Waheed Final Rport PDF

CHAPTER 01
INTRODUCTION
PRODUCTION OF VAM 1
1.1 Introduction:
Vinyl acetate is a colorless, flammable liquid that also has a characteristic smell that can quickly
become irritating. This monomer is used principally in the production of polyvinyl acetate (PVAc)
and other vinyl acetate copolymers. Polyvinyl acetate is a precursor of polyvinylic alcohol and
polyvinyl acetate resins (PVA). Vinyl acetate is also copolymerized as a minor raw material for
vinyl chloride and ethylene to form commercial
Polymers and acrylic fibers.
Vinyl acetate is completely soluble in organic liquids but not in water. At 20 degree centigrade a
saturated solution of the monomer in water can contain between 2-2.4% of vinyl acetate, while a
saturated water solution in vinyl acetate contains 1% of water. At 50 degree centigrade the
solubility of the monomer in water increases in 0.1% in regards to 20 degree centigrade, while the
solubility of water in vinyl acetate doubles at 50 degree centigrade. The most important reaction
of vinyl acetate is the polymerization by free radicals which is fast and exothermic. The speed of
hydrolysis of the vinyl acetate is 1,000 times greater than its saturated analogous in a alkaline
medium, and it was researched that its speed of hydrolysis is significantly lower at a pH of 4.4.
1.2 Physio-Chemical Properties:

Table 1.1 Physical & Chemical Properties [1]
Properties Values
Molecular weight 86.09
Vinyl ester content ≥ 99.9%
Distillation range (101.3 kPa) 72 – 73 °C
Freezing point − 93 °C
Water Max. 400 ppm
Acid content (acetic acid) Max 50 ppm
Acetaldehyde Max 100 ppm
Inhibitor content 3 – 5 ppm
Liquid viscosity at 20 °C 0.41 Cp
Solubility VAM - water/water - VAM at 0.9%/2.3%
25 °C
Solubility in organic solvents Complete
Upper/lower explosion limit vapor in air at 2.6/13.4% vol.
20 °C
PRODUCTION OF VAM 2
1.3 Applications:
The vinyl acetate monomer (VAM) is large scale commodity chemical mostly used in
manufacturing polyvinyl acetate, the basic ingredient in water soluble acrylic paints. Other
applications are coatings for textile and paper industries, laminated safety glass, packaging,
automotive fuel tanks and acrylic fibers. The worldwide production of vinyl acetate was about 5
million tons per year in 2005[2], with rapid growth in the emerging markets. Higher efficiency can
be achieved by upstream integration with the production of low cost acetic acid, as well as by
downstream integration with the manufacturing of polyvinyl acetate and polyvinyl alcohol.
• Plastics
• Films
• Lacquers
• Laminating adhesives
• Inks
• Elastomers
• Adhesives
• Paper coating
• Finishing and impregnation materials
• Water based emulsion paints
• Floor tiling
• Safety Glasses
• Building construction
• Acrylic fibers
• Glue
• Cosmetics and personal care products
• Textile finishing and non-woven products
PRODUCTION OF VAM 3
CHAPTER 02
PROCESS SELECTION
PRODUCTION OF VAM 4
2.1 Manufacturing Routes:
Three main routes for vinyl acetate manufacturing are employed today, as follows:
2.1 .1 Acetic Acid and Acetylene

The process is based on the reaction:
HC≡CH+ CH3COOH → H2C=CH-O-(CO) CH3 ΔH = −118 kJ/mol
The operating conditions are gas phase at 170 – 250 °C and Zn catalyst impregnated on charcoal.
Per - pass acetylene conversion is 60 – 70% with a selectivity of 93% acetylene and 99% acetic
acid [3]. High acetylene cost and safety problems make this process less competitive today.
2.1.2 Acetaldehyde and Acetic Anhydride

The process takes place in two stages. Firstly, acetaldehyde and acetic anhydride form ethylidene
diacetate in liquid phase at 120 – 140 °C with FeCl3 as a catalyst:
CH3CHO + (CH 3CO)2O → CH3CH(OCOCH3 )2
In the second step the intermediate decomposes at 120 °C with acid catalyst:
CH3CH (OCOCH3)2 → H2C=CH-O-(CO) CH3 + CH3COOH
Note that this process may rely completely on renewable raw materials.
2.2 Acetic Acid, Ethylene and Oxygen

This route dominates today and it will be adopted in this project. In older technologies, the reaction
was conducted in liquid phase at 110 – 130 °C and 30 – 40 bars in the presence of a redox catalyst
PdCl 2 /CuCl 2, but corrosion raised problems. Modern processes operate in gas phase with Pd -
based catalysts. A highly undesired secondary reaction is the combustion of ethylene to CO2. With
modern Pd/Au catalysts the selectivity may reach 94%, based on ethylene and 98 – 99% based on
acetic acid [3]. The removal of CO2 usually by a wash with hot KOH solution negatively affects
the overall economics. Hoechst/Celanese and Bayer/DuPont are the most widespread processes,
the main difference being in the formulation of the catalyst. With respect to reaction engineering
a multi-tubular fixed bed reactor is employed, where the operational difficulty is mastering the
occurrence of excessive temperature rise (hot spot). Recently, fluidized bed reactor technology
was developed with better productivity and 30% lower investment.
PRODUCTION OF VAM 5
2.3 Selection of the Process:
Table 2.1 Process Comparison
Process Advantages Disadvantages

Acetic acid and Acetylene Single step process Low conversion per pass
Acetaldehyde and acetic Renewable Raw materials Corrosion problem due to
anhydride liquid phase reaction.
Acetic acid, ethylene and Better productivity and higher By-product CO2 is produced.
oxygen per pass conversion
We have selected the vinyl acetate monomer production from Acetic acid, ethylene and oxygen
because selectivity may reach 94 % by ethylene and 98 to 99 % by acetic acid. [4]
PRODUCTION OF VAM 6
CHAPTER 03
CAPACITY SELECTION
PRODUCTION OF VAM 7
3.1 Capacity Selection:
• The worldwide production capacity of vinyl acetate monomer (VAM) was estimated at
6,154,000 tonnes/annum in 2007, with most capacity concentrated in the United States
(1,585,000 all in Texas), China (1,261,000), Japan (725,000) and Taiwan (650,000). The
average list price for 2008 was $1600/tonne[4].
• The market for vinyl acetate monomer (VAM) is driven by high demand for adhesives
from end-user industries such as construction, auto-motives and furniture. Moreover, the
global vinyl acetate monomer market is driven by increasing demand for VAM copolymers
from paints and coatings industry. Vinyl acetate monomer (VAM) is one of the key
polymers used in manufacture of adhesives and emulsions. Increasing demand for
ethylene-vinyl acetate and ethylene-vinyl alcohol from solar PV cells and the food
packaging industry respectively are likely to provide better opportunities for the vinyl
acetate monomer (VAM) market over the forecast period. However, highly volatility of
raw material prices, limited technology and over production in the market is anticipated to
hinder the growth of the market in near future.
• With over 40% share in total demand, Asia Pacific dominated the demand for vinyl acetate
monomer in 2013[4]. The region is projected to demonstrate latent growth for the vinyl
acetate monomer (VAM) market during the forecast period. In terms of market share, Asia
Pacific was followed by Europe and North America, both of which are projected to exhibit
relatively slower growth numbers for the vinyl acetate monomer market during the forecast
period. The demand for vinyl acetate monomer is increasing slightly in North America
region due to an increasing demand from the adhesives and packaging industries. Rest of
the World is anticipated to witness stable demand for vinyl acetate monomer between 2014
and 2020[4].
PRODUCTION OF VAM 8
• In Pakistan there is no company which is producing VAM. So, we have decided to
produce Vinyl acetate monomer with the capacity of 34 ktonnes per annum.
Figure 3.1[4] Vinyl Acetate consumption
PRODUCTION OF VAM 9
CHAPTER 04
PROCESS DESCRIPTION
PRODUCTION OF VAM 10
11
4.1 Process Flow Diagram:
PRODUCTION OF VAM
Figure 4.1 Process Flow Diagram for Production of VAM
4.2 Process Description:
The process is centered on the reaction between ethylene, oxygen and acetic acid in order to
produce vinyl acetate and water. There is a second unwanted reaction in the process based on the
ethylene oxidization to produce water and carbon dioxide. The gaseous effluents from the reactor
are cooled trying to have a partial condensation of the stream. Next, the gas is separated from the
liquids in a phase separator. The gas is washed with acetic acid from a recycle stream. This helps
to recover the vinyl acetate in the absorber. Afterwards, there is a process to eliminate the CO2
from the gas phase and recycle it back in to the reactor the Ethylene is necessary.
The liquids that come out from the separator and the acetic acid used in the washing process enter
an azeotropic distillation tower. In this part of the process, the main objective is to separate the
acetic acid (bottoms) form the water and vinyl acetate mixture (distillate). The distillate enters to
a decantation process in which its organic product (mainly vinyl acetate) divides into a reflux
stream that heads back to the distillation column and another stream that enters a separation train
process where the proper concentration level of vinyl acetate is achieved to comply with the
wanted specifications. The aqueous stream from the decanter is discarded.
A portion of the bottoms stream from the distillation column (mainly acetic acid) is used in the
washing process in the absorber, while the other portion of the bottom stream is mixed with pure
acetic acid from the feed streams to later on enter to an evaporation process. The gaseous acetic
acid obtained is mixed with the recycle gas, oxygen and ethylene to form the feed to the reactor.
The reaction that produces the vinyl acetate takes place in a P.B.R. reactor where a gaseous mixture
of ethylene, acetic acid, and air (with small presence of CO2 and water from the recycle streams)
are fed to the reactor. To obtain an annual production of in thousands of tons of vinyl acetate, with
a molar composition of 0.5 of ethylene, 0.07 of oxygen and 0.15 acetic acid have to be fed. An
excess of ethylene over acetic acid (3:1) must be guaranteed. The concentration of oxygen must
be kept below 8 % molar because at higher concentrations it breaches the explosive limit of the
mixture.
4.3 Process Constraints
Two key safety constraints exist in the process.First, the oxygen composition must not exceed 8
mol %anywhere in the gas recycle loop to remain outside the explosivity envelope of ethylene[5].
Continuous and reliable O2 analyzers will be installed in the process at the inlet of the reactor to
monitor oxygen composition. Second, the pressure in the gas recycle loop and distillation column
cannot exceed 140 psia because of the mechanical construction limit of the process vessels.
Pressure measurements are readily available and will be installed at appropriate locations.
Exceeding either the oxygen concentration or pressure limits will shut down the process via
interlocks.
Several other operational constraints must also be satisfied during process operation. The peak
reactor temperature along the length of the tube must remain below 200 oC, otherwise mechanical
damage occurs to the catalyst requiring shutdown. Liquid levels in the vaporizer, separator,
absorber base, distillation column base, and decanter must operate within the limits of 10 to 90%.
The vessel volumes listed have been proposed for the working liquid inventories between the level
taps. Reactor inlet temperature must exceed 130 oC to prevent condensation of liquid in the reactor.
The hot side exit temperature from the feed effluent heat exchanger (FEHE) must remain above
130oC to avoid condensation in the exchanger, which has been designed to handle only vapor-
phase flow.
CHAPTER 05
MATERIAL AND ENERGY
BALANCE
Material and Energy Balance
5.1 Assumptions
• Capacity:4353kg/hr
• Days of operation:330
• Basis: 1 hour operation
• Tref = 30 oC
• Steady state condition
• min = mout
• Ein = Eout
5.1 Over All Mass Balance
Table 5.1 Stream Balance
stream stream stream stream stream stream stream

Component 3 1 2 15 17 20 22
Oxygen 1218 0 0.7
CO2 0 378 3
C2H4 0 1545 0 21
C2H6 0 2 0 2
VAM 0 0 4198 101 0 0
ACID 0 0 3146 11 125 0 0
WATER 0 0 46 1039 0 0
1218 1547 3146 4256 1266 378 26.7
5912kg 5912kg
5.1.1 Section 1
Figure 5.1 Reactor section
Table 5.2 Balance of Reactor Section
component stream 1 stream 3 stream 5 stream 19 stream 23

30 oC 30 oC 159 oC 107 oC 81 oC
Oxygen 1218 625 624
CO2 2627 2246
C2H4 1545 20253 20232
C2H6 2 1600 1598
VAM 4305 3 0
ACID 4503 4357 2
WATER 1226 131 15
1547 1218 35142 4491 24719
∆H(Kj/hr) 0 0 1656 555 756
5.1.2 Section 2
Figure 5.2 Separation Section

Table 5.3 Balance of Separation Section
stream stream stream stream stream stream Vent

Component 2 13 15 17 18 19
30 oC 42 oC 40 oC 40 oC 107 oC 107 oC
oxygen
CO2
C2H4
C2H6
VAM 4304 4198 101 1 3
ACID 3146 6836 11 125 2342 4357
WATER 1260 46 1038 70 131
Total 3146 12401 4256 1265 2414 4491 negligible
∆H(Kj/hr) 0 347 202 122 285 555
5.1.3 Section 3
Figure 5.3 Absorber Section
Table 5.4 Balance of Absorber Section
stream stream stream stream stream stream stream

Component 7 9 12 18 20 21 22
40 oC 40 oC 54 oC 42 oC 45 oC 45 oC 45 oC
Oxygen 625 624 0.7
CO2 2627 378 2246 3
C2H4 20253 20232 21
C2H6 1600 1598 2
VAM 4305 3801 503 2 0 0
ACID 4503 4416 2420 2342 1 0
WATER 1226 1189 71 70 15 0

35142 9406 2995 2414 378 24719 26.7
∆H(Kj/hr) 567 297 221 179 75 273 negligible
5.2 Reactor
Figure 5.4 Plug Flow Reactor
5.2.1 Reactor Mass Balance
Table 5.5 Reactor Material Balance
Reactor inlet Reactor outlet
5.2.2 Energy balance
Equation for energy balance is:
dQ/dt = ∆𝐻1 - ∆𝐻2 + Q - ∆𝐻𝑟
Q = ∆𝐻2 − ∆𝐻1 + ∆𝐻𝑟
T
Tref = 150oC ∆H2 = Cp dT = ∫T 2 (A + BT + CT 2 + DT 3 )dT
ref
So, ∆𝐻1 = 0
∆𝐻2 = 5.9×104 kJ/kmol
∆𝐻𝑟= ∑(𝑛𝑖 ∆𝐻𝑓 )𝑝 − ∑(𝑛𝑖 ∆𝐻𝑓 )𝑟
(∆𝐻𝑟)1 = -1.7×105 kJ/kmol

(∆Hr)2 = - 1.3×106 𝑘𝐽/kmol
𝑄 = ∆𝐻2 + (𝜉1 ∗ ∆𝐻𝑟)1 − (𝜉2 ∗ ∆𝐻𝑟)2
𝜉1 = 50, 𝜉2 = 4.3
Q = 59962.3 + ( -176407.1*50 -1322137.3*4.3)
Q = -1.4×107 𝑘𝐽/ℎ𝑟
Utility flow rate

BFW inlet temp = 145 OC
QH=QC=m.Hvap
QH=-1.4×107 =m × 2740 Hvap=2740kJ/kg
m= 5109kg/hr
5.2 FEHE Energy Balance
Figure 5.5 Feed Effluent Heat Exchanger
𝑇𝑖𝑛 = 160℃ 𝑄𝑐 = −𝑄ℎ

𝑇𝑜𝑢𝑡 = 134℃ 𝑄ℎ = −1.4×106 𝑘𝐽/ℎ𝑟
For cold side
𝑇
𝑇𝑖𝑛 = 45℃ 𝑄 = 𝑛𝑖 ∫𝑇 2(𝐴𝑖 + 𝐵𝑖 𝑇 + 𝐶𝑖 𝑇 2 + 𝐷𝑖 𝑇 3 )𝑑𝑇= 1.4×106 𝑘𝐽/ℎ𝑟
1
𝑇𝑜𝑢𝑡 = 81℃
5.3 Cooler Before Flash Energy Balance
Figure 5.6 Cooler

𝑇
Q = 𝑛𝑖 (∫𝑇 2(𝐴𝑖 + 𝐵𝑖 𝑇 + 𝐶𝑖 𝑇 2 + 𝐷𝑖 𝑇 3 )𝑑𝑇) + 𝑛𝑖 𝜆𝑖
1
Qh = -1.23×107 kJ/hr
Assuming no heat losses
Qh = Qc
Cp = 4.18 kJ/kg.K
∆T = 15 K
Mass flow rate of water = Qh/(Cp. ∆T)
= 1.9×105 kg/hr
5.4 Flash Drum
𝑍𝑖 𝐾𝑖 𝑦 Figure 5.7 Flash Vessel

∑ =1 𝑥𝑖 = 𝑘𝑖
1+𝑉(𝐾𝑖 −1) 𝑖
𝑍𝐾
𝑖 𝑖
where v = vapor fraction 𝑦𝑖 = 1+𝑉(𝐾
𝑖−1)
Table 5.6 Material Balance of Flash Vessel
5.5 Compressor Energy Balance
Tin = 40℃ Pin = 592 kPa
Tout = 80℃ Pout= 882 kPa
Compression Ratio = 1.5
Compressor Work = m*(∆𝐻)
Where ∆𝐻 = H2 – H1
W = 1.7×106 kJ/hr
Actual Work = W/efficiency = 1.7∗ 106 /0.75 = 2.26×106 kJ/hr
Power required = Actual Work/efficiency = (2.26×106 )/0.85
= 2.6×106 kJ/hr
= 738 kW
5.6 Absorber
Figure 5.8 Absorber
5.6.1 Absorber Material Balance
RECOVERY [6]
VAM = 99.9%
Acid = 98%
Table 5.7 Material Balance of Absorber
Inflow Out flow
5.6.2 Absorber Energy Balance

Overall energy balance on absorber
Hgas,in + Hsolvent,in = Hgas,out + Hsolvent,out+ Qc
Hgas,in = 2018065kj/hr
Hsolvent,in = 65197kJ/hr
Hgas,out = 576135kJ/hr
Hsolvent,out= 225723 kJ/hr
Qc= 1.2×106 kJ/hr
5.7 Distillation Column
Figure 5.9 Distillation Column
5.7.1 Material Balance of Distillation

VAM = 99.9% (top)[6]
Acid = 98% (bottom)
Table 5.8 Material of Distillation Column
5.7.2 Distillation Column Energy Balance
Figure 5.10 Heat Exchanger

𝑇
1
Condenser
Saturated vapor at T=97ºC
Condenser outlet T=40ºC
So, latent and sensitive heat is involved.
Q=4.74×106 kJ/hr
Utility flow
Mass of water=Q/(Cp*dt)
Where Cp=4.18kJ/kg.K
dT = 15ºC
Mass flow rate of water=75645.13kg/hr
Reboiler
Overall energy balance on distillation column
HF +QR= HD + HW + Qc
HF=3397691.15kJ/hr
HD=132108.4kJ/hr
HW=1747707 kJ/hr
QC=4742950 kJ/hr
QR=3.2×106 kJ/hr
5.8 Vaporizer Energy Balance
𝑇
1
Tin = 87oC Tout = 120oC

Qv = Hout - Hin
Hout=8772360kJ/hr
Hin=3347975kJ/hr
Qv=5.42×106kJ/hr
5.9 Pre-Heater Energy Balance

Tin = 120oC
Tout = 152oC
Qh = -8.17×106 kJ/hr
Assuming no heat losses
Qh = Qc
QH = mHvap
8.17×106 = m×2740 Hvap=2740 kJ/kg
m = 2980 kg/hr
CHAPTER 06
EQUIPMENT DESIGN
6.1 REACTOR DESIGN
Reactor
6.1.1 Reactor Design
Reactor is the heart of a chemical process. Reactor is the equipment where the main chemical
reaction takes place. Following the reactor are the preliminary treatment and raw material
preparation steps whereas followed by the reactor are product enrichment and purification steps.
The main objective in this chapter is to determine what type and size of the reactor and mode of
operation would be the best to get the desired yield and purity of Vinyl Acetate Monomer.
6.1.2 Reactor Selection Criteria

Selection of the appropriate reactor for the process is as important as the accurate temperature and
pressure conditions for carrying out the reaction. Selection of the reactor depends on the following
factors;
• Mode of operation
• Type of flow
• Reaction phase
• catalyst bed
6.1.3 Mode of Operation

In a batch reactor, the reacting contents are fed into a vessel all at a time and then removed some
time later. This is a closed system w.r.t mass i.e. no mass can cross the boundaries of the vessel
during the reaction residence time. If certain reagents are fed into the vessel while it is processing
a part of them, the reactor is termed as semi-batch. A continuous reactor is one that permits the
input and output of reagents during process.
A comparison of batch and continuous process is shown below; [7]
Table 6.1 Comparison of Batch & Continuous Reactor
Parameters Continuous Reactor Batch Reactor

Residence Time Low High
Operating Cost Low High
Rate of Production High Low
Work Force Low High
Ease of Automation Easy Difficult
Down Time Low High
Equipment Cost High Low
For the same production, the size of batch reactor is much larger as compared to a continuous
reactor. As the annual production capacity of the plant has been selected to be 34 k-tons per annum,
continuous mode of operation is selected for the reactor.
6.1.4 Type of Flow
On the basis of interaction of the reagents in the reactor, the reactors are classified as:
• Continuous Stirred Tank Reactor (CSTR)
• Plug Flow Reactor (PFR)
A CSTR is equipped with an impeller. One or more reagents, which may be solid or fluid are fed
into the reactor. The impeller agitates the reaction mixture at a set RPM to ensure homogeneous
mixing throughout. Contrary to CSTR, the reactants move in tubes without any axial mixing in a
PFR. The tubing is divided into small segments, each segment termed as a plug. A brief
comparison of PFR and CSTR is shown below: [7]
Table 6.2 Comparison of CSTR & PFR
Parameters CSTR PFR

Composition Uniform Varies along the length of reactor
Mixing Axial Perpendicular to the direction of
flow
Agitation Required Prohibited
Temperature Uniform Varies along the length
Reactor Volume More Less
Figure
6.1.5 Reaction Phase
Since, the production of Vinyl Acetate Monomer is a gas phase reaction, CSTR cannot be used.
To choose the appropriate reactor, PFR is studied further. Before going into the detail of reactor,
the reaction characteristics should be known i.e. whether the reaction is catalytic or non-catalytic.
And if the reaction is catalytic, it is homogeneous or heterogeneous.
Literature survey reveals that production of VAM from ethylene is a gas phase and takes place in
the presence of Palladium-gold catalyst. Catalyst properties would be discussed in detail later on
in this chapter. Catalysis can be of two types;
• Homogeneous catalysis
• Heterogeneous catalysis
6.1.6 Catalyst Bed
Industrially, there are two practices by which heterogeneous catalysis is carried out. The catalyst
bed can either be packed bed or fluidized bed. Reactors in which the solid catalyst particles remain
static at their position relative to other particles are the fixed bed particles. Whereas the reactors in
which the particles are suspended in the fluid, solely due to upward pressure of fluid are termed as
fluidized bed reactors.
Table 6.3 Comparison of Fixed Bed Reactor& Fluidized Bed Reactor [7]
Properties Fixed Bed Fluidized Bed

Contact Phases Solid-liquid or solid-gas Solid-gas
Residence Time Less High
Pressure Drop High Low
Catalyst Loss No loss Possible
Catalyst Handling No difficulty Technical difficulties
Maximum opt. Pressure High operating pressure 10-12 MPa
Operating Cost Low High
Supporting Equipment Not Required Required
Keeping in view all the selection parameters, discussed above, the reactor selected for the
production of VAM from ethylene is fixed bed, heterogeneous catalytic plug flow reactor. The
major plus points of the selected reactor can be summarized as follows;
• Small residence time

• Ease of operation
• Efficient heat transfer/removal
• High operating pressure
6.1.7 Design Parameters
• Volume of catalyst
• Number of tubes
• Shell diameter
• Shell side heat transfer coefficient
• Tube side heat transfer coefficient
• Shell area
• Tube area
6.1.8 Reactor Specifications

• Temperature = 423 K
• Pressure = 811 kPa
• Catalyst used: Palladium Gold
• Reaction: Exothermic
• Coolant: Water
• Steady state process
• Isothermal process
6.1.9 Catalyst Specifications

• Palladium-Gold catalyst
• Bed density =ƍ = 833 kg/m3
• Pallet diameter = dp =3 * 10-3 m
• Void fraction = 𝛆 = 0.4
6.1.10 Chemical Reaction

• C2H4 (g) + CH3COOH (g) + 0.5O2 (g) → C4H6O2 (g) + H2O (g)
• Heat of Reaction = -176.2 kJ/mol
• Temperature = 423 K
• Pressure = 811 kPa
6.1.11 Reaction Kinetics

-rVA = k1 ( P(C2H4) )0.35 ( P (O2) ) 0.192
k1 = k0 exp (–Ea/RT)
T = 423 K
R = 8.314 J/mol. K
Ea = 15000 J/mol.
k0 = 9.7 * 10 -05
k1 = 1.38 * 10 -06
6.1.12 Design Steps
The general design steps for the design of multi-tubular packed bed plug flow reactor are as
follows:
1. Calculate the weight of catalyst required using the performance equation:
𝑊 𝑥 dxA
= ∫0 𝐴
𝐹𝐴0 −rA
2. Calculate the volume of the catalyst
𝑉𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡 = 𝑊/𝜌𝑏𝑢𝑙𝑘
3. Calculate reactor volume
𝑉𝑟𝑒𝑎𝑐𝑡𝑜𝑟 = 𝑉𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡 / (1−𝜖)
4. Select tube size, length and pitch by using empirical relations
5. calculate volume of one tube
𝑉𝑡𝑢𝑏𝑒 = (𝜋 𝐷𝑖2 𝐿)/4
6. Calculate total number of tubes, total surface area for heat transfer and bundle diameter
𝑇𝑜𝑡𝑎𝑙 𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑇𝑢𝑏𝑒𝑠 = 𝑁𝑡𝑢𝑏𝑒𝑠=𝑉𝑟𝑒𝑎𝑐𝑡𝑜𝑟/𝑉𝑡𝑢𝑏𝑒

𝐴 = 𝑁𝑡𝑢𝑏𝑒𝑠 ∗(𝐿𝑒𝑛𝑔𝑡ℎ) ∗(𝑆𝑢𝑟𝑓𝑎𝑐𝑒 𝑝𝑒𝑟 𝑙𝑖𝑛𝑒𝑎𝑟 𝑚𝑒𝑡𝑒𝑟)
7. Calculate the tube bundle diameter
𝐷𝑏 = 𝑑𝑜 (𝑁𝑇/𝑘1)1/𝑛
8. Calculate Shell Inside Diameter and Length
4/𝛱 𝑁𝑡𝑢𝑏𝑒𝑠 𝑃𝑡 2
𝐷𝑖 = √
0.99
9. Calculate the heat duty Q and LMTD
10. Calculate overall heat transfer co-efficient (U)
1/𝑈=1/ℎ𝑖 + 1/ℎ𝑜
11. Calculate Tube side pressure drop using following equation.
fGt^2 ∗L n
Δ𝑃 =
5.22 ∗ 10^10 ∗ Dp sφs
12. Calculate shell side pressure drop using the following equation
f Gs2 Ds (N+1)
Δ𝑃 =
5.22 ∗ 10^10 ∗De ∗s∅s
6.1.13 Design Calculations
STEP 1
Calculate the weight of catalyst required using the performance equation

W 𝑥 dxA
= ∫0 𝐴
FA0 −rA
As,
CA0 = 0.23 mol./m3
V = 569 m3 /hr
𝛆 = -0.2
𝑃𝐶2𝐻4(1−𝑥𝐴) 0.35 𝑃𝑂2(1−𝑥𝐴) 0.192

-rva = k1 [( ) ( ) ]
1−0.2𝑥𝐵 1−0.2𝑥𝐴
0 to 40 % conversion, plot graph between conversion XA and (1 / -rVA)
Table 6.4 Conversion & Reaction Rate
XA rVa 1/ -rVA
0 0.0028 358
0.1 0.0023 437
0.15 0.002 488
0.2 0.0018 547
0.25 0.0016 619
0.3 0.0014 707
0.35 0.0012 815
0.40 0.0010 910
Graph between XA and 1/ -rVA
1000
900
800
700
600
500
400
300
200
100
0
0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0.4 0.45
Figure 6.1 Conversion vs Inverse of Rate
Weight of catalyst = Density * volume of catalyst bed

Density of catalyst = 833 kg/m3
Weight of catalyst = 4740 kg
STEP 2
Calculate the volume of the catalyst
𝑉𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡 = 𝑊 / 𝜌𝑏𝑢𝑙𝑘
𝜌𝑏𝑢𝑙𝑘 = 833 kg/m3
Volume of the catalyst bed = 5.7 m3
STEP 3
Calculate reactor volume
𝑉𝑟𝑒𝑎𝑐𝑡𝑜𝑟= 𝑉𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡 / (1−𝜖)
Volume of the reactor = VReactor = 9.5 m3
𝜋
Volume of Reactor = VR = D2 L
4
Let,
L/D=3
Diameter of Reactor = 1.59 m
Length of Reactor = 4.78 m
STEP 4
Select tube size, length and pitch by using empirical relations
To calculate the length of the tubes, we will consider the reactor as a heat exchanger.
Selected Pipe Size
ID = 0.0312”
OD = 0.0315”
14 BWG
Length = 4 m
Square Pitch = Ps = 0.0437
Tube diameter is selected such that ratio of tube diameter to particle diameter should be greater
than 10. [7]
Diameter of the tube selected = 0.0315 m

Diameter of particle = 0.003 m
Dt / Dp = 11 > 10
So, selected tube diameter is correct.
STEP 5
Calculate volume of one tube

𝑉𝑡𝑢𝑏𝑒 = (𝜋 𝐷𝑖2 𝐿)/4
Volume of one tube of reactor = Vtube = 0.0083 m3
STEP 6
Calculate total number of tubes and total surface area for heat transfer
𝑇𝑜𝑡𝑎𝑙 𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑇𝑢𝑏𝑒𝑠 = 𝑁𝑡𝑢𝑏𝑒𝑠 = 𝑉𝑟𝑒𝑎𝑐𝑡𝑜𝑟 / 𝑉𝑡𝑢𝑏𝑒
Total Number of tubes in reactor = Ntubes = 1133
𝐴 = 𝑁𝑡𝑢𝑏𝑒𝑠 ∗𝐿𝑒𝑛𝑔𝑡ℎ ∗𝑆𝑢𝑟𝑓𝑎𝑐𝑒 𝑝𝑒𝑟 𝑙𝑖𝑛𝑒𝑎𝑟 𝑚𝑒𝑡𝑒𝑟

Total surface area for heat transfer = A = 145 m2
STEP 7
Calculating the tube bundle diameter
𝐷𝑏 = 𝑑𝑜 (𝑁𝑇/𝑘1)1/𝑛
Db = bundle diameter
do = tube OD = 0.0315 m
Nt = number of tube = 1133 tubes
K1 and n are constants from table
Table 6.5 Tube Pitch
Triangular Pitch Pt = 1.25 do

Number passes 1 2 4 6 8
K1 0.319 0.249 0.175 0.0743 0.0365
n 2.142 2.207 2.265 2.499 2.675
Square Pitch Pt = 1.25 do
K1 0.215 0.156 0.158 0.0402 0.0331
n 2.207 2.291 2.263 2.617 2.643
Bundle diameter = Db = 1.53 m
STEP 8
Calculate Shell inside Diameter
4/Π Ntubes Pt2

𝐷𝑖 = √
0.99
Shell Inside Diameter = Di = 1.67 m

Shell inside diameter should be greater than tube bundle diameter.
STEP 9
Calculate the heat duty Q and LMTD

( T2−t1 ) −( 𝑇1−𝑡2 )
ΔT LM = ( T2−t1 )
[𝑙𝑛( ]
𝑇1−𝑡2 )
ΔT LM = 121.6 K
Q = m*Cp* ΔT LM
Q = 2.78 * 10 6 kJ / hr
STEP 10
Calculate overall heat transfer co-efficient (U)
1) Shell and tube side specifications

• Reaction mixture is hot so taken on tube side.
• Water on shell side.
• Shell ID = Dx = 1.57 m
• Baffle spacing = 0.4 * Dx = 0.628 m
• Shell passing = ns = 1
• Tube passing = nt = 1
• Number of tubes = 1133
• Length of tubes = 4m
• 14 BWG
• Tube OD = d0 = 0.0315 m
• Tube ID = di = 0.0312 m
• Square pitch = Ps = 0.0437 m
2) Physical properties data
Table 6.6 Physical Properties [8]
Properties Shell side ( Water ) Tube side ( Reaction media)

Thermal conductivities 0.606 0.029
(W/m K )
Specific heat capacity 4.18 2.04
(kJ/kg.K)
Viscosity (kg/m.s) 9.59 * 10 -04 1.5 * 10 -05
Density (kg/m) 997 7.45
TEntering 298 433
TLeaving 313 423
Flow rate (kg/sec) 1.55 9.76
3) Tube side heat transfer coefficient
Flow area for selected tube diameter = a = 7.64 * 10 -04

Flow area for all tubes = at = 1133 * 7.64 * 10 -04 = 0.86
Mass velocity = Gt = W/at = 11.34 kg/m2.s
(di Gi)
Re. No = = 23587.2
µ
Pr = (Cp µ)/k = 0.00105
𝑁𝑢 # = 0.203 (𝑅𝑒 𝑃𝑟)0.33+0.22𝑅𝑒0.8 𝑃𝑟0.4
𝑁𝑢 # = 45
ℎ𝑖=𝑁𝑢 𝑘/𝐷
hi = 42 W/m2.K
hio = hi * (ID/OD) = 41.6 W/m2.K
4) Shell side heat transfer coefficient

𝐷𝑠( 𝑃𝑡−𝑑𝑜 )𝐵
Shell side flow rate = as =
𝑃𝑠
as = 0.315 m2
Mass velocity = Gs = W/as = 4.92 kg/m2.s
(de Gs)
Re. No =
µ
4( 𝑃𝑡 2 −0.25𝜋𝐷𝑒 2 )
De =
𝜋𝐷𝑒
De = 0.033 m
Re # = 169.3
Pr # = 6.6 * 10 -03
Nu # = 3.6 ( Re ) 0.7 ( Pr ) 0.33
hs = 458.13 W/m2.K
5) Overall heat transfer coefficient

a) Clean overall heat transfer coefficient.
ℎ𝑠∗ℎ𝑖𝑜
Uc = = 38.14 W/m2.K
ℎ𝑠+ℎ𝑖𝑜
b) Design overall heat transfer coefficient
Surface area per linear m = a” = 0.0318 m2/linear m

Total surface area = At = Nt * L * a”
At = 144 m2
Uo = Q/ (ΔT LM A ) = 10.03 W/m2.k
c) Dirt factor.
𝑈𝑐−𝑈𝑜
Rd = = 0.0735
𝑈𝑐∗𝑈𝑜
STEP 11
Tube side pressure drop
𝑓∗𝐺𝑡 2 ∗𝐿𝑛
ΔPt =
5.22∗1010 ∗𝐷𝑡∗𝑆∗𝜑𝑠
Friction factor = f = 0.0005

Specific gravity = s = 0.59
ΔPt = 0.0035 kPa
STEP 12
Shell side pressure drop
𝑓∗𝐺𝑡 2 ∗(𝑁+1)𝐷𝑠
ΔPs =
5.22∗1010 ∗𝐷𝑒∗𝑆∗𝜑𝑠
Friction factor = 0.0013

Specific gravity = s = 1
# of crosses = N+1 = L/B
ΔPs = 0.249 kPa
Design Temperature
Operating Temperature = 423 K

Design Temperature = 1.1 * 423 = 465.3 K
Design Pressure
Operating Pressure = 811 kPa
Design Pressure = 1.1 * 811 = 892.1 kPa
6.1.14 Specification Sheet
Table 6.6 Specification Sheet of Reactor
Identification
Item Reactor
Item Number R-1
Type Multi-tubular fixed bed Reactor
Function
Production of Vinyl acetate
Design Specification
Operating Temperature 423 K
Operating Pressure 811 kPa
Design Temperature 465.3 K
Design Pressure 892.1 kPa
Diameter of Reactor 1.59 m
Length of Reactor 4.78 m
Volume of Reactor 9.5 m3
Length of Tube 4m
Diameter of Tube 0.0315 m
Thickness of Tube 0.003 m
Overall heat transfer Coefficient 10.3 W/m2.K
Pressure drop tube side 0.0035 kPa
Pressure drop shell side 0.245 kPa
Catalyst Palladium-Gold
Catalyst shape Spherical
Number of Tubes 1133
6.2 SHELL AND TUBE
HEAT EXCHANGER
Shell and Tube Heat Exchanger
6.2.1 Heat Exchanger
Heat exchanger is an operating device used to exchange heat between two fluids. Fluids may be
liquid, gases and vapors. The most commonly used is the shell and tube heat exchanger. It is used
as condenser, reboiler etc. and in petroleum industry and can be used for high temperature
scenarios.
6.2.2 Features of Shell and Tube Heat Exchanger

Table 6.8 Features of Shell & Tube Heat Exchanger [8]
Type TEMA code Advantages Limitations

fixed tube sheet Mechanical cleaning of
outer side of tube and shell
is not possible
Provides largest HT No allowance for thermal

expansion between the
area for a particular
shell and the tube.
shell and tube Allowance can be provided
diameter by using expansion joint on
shell side.
Less expensive than
BEM, AEM, NEN other bundle designs
Floating head For large no. f tubes, bolt
requires space
Can’t bear large thermal

There is allowance for
shocks as tubes can’t
thermal expansion expand
Mechanical cleaning is Design temperature and
AEW, BEW, BEP, possible pressure are limited by
AEP, AES, BES packing material
U-tube Thermal expansion Some center tubes are
allowance is there for omitted due to U-bend
Individual tubes as
well as between tube Tubes can only be
bundle and shell chemically cleaned
because of U-bend
Mechanical cleaning is
Difficult to replace
possible individual tubes
Comparatively Single tube pass or
inexpensive countercurrent flow
BEU, AEU arrangement is not possible
6.2.3 Thermal Design Considerations
The flowrates, terminal temperatures and properties of both hot and cold fluids are basic inputs
of heat exchanger’s thermal design. Thermal design consists of calculation of
• Heat transfer area
• No. of tubes
• Tube length and dia.
• Tube layout
• No. of passes
• Heat exchanger type
• Tube pitch
• No. of baffles
• Type and size of baffle
• Shell and tube side pressure drop etc.
6.2.4 Shell Side

It contains shell fluid and tube bundle is placed inside it. Its dia. Is selected to give a close fit with
the tube bundle. Clearance between shell and bundle depends on heat exchanger type. Standard
steel pipes are used to fabricate shells and corrosion allowance is always provided. 3/8inch shell
thickness for 12-24inch shell dia. can be used for up to 300psi of operating pressure.
6.2.5 Tube Side

¾ and 1inch outer dia. are very common for designing a compact heat exchanger [8]. Maximum
heat transfer occurs if we have maximum no. of tubes which increases turbulence. Tube thickness
should withstand internal pressure along with providing allowance for corrosion resistance. Tube
thickness is expressed by
• Birmingham wire gauge (BWG)
• True outside diameter (OD)
Frequently used tube lengths are 6, 8, 12, 16, 20 and 24ft. Finned tubes are used in case of fluids
with low HT coefficient. Stainless steel, brass, bronze, admiralty and copper-nickel alloys are
commonly used tube materials.
6.2.5.1 Tube Pitch:

It is center to center distance between two adjacent tubes. General tube patterns are square,
triangular and rotated square.
6.2.5.2 Tube Count:
It is the no. of tubes that can be placed in a shell. It depends on
• Shell ID
• Tube OD
• Tube pitch
• No. of passes
• Tube layout
• Type of heat exchanger and
• Design pressure
Table 6.9 Tube Specifications [8]
Tube OD, inch Pitch type Tube pitch, inch

¾ Square 1
1 Square 11/4
¾ Triangular 15/16
¾ Triangular 1
6.2.5.3 Tube Passes

No. of tube passes is selected based on
• Velocity of tube side fluid
• Large HT coefficient
• Reduce scale formation
No. of passes vary from 1 to 16. Commonly used passes are 1, 2 and 4 [9]. Tube side flow is
directed with help of partition plate also called as pass partition.
6.2.5.4 Tube Sheet

Tube sheets are used to fix tubes and they act as a barrier between shell and tube side fluids.
Grooves attach tube to tube sheets in the wall by tube rolling and an excellent seal is developed.
This is the most common type of arrangement. Thickness of tube sheet should be greater than tube
OD in order to form a good seal. TEMA standards are used to select tube sheet thickness.
6.2.6 Baffles
They increase fluid velocity to obtain high HT coefficient by diverting fluid flow across tube
bundle. The distance between two adjacent baffles is called baffle spacing and it is 0.2-1 of shell
inside diameter. Baffle spacers hold baffles in their position. High HT coefficient is achieved if
baffle spacing is small. 15-45 % baffle cuts are commonly used. High HT coefficient with
reasonable pressure drop is achieved with 20-25 % baffle cut. The % cut for segmental baffle refers
to the cut away height from its diameter.
6.2.7 Fouling Considerations
Most process fluids cause fouling of HT surface. It reduces relative HT rate due to lower K
value. It also increases cost of
• Construction due to oversizing
• Additional energy due to poor performance
• Maintenance and cleaning
Usually, a secondary exchanger is available for uninterrupted service. This effect is considered in
design in terms of shell and tube side fouling resistance.
6.2.8 Selection of Fluids for Tube and Shell Side

Tube and shell side fluid routes have a considerable effect on heat exchanger design. Guidelines
for shell and tube side fluids are given in table.
Table 6.10 Location of Fluid
Tube side fluid Shell side fluid

Corrosive fluid Condensing vapor (unless corrosive)
Cooling water Fluid with large temperature difference
(>40C)
Fouling fluid
Less viscous fluid
High pressure steam
Hotter fluid
6.2.9 Design Problem

Thermal Design:
Given data:
Hot fluid inlet temperature (T1) = 160°C

Cold fluid inlet temperature (t1) = 45°C
Cold fluid outlet temperature (t2) = 81°C
Pinlet (for hot fluid) = 882kPa, Pout = 882kPa
Pinlet (for cold fluid) = 620kPa, Pout =
620kPa
Energy Balance
Assume no heat loss to the surrounding.

Qh = Qc = mc Cc (t2 - t1) = mh Ch (T1 -T2) = 1.4*106kJ/hr
T2 = 134°C
LMTD = ((T2 – t1) – (T1 – t2 ))/ln (T2 – t1)/ (T1 – t2)
LMTD = 83.90°C
Calculation of Heat Transfer Area and Tube Numbers

Assuming 1 shell pass and 2 tube pass shell and tube exchanger with following dimensions and
considerations.
• Fixed tube plate

• 20mm OD tubes (do) (16 BWG) on 25mm triangular pitch (PT)
• Outer diameter of tube = 20mm
• Tube length (Lt) = 4.88m
• Tube ID (di) = 16mm
Fluid arrangement: Cold fluid is placed in tube side because it has the higher fouling tendency
The log mean temperature correction factor (FT) for 1-2 shell and tube exchanger:
√𝑅2 + 1 ln(1 − 𝑆)
1−𝑅𝑆
FT =
(𝑅−1)ln{2−𝑆(𝑅+1− √(𝑅2 +1) ) }
2−𝑆(𝑅+1+ √(𝑅2+1) )
√(0.89)2 + 1 ln(1 − 0.529)

1−𝑅𝑆
FT =
(0.89 −1)ln{2−0.529(0.89+1− √((0.89)2+1) ) }
2−0.529(0.89+1+ √((0.89)2 +1) )
= 0.977
Where R = 0.72222, S = .3130
FT = 0.977
LMTDcorr = FT * LMTD = 81.9703°C
Determining The Heat Transfer Area (‘A’):
The assumed value of overall heat transfer coefficient (Ua) of 30 Wm-2°C-1 is assumed to initiate
the design calculation for the heat exchanger. The approximate range of overall heat transfer
coefficient depending on the hot and cold fluid can be found out from text books.
A = Q/Ua * LMTDcorr = 158.1422m2
Calculating No. Of Tubes (Nt)
Surface area of one tube = π*do*Lt = 0.303m2

No. of tubes = 158.1422/0.303 = 522
For Triangular Pitch
Pt = 1.25do = 25mm
No. of tube passes = 2
Bundle Diameter
Db = do (Nt /K1)1/n1 = 20*10-3 (522/0.249) 1/2.207 = 0.64m

Table 6.11 Tube Pitch
Triangular Pitch Pt = 1.25 do

K1 0.319 0.249 0.175 0.0743 0.0365
N 2.142 2.207 2.265 2.499 2.675
Square Pitch Pt = 1.25 do
K1 0.215 0.156 0.158 0.0402 0.0331
N 2.207 2.291 2.263 2.617 2.643
Using Split Ring Floating Head

Db = 0.64m
Clearance = 62mm
Shell dia.(Ds) = 0.64 + clearance = 702mm
Heat Transfer Coefficient
Tube Side
Mean temperature = (45 + 81)/2 = 63°C
Tube cross-sectional area = πdi2/4 = 201mm2
Tubes per pass = 522/2 = 261
Total flow area = 261*201*106 = 0.0525m2
Mass velocity = Gc = mc/total flow area = 6.8714/0.0525 = 130.884kgm-2s-1
Linear velocity = v = Gc/ρ = 130.884/6.10 = 21.4564ms-1
Prandtl no. = 0.85 (for gases, 0.7 to 1)
Thermal conductivity = k = 0.05 (for gases, 0.006 to .01)
Re = ρdiv/µ = 40981 jh = 3.3*10-3
Figure 6.2 Re vs Heat Transfer Coefficient [10]
hi*di/kc = jh*Re*Pr0.33*(µ/ µw)^0.14

hi = 4005.54Wm-2°C-1
Shell Side
Baffle spacing = Ib = 0.2 to 1(shell dia.)
Area of cross flow AS for hypothetical row at shell equator is
AS = (PT – do) Ds*Ib/ PT = 0.0197m2
Mass velocity = Gh = mh/As = 9.7614/0.0197 = 495.502 kgm-2s-1
Velocity = u = Gh/ρ = 495.502/23.5 = 21.0852m s-1
Equivalent Diameter
De = 4(PT*0.87 PT/2 – 1/2πdo2/4)/(πdo/2)
De = 0.0142m = 14.2mm
Mean temperature = (160+134)/2 = 147°C
Prandtl no. = 0.85 (for gases, 0.7 to 1)
Thermal conductivity = k = 0.053 (for gases, 0.006 to .01)
Re = ρdeu/µ = 77320 jh = 2.3*10^-3
hs*de/kh = jh*Re*Pr0.33*(µ/ µw)0.14 µ/ µw = 1.781
hs = 761.087 Wm-2°C-1
Figure 6.3 Re vs Heat Transfer factor[10]
Pressure Drop
Tube Side
ΔPt = Np(8*jh*(L/di) (µ/ µw) + 2.5) ρv2
ΔPt = 58.792kPa = 4psi
Shell Side
ΔPs = 8* jh*(ds/de) (L/Ib) ρu2/2
ΔPs = 165kPa = 11.235psi
Which is almost acceptable
Typical pressure drops are 30-60 kPa (5-8 psi) on the tub side and 20-30 kPa (3-5 psi) on the
shell side and may reach 10 psi.
Overall Heat Transfer Coefficient
1/Uo = 1/ho + 1/ hod + (do/2Kc) ln(do/di) + (do/di) 1/hid + (do/di) 1/hi

Uo = 21.40 Wm-2s-1
Where
hod = 5000 Wm-2s-1
hod = 4000 Wm-2s-1
Table 6.12 Specification Sheet of Shell & Tube HX
IDENTIFICATION
Item Heat Exchanger
Item number HX-1
Type Shell and Tube HX
DESIGN SPECIFICATION
Length of Tube 4.88m
Outside Tube Diameter 0.02m
Baffle Spacing 0.1404m
No. of Tubes 522
Inside Shell Diameter 0.702m
Shell Passes 1
Tube Passes 2
Pitch 0.025m
Tube Pressure Drop 58.792kPa
Shell Pressure Drop 165kPa
BWG 16
Surface Area 158.1422m2
Tube Heat Transfer Coefficient 4005.54W/m2K
Shell Heat Transfer Coefficient 761.09 W/m2K
6.3 DESIGN OF FLASH
VESSEL
Flash Vessel
6.3.1 Vapor-Liquid Separator
6.3.2 Basic Objectives & Principles
• The primary job of the gas liquid separators is to separate vapor and liquid, but they may
also serve as liquid surge drums.
• The basic design principle of a vapor liquid separator is to provide a sufficiently low gas
velocity so that liquid and vapor will separate.
• The separation of the mixture is actually done due to the actions of gravity and impaction
and also on density.
6.3.3 Selection Criteria
• Length to diameter ratio.

• Separator liquid surge characteristics.
6.3.4 Types of Vapor-Liquid Separator
• Knockout drums.
• Vertical gas liquid separator.
• Horizontal gas liquid separator.
6.3.5 Vertical Gas Liquid Separators

The liquid and gas mixture is separated on the basis of gravity and impaction. The gas liquid
mixture enters the mid of the vessel and strikes with a splash plate which is use for momentum
break and to deflect the stream downward. The gas moves upward and liquid moves downward.
Some vapors carry over the liquid drops and as the drops become large they settle down on the
bottom of vessel due to gravity. If we want a separator of efficiency greater than 95% then we have
to use a demister pad (mist eliminator), by using mist eliminator very small liquid drops can be
from vapor stream. In vertical gas liquid separators L/D should be in the range of 3 to 5 [11].
Figure 6.4 Vertical Flash Vessel
6.3.6 Horizontal Gas Liquid Separator
If L/D is greater than 5 then we use Horizontal Gas Liquid Separator [11]. Designing of this
separator is same as vertical gas liq. Separators except increase Kv by 25%, and the minimum area
of gas flow should be at least 20% of total cross-sectional area of the separator. In this mist
eliminator can be used internally or externally.
Figure 6.5 Horizontal Flash Vessel
6.3.7 Types of Mist Eliminators

• Knitted wire mesh
• Vane type mist eliminator
6.3.8 Mesh Eliminators

Mesh eliminators are made up of plastic or stainless-steel wire with diameter of 0.006-0.011 inch
Figure 6.6 Mesh Type Mist Eliminator
6.3.9 Vane Type Mist Eliminators
Vane eliminators consists of closely spaced plates mist strikes on adjacent vane there they held
by surface force
.
Figure 6.7 Vane Type Mist Eliminator
6.3.10 Design Considerations

• Pressure
• Temperature
• Mass flow rate of liquid
• Mass flow rate of vapor
• Liquid Density
• Vapor Density
• Volumetric flow rate of vapors
• Volumetric flow rate of liquid
6.3.11 Design Procedure

1. Calculate separation factor
2. Calculate the value of Kv using graph or equation.
3. Calculate the minimum cross-sectional area.
4. Calculate the minimum diameter and diameter based on 6 inches increment.
5. Calculate the liquid hold up Ll.
6. Calculate (Umax)nozzle and (Umin)nozzle.
7. Calculate the volume of vapor and Lv.
8. Calculate the length of separator.
9. Check L/D ratio.
10. Calculate the wall thickness.
11. Calculate the nozzle diameter.
This graph is used for the calculation of Kv.
Figure 6.7 [11]
6.3.12 Design of Flash Vessel

Table 6.13 Mass Balance of Flash
Feed Kg/hr K values Liquid(Kg/hr) Vapor(Kg/hr)

O2 625 29.75 0 625
CO2 2627 7.5 0 2627
C2H4 20253 7.37 0 20253
C2H6 1600 5.25 0 1600
C4H6O2 4305 0.14 2659 1646
C2H4O2 4503 0.00418 4330 173
H20 1226 0.0196 1123 103
Total 35141 8112 27029
Table 6.14 Densities of Components
Components 𝝆𝑳 (kg/m3) 𝝆𝑽 (kg/m3)

O2 - 7.27
CO2 - 10
C2H4 - 6.36
C2H6 - 6.82
C4H6O2 941.42 19.55
C2H4 1027.19 13.64
H20 992.2 4.09
Table 6.15 Mass Fractions
Components Liquid Fractions Vapor Fractions

O2 0 0.023
CO2 0 0.097
C2H4 0 0.749
C2H6 0 0.059
C4H6O2 0.327 0.06
C2H4O2 0.533 0.0064
H20 0.138 0.00381
𝜌𝐿 = 992.25 kg/𝑚3
𝜌𝑣 = 7.61 kg/𝑚3
𝑊𝐿 = 8112 kg/ℎ𝑟
𝑊𝑉 = 27029 kg/hr
6.3.12.1 Separation Factor
WL ρV
Separation Factor = K = √
WV ρL
27029 7.61
K= √
8112 992.25
K = 0.29
x = ln(0.29)
x = −1.23
K V = exp(A + Bx + Cx 2 + Dx 3 + Ex 4 + Fx 5 )
A = −1.942 , B = −0.814 , C = −0.197
D = −0.0125 , E = 0.00038 , F = 0.000259
Kv = 0.32
6.3.12.2 Maximum Vapor Velocity
ρL− ρv 0.5
Uvap.max = 0.305K V ( )
ρV
Uvap.max = 1.1m/s
8112×1
QL =
3600×992.25
QL = 2.27×10−3 m3 /s
29027×1
QV =
3600×7.61
QV = 1.05m3 /s
6.3.12.3 Minimum Cross-Sectional Area

1.05
A=
1.1
A = 0.96m2
6.3.12.4 Minimum Vessel Diameter
4A
D=√ = 1.105m
3.14
An increment of 6 inch.
D = 1.13m
6.3.12.5 Hold Up Calculation

VL = QL (Residence Time)
m3 60s
VL =2.27×10-3 ×4min× 1min
s
VL = 0.544m3
0.544 (1.132 )4
Liquid Height = , A= = 1m2
A 3.14
HL = 0.54m
6.3.12.6 𝐇𝐕 Calculation
ρmix = (0.23×992.25) + (0.769×7.61)
ρmix = 234.07kg/m3
100
(Umax. )nozzle= = 6.53ft/s
√ρmin
(Umax. )nozzle = 1.99m/s

60
(Umin. )nozzle= = 3.92ft/s
√ρmin
(Umin. )nozzle = 1.26m/s

4 1.5
HV = (1.99× ) + (1.99× )
3.28 3.28
HV = 3.336m
6.3.12.7 Length of Separator

L = HL + HV = 3.336 + 0.54
L = 3.87m
L
6.3.12.8 Ratio
D
L 3.87
=
D 1.13
L L
= 3.43 3≤ ≤5
D D
6.3.12.9 Calculation of Wall Thickness
t s = α. D + t ′ c
1
t′c = inches
8
t ′ c = 0.0317m
P
αs =
2×ϵs (S) − 1.2P
S = Max. Allowable Stress = 137800kPa [8]
ϵ = Welding Efficiency = 1 [12]
P = 592kPa
αs = 0.00215
t s = (0.00215×1.13) + 0.00317
t s = 0.0056m = 5.66mm
t s = 5.66mm
6.3.12.10 Calculation of Nozzle Diameter
4Qmix
Dnozzle = √
π×60√ρmix
Dnozzle = 0.4m
6.3.13 SPECIFICATION SHEET
Table 6.16 Specifications of Flash Vessel
IDENTIFICATION
Item Flash Vessel
Item number F-1
Type Vertical Flash Vessel
FUNCTION
Gas Liquid Separation
DESIGN SPECIFICATION
Operating Temperature 400C
Operating Pressure 592kPa
Vessel Diameter 1.13m
Hold Up 0.54m
Vessel Height 3.36m
Material Carbon Steel
Wall Thickness 5.6mm
Allowable Stress 137800kPa
Nozzle Diameter 0.4m
6.4 ABSORBER DESIGN
Absorber
6.4.1 Absorption
Absorption is a physical or chemical phenomenon or a process in which atoms, molecules or ions
and some bulk phase-gas, liquid or solid material and since molecules taken up by the volume not
by the surface as in adsorption.
In gas absorption, a soluble vapors or gas is absorbed in the solvent from its mixture with gas
mixture. The 'purpose of such gas scrubbing operations may be any of the following;
• For Separation of component having the economic value.
• As a stage in the preparation of some compound.
• For removing of undesired component (pollution).
Solvent
Liquid applied to remove the solute from a gas stream.
Solute
Components to be removed from an entering stream
6.4.2 Absorber System Configuration

Gas and liquid flow through an absorber may be countercurrent, crosscurrent, or co-current.
The most commonly installed designs are countercurrent, in which the waste gas stream enters at
the bottom of the absorber column and exits at the top. Conversely, the solvent stream enters at the
top and exits at the bottom. Moreover, countercurrent designs usually require lower liquid to gas
ratios than co-current and are more suitable when the loading is higher because of higher intimate
contact between liquid and gas /vapors.
In a crosscurrent tower, the waste gas flows horizontally across the column while the solvent
flows vertically down the column. As a rule, crosscurrent designs have lower pressure drops and
require lower liquid-to-gas ratios than both co-current and countercurrent designs. They are
applicable when gases are highly soluble, since they offer less contact time for absorption.
In co-current towers, both the gas and solvent enter the column at the top of the tower and exit at
the bottom. Co-current designs have lower pressure drops, are not subject to flooding limitations
and are more efficient for fine mist droplets removal. Co-current designs are only efficient where
large absorption driving forces are available [13]. Removal efficiency is limited since the gas-liquid
system approaches equilibrium at the bottom of the tower.
6.4.3 Types of Absorption

• Physical Absorption/ Physio sorption
• Chemical Absorption /Chemisorption
Physical Absorption
In physical absorption mass transfer take place, purely by diffusion and physical absorption
is governed by the physical equilibrium. Physical absorption is easy to handle and it has no heating
effects.
Chemical Absorption
In this type of absorption as soon as a component encounters the absorbing liquid a chemical
reaction take place. Then by reducing the concentration of component in the liquid phase, which
enhances the rate of diffusion.
In our process, the vinyl acetate Is absorbing into acetic acid solution the case under study is
physical absorption.
6.4.4 Types of Absorption Equipment

• Packed Column
• Tray column
• Spray Column
6.4.5 Comparison Between Packed and Plate Column

• Plate columns can be designed to handle a wider range of liquid and gas flow-rates than
packed columns [13].
• Packed columns are not suitable for very low liquid rates.
• The efficiency of a plate can be predicted with more certainty than the equivalent term
for packing (HETP or HTU).
• Plate columns can be designed with more assurance than packed columns. There is
always some doubt that good liquid distribution can be maintained throughout a packed
column under all operating conditions, particularly in large columns.
• It is easier to make provision for cooling in a plate column; coils can be installed on the
plates.
• It is easier to make provision for the withdrawal of side-streams from plate
• columns.
• If the liquid causes fouling, or contains solids, it is easier to make provision for cleaning
in a plate column; manways can be installed on the plates. With small diameter
columns, it may be cheaper to use packing and replace the packing when it becomes
fouled.
• For corrosive liquids, a packed column will usually be cheaper than the equivalent plate
column.
• The liquid hold-up is appreciably lower in a packed column than a plate column. This
can be important when the inventory of toxic or flammable liquids needs to be kept as
small as possible for safety reasons.
• Packed columns are more suitable for handling foaming systems.
• The pressure drops per equilibrium stage (HETP) can be lower for packing than plates;
and packing should be considered for vacuum columns.
• Packing should always be considered for small diameter columns.
6.4.6 Packing
The packing is the most important component of the system. The packing provides sufficient area
for intimate contact between phases. The efficiency of the packing with respect to both HTU and
flow capacity determines to a significance extent the overall size of the tower. The economics of
the installation is therefore tied up with packing choice.
The packings are divided into those types which are dumped at random into the tower and these
which must be stacked by hand. Dumped packing consists of unit 1/4 to 2 inches in major
dimension and are used roost in the smaller columns [14]. The units in stacked packing are 2 to
about 8 inches in size, they are used only in the larger towers.
The Principal Requirement of a Tower packing are:

• It must be chemically inert to the fluids in the tower.
• It must be strong without excessive weight.
• It must contain adequate passages for both streams without excessive liquid hold up or
pressure drop.
• It must provide good contact between liquid and gas.
• It must be reasonable in cost.
Thus, most packing are made of cheap, inert, light materials such as clay, porcelain, or
graphite. Thin-walled metal rings of steel or aluminum are sometimes used [13].
Common Packings are:
• Berl Saddle
• Intalox Saddle
• Rasching rings
• Lessing rings
• Cross-partition rings
• Spiral rings
6.4.7 Selection of Tray Column
• Plate column can be designed with more assurance than packed columns. There is always
some doubt that good liquid distribution can be maintained throughout a packed column
under all operating condition, particularly in large columns that lead to selection of plate.
• Presser drop per equilibrium stage (HETP) can be lower for packing than plates and and
packing should be considered for vacuum columns. As pressure is high in plate column is
selected.
• Plate should always be considered for large diameter columns say greater than 0.6m, where
plates would be easy to install and less expensive
• Plate columns are more suitable for handling non-forming systems as the systems is non-
foaming therefore plate column is selected [15].
From the above consideration, tray column is selected as the absorber, because in our case the
pressure is not very low.
6.4.8 Process of Absorption

• Changing the conditions of the absorption column can influence the effectiveness and
efficiency of absorption. Some important controllable conditions are as follows:
• Pressure of the column.
• Temperature of entering liquid and gas streams.
• Humidity of the gas stream.
• Ratio of the liquid and gas stream rates.
Raising the total pressure of the column may increase the efficiency of the separation because
increasing the pressure decreases the liquid flow rate and increases the concentration of the gas.
The temperature of entering liquid effect absorption in that it effects the flow rate of liquid required
for the separation with a given number of stages. Increasing the temperature of the entering solvent
increases the liquid flow rate required.
Inlet gases of the absorber with high humidity at a high temperature effect the capability of the gas
to consume latent heat hindering the absorption process. Therefore, dehumidification of the inlet
gas should be considered for absorbers with large heat effects. The ratio of the liquid to gas stream
rates in that if the ratio is too low, the solute builds in the upper portion of the column causing a
higher temperature profile in the top of the column. As a result, internal cooling maybe necessary
for lower liquid to gas ratios so we are using a cooler to decrease the temperature and enhancing
the absorption process.
6.4.9 Selection of Solvent
The ideal absorbent should have:
• have a high solubility for the solute
• have a low volatility to reduce loss of absorbent
• have a low viscosity to provide a low pressure drop
• be non-toxic
• Easily available and not expensive.
An organic solvent, vinyl acetate, is preferred because they are chemically stable. During mass
transfer in the absorption column small quantities of solvent are lost, and the energy consumption
is low because water evaporation is not required and the production of the by-product is also low.
6.4.10 Design Consideration

Design of the absorber involves the following parameters
• Capacity
• Column height
• Type and size of packing
• Pressure drop
• Flooding velocity
• Column internals
• Mechanical design
Objective
To remove vinyl acetate
Media for Absorption

Acetic acid
Equipment
Tray column
Operating Conditions
Inlet flow rate of the gas = 27029 kg/hr
Operating temperature = 353K
Operating pressure = 885kPa
Inlet flow rate of vinyl acetate = 26.54 kgmol/hr
Inlet flow rate of vinyl acetate=.025kgmol/hr
Specifications:
K=Pi/Xi *P=.036(equilibrium constant)
Ai=(L/V) *K=1.26(Absorption factor)
Minimum(Lo/VN+1) for C4H6O2
(Lo/VN+1) = KiEai=.0356
Operating (L0/VN+1)0=.049
Operating absorption factor
(Aio)=(L0/VN+1) (1/Ki)
=1.36
For optimum design
1.2 < Aio < 2.0 [15]
As the value in the range so, our design is optimum
Theoretical number of stages at operating(L0/VN+1)

Eai=(AN+1-A)/(AN+1-1)
After solving the equation by iterative method, we have N=10
Actual number of stages at operating (L0/VN+1)

Eo around 40-50% (stage efficiency)
Actual trays Nact=N/Eo=10/.45=22 stages
Nact:actual no of stages
N: theoretical no of stages
Diameter evaluation:
Vsf=Csb(α/20)0.2/ (ρL- ρg)/ ρg)0.5
Vsf : net vapor velocity at flooding velocity m/s
α: Surface tension
ρg: density of gas
ρL: density of liquid
Csb:souder and brown factor at flood conditions m/s
Csb is obtained after specifying a reasonable tray spacing. Standard tray spacing for large
diameter column area is 0.4 or 0.6m
Tray spacing of 0.45m is selected
Vsf= 0.635 m/s
VN=0.7(Vsf)=0.539m/s
An=mv/VN=11.93m2
An: is the net column area
VN: actual vapor velocity
Ac=85% of An
An/0.85=11.93/0.85=14.04m2
D=(4Ac/3.14)0.5=4.8m
Where Ac is cross sectional area of the column and D is diameter of column
Height evaluation:
Hact=(Nact-1) Hs+dH
=10.8
Hact=Actual column height
Hs=Plate spacing (selected as 0.45m)
dH= additional height required for column operation
dH=3*Hs=1.35m
Specification of tray layout:

Ad (down comer Area) =0.12 *Ac
=2.1m2
Aa (Net actual Area) =Ac-Ad
Aa (actual area) =Ac-2Ad=9.88m2
Lw (weir length) = is 0.85 of the weir diameter
=4.13mm
hw (weir height) =50mm
dh (hole diameter) =5mm
Plate thickness =3mm
hwc=750(Lw/ρLw)2/3
=2.8mm of liquid
Weep point calculation:

hw=(k2-0.90(25.4-dn)/ (ρv)1/2
hw=50mm
hw+hwo=52.8
Minimum vapor velocity through holes
ub=(k2-0.90(25.4-dn)/ (ρv)1/2
so, un=22.87 m/s
Actual vapor velocity through holes
Ah=0.589m2
Uact=-0.7(Vm/Ah) =27m/s
As Uact>Uhmin so weeping will not occur.
Pressure drop calculations
The ratio of hole to perforated area
An/Ap=0.9(dn/Ip)2
Ip(hole pitch): between 2.5-4 times dn.
Ap=6.40m2
AN/Ap*100=10
Pitch thickness of 3mm is selected
hd=51(ub/a)2 ρv/ρL
hd=pressure drop per stage
hr=12.5*103/ρL
h=residual head=13.09mm of liquid
hf=hd+(hw+hwo)+hr
Actual plate drop=hf
hf=80.57mm of liquid
dP=for one tray=0.009*ht*ρ
=0.75kPa
Pressure drop for column=N*dP
=16.6kPa
6.4.11 Specification sheet
Table 6.17 Specifications of Absorber
IDENTIFICATION
Item Plate absorber
Type Plate column
No of items 1
FUNCTION
Removal of vinyl acetate from gas mixture
COLUMN DESING SPECIFICATION
Operating temperature 353K
Operating pressure 885kPa
Design temperature 361K
Design pressure 920kPa
Number of actual stages 22
Net area of column 11.9m2
Column diameter 4.8m
Height of column 10.8m
Total pressure drop 16.6kPa
%flooding 80%
Contacting device Trays
Tray type Sieve type
Column cross sectional area 14m2
Material of construction Stainless steel
6.5 DISTILLATION
COLUMN DESIGN
Distillation
In an industry, in order to gain purified product distillation columns are used. Distillation column
is a mass transfer equipment in which on the basis of relative volatility components of mixture are
separated. There are two major sections, stripping and rectification section. Lighter components
will be obtained at the upper end and heavy products will be obtained from bottom.
In engineering terms, distillation columns have to be designed with a larger range in capacity than
any other types of processing equipment, with single columns 0.3–10 m in diameter and 3–75 m
in height [15]. Designers are required to achieve the desired product quality at minimum cost and
also to provide constant purity of product even though there may be variations in feed composition.
6.5.1 Types of Distillation Column
6.5.2.1 Batch Distillation Column

In batch operation feed the feed is introduced batch wise. The column is charged with the batch
and then distillation process is carried out. When the desired task is achieved, a next batch of feed
is introduced.
6.5.2.2 Continuous Distillation Column

In contrast, continuous columns process a continuous feed. No interruption occurs unless there is
problem with column or surrounding process units. They are capable of handling of high
throughputs and is the most common of the two types. We shall concentrate only on this type of
column.
6.5.3 Selection of Column Type
Following are the two types of distillation column

• Packed column
• Tray column
Random packed columns are generally not designed with diameters larger than 1.5 m and diameters
of commercial tray columns are seldom less than 0.67 m. [15]
Since diameter is greater than 1.5 m so we will use tray column
Further benefits of tray column over packed column are following:
• Plate columns have ability to handle wide variety of liquid flow rates as compared to
packed column.
• If liquid flow rate is lower than vapor flow rate then tray columns are preferred because
this situation can cause dispersion. And dispersion can be easily handled in tray column.
• For dirty fluids when cleaning is required, man holes can be provided for this purpose
in tray column. While in packed column removal of packing is needed to be done for
this purpose.
• To handle non-foaming systems, plate columns are generally used.
• For high height columns, weight of plate column is less as compared to packed column.
• Design data for plate column is swell established and easily available.
• If there are temperature variations, then plate columns are best to used.
• For larger diameters, plate columns are used.
6.5.4 Types of Plates
There are three types of plates including

• Sieve plate
• Bubble cap
• Valve plates
6.5.5 Application of Sieve Plates

• Pressure drop in sieve plate is lower than others
• Their design data is well established
• They are economical. Their cost is low
• They are lighter in weight
• Cleaning is easy in sieve plates
6.5.6 Design Steps of Distilation Column

• Calculation of minimum number of stages
• Calculation of minimum reflux ratio
• Calculation of actual reeflux ratio
• Calculation of theoratical number of stages
• Calculation of actual number of srages
• Calculation of diameter of column
• Calculation of weeping point
• Calculation of pressure drop
• Calculation of thichness of shell
• Calculation of height of column
6.5.6.1 Basic Deta For Design of Distillation Column
Figure 6.8 Distillation Column

Table 6.18 Material Balance of Distillation Column
Feed (mol frac) Top (mol frac) Bottom (mol frac)

Vinyl acetate 0.21 0.45 0.0004
Acetic acid 0.5 0.02 0.91
Water 0.29 0.53 0.09
Liquid density 920 kg/m3 940 kg/m3
Vapor density 1.698 kg/m3 2.086 kg/m3
Heavy key = acetic acid
Light key = vinyl acetate monomer(VAM)
6.5.6.1.1 Nature of Feed
By bubble T calculation
TB = 98Oc which is greater than feed temperature Tf = 42.5 oC
So, feed is subcooled liquid at Tf = 42.5 and Pf = 26.7 psia
6.5.6.2 Calculation of Minimum Number of Stages

𝑥 𝑥
𝑙𝑜𝑔 [(𝑥 𝐿.𝐾 ) ( 𝑥𝐻.𝐾 ) ]
𝐻.𝐾 𝐷 𝐿.𝐾 𝐵
𝑁𝑚𝑖𝑛 =
𝑙𝑜𝑔(𝛼𝑎𝑏 )𝑎𝑣𝑔
where 𝛼𝐴𝐵 is the average relative volatility of the light key (VAM) with respect to the heavy
key (acetic acid), and XLK and XHK. are the light and heavy key composition. The relative
volatility is taken as the geometric mean of the values at the column top and bottom
temperatures.
(𝛼𝐴𝐵 )𝑎𝑣𝑔 = √(𝛼𝐴𝐵 )𝐷 (𝛼𝐴𝐵 )𝐵
=4.20
0.45 0.91
𝑙𝑜𝑔 [(0.02) (0.0004) ]
𝐷 𝐵
𝑁𝑚𝑖𝑛 =
𝑙𝑜𝑔(4.20)
𝑁𝑚𝑖𝑛 = 8 (𝑟𝑒𝑏𝑜𝑖𝑙𝑒𝑟 𝑖𝑠 𝑒𝑥𝑐𝑙𝑢𝑑𝑒𝑑)
6.5.6.3 Calculation of Minimum Reflux Ratio
As feed is subcooled so we can calculate q using following equation

𝐶𝑃𝐿 (𝑇𝐵 −𝑇𝐹 )
𝑞 =1+
𝜆
Where
28094𝐽
𝐶𝑃𝐿 = 123𝐽/𝑚𝑜𝑙 𝜆= TB = 98 oC and TF = 42.5 oC
𝑚𝑜𝑙
By putting all these values, we get q = 1.333
Now from Underwood equitation
𝑛
𝛼𝑖 𝑋𝐹𝑖
∑ =1−𝑞
𝛼𝑖 − 𝜃
𝑖=1
𝜃 = 2.75
Bu using equation of minimum reflux ratio
𝑛
𝛼𝑖 𝑋𝐷𝑖
∑ = 𝑅𝑚𝑖𝑛 + 1
𝛼𝑖 − 𝜃
𝑖=1
𝑅𝑚𝑖𝑛 = 0.59
6.5.6.4 Actual Reflux Ratio

To calculate the actual reflux ratio, we used the following rule of thumb
𝑅 = (1.2 … … … 1.5)𝑅𝑚𝑖𝑛 [16]
𝑅 = (1.37)0.59
R = 0.81
6.5.6.5 Theoretical Number of Plates

From Gilliland correlation
𝑁 − 𝑁𝑚𝑖𝑛 𝑅 − 𝑅𝑚𝑖𝑛 0.566

= 0.75 [1 − ( ) ]
𝑁+1 𝑅+1
By putting the values of “R” and “Nmin”

N=18
6.5.6.6 Actual number of trays
Overall tray efficiency

The overall column efficiency is correlated with the product of the relative volatility of the light
key component (relative to the heavy key) and the molar average viscosity of the feed, estimated
at the average column temperature.
Eduljee has expressed the O'Connell correlation in the form of mathematical expression
Eo  51  32.5log[( AB )av .( av )] [17]

Where
µavg = molar average liquid vscosity mNS⁄m2
𝛼𝑎𝑣𝑔 = average relative volatility of the light key = 4.20
Average temperature of column = (116+82)/2 = 99 oC
𝜇𝑎𝑣𝑔 = 0.092 𝑚𝑁𝑆⁄𝑚2
EO = 65 %
18
𝑎𝑐𝑡𝑢𝑎𝑙 𝑡𝑟𝑎𝑦𝑠 =
0.65
𝑁𝑜 𝑜𝑓 𝑎𝑐𝑡𝑢𝑎𝑙 𝑡𝑟𝑎𝑦𝑠 = 27
The Kirk bride method is used to determine the ratio of trays above and below the feed point.
2
𝑁𝐷 𝐵 𝑥𝐻.𝐾 (𝑥𝐿.𝑘 )𝐵
log = 0.206 log [( ) ( ) ( ) ]
𝑁𝐵 𝐷 𝑥𝐿.𝐾 𝐹 (𝑥𝐻.𝐾 )𝐷
Where
ND = number of stages above the feed, including any partial condenser,
NB = number of stages below the feed, including the reboiler,
B = molar flow bottom product,
D = molar flow top product,
Xf,HK = concentration of the heavy key in the feed,
Xf,LK = concentration of the light key in the feed,
Xd,HK = concentration of the heavy key in the top product,
Xb,LH = concentration of the light key if in the bottom product.
2
𝑁𝐷 122 0.5 (0.0004)𝐵
log = 0.206 log [( )( ) ( ) ]
𝑁𝐵 111 0.21 𝐹 (0.02)𝐷
𝑁𝐷
= 0.2433
𝑁𝐵
NB +ND = 27
Simultaneously solving both equation, we get
ND = 6 and NB = 21
6.5.6.7 Calculation of Column Diameter
Basic calculations are
Table 6.19 Distillation Data
Top condition Bottom condition

LN = 90 kgmol/hr Lm = 323 kgmol/hr
VN =200 kgmol/hr Vm = 201kgmol/hr
MWT = 50 kg/kgmol MWT = 56kg/kgmol
T =82 OC T = 116 OC
Density = 920 kg/m3 Density = 940 kg/m3
Flow Parameter
Liquid vapor factor
𝐿𝑁 𝜌𝑉 0.5
𝐹𝐿𝑉 = ( )( )
𝑉𝑁 𝜌𝐿
FLV = 0.02
Capacity Parameter
Tray spacing = 0.6 m
From figure 15.5 we get Csb =0.06
𝑑𝑦𝑛𝑒𝑠
𝑠𝑢𝑟𝑓𝑎𝑐𝑒 𝑡𝑒𝑛𝑠𝑖𝑜𝑛 𝑜𝑓 𝑚𝑖𝑥𝑡𝑢𝑟𝑒 = 𝜎 = 20
𝐶𝑚
Flooding velocity
𝜎 0.2 𝜌𝐿− 𝜌𝑉 0.5
𝑉𝑛𝑓 = 𝐶𝑠𝑏 ( ) ( )
20 𝜌𝑉
Vnf = 0.22 m/s
Assume 80% of flooding, then actual vapor velocity
Vn=0.80(Vnf)
Vn = 0.17 m/s
Net area used
𝑚̇ 𝑣
𝐴𝑛 =
𝑉𝑛
𝑣𝑎𝑝𝑜𝑟 𝑚𝑜𝑙𝑎𝑟 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒×𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑒𝑟 𝑤𝑒𝑖𝑔ℎ𝑡
Volumetric flow rate of vapor = 𝑚𝑣 =
𝑑𝑒𝑛𝑠𝑖𝑡𝑦×3600
ṁ v
An = = 1.362m2
Vn
Assume the down comer occupies 17% of cross sectional area of column(AC)
𝐴𝑐 = 𝐴𝑑 + 𝐴𝑛
𝐴𝑐 = 0.17(𝐴𝑐 ) + 𝐴𝑛
𝐴𝑛
𝐴𝑐 = = 2.243 𝑚2
0.83
So the dia of the column is
4×𝐴𝑐
𝐷𝑐 = √ = 1.69 𝑚
𝜋
6.5.6.8 Liquid Flow Arrangement
In order to find liquid arrangement, first we find the maximum volumetric liquid flow rate.
Maximum liquid flow rate is at the bottom of the column that is Lm
𝑣𝑎𝑝𝑜𝑟 𝑚𝑜𝑙𝑎𝑟 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒×𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑒𝑟 𝑤𝑒𝑖𝑔ℎ𝑡
Volumetric flow rate of liquid = 𝑞𝐿 = 𝑑𝑒𝑛𝑠𝑖𝑡𝑦×3600
=0.0055m3/s
from figure, cross flow single pass plate is selected
Figure 6.9 [15]
6.5.6.9 Provisional Plate Design
Column Diameter = Dc = 1.69 m

Column Cross sectional Area = Ac = 2.243 m2
Down comer area = Ad = 0.17(2.243) = 0.3814
Net Area = An = Ac - Ad = 1.862 m2
Active Area = Aa = Ac - 2Ad = 1.681 m2
Hole Area = Ah = 0.06(1.681) = 0.1 m2
Weir Length
𝐴𝑑 0.381
= = 0.17
𝐴𝑐 2.243
From figure 11.31 (Coulson & Richardson vol 6)
𝑙𝑤
= 0.82
𝐷𝑐
lw = 0.82 × 1.69 = 1.38 m
Take weir length, hw = 40 mm
Hole diameter, dh = 3mm
Plate thickness = 3mm
6.5.6.10 Check Weeping Figure 6.10 [15]
The lower limit of the operating range occurs when liquid leakage through the plate holes become
excessive. This is known as the weep point. The vapour velocity at the weep point is the minimum
value for stable operation
[K 2 − 0.9(25.4 − dh )]
Uh =
√ρv
Uhmin = minimum vapour velocity through the holes (based on the hole area), m/s,
dh = hole diameter, mm,
K2 = a constant, dependent on the depth of clear liquid on the plate, obtained
from Figure 11.30
to find out value of constant K2, we should find the height of the liquid crest over the weir
2
Lw 3
how = 750 [ ]
ρL lw
Lw = weir length, m = 1.38 m
Lw = liquid flow-rate, kg/s. = 5kg/s
At maximum flow rate,
2
5 3
how = 750 [920×1.38] = 18.76mm
Minimum flow rate = 70% of Lm

(which is5 kg/s)
At minimum flowrate Figure 6.11 [15]

2
0.7×5 3
ℎ𝑜𝑤 = 750 [ ] = 14.79𝑚𝑚
920×1.38
ℎ𝑤 + ℎ𝑜𝑤 = 40 + 14.79
= 54.14 𝑚𝑚 Figure 6.12
Now from figure 11.30 (Coulson & Richardson vol 6)

𝐾2 = 30.1
So, minimum design velocity is given by
[30.1−0.9(25.4−3)] 𝑚
𝑈ℎ = 𝑈ℎ = 6.9 𝑠 Actual Uh(min) on base of active hole area
√2.086
min 𝑣𝑎𝑝𝑜𝑟 𝑓𝑙𝑜𝑤 𝑉𝑉

𝑈ℎ(min) = = 0.7 [ ]
ℎ𝑜𝑙𝑒 𝑎𝑟𝑒𝑎 𝜌𝑣 𝐴ℎ
2.77 𝑚
𝑈ℎ(min) = 0.7 [ ] = 9.307
2.08×0.1 𝑠
So, the minimum vapor rate will be well above the weeping point
6.5.6.11 Plate Pressure Drop
The pressure drop over the plates is an important design consideration. There are two main sources
of pressure loss: that due to vapour flow through the holes (an orifice loss), and that due to the
static head of liquid on the plate.
Dry Plate Pressure Drop

Maximum vapor velocity through holes
max vapor flow
Uh =
hole area
2.77 m
UH = [ ] = 13.35
2.08×0.1 s
plate thickness 3
= =1
hole dia 3
Ah Ah Ah
≅ ×10
AP Aa Aa
0.1 Figure 6.12 [15]

= ×100 = 5.95
1.68
From figure 11.34
(Coulson & Richardson vol 6)
Co = 0.81
Uh 2 ρV
hd = 51 ( )
C0 ρL
13.35 2 2.08
hd = 51 ( ) = 32mm
0.81 920
Residual Head
12.5×1000
hr =
ρL
12.5×1000
hr = = 13.6 mm
920
Total pressure drop is
ht = hd + hw + how + hr
ht = 32 + 54.24 + 14
ht = 100 mm
Total Column Pressure Drop Per Plate
9.81×ht ×ρl
∆Pt =
1000
9.81×100×920
∆Pt = = 903 pa
1000
∆Pt = 0.13 psia
6.5.6.12 Downcomer Liquid Back-Up
Downcomer liquid back-up is caused by pressure drop over the plate and resistance to flow in
downcomer itself,
ℎ𝑏 = ℎ𝑑𝑐 + (ℎ𝑤 + ℎ𝑜𝑤 ) + ℎ𝑡
where hb = downcomer back-up, measured from plate surface, mm,
hdc = head loss in the downcomer, mm.
𝐿𝑤𝑑 2
ℎ𝑑𝑐 = 166 [ ]
𝜌𝐿 𝐴𝑚
Lwd = liquid flow rate in downcomer, kg/s,
Am = the clearance area under the downcomer
ℎ𝑎𝑝 = ℎ𝑤 − (5 𝑡𝑜 10 𝑚𝑚)
ℎ𝑎𝑝 = 40 − 10 = 30 𝑚𝑚
𝐴𝑎𝑝 = ℎ𝑎𝑝 𝑙𝑤
𝐴𝑎𝑝 = 0.03×1.38 = 0.0414 𝑚2
Which is less than Ad so Aap use to find hdc

2
5
ℎ𝑑𝑐 = 166 [ ] = 2.9 𝑚𝑚
920×0.0414
so
ℎ𝑏 = 2.9 + 54.14 + 100 = 157 𝑚𝑚
ℎ𝑏 = 0.157 𝑚
As,
𝑡𝑟𝑎𝑦 𝑠𝑝𝑎𝑐𝑖𝑛𝑔 + 𝑤𝑒𝑖𝑟 ℎ𝑒𝑖𝑔ℎ𝑡
ℎ𝑏 <
2
0.6 + 0.04
ℎ𝑏 <
2
0.157 < 0.32
So, tray spacing is acceptable
6.5.6.13 Check Residence Time
Sufficient residence time must be allowed in the downcomer for the entrained vapour to
disengage from the liquid stream; to prevent heavily "aerated" liquid being carried under
the downcomer.
A time of at least 3 seconds is recommended.
The downcomer residence time is given by:
Ad hbc ρL 0.3814×0.157×920
tr = =
Lwd 5
t r = 11 sec
That is greater than 3 secs, so it is satisfactory.
6.5.6.14 Check Entrainment
Actual velocity = 0.17 m/s

Flooding velocity = 0.21 m/s
Percent flooding = 80%
FLV = 0.09
FROM FGURE 11.29
𝜑 = 0.03
That is well below upper limit that is 0.1
6.5.6.15 Number of Holes
Figure 6.13 [15]

π π
Area of a hole = dh 2 = 0.0032
4 4
= 7.1×10−5 m2
Area of n hole = 0.1 m2
0.1
number of hole =
7.1×10−5
number of holes = 1428
6.5.6.16 Height of Column
Hc = (Nactual − 1)HS + ∆H
∆H = 1 − 1.5% of total height for liquid hold up
= 0.5
tray thickness = 3mm
total tray thickness = 0.003×27 = 0.08m
Ht = (26×0.6) + 0.5 + 0.08
= 16m
L
= 9.4 < 20
D
Its value should be preferable less than 20
Table 6.20 Specification Sheet of Distillation Column
Identification
Item Distillation column
Type Plate column
No. of items 1
Function
Separation of acetic acid from vinyl acetate and water
Column design data
Operating temperature 373 K
Operating pressure 101.325 kpa
Design temperature 410 K
Design pressure 111 kpa
Actual no. of stages 27
Net area of column 1.362 m2
Column diameter 1.69 m
Height of column 16 m
Total pressure drop 1.3 kpa
%flooding 80%
Entrainment 3%
Tray type Sieve tray
Plate thickness 3 mm
Reflux ratio 0.81
Hole diameter 3 mm
Number of holes 1428
Column cross-sectional area 2.243 m2
Weir height 40 mm
Weir length 1.38 m
Tray spacing 0.6 m
Material of construction Stainless steel
CHAPTER 07
INSTRUMENTATION AND
CONTROL
Instrumentation and Control
Instrumentation is provided to monitor the key process variables during plant operation. They may
be incorporated in automatic control loops or used for the manual monitoring of the process
operation. They may also be part of an automatic computer data logging system. Instruments
monitoring critical process variables will be fitted with automatic alarms to alert the operators to
critical and hazardous situations. It is desirable that the process variable to be monitored can be
measured directly; often, however, this is impractical and some dependent variable that is easier to
measure is monitored in its place.
7.1 Instrumentation and Control Incentives

There are three primary objectives of instrumentation and control schemes [18]
• To minimize the influence of external disturbances
• To ensure the stability of the process
• To optimize the operation of the chemical plant
7.2 Control Parameters

In most of the plants, the parameters that are to be measured, controlled and monitored are almost
the same. These are level, temperature, pressure and flow rate.
7.3 Controllers
Based upon the parameters that can be controlled, there are mainly four types of controllers;
7.3.1 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 [18]. Venture tubes and turbine meters are also used.
7.3.2 Temperature Controllers
Thermocouples are the most commonly used temperature sensing devices. The two dissimilar
wires produce a produces voltage difference when they are subjected to temperature difference.
7.3.3 Pressure Controllers
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.
7.3.4 Level Controllers
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).
• 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.
7.4 Types of the Control Loops
For instrumentation and control of different sections and equipment of plants, following control
loops are most often used.
1. Feedback control loop

2. Feed forward control loop
3. Ratio control loop
4. Auctioneering control loop
5. Split range control loop
6. Cascade control loop
7.5 Control Scheme of Shell and Tube Heat Exchanger

7.5.1 Objective
Our control objective is to maintain the temperature of outlet process stream at 40oC.
7.5.2 Manipulated Variables
The manipulated variables in our case can be
Flow rate of the utility stream
7.5.3 Loads or Disturbances
Following are typical disturbances
• Change in the temperature of the utility stream
• Change in the temperature of the process stream
• Change in flow rate of utility stream
• Change in flow rate of process stream
.
7.5.4 Control loop of Shell and Tube Heat Exchanger
Figure 7.1 Instrumentation & Control of Shell & Tube HX
CHAPTER 08
HAZOP ANALYSIS
HAZOP Analysis
It is important to evaluate and identify the problems and hazards that cause the process parameters
to deviate from intended design. For this purpose a detailed hazard analysis is done under a multi-
disciplinary team. The more formalized hazard assessment technique is HAZOP.
HAZOP is a structured and systematic technique to assess and evaluate potential hazards in a
chemical process and identifying the operability problems that may lead to risk to personnel or
equipment, or prevent efficient operation. HAZOP is based on a theory that assumes risk events
are caused by deviations from design conditions.
HAZOP studies have been used with great success within chemical and the petroleum industry to
obtain safer, more efficient and more reliable plants. It’s a well-known and well documented study
and is used as a part of Quantitative Risk Assessment (QRA). A HAZOP analysis provides a full
review of a process system and systematically questions every part of it to establish how deviations
from design intensions might arise.
8.1 HAZOP Effectiveness

The success or failure of HAZOP depends upon several factors:
• The completeness and accuracy of drawings (P&ID) and information available to the
team- the information should be updated.
• The technical skills and insights of the team
• The ability of the team to concentrate on the more serious hazards identified.
• The ability of the team to use the systematic approach of their imagination as an aid in
visualizing deviations, causes and consequences.
8.2 HAZOP Methodology
The HAZOP analysis is executed in four steps:
8.2.1 Definition
• Define scope and objectives

• Define responsibilities
• Select team
8.2.2 Preparation
• Plan the study

• Collect data
• Estimate time Estimate time
• Arrange a schedule
8.2.3 Examination
• Divide the system into parts

• Select a part and define design intent
• Identify deviation by using guide words on each element
• Identify consequences and causes
• Identify whether a significant problem exists
• Identify protection, detection, and indicating mechanism
• Identify possible mitigating measures
• Repeat for each element and then for each part
8.2.4 Documentation and Follow Up
• Record the examination

• Sign off the documentation
• Produce the report of the study
• Follow up that actions are implemented
• Re-study ay part of the system if necessary
• Produce final output report
8.3 HAZOP Terminologies
System:
The location at which the process parameters are investigated for deviations For example, heat
exchanger, reactor, pump, compressor, valve or pipelines.
Intension:
The intension defines how the system is intended to operate in the absence of deviations.
Deviations:
It’s a way in which process conditions deviate from the design intentions which are discovered by
applying the guide words.
Causes:
These are the reasons why deviations might occur. These causes can be hardware failure, human
errors or external disruption.
Consequences:
These are the results of the deviations. Consequences may comprise both process hazards and
operability problems.
Guide Words
These are the simple words applied on process parameters used to identify possible deviations.
HAZOP Analysis
Table 8.1 Guide Words [19]
GUIDE WORDS MEANINGS

No or not No part of the intent is achieved, and nothing else occurs
Less Quantitative decrease
More Quantitative increase
Part of Qualitative decrease (i.e. only one of the two components in a
mixture)
As well as Qualitative decrease (e.g. an impurity)
Reverse Opposite
Other than Complete substitution
8.4 Steps in HAZOP
The HAZOP process can be organized into the following steps:
• Divide the process into sections. (i.e. reactor, heat exchanger)

• Choose a study note. (i.e. line, vessel, pump)
• Describe the design intent.
• Select a process variable.
• Apply a guide word.
• Identify the deviations of the process from the intended design
• Determine possible causes of the deviations.
• Evaluate consequences.
• Recommend action.
• Record information.
• Repeat procedure for other sections of the process.
8.5 HAZOP of Acetic Acid Tank
Table 8.2 HAZOP of Acid Tank
Variable Operating Event Consequences Process

condition indications
Level Less Runs dry Cavitation LIA-1
rupture Fire FICA-1
V-3 open Reagent release LIA-1
V-1 open Reagent release LIA-1
Rupture Reagent release LIA-1
More Unload Overfill LIA-1
too much
Reverse Overfill LIA-1
flow
No Same as
less
Pressure Less Break in Reagent release PICA-1
line
Lose N2 Implosion PICA-1
PV-2 fail Implosion PICA-1
PICA-1 fail Implosion PICA-1
More PICA-1 fail Reagent release PICA-1
via RV-1
PV-1 fail Reagent release PICA-1
via RV-1
V-7 Reagent release PICA-1
closed via RV-1
Overfill Reagent release PICA-1
via RV-1
Temperature Less inlet is Thermal stresses PICA-1
less
Low Thermal stresses PICA-1
pressure
More Inlet is Reagent release PICA-1
high T via RV-1
External Tank fail PICA-1
fire

TO ATMOSPHERE
TO FLARE
RV-1 Nitrogen
V-7
PIC
A-1 PV
-1
FROM LIA-1
DISTILLATION Acetic acid
COLUMN storage Tank T-1
FICA-1
V-1 PI-1
V-7
P-1
FV-1
V-4
V-3
Figure 8.1 HAZOP diagram of the storage tank

CHAPTER 09
ENVIRONMENTAL
IMPACTS ASSESSMENT

9.1 General Substance Information
CAS Number: 108-05-4 [20]
EINECS Number: 203-545-4 [20]

IUPAC Name: vinyl acetate
Molecular weight: 86 g/mol
Molecular formula: C4H6O2
Structural formula:
O
CH
H2C O CH3
Purity
Purity: 99.8 % w/w
Impurities: ≥ 0.03 - 0.1 % w/w water
≥ 0.005 - 0.01 % w/w acetic acid
≥ 0.005 - 0.02 % w/w acetaldehyde
Additives: Hydroquinone/hydroquinone mono methyl ether for stabilization
0.00015 - 0.002 % w/w [20]

9.2 Classification
Table 9.1 Classification of Hazards [20]
Harmful R 20 Harmful by inhalation

Irritant R 37 Irritating to respiratory system
Carcinogenic, Cat. 3 R 40 Limited evidence of a carcinogenic effect
The only valid test i.e. RCC, 2003 showed mild irritation effects on skin of rabbits that don’t need
classified. Its eye irritation potential seems to be mild as found by eye irritation tests with rabbits.
So, it does not need any classification about eye irritation. Severe irritation was found by testing
on rats in respiratory tract.
Skin sensitization study results (Buehler Test) on animals showed mild effects on commercial
grade. Local Lymph Nodes Assay (LLNA) showed no significant positive stimulation responses
at concentrations of 5% - 100% [20]. Overall, the results of both studies indicated that vinyl acetate
has mild skin effects.
Clear evidence for carcinogenic effect of vinyl acetate is there. The carcinogenic potential is by
inhalation and oral route of exposure. Its exposure also produces tumors at first contact along
exposure routes. The tumor responses are due to site-specific enzymatic activities.
9.3 General Information on Exposure

9.3.1 Production
Vinyl acetate can be produced by a vapor phase reaction between ethylene and acetic acid in gas,
liquid phase or a fluidized-bed process in presence of catalyst. Five manufacturers of VAM were
identified in Western Europe with a manufacturing capacity of 800,000 t/a (CEFIC). Changing
operating capacity makes it hard to give a general figure about the annual production of VAM in
the EU [21].
From almost 1045000 tonnes total supply, some unmeasured amounts were exported outside
Western Europe. With an end stock2 of about less than 50000 tonnes in 2002, approximately
750,000 tonnes of VAM were marketed in Western Europe that year (figures provided by CEFIC
Acetyls Sector Group) [21].
9.3.2 Uses
Vinyl acetate monomer is only used as an intermediate for manufacturing of vinyl acetate
(co)polymers. Hence it is concluded that all the volume of VAM is used for the manufacturing
different polymers mainly polyvinyl acetate. Besides the manufacture of homo-polymers, VAM is
combined with other monomers like ethylene, vinyl chloride and acrylic acid esters to produce
various types of co-polymers.
Polymers manufactured from VAM are used in a broad spectrum of products including water based
paints, printing inks, lacquer, ceramic, adhesives for packaging and construction, paper finishing
and protective colloids for various materials. Other important products include textile fibers, paper
coating and inks.
VAM is used as feed for manufacturing vinyl alcohol (co)polymers (e.g. polyvinyl alcohol).

9.4 Environmental Exposure
As VAM is used as an intermediate in manufacturing of a wide range of polymeric materials, its
release into the environment is definite during various life cycle stages and from the final products
and other substances produced from VAM. It is comparatively volatile substance that evaporates
into the atmosphere primarily via off-gas. Also, due to high-water solubility of VAM, emissions
may occur to the aqueous phase if it gets in contact with water. Therefore, waste water may in turn
be a source for its emission into the atmosphere during post-treatment (e.g. stripping).
9.5 Effects Assessment

9.5.1 Acute Toxicity
Human data on the acute toxicity of VAM are not available. In tests with rats LD50 values in two
studies were 3470 and 3500 mg/kg, respectively. A dermal LD50 value of 7440 mg/kg was found
from a range finding study with rabbits. Thus, it does not need to be labelled according to EU
criteria with respect to acute oral and dermal toxicity. Inhalation toxicity testing, however, resulted
in LC50 values of 15.8 mg/l/4 hours and 14.1 mg/l/4 hours in rats which requires its classification
as harmful and need to be labelled with “R 20” i.e. harmful by inhalation [22].
9.5.2 Irritation
Except a general notice from occupational use, no substantiated human data about irritation caused
by VAM are available.
Based on only valid tests (RCC, 2003a and c), mild irritation effects on the skin and eyes of rabbits
were observed that do not need classification. Earlier studies indicated pronounced irritation of
skin after extended exposure periods but they were less reliable.
Acute inhalation on rats demonstrated severe irritation in animal respiratory tract. Thus, VAM
should be labelled “R 37” i.e. irritating to respiratory system. In September 2007, the TC C&L
agreed on R37 [22].
9.5.3 Corrosiveness
There is no evidence about corrosiveness of VAM based on data about irritation.
9.5.4 Sensitization
There haven’t been any cases of skin sensitization due to VAM contact. However, the data about
humans obtained at the workplace is of limited importance for assessment of skin sensitizing
potential of VAM. No data is there to conclude that it has no sensitizing effect on skin.
9.5.5 Carcinogenicity
Inhalation of monomer leads to a number of nasal tumors (largely papillomas and squamous cell
carcinomas) in various parts of rat’s nasal mucosa. The number of incidents rose significantly at
600 ppm (2142 mg/m3) but with a condition that single papilloma was already developed at 200
ppm. However, no significant response of tumor was found in mice cancer bioassay. Occasionally,
a single squamous cell tumors happened to occur at other areas of the rats and mice respiratory
tract [22].
VAM is considered to be a threshold carcinogen because it is thought that the carcinogenic action
affects the site or area of the first contact only if it has a high concentration.

CHAPTER 10
COST ESTIMATION

Cost Estimation
Table 10.1 Cost Estimation [23]
Equipment Number of Items Company Name Prices ($)

Vaporizer 1 Taco PF Series 975000
Heater 1 Taco PF Series 686000
Reactor 1 Foshan JCT 8395000
Heat Exchanger 1 Siemens 1050000
Cooler 3 Siemens 686400
Flash Drum 1 Alfa Laval 97700
Compressor 1 Alfa Laval 230000
Storage Tank 1 Local Company 150000
Pump 2 Alfa Laval 120000
Absorber Column 1 Talshan Group 750000
Distillation Column 1 JX Series 2997980
Total purchase equipment cost = 16138080 ($)
10.1 Estimation of Total Capital Investment:

10.1.1 Direct Cost
Purchased equipment cost = 16138080 ($)
Purchased equipment installation = 0.47 * 16138080 = 7584898 ($)
Instrumentation and process control = 0.12 * 16138080 = 1936569 ($)
Piping (installed) = 0.66 * 16138080 = 10651133 ($)
Building (including services) = 0.18 * 16138080 = 2904854 ($)
Yard improvements = 0.1 * 16138080 = 1613808 ($)
Service facilities (installed) = 0.7 * 16138080 = 11296656 ($)
Land required = 0.06 * 16138080 = 968285 ($)
Total Direct Cost = 53094283 ($)

10.1.2 Indirect Cost
Engineering and Supervision cost = 0.33 * 16138080 = 5325566 ($)
Construction expenses = 0.41 * 16138080 = 6616613 ($)
Total Indirect Cost = 11942179 ($)
Total cost = total direct cost + total indirect cost = 54288462 ($)
Contractor’s fee = 0.05 * total cost = 2714423 ($)
Contingency = 0.1 * total cost = 5428846 ($)
Fixed capital investment = total direct cost + total indirect cost + contractor’s fee +
contingency [19]
F.C.I = 62431731 ($)
Total capital investment = fixed capital cost + working cost
Working cost = W.C = 0.15 * (T.C.I) = 0.15 * (F.C.I + W.C) = 11017364 ($)
Total Capital Investment = T.C.I = F.C.I + W.C = 73449098 ($)
10.2 Product Cost

Depreciation = D = (V – Vs)/N [19]
V = F.C.I = 62431731 ($) [12]
Vs = 5% of F.C.I = 3121587 ($)
N = number of years = 20
D = 2965507 ($)
Total product cost = T.C.I – D
T.P.C = 70483588 ($)
Fixed charges = 0.12 * T.P.C = 8458030 ($)
Direct product cost = 0.55 * T.P.C = 38765973 ($)
Plant overhead = 0.1 * T.P.C = 7048359 ($)
Manufacturing cost = Direct product cost + fixed charges + plant overhead cost
= 54272362 ($)

10.3 General Expenses
General expenses = Administrative cost + Distribution and selling cost + Research and
development cost + Financing [19]
Administrative cost = 0.05 * T.P.C = 3524179 ($)
Distribution and selling cost = 0.2 * T.P.C = 14096718 ($)
Research and development cost = 0.05 * T.P.C = 3524179 ($)
Financing (interest) = 0.08 * T.C.I = 5875928 ($)
General expenses = 27021004 ($)
T.P.C = manufacturing cost + General expenses
T.P.C = 81293366 ($)
10.4 Gross earning in terms of VAM production:

Wholesale selling price of VAM per ton = 3000 ($)
T.P.C = 81293366 ($)
Total income = selling price * quantity of product manufactured
= 102000000 ($)
Gross income = total income – T.P.C
= 20706634 ($)
Let tax rate is 50%;
Taxes = 0.5 * Gross income = 10353317 ($)
Net profit = Gross income – Taxes
Net profit = 10353317 ($)
10.5 Rate of Return

ROR = (Net profit * 100)/Total investment
= (10353317 * 100)/81293366
ROR = 12.74 %

References
[1] Carl L.Yaws Chemical properties handbook New York, USA: McGraw-Hill
[2] Silsbv R.I Sawyer E. W., “ The Kinetics and Mechanism of Vinyl Acetate Monomer
Production” J. Appl. CHEM. ,6:347 (August 1956)
[3] Kumar, D., et al., “ Synthesis of Vinyl Acetate on Pd-Catalysts, Catalyst Today Journal,
Vol. 123, 2007, pp. 4-7
[4] Durston, P., et al., Production of Vinyl Acetate, United States Patent Office, Patent No.
3.306.930, February 28 of 1967
[5] Flammability of Gases and Vapors by H.F Coward & G.W Jones (1952).
[6] Serge Ravees, Thermal and Catalyst Processes in Petroleum Refining. Marcel dekker, inc.
New York basel
[7] J.D. Seader Product and Process Design Principles. John Wiley & sons, inc.
[8] Bruce E poling. Properties of Gases and Liquids. McGraw Hill
[9] Process Heat Transfer by Donald Q. Kern
[10] Unit Operation of Chemical Engineering by Warren L. McCabe, Julian C. Smith and
Peter Harriot 7th edition
[11] Rules of Thumb for Chemical Engineers by Carl R Barnan, 4th edition
[12] Dimian, A., Bildea, C.S., Chemical Process Design, Wiley-vch, (2008), pp, 287.
[13] Chemical Engineering, Volume 6, Third editionChemical Engineering Design
R. K. Sinnott
[14] Douglasm J.M. (1998). Conceptual design of chemical process. New York, USA:
McGraw Hill
[15] Encyclopedia of Physical Science & Technology by James R. Fair and Henry Z.
Kister and Narses Barona, 3rd edition.
[16] Vinyl Acetate from ethylene, acetic acid and oxygen Industrial Plant Simulation.
J.P. Contreras, J.C. Naranjo, S. Ramírez & D.M. Martínez
[17] G.S. Grover, R.V. Chaudhari, Chem. Eng. J. 32 (1986) 93
[18] Stephanoplous, G. (1984). Chemical Process Control. New Jersy, USA: Prenice-Hall I
International Editions
[19] Downs, J.J. and Vogel, E.F. (1993) A plant-wide industrialprocess control problem.
Computers in Chemical Engineering
[20] G. Reinacker, S. Engels, Z. Anorg. Allg. Chem. 336 (1965) 259
[21] Coward, H.F. and Jones, G.W. (1952) Limits of ßammability of gases and vapors.
Bulletin 503, Bureau of Mines.
[22] Peter M.S., Timmerhaus K.D., Plant Design & Economics for chemical engineers.
Fourth edition. New York: McGraw-Hill

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CHAPTER 01

1.2 Physio-Chemical Properties:

2.1 .1 Acetic Acid and Acetylene

HC≡CH+ CH3COOH → H2C=CH-O-(CO) CH3 ΔH = −118 kJ/mol

2.1.2 Acetaldehyde and Acetic Anhydride

CH3CHO + (CH 3CO)2O → CH3CH(OCOCH3 )2

CH3CH (OCOCH3)2 → H2C=CH-O-(CO) CH3 + CH3COOH

2.2 Acetic Acid, Ethylene and Oxygen

Table 2.1 Process Comparison

Process Advantages Disadvantages

Figure 3.1[4] Vinyl Acetate consumption

4.3 Process Constraints

Table 5.1 Stream Balance

stream stream stream stream stream stream stream

Figure 5.1 Reactor section

Table 5.2 Balance of Reactor Section

component stream 1 stream 3 stream 5 stream 19 stream 23

Figure 5.2 Separation Section

stream stream stream stream stream stream Vent

Figure 5.3 Absorber Section

Table 5.4 Balance of Absorber Section

stream stream stream stream stream stream stream

Oxygen 625 624 0.7

CO2 2627 378 2246 3

C2H4 20253 20232 21

C2H6 1600 1598 2

VAM 4305 3801 503 2 0 0

ACID 4503 4416 2420 2342 1 0

WATER 1226 1189 71 70 15 0

Figure 5.4 Plug Flow Reactor

5.2.1 Reactor Mass Balance

Table 5.5 Reactor Material Balance

Reactor inlet Reactor outlet

(∆𝐻𝑟)1 = -1.7×105 kJ/kmol

Utility flow rate

Figure 5.5 Feed Effluent Heat Exchanger

𝑇𝑖𝑛 = 160℃ 𝑄𝑐 = −𝑄ℎ

5.3 Cooler Before Flash Energy Balance

Figure 5.6 Cooler

𝑍𝑖 𝐾𝑖 𝑦 Figure 5.7 Flash Vessel

Table 5.6 Material Balance of Flash Vessel

Figure 5.8 Absorber

Inflow Out flow

5.6.2 Absorber Energy Balance

Figure 5.9 Distillation Column

5.7.1 Material Balance of Distillation

Figure 5.10 Heat Exchanger

Tin = 87oC Tout = 120oC

5.9 Pre-Heater Energy Balance

6.1.2 Reactor Selection Criteria

6.1.3 Mode of Operation

Parameters Continuous Reactor Batch Reactor

Parameters CSTR PFR

Properties Fixed Bed Fluidized Bed

• Small residence time

6.1.8 Reactor Specifications

6.1.9 Catalyst Specifications

6.1.10 Chemical Reaction

6.1.11 Reaction Kinetics

1. Calculate the weight of catalyst required using the performance equation:

2. Calculate the volume of the catalyst

3. Calculate reactor volume