0305 cm/sec
OVERALL RATE CALCULATION

H
1765.4
pp H2 =
35 atm
ac
160.45 cm2 /cc
51
= 8.931 x 10-4 gmol/cc
rv = 2.476 x 10-6 mol of benzene/cc-sec
REACTOR VOLUME CALCULATION
V = volume of slurry cm3

Xe Xi = 0.95
rv = 2.476 x 10-6 mol of benzene/cc-sec
F = 5.74 gmol/sec
V = 2202431.43 cm3 =2.20 m3
Reactor volume is obtained by 25 % increment

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
Diameter of vessel = 0.96 m
Height of vessel
= 3.83 m
52
RESIDENSE TIME CALCULATION
Volume of vessel = 2.75 m3

Volumetric flowrate = 0.0234 m3/sec
= 1.958 min
SPARGER SELECTION
Porous plate distributor is selected because
Low price
Easy manufacturing
Variety of specfications
53
PRESSURE DROP CALCULATIONS

P across sparger = 0.1-0.3 atm
Let P be 0.2 atm
P due to liquid head = 0.175 atm

Total P = 0.375 atm
SPECIFICATION SHEET
Identification
Item
Reactor
Item No.
R-101
No. required
Position
Vertical
54
Function
Production of cyclohexane from benzene hydrogenation
Operation
Continuous
Type
Catalytic
Slurry Bubble Column Reactor
Chemical Reaction
C6H6 + 3H2
Catalyst
C6H12
H = -214 KJ/mol
Raney Nickel
Shape : Spherical
Size
: 150 oA
Material Contained
Benzene
Quality of material
Slightly Corrosive
Working Volume
2.20 m3
Design Volume
2.75 m3
Residense time
1.958 min
Temperature (process 2047.4 oC

temperature)
Working Pressure
35 atm
Diameter of Vessel
0.96 m
Height of Vessel
3.83 m
Height to Dia Ratio
4:1
55
56
VERTICAL VAPOR LIQUID SEPARATOR
57
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).
SELECTION CRITERIA FOR VAPOR LIQUID SEPARATORS

The configuration of a vapor/liquid separator depends on a number of factors. Before
making a vessel design one has to decide on the configuration of the vessel with respect
to among others:
Orientation
Type of feed inlet
Type of internals
Type of heads
Orientation of the Vessel

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.
Advantages of a vertical vessel are:
a smaller plot area is required (critical on offshore platforms)

58
it is easier to remove solids
liquid removal efficiency does not vary with liquid level because the area in the
vessel available for the vapor flow remains constant
generally the vessel volume is smaller
Advantages of a horizontal vessel are:
it is easier to accommodate large liquid slugs;
less head room is required;
the downward liquid velocity is lower, resulting in improved de-gassing and foam
breakdown;
additional to vapor / liquid separation also a liquid / liquid separation can be

achieved (e.g. by installing a boot).
The preferred orientation for a number of typical vapor / liquid separation applications
are:
Application
Preferred orientation
Reactor Effluent Separator (V/L)
Vertical
Reactor Effluent Separator (V/L/L)
Horizontal
Reflux Accumulator
Horizontal
Compressor KO Drum
Vertical
Fuel Gas KO Drum
Vertical
Flare KO Drum
Horizontal
Condensate Flash Drum
Vertical
59
Steam Disengaging Drum
Horizontal
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 slotted tee distributor
a half-open pipe
a 90 elbow
a tangential inlet with annular ring
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
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 twophase feed.
Normally the selected inlet device for a horizontal drum shall be:
a 90 elbow or a slotted diverter in case of an all liquid or vapor-liquid feed
a submerged pipe when the feed is a subcooled liquid and the mixing of liquid and
blanket gas is to be minimized
two 90 elbow inlets in case of high vapor loads
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
To reduce the size of a vessel
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
Major disadvantages of wire mesh demisters are:
They are not suitable for fouling services
Their liquid removal decreases significantly at reduced throughput

61
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
A hemispherical head should be considered for an extremely large, high-pressure vessel
A dished head should be considered in the case of a large diameter, low-pressure

vessel
62
INLET STREAM
C.H= 1666.545 kg/hr
M.C.P= 0.367 kg/hr
Benzene= 0.0167 kg/hr
Impurities= traces
S= traces
H2=150-120= 30 kg/hr+ XH2R
CO2= 0.0327 kg/hr+ X CO2R
CO= 0.02 kg/hr+ X CO R
CH4=14.5 kg/hr+ X CH4R
INPUTS
Operating pressure : P=10 atm
Vapour mass flow rate: WV = 56.05 kg/hr
63
Vapor density = 1.23 kg/hr

Liquid mass flow rate : WL = 1669 kg/hr
Liquid density : = 39.6 kg/m3
VAPORS
H2= 30 kg/hr
CO2= 0.0327 kg/hr
CO= 0.02 kg/hr
CH4=26 kg/hr
LIQUID
C.H= 1666.545 kg/hr
M.C.P= 0.367 kg/hr
Benzene= 0.0167 kg/hr
Impurities= traces
S= traces
Kg mole of Gases
H2= 15 kg mole
CO2= 1.36310-3 kg mole
CO= 1.4285710-3 kg mole
64
CH4=1.625 kg mole
VOLUME OF GASES
n= total moles=16.627 kg mole
= 16.6270.082335/10
kgmoleatmm3k / atm kg molek
= m3
V= 45.676 m3/ hr
V=0.76 m3/ min
Density of vapours
Mass = 56.1 kg/ hr

= 0.935 kg/min
v
= 0.935/0.76
= 1.23 kg/ m3
65
Density of liquid
n= total moles=19.84 kg mole
Specific gravity = 0.313
Density of liquid = 31.3 kg/m3
STEPS
Vv=A Uv
Uv = kv {(L - v)/ v}1/2
kv= 0.0107 m/s with a mist eliminator
A=D2/4
LLA=ts VL
3 ts 5
L=LL+1.5D+1.5ft
CALCULATIONS
First we find velocity of gase
Uv = kv {(L - v)/ v}1/2
= 0.0579m/s
Now we find area
Vv=A Uv
A= Vv/ Uv
66
0.76 m3
min
1 min
sec
60 sec
0.05798 m
= 0.218 m2
= 2.346 ft2
DIAMETER
D= 1.72 ft
= 1.75 ft
LENGTH OF LIQUID ENTRAINED

LLA=ts VL
ts= 4 min
We assume 5 percent of entrainment of liquid in vapors
VL= VL 5 %
= 0.908 5 %
= 0.0454 m3 / min
LLA=ts VL
67
LL=ts VL/ A
= 0.0454 4 / 0.218 m2
m3 / minmin1/ m2
=0.633027 m
= 2.73 ft
= 2.75 ft
L= LL+1.5D+1.5 ft
= 6.875 ft
Minimum length should be 8.5 ft
According to vertical and horizontal vap liq separator design
So length is 8.5 ft
L/D= 8.5/1.75
= 4.85
L/D < 5 for vertical separator
68
69
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.
A typical design of stabilization column is the cold feed
stabilizer with out reflux.
The stabilizer is a conventional distillation column with
reboiler but no overhead condenser. The lack of overhead
condenser means there is no liquid reflux from the overhead
stream. Therefore feed is provided on the top of column and
must provide all the cold liquor for the tower.
Fig.4.1 Cyclohexane stabilizer column
This type of design can be used when operating pressures are
high; typically stabilizers operate in the range of 700kpa -1400kpa.
High pressure
eliminates the need of cold reflux stream. Also as the pressure of system is high, the
flashing of feed is avoided. At the bottom a product cooler is install whose temperature
varies between 90-200oC depending upon operating pressure.
70
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 reboilers 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:
Feed
Components
Bottoms
Overheads
Mol
Kg-
Mol
Kg-
Mol
Kg-
fraction
mol/hr
fractio
mol/hr
fraction
mol/hr
xf
xd
xb
C6H6
0.9733
19.841
0.9998
19.841
0.995
0.4851
2.6x10-5
1.9x10-4
9.9x10H2
0.0245
0.498
5.0x10-4
2.0x10- 1.07x10 2.1x101.0x10-5
-7
71
3.0x10CO
1.5x10-7
3.0x10-7
3.0x10-6
3.0x10-7
3.0x10-6
3.65x10-4 3.7x10-3
3.0x10CO2
1.5x10-7
3.7x10CH4
1.8x10-4
2.19x10 4.3x10MCP
2.15x10-3
0.043
-7
2.7x10-5
0.0429
Total
1.0
20.385
1.0
19.845
1.0
0.540
DESIGNING OF COLUMN
The general design of stabilization column include following steps:

1) Selection of tray or packed column
2) Selection of packing
3) Calculation of Diameter and Area of column
4) Calculation of pressure drop
5) Calculation of Number of transfer units
6) Estimation of height of transfer units
7) Height of Column
8) Calculation of Liquid Hold Up
72
Step # 1: SELECTION OF COLUMN: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.
1- Breaking up gas into small bubble into continuous liquid stream
(Tray Column)
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)
Tray Column
It is used for non corrosive,
Packed Column
These are preferred for
non-foaming and clean
corrosive liquids.
liquids.
Tray columns are for large
They are efficient in small
installations
installations.
It is used for low to medium
For high liquid to gas ratios,
liquid flow-rates
They are preferred when
packed columns are installed.

For low pressure drop application
internal cooling is required
they work best.
between stages
I have selected packed column because cyclohexane is slightly corrosive

and as it is very small scale plant. Also packed columns are less expensive than
plate columns for small column diameter (<0.6 m).
Above this the fabrication of trays in small diameter column is a difficult job.
73
The main components of packed columns are given bellow:

1. Shell
2. Packings
3. Packing support
4. Liquid distributor
Figure 4.2: Packed column with

its internals
Step # 2: SELECTION OF PACKING TYPE :The distributor and packing are the heart of the performance of this
equipment. Their proper selection entails an understanding
of packing operational characteristics and the effects on performance.
The broad classes of packings for vapor-liquid contacting are either
random or structured . The former are small, hollow structures with large
surface per unit volume that are loaded at random into the vessel.
Structured packings may be layers of large rings or grids, but are most
74
commonly made of expanded metal or woven wire screen that are stacked
in layers or as spiral windings.
GENERAL CRITERIA FOR SELECTION OF PACKING :

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.
Most commonly used packings include:
75
Figure 4.3 Examples of some packing

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 .

On the other hand comparative analysis of different random packings
supports Pall rings with respect to availability, cost and pressure drop
features.
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
76
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 .
Recommended sizes are given below
Column diameter
Packing sizes
<0.3m
<25mm
0.3-0.9
25-38mm
>0.9
50-75mm
The design data of different rings is given in appendix, Figure 4.1.
Step # 3: COLUMN DIAMETER CALCULATIONS :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.
In calculation of appropriate diameter for column the steps followed are
given below:
a)
Find percentage flooding
With the help of calculated F LV , flow parameter, read values of
K4 & K
from Figure 4.3 given in appendix.

77
The formulae to calculate flow parameter and percentage flooding are

given below with:
F L v = L/V( v / l )
Where;
L = Mass flow-rate of liquid in kg/sec
= 0.46kg/sec
V = Mass flow-rate of vapor in kg/sec
= 0.0143 kg/sec
l = Density of liquid, kg/m 3
= 778kg/m 3
v = Density of vapor, kg/m 3
=1.5kg/m 3
F LV = 2.3
Percentage flooding = (K 4 /K 4 / ) 0 . 5 x 100

Assume pressure drop per unit height of packing to be 21mm/m height of
packing
K 4 = 0.13
K 4 / = 0.23
% flooding = 75%
Percentage flooding is in satisfactory range.
b)
Find Vapor Mass velocity kg/m 2 -sec
The formula to be used is given below;

78
v = Density of liquid,kg/m 3 = 778kg/m 3

l =Density of vapor ,kg/m 3 =1.5kg/m 3
l =Viscosity of liquid ,Nm/s 2
Fp
Packing factor m - 1
= 160 (taken from Richardson and coulson Vol. 6)
G = 0.367 kg/m 2 -sec
c) Required Area= V/G m 2

V = 0.0142 kg/sec
G = 0.367 kg/m 2 -sec
Area ,A= 0.039 m 2
Diameter, D = (4xA)/3.14
D= 0.223m
Actual area comes out to be;
A= /4(D 2 )
A= 0.039 m 2
79
Step
4:
CALCULATION
OF
PRESSURE
DROP
IN
PACKING :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
The X and Y co-ordinates are given below:
X- Coordinate;
G x /G v ( v / x - v )
Y-Coordinate;
G v 2 F p x 0 . 1 /g c ( x - v ) v
Pressure drop per unit height of packing has been calculated with the help
of graph given in appendix Figure 4.2.
P = Pressure drop in inches of water /ft of the packing height
G = Gas superficial mass velocity lb/s-ft 2 tower cross section
=0.07414 lb/s-ft 2
L = liquid superficial mass velocity lb/s-ft 2 tower cross section
=2.419lb/s-ft 2
g =Gas density ,lb/ft 2
g c = 32.14 lb m -ft/lb f -sec 2
F p =48.48
X=1.596
80
Y=0.0002
P = 0.2424 in H 2 O/ft of packing
=20mm H 2 O/m of packing
Assumed value was 21mm H2O / m Height of packing calculated value is
close to assumed value so it is acceptable.
Step # 5: CALCULATION OF NUMBER OF TRANSFER

UNITS :Number of transfer units has been calculated with the help of Kremsers
Equation given below;
N+ 1
(S
S) / (S
N+1
1)
= Mol fraction of solute gas stripped
This equation is applicable because the equilibrium data of hydrogen

desorption from cyclohexane is straight line. Equilibrium constant,K, has
been measured by using graph given in appendix Table 4.4
Whereas nomenclature used is given below :
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
81
K=
76
S=
2.024
N=
The number of transfer units for required separation is 8.
Step #6: HEIGHT OF TRANSFER UNITS :Height of transfer units is the height of packing that is required to change
the mol fractions of components equivalent to one theoretical plate in tray
column. It is some time called the efficiency calculation of packed
column.
It is calculated by using the concept of Height equivalent to theoretical
plate, HETP, given by peters.
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 ones. 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
82
H O G =Vapor phase height of transfer unit

As rule of thumb in when D<0.5m
[7]
HETP=D
HETP=0.233m
HOG
= 0.54m
Step #7: HEIGHT OF COLUMN :-
Z =N x H O G
Z = Height of Packing in meters
Z=8x0.54
Z =4.32m
Z t = Z +H d +H b
Height for the disengagement region, H d =0.289m
Height for the Bottom, H b =0.4365m
Z t = Total height of the column
= 5.04m
Step # 8: LIQUID HOLD UP CALCULATIONS :-
HLw = 0.0004(Lm/Dp)0.6
83
Dp =equivalent spherical packing diameter (inches)

Lm =liquid rate ( lb/s-ft2 )
Hlw=0.050m3/m3 of packing
PROCESS SPECIFICATION SHEET FOR STABILIZATION COLUMN
84
1.
Item Number
V-02
Type:Packed
Service
Cyclohexane Stabilizer
3.
NO OF EQUIPMENTS
4.
OPERATION
CONTINUOUS
PROCESS CONDITIONS
5.
Liquid Handled
6.
Liquid Flow-rate
7.
Kg-mol/hr
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
Cyclohexane
20.385
OPERATIONAL CONDITIONS
14.
Nature of operation
Stripping
15.
Feed nozzle location
Top/Sat. liquid
16.
Temperature
442
K
17.
Percentage Flooding
75%
COLUMN INTERNALS
18.
Packing Size
mm
25
19.
Nature of packing
Pall rings
20.
Material of Packing
Metallic, Carbon Steel
21.
Liquid Distributor
Spray nozzles
85
HEAT EXCHANGER DESIGN

HEAT EXCHANGER
Heat exchanger is a device that is used to transfer heat between two fluids at different
temperature.
DIFFERENT TYPES OF HEAT EXCHANGERS

The principle types of heat Exchanger used in Chemical and allied industries are as follows:
1.
2.
3.
4.
5.
6.
Double Pipe heat Exchanger

Shell and Tube Heat Exchanger
Plate and Frame Heat Exchanger
Plate and Fin Type Heat Exchanger
Spiral Type Heat Exchanger
A Cooled: Cooler and Condenser
SELECTION CRITERIA
Selection process includes a No. of factors all of these are related to the heat transfer
application.
1.
2.
3.
4.
5.
6.
Thermal Requirements
Material Compatibility
Operational Maintains
Environmental, Health & Safety Consideration
Availability
Cost
SHELL & TUBE HEAT EXCHANGER

Basic Construction of Shell & Tube Heat Exchangers
Shell and tube heat exchangers represent the most widely used vehicle for the transfer of
86
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 tradeoffs in fluid allocation in heat transfer coefficients, available pressure drop, fouling
tendencies and operating pressure.
87
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
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
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.
90
End Channels and Bonnets

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.
91
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
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 4045% 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
93
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.
STANDARD DESIGN STEPS

a.
b.
c.
d.
e.
f.
g.
Define the duty; Heat Transfer Rate and Temperature

Collection of Fluid Physical Properties
Assume the value of Heat Transfer Coefficient
Calculate the Mean Temperature Difference
Calculate the Area Required
Decide the Heat Exchanger Layout
Calculate the Pressure
STREAM CONDITIONS
HOT FLUID
Inlet Temperature T1 =184 C
Outlet Temperature T2 =30 C
Mass flow rate mh =1669 kg/hr
COLD FLUID
Inlet Temperature t1 =25 C
Outlet Temperature t2 =43 C
Mass flow rate
mc =7969 kg/hr
PHYSICAL PROPERTIES
HOT FLUID
94
Specific heat Cp =2.186 kJ/kg K

Thermal conductivity k =0.1041 W/m K
Density
=695.2 kg/m3
Viscosity =1.88 kg/m sec

COLD FLUID
Specific Heat Cp =4.17 kJ/kg K
Thermal conductivity k = 0.590W/m K
Density = 995kg/m3
Viscosity =2.37 kg/m sec
HEAT LOAD
Using Hot Fluid
Q = m Cp T
=5.62 103 kJ/hr
LOG MEAN TEMPERATURE DIFFERENCE

T1
Hot Fluid
184 C
T2
30 C
t2
Cold Fluid
43 C
t1
25 C
T1 = T2-t1
T2=T1-t2
95
LMTD = (T1- T2)/(ln T1/ T2)

LMTD = 41.72 K
Ft Factor
R= (T1-T2)/(t2-t1)
= 8.55
S=(t2-t1)/(T1-t1)
=0.113
Ft=0.976
Tm=0.96741.72= 38.684K
ASSUMED OVERALL COEFFICIENT Ud

Ud =100 W/m2K
APPROXIMATE AREA
A=Q/Ud Tm
=40.35m2
TUBE SPECIFICATIONS
Outside Dia of Tube (OD) = 0.019m
Inner Diameter of Tube (ID) = 0.016m
Tube Pitch
Thickness
Pt = 0.024m
= 16 BWG
Area of a Single Tube a = 0.2911m2
96
No of Tubes
A/a=139
TUBE SIDE CALCULATIONS

Mass Flow rate (mc) = 7969 kg/hr
Total Area of Tubes (at) = 0.0125 m2
Mass Velocity Gt = (mc/at ) = 63752 kg/hr.m2
Calculation of Reynolds Number

Reynolds Number (NRe) = DGt /
= ( 0.016 63752)/2.37
= 5425.70
TUBE SIDE HEAT TRANSFER

hi = [4200(1.35+0.02t)]/ID0.2
= 4877.57W/m2K
=4107.43W/m2K
SHELL SIDE CALCULATIONS

Internal Diameter of Shell (ID) = 0.387 m
Tube Clearance
(C) = 0.0048m
Baffle Spacing
(B) = 0.2035 m
FLOW AREA
97
= (0.3870.0040.205 )/0.024
= 0.011 m2
MASS VELOCITY
Mass velocity
= 1669/0.011
= 151727kg/hr.m2
SHELL SIDE EQUIVALENT DIAMETER

Shell Side Equivalent Diameter
(De )= 0.0139 m
Reynolds Number
= (0.0139151727)/1.88
= 24434.5
Jh = 90
Prandtl Number
98
Pr
= Cp/k
= (2.1861.88 )/0.104
=1.3
OUTSIDE HEAT TRANSFER COEFFICIENT
[900.104(1.3)1/3]/0.0139
876.23W/m2 K
CLEAN OVERALL COEFFICIENT
= 742W/m2K
ACTUAL AREA Ac
=40.70m2
CORRECTED Ud
(156103)/(40.7038.684)
99.15 W/m2K
DIRT FACTOR
99
Dirt factor
=0.0087 W/m2K
SHELL SIDE PRESSURE DROP CALCULATION

Friction factor (f) = 0.0051
Eq., Diameter Of Shell (De) = 0.0139m
Specific Gravity (S) =0.79
Number of crosses (N+1) = L/B=23.98
Gs
= 42.27kg/sec .m2
SHELL SIDE PRESSURE DROP
= 741.98N/m2
TUBE SIDE PRESSURE DROP CALCULATION

Friction factor (f)
= 0.0025
Inside Diameter (I.D) = 0.016m

Specific Gravity (S) =1
Length L = 4.88m
n=139
Gt = 177kg/sec.m2
100
TUBE SIDE PRESSURE DROP
=239.45 N/m2
101
SPECFICATION SHEET
I Item
S Shell & Tube Heat Exchanger
F Function
S Stabilizer Product Cooler
P Position
N No. of Unit
Horizontal
N One
1
N No. of Shell Passes
11
No. of Tube Passes
22
Heat Transfer Area
440.7m2
Diameter of Shell
0 0.387m
P Pitch (Triangular Pitch)
No. of Tubes
0 0.025m
1 139
102
T Type of Tube Used
1 16BWG
T Tube Length
4 4.88m
I ID & OD of tube
0 0.0157m, 0.01908m
hi
4 4877.57W/m2K
ho
8 876.23W/m2 K
P Pressure drop on Shell Side
7 41.98N/m2
Chapter # 5
MECHANICAL DESIGN
103
MECHANICAL DESIGN OF SHELL & TUBE HEAT

EXCHANGER
SHELL SIDE
SHELL THICKNESS
ts=Shell thickness =?
P=Design Pressure=1.51N/mm2
Ds=Inner Diameter of Shell=387mm
Permissible Strength for Carbon Steel
f=95N/mm2
Joint factor=J = 85%

So
ts =3.65
Allowable Corrosion allowance C =4mm

So the Shell Thickness
ts =3.65+4
=7.65mm
NOZZLE DESIGN FOR SHELL SIDE

Material used Carbon Steel
For Shell Fluid Inlet Nozzle
104
Mass Flow Rate of Shell Side fluid =1669kg/hr

Density of the Shell side Fluid=695.2kg/m3
Velocity of Shell Side Fluid= 218m/hr
A =m/v= 0.011m2
Dn = 118mm
Outer Nozzle also has the same Diameter
NOZZLE THICKNESS
C = Corrosion allowance
=5.11mm
HEAD THICKNESS
P = Design Pressure = 4 N/mm2
Rc =Outer Radius of Shell = 200mm

Rk = Kunckle Radius of Shell = 0.06Rc =12mm
W= 1.7706
105
th = 7.270mm
BAFFLE DIAMETER
(Using 25% Cut Baffle)
Db = Ds -4.8
=382.2mm
TUBE SIDE
Material Used Carbon Steel
No. of Passes = 2
No. of Tubes = 139
Outside Diameter = 0.019m
Inside Diameter = 0.016m
Wall Thickness of Tube= 0.165m
Length of Tube= L=4.88m
Tube Pitch Pt =0.025m
Working Pressure =0.6 N/mm2
Design Pressure =0.66 N/mm2
NOZZLE DESIGN FOR TUBE SIDE

Material Used Carbon Steel
Mass Flow Rate of Tube Side Fluid = 7969kg/hr
Density of Cold Fluid =995 kg/m3
Velocity of Tube Side Fluid = v =640.72m/hr
106
= 0.0125m2
Dn = 126.18mm
NOZZLE THICKNESS
tn = 0.51
Nozzle thickness with Corrosion Allowance
tn = 0.51+4
= 4.51mm
Chapter # 6
INSTRUMENTATION &
PROCESS CONTROL
107
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.
It is desirable that the process variable to be monitored be measured directly, often,
however, this is impractical and some dependent variable that is easier to measure is
monitored in its place. For example, in the control of distillation columns the continuous on
line, analysis of the overhead product is desirable but difficult and expensive to achieve
reliably, so temperature is often monitored as an indication of composition. The temperature
instrument may form part of a control loop controlling, say , reflux flow ; with the
composition of the overhead checked frequently by sampling and laboratory.
INSTRUMENTATION & CONTROL OBJECTIVE

The primary objective of the designer when specifying instrumentation and control schemes
are:
Safer Plant Operation
a. To keep the process variable within known safe operation limits
b. To detect dangerous situation as they develop and to provide alarms and
automatic shut down system.
c. To provide inter locks and alarms to prevent dangerous operating
procedures.
Production Rate
To achieve t6he design product output
Product Quality
To maintain the product composition within the specified quality standards
Cost
To operate at the lowest production cost, commensurate with the other
objectives.
108
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.
COMPONENTS OF A CONTROL SYSTEM

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.
Analysis of measurements Variable to be measured

1.
2.
3.
4.
Pressure measurements
Temperature measurements
Flow Rate measurements
Level measurements
Variable to be Recorded
Indicated Temperature, Composition, Pressure etc
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.
109
Final Control element

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.
ii)
The pneumatic controller appears to be safer in a potentially explosive

atmosphere which is often present in the petro-chemical industry.
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:
110
i)
On-off Control
ii)
Integral Control
iii)
Proportional Control
iv)
Rate or Derivative Control

In industry purely integral, proportional or derivative modes seldom occur alone
in the control system.

The On-off controller in the controller with very high gain. In this case the error
signal at once off the valve or any other parameter upon which it sits or completely sets
the system.
ALARMS AND SAFETY TRIPS AND INTERLOCKS

Alarms are used to alert operators of serious, and potentially hazardous,
deviations in process conditions. Key instruments are fitted with switches and relays to
operate audible and visual alarms on the control panels.
The basic components of an automatic trip systems are:
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.
111
A safety trip can be incorporated in control loop; as shown in figure . In this

system the high-temperature alarm operates a solenoid valve, releasing the air on the
pneumatic activator closing the valve on high temperature.
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.
DIFFERENT TYPES OF CONTROLLERS

Flow Controllers
These are used to control feed rate into a process unit. Orifice plates are by far the
most type of flow rate sensor. Normally, orifice plates are designed to give pressure drops
in the range of 20 to 200inch of water. Venture tubes and turbine meters are also used.
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 1300F 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).
112
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.
113
CONTROL OF HEAT EXCHANGER

1. The Normal Way
The normal method for controlling a heat exchanger is to measure exit
temperature of the process fluid and adjusts input of heating or cooling medium to hold
the desired temperature.
2. Cascade Control
The control objective is to keep the exit temperature of stream 2 at a distance
value. The secondary loop is used to compensate for the changes in the flow rate of
stream 1.
In chemical process, flow rate control loops are almost always cascade with other control
loops.
CONTROL SCHEME
The figure shows a cascade control in which the hot fluid temperature is constantly
measured by the temperature transmitter. The temperature is matched with the set point
when the temperature changes, the deviations are communicated to the secondary controller
which is then adjusted the flow rate of the cold fluid.
114
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.
115
The objectives of a HAZOP study can be summarized as follows:

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.
3)
To familiarize the study team with the design information available.
4)
To ensure that a systematic study is made of the areas of significant hazard

potential.
5)
To identify pertinent design information not currently available to the team.
6)
To provide a mechanism for feedback to the client of the study team's detailed
comments.
BASIC PRINCIPLES OF HAZOP STUDY

The basic concept of the hazard and operability study is to take a full description of
process and to question every part of it to discover what deviation from the intention of
the design can occure and what can be their causes and consequences.
The seven guide words recommended in the chemical industries association
(CIA) booklet are used. In addition to these words, the following words are also used
with precise meaning.
Intention
Deviation
Causes
Consequences
Hazards
116
In HAZOP study, each segment (pipeline, piece of equipment, instrument

etc) is carefully examined and all possible deviations from normal operating conditions
are specified. Some of guide words works recommended by CIA are given in the
following Table.
Table: HAZOP Guide Words and Meanings

Guide Words
No
Meaning
Negation of design intent
Less
Quantitative decrease
More
Quantitative increase
Part of
Qualitative decrease
As well as
Qualitative Increase
Reverse
Logical opposite of the intent
Other than
Complete substitution
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.
A HAZOP study is conducted in the following steps:
1)
Specify the purpose, objective, and scope of the study. The purpose may be
the analysis of a yet to be built plant or a review of the risk of an 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
117
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.
118
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.
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.
119
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.
120
HAZOP STUDY OF GAS/LIQUID SEPARATOR

Deviation from
Events cause
Consequence of
Operating
deviation
Deviation
Notes
conditions
Level
1. Inlet flow
1. Lowering of
stops
pressure
2. temp, rises
2. Separator dries
Check for any

valve failure
Check condenser
121
out
Less
temp rise
3. Pressure
3. Feed to
See the vent
lowers
Stabilizer
valve
interrupted
4. Vent on
4. Purge
Condenser is
composition
uncontrolled
changes
Check the purge

composition
Leakage
detection
5. Reflux is
5. Feed to
Check for any
interrupted
Stabilizer
valve failure
interrupted
1. Temp, drops
1. Pressure
increases
More
2. Pressure
2. Separator over-
increased
loaded
3. Feed
3. More
vaporized
vaporizing steam
Consider for
column
shut down
Check reflux
quantity
plugged
4. High temp of
See reflex
reflux condenser
condenser
No
Same as less
Temperature
1. Subcooling in
1. Less flashing
condenser
2. Pressure
Check flow from

condenser
2. Purge / recycle
Vent/purge
122
Less
drops.
composition
change
3. Reflux temp,
3. Level builds-up
drops
composition
analysis
Check flow from
condenser
More
Opposite to less
No
Same as less
Pressure
1. Purge valve
1. Composition of
openned/uncontr purge / recycle
Less
Check for gas

composition
olled
changed
2. Temp, drops
2. Quanity to feed
Follow the
from condenser
vaporizer changes
process
conditions
3. Temp, drops
3. Composition of
Consider the
from refluxed
purge / recycle
vaporizer &
condenser
changed
compressor shut
down
More
Opposite to less
No
Same as less
123
Chapter # 8
ENVIRONMENTAL IMPACTS
OF CYCLOHEXANE PLANT
Chemicals can be released to the environment as a result of their manufacture,
processing, and use. EPA has developed information summaries on selected chemicals to
describe how you might be exposed to these chemicals, how exposure to them might
affect you and the environment, what happens to them in the environment, who regulates
them, and whom to contact for additional information. EPA is committed to reducing
environmental releases of chemicals through source reduction and other practices that
reduce creation of pollutants.
HOW MIGHT I BE EXPOSED TO CYCLOHEXANE?

Cyclohexane is a colorless, flammable liquid. It occurs naturally in petroleum crude
oil, in volcanic gases, and in cigarette smoke. It is produced in large amounts (an
estimated 338 million gallons in 1992) by four companies in the United States. US
demand for cyclohexane is likely to increase at a rate of 2% to 2.5% per year. The largest
users of cyclohexane are chemical companies that make adipic acid and caprolactam,
chemicals used to make nylon. Chemical companies also use cyclohexane to make
124
benzene, cyclohexanone, and nitrocyclohexane. Cyclohexane can be added to lacquers

and resins, paint and varnish removers, and fungicides. It is also used as a fuel for camp
stoves.
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. 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.
WHAT HAPPENS TO CYCLOHEXANE IN THE ENVIRONMENT?

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
1. Absorption - Cyclohexane is absorbed following inhalation and nominally by the
skin. Massive applications of the chemical to the skin of rabbits have produced
125
microscopic changes in the liver and kidneys. Systemic toxicity observed in animals
exposed orally to cyclohexane indicates that gastrointestinal 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.
2. Distribution - Following inhalation exposure of Wistar rats to
concentrations
of cyclohexane ranging from 300-2000 ppm, perirenal fat concentrations of the chemical
were 23- to 38-fold greater than brain concentrations after one week of exposure and 50to 80-fold greater than brain concentrations, after two weeks. No information was found
regarding distribution to other organs.
3. Metabolism - Cyclohexane is metabolized via the hepatic, vascular, and renal
systems. Microsomal hydroxylases oxidize cyclohexane to cyclohexanol in the presence
of NADPH and oxygen. Other metabolites identified in mammalian systems include
trans-cyclohexane-1,2,-diol, cyclohexanone, and adipic acid.
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.
1. Humans - According to one source, cyclohexane is detectable by odor and is
irritating to the eyes at 300 ppm; another source suggested 25 ppm as the odor threshold
(ACGIH 1991). Undiluted cyclohexane is also irritating to the skin. No other
information was found in the secondary sources searched for the acute toxicity of
cyclohexane to humans.
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
126
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
Cyclohexane administered subchronically is of low toxicity, producing
neurological effects, ocular, gastrointestinal, and respiratory effects in animals at very
high, lethal concentrations.
1. Humans - No information was found for the subchronic/chronic toxicity of
cyclohexane in humans in the secondary sources searched.
2. Animals - No effects were observed in rabbits exposed to 434 ppm
cyclohexane for fifty 6-hour periods or in rhesus monkeys exposed to 1234 ppm under
identical exposure conditions. Concentrations of 7445 ppm, 6 to 8 hours/day for 2 to 26
weeks were lethal to rabbits, producing neurological effects as well as closure of the eyes,
conjunctival infection, salivation, labored respiration, cyanosis and diarrhea prior to
death. Rats exposed by inhalation to 1500 or 2500 ppm cyclohexane for 9-10 hours/day,
5 days/week for 7, 14, or 30 weeks exhibited no adverse effects.
D. Carcinogenicity
1. Humans - No information was found in the secondary sources searched
regarding the carcinogenicity of cyclohexane in humans.
2. Animals - No information was found in the secondary sources searched regarding
the carcinogenicity of cyclohexane in animals.
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.
127
F. Developmental/Reproductive Toxicity
1. Humans - No information was found in the secondary sources searched
regarding the developmental/reproductive toxicity of cyclohexane in humans.
2. Animals - No information was found in the secondary sources
searched
regarding the developmental/reproductive toxicity of cyclohexane in animals.
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.
1. Humans - At high concentrations, cyclohexane is a central nervous system
depressant and may cause dizziness and unconsciousness.
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 7445 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
128
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.
A. Toxicity to Aquatic Organisms

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.
B. Toxicity to Terrestrial Organisms

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
Limited information indicates cyclohexane may have potential to contribute to the
formation of photochemical smog. The ozone-forming potential for cyclohexane has
been measured as 2 on a scale of 5. Ozone-forming potential is an indicator of the smogforming potential of a chemical.
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.
129
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.
ECONOMICS & BUSINESS

A huge amount of finances are spent as fixed and working capital of the project.
New markets will be explored and captured. Existing financial activity (imports etc.) will
be affected. Also the living status of the people involved will be changed.
POPULATION THICKENING EFFECTS

If the plant is to be installed near to a thickly populated area, the necessities like
accommodation, transportation, schooling etc. may get sever.
130
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.
IMPORTANT MATERIAL AVAILABLE

Material of construction may be divided into two general classifications of metals
and non-metals. Pure metals and metallic alloys are included under the first classification.
1)
Iron and Steel

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
131
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.
3)
Nickel and its Alloy

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 100C, the corrosion rate of copper is comparatively small.
However, the corrosion rate of 100C 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
132
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
The beneficial effects of nickel, chromium, and molybdenum arc combined in
Hastelloy C to give an expensive but highly corrosion-resistant material. A typical

analysis of this shows 56% nickel, 17 molybdenum, 16% chromium, 5% iron and 4%
tungsten with manganese, silicon, carbon, phosphorus, and sulfur making up the balance.
Hastelloy C is used where structural strength and good corrosion resistance are necessary
under conditions of high temperature. The material can be machined and is easily
fabricated.
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.
133
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
134
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.
ESTIMATION OF EQUIPMENT COST

STORAGE TANK
TK-1
3.1 x 106 rupees
TK-2
3.54 x 106 rupees
P-01
3.54 X 105 rupees
P-02
2.88 x 105 rupees
P-03
6.64xl04 rupees
PUMPS
COMPRESSORS
135
C-01
5.7.6x106 rupees
HEAT EXCHANGERS
E-01
1.45 xlO5 rupees
E-02
7.27xl05 rupees
E-03
5.8x105 rupees
E-04
5.8xl05 rupees
E-05
2.2xl05 rupees
E-06
9.25 xlO5 rupees
R-01
3.76xlO5 rupees
R-02
9.5xl04 rupees
V-01
3.3 x 105 rupees
V-02
l.lxlO5 rupees
VESSELS
STABALIZER (V-03)
=
3.54xlO5 rupees
Packing cost =
1.94 x 104rupees
Total cost
3.73xlO5 rupees
Shell cost
Total purchased equipment cost
Rs. 2.56xl07 rupees
ESTIMATION OF TOTAL CAPITAL INVESTMENT

136
Direct Cost (Rs)

Installation costs
4.61x105 rupees
Instrumentation & control, installed

Piping, installed
1.15x105 rupees
Electrical, installed
6.4 xlO4rupees
Building, process & auxiliary
1.28 x 106rupees
1.8x105 rupees
Service facilities & yard improvement =
6.4 x 105 rupees
Land
1.53 x 106 rupees
Total direct cost
8.68 x 106rupees
Indirect Cost
Engineering & supervision
1.514x106 rupees
Construction & contractor's fee=
1.56x106 rupees
Contingency
1.33 x 107 rupees
Total indirect costs
4.41 x 107 rupees
Total fixed capital investment
1.31x107 rupees
Working capital
3.3x106 rupees
1.64x107 rupees
Total capital investment
137
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.
3) John B. Butt, Reaction kinetics and reactor design
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.
6) William L. Luyben, Chemical Reactor Design and Control
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.
9) J.M.Smith, Chemical engineering kinetics.
10) Coulson, J.m., and Richardson, J.F., Chemical Engineering, 4 th ed, Vol.2, Butterworth
Heminann, 1991.
11) E.Bruce Nauman, Chemical Reactor Design,optimization and scaleup.
12) Charles G.Hill,JR, An Introduction to Chemical Engineering kinetics & reactor design
138

13) Peacock, D.G., Co ulson & Richardsons Chemical Engineering, 3rd ed, vol,
Butterworth Heinenann, 1994.
14) Sinnot, R.K., Coulson and Richardsons 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): Perrys 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
20)
petrol),U.S. Patent 3,202,723, Aug.24 1965.

Maurice Stewart, Emulsion and Oil Treating Equipments,vol.5;Gulf
21)
Professional Publishers,1972.
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
23)
Publishers, 1998.
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,
26)
vol.6;McGraw Hill, New York, 1997.

Ernest,L.E., Applied Process Design For Chemical And
Petrochemical Plants,edit.3;vol.2; Gulf Professional Publishers.
139
APPENDIX
Figure 4.1
Figure 4.2
140
Figure 4.3
141
Figure 4.4
142
143

Production of Cyclohexane From Benzene

Hochgeladen von

Dokumentinformationen

Originalbeschreibung:

Originaltitel

Copyright

Verfügbare Formate

Dieses Dokument teilen

Dokument teilen oder einbetten

Freigabeoptionen

Stufen Sie dieses Dokument als nützlich ein?

Sind diese Inhalte unangemessen?

Copyright:

Verfügbare Formate

Production of Cyclohexane From Benzene

Hochgeladen von

Copyright:

Verfügbare Formate

Production of Cyclohexane from Benzene

DEPARTMENT OF CHEMICAL ENGINEERING

This report is submitted to department of Chemical

DEPARTMENT OF CHEMICAL ENGINEERING

We pay special homage to our respective teachers; Dr.