Chapter 5 - Chemical DSGN

Production of 100,000 Tonnes Per Year of Butyl Acetate
CHAPTER 5
CHEMICAL DESIGN
SECTION 1 DESIGN OF CONTINUOUS STIRRED TANK REACTOR (CSTR-100)
5.1 INTRODUCTION
The reactor is the most important unit operation in chemical process. This is the only
place in the chemical process where the raw materials which are methyl acetate and
butanol are converted into products which are butyl acetate and to design the
reactor is a vital step in the overall design of the process.
The type of reactor that been choose is Continuous Stirred Tank Reactor (CSTR)
including jacket there. The rationales of CSTR as our chemical reactor because:-
a. The composition is constant. To maintain its composition of the products, the

reactor needs to be operated in continuous process and CSTR is the best reactor.
b. CSTR is the reactor that easy to maintain the temperature which is 110℃ or in
other words is easy to maintain the temperature control because it‘s perfectly mixed.
c. To maintain high conversion. The amount of the product is quite huge

(100000MT/yr). The benefits used CSTR are the right reactor for huge amounts of
productions and can maintain high conversion which is 90%. The power will depend
on the degree of agitation required and will range from about 0.2kW/m 3 for moderate
mixing to 2kW/m3 for intense mixing.
d. Cheap to construct. CSTR is cheap to construct. It‘s very economic where the
cost of construction can be minimized.
.
Some assumptions are made for CSTR:
a) Steady state condition
120
b) No radial variation in concentration, in the reactor.
c) The concentration of reactants and products are varies continuous in the axial
direction through the reactor.
d) No temperature change in the reaction.
e) Adiabatic condition.
CHEMICAL ENGINEERING DESIGN
5.1.1 Determination of Reaction Rate
Butyl acetate can be produced by the reaction of methyl acetate with butanol in a
reversible, liquid-phase, mildly exothermic reaction. Methanol is the by-product. The
reaction is isothermal reaction. Assuming a catalyst density of 2000 kg/m3 and a
void fraction of 0.5, the kinetic expressions used are given below, with the overall
reaction rate R having a first-order dependence on the two reactants and products.
Concentrations are in molality (kmol/m 3). Activation energies are in J/kmol, and the
reactor temperature is in K. The reaction has been catalyzed by the acidic ion-
exchange resin, Amberlyst 15. The liquid-phase second order reversible reaction
considered is the kinetics for the forward and reverse reactions are based on those
given by Jimenez and Costa-Lopez.
CH3COOCH3 (l) + CH3(CH2)3OH (l) ↔ CH3COO(CH2)3CH3 (l) + CH3OH (l)
r = kFCMeAcCBuOH - kRCMeOHCBuAc
kF= 1.246 × 105e-71960/RT
kR = 1.696 × 105e-72670/RT
121
Table 5.1: The flowrate and the concentration of the component inlet and outlet of
reactor (CSTR-100).
Component Volumetric Mole Flowrate Concentration

flowrate (kmol/h) (kmol/m3)
(m3/h)
inlet outlet inlet outlet inlet outlet
Methyl Acetate 31.86 31.47 137.5210 52.8280 4.3164 1.6787
Butanol 31.86 31.47 105.0767 20.3833 3.2981 0.6477
Methanol 31.86 31.47 284.1020 368.7953 8.9172 11.7189
Butyl acetate - 31.47 - 84.6934 - 2.6912
T=The reactor temperature is 383 K

R=8.314 J/kmol K
Hence,
k F  1.907  10 5 m 3 kmol1 s 1
k R  2.075  10 5 m3 kmol1 s 1
r  6.3369  10 4 kmol s 1 m 3
From the table above, the conversion of methyl acetate in CSTR-100 is 61%.
5.1.2 Determination of The Reactor Volume
Now the volume can be calculated using the formula [Levenspiel, 1999],
V C A0  C A

v0 r
Where,
CA0 = inlet concentration of Methyl Acetate
CA = outlet concentration of Methyl Acetate
v0  the volumetric flowrate, 31.86 m 3/h
122
Rearramge equation
C A0  C A
V  v0
r
kmol kmol
4.3164  1.6787
m 3
m  3 m 
3
V    

  6.3369  10  4 kmol s 1 m 3 8.85 10
s 
 36.8376 m 3  37 m 3
The shape of the reactor is to be a cylinder and take the height of the reactor is 3
times of the diameter, for better mixing in the reactor by the impeller [Sinnot, 1999].
V   r2H
Where H  6r
V  6r 3
Hence the radius, ractual  V 6 

1 3
 37 6 
1 3
 1.25 m (round up to1.5)

The diameter, Dactual  1.5 m  2
 3m
The height, H actual  3 m  3
9m
Vdesign volume  3.142 * 1.5 * 9  63m 3

2
123
5.1.3 Determination of The Reactor Residence Time
The calculation of reactor residence time, shown below [Levenspiel, 1999]:
V 37m 3
 
v0 m3
0.531
min
 69.6798 min
≈ 70 min
Hence, the reactor residence time,   70 min
where v o is the inlet volumetric flow rate
5.1.4 Rate of Change
From the mass balance equation:
Input = Output
d(ρV)/dt = mass in – mass out (unit mass /time)
Since the mass in is equal to mass out, so the rate of change of volume remain zero
The mole balance for the equation is;
Rate change of component = input – output + generation – consumption (unit

mol/time)
V d(CA)/dt = F0 CA– Fi CA– Vr1 + Vr2
Since the volume is constant;

From the rate value above;
d [CH 3 COOCH3 ] F
 (Cin  Cout )  (r1  r2 )
dt V
d [CH 3 (CH 2 ) 3 OH ] F
 (Cin  Cout )  (r1  r2 )
dt V
d [CH 3 OH] F
 (Cin  Cout )  (r1  r2 )
dt V
124
d [CH3COO(CH2 ) 3 CH 3 ] F
 (Cin  Cout )  (r1  r2 )
dt V
We used Euler Algorithm to solve the mathematical model ,
dx/dt = f (x,t)
at x(0) = x0 at t=0
the derivative of x times the step size.
x(Δt) = x(0) + (dx/dt) t=0 Δt
x1 = x0 + f (x0,0) Δt
Table 5.2 The change of concentration profile of each components in reactor

Final Final Final Final
concentration of concentration of concentration of concentration of
Methyl Acetate Butanol Methanol Butyl acetate
Time(min) (kmol/m3) (kmol/m3) (kmol/m3) (kmol/m3)
0 4.3200 3.2981 8.9172 0.0000
5 4.1800 3.1600 9.0500 0.0136
10 4.0700 3.0500 9.1700 -0.0032
15 3.9500 2.9300 9.2844 0.1153
20 3.8494 2.8321 9.3832 0.2144
25 3.7668 2.7495 9.4658 0.2973
30 3.6979 2.6806 9.5347 0.3665
35 3.6403 2.6230 9.5923 0.4243
40 3.5922 2.5749 9.6403 0.4727
45 3.5521 2.5348 9.6805 0.5130
50 3.5186 2.5013 9.7140 0.5469
55 3.4907 2.4734 9.7419 0.5751
60 2.5800 2.4500 9.7700 0.5990
65 1.5800 0.5200 11.800 1.6000
70 1.5300 0.5100 11.1200 4.5000
125
Concentration Profile
1.40E+01
1.20E+01
1.00E+01
8.00E+00
6.00E+00
4.00E+00
2.00E+00
0.00E+00
-2.00E+00 0 10 20 30 40 50 60 70 80
Methyl Acetate Butanol Methanol Butyl Acetate
Figure 5.1 The graph above show the change of concentration profile of each
component in reactor with time for the first reactor and the residence time taken is
70 min.
From the graph the concentration of methanol is higher than the product at 70
minutes, butyl acetate. The patent also suggested that the ratio of feed methanol
must higher than the feed of metyl acetate n butanol. This is because the reaction is
reversible. The reaction may occur in forward and reverse reaction. In order to
reduce the concentration of methanol, the next action is to install another
continuous ctirred tank reactor (CSTR-101) in series to get higher concentration of
butyl acetate and the conversion of methyl acetate in CSTR-101 is 71%.
5.1.5 Determining the Weight of Catalyst
The next step in chemical design is to calculate the weight of catalyst (acidic ion-
exchange resin, Amberlyst 15. By Jimenez and Costa-Lopez the bulk density of the
Amberlyst 15 is 600 kg/m 3 and the void fraction is 0.5. The equation used is as
follow [Coulson & Richardson’s, Volume 6]:
The bulk density,

 b  1    B
 1  0.5600 
kg
 300 3
m
126
The volume of catalyst,

VC  Vreactor (1   )
VC  37(1  0.5)
VC  18.5m3
The weight of the catalyst,

W  VC  b
Where,
W  mass of catalyst,kg
V  reactor catalyst,37 m 3
kg
 b  assuming bulk density,300
m3
kg
W  18.5m 3  300  5550kg catalyst
m3
5.1.6 The Volume of Cooling Water
The amount of heat absorbed by the cooling water is equal to the amount of heat
generated by the exothermic reactions. First, the amount of heat generated shall be
determined. Water jacket is needed in order to maintain the operating temperature
of the reactor, which is at 120℃.
Based on the simulation result;

Duty of the reactor, Q  2.31 10 6 kJ h
Hence the amount of heat that shall be absorbed by the cooling water is -2.31x106
kJ/h.
For cooling purpose of the reactor, half pipe jackets is installed outside the reactor
since half pipe jacket provides higher heat transfer rate when compared to
conventional cooling jacket (Sinnot, 1999).To determine the flow rate of cooling
water to the coil, m, it is assumed that the inlet cooling water mean temperature, T m,i
and the outlet temperature Tm,o is 22 oC and 80 oC respectively.
127
By using the equation [Incropera, 2002],
Q  H  mC p Tin  Tout 
(1.23)
Where heat capacity of water Cp = 4.181 kJ/kg.K

Hence, m  H C p 80  22

 2.31 10 6 kJ h 4.181 58 
 9525.8518 kg h
Now, the length of the cooling coil is determined using following formula [Incropera,
2002];
As  Dt ,i L  mCP Tm,o  Tm,i  Q Ar 
(1.24)
Rearraging, L  mCP Tm,o  Tm,i  Q Ar   Dt ,i
Where, As is the heat transfer area of the coil, A r is the heat transfer area of the
reactor and Dt,i is the inside diameter of the coil (which is assumed to be 0.3 m)
Ar  DH
 3.142  3  9
 84.8340 m 2
(1.25)
 
Hence, L  84.834  4.18158 2.301 10 6 84.834    0.3 m  90 m
The number spiral formed by the cooling coil around the reactor can be calculated
by dividing the length of the coil by the reactor circumference,
Number of spiral,
 98 D
 9.5481 m (round up to 10 m)
128
Table 5.3: Specification sheet for chemical design for reactor
SPECIFICATION DATA
CHEMICAL DESIGN
Identification
Type of reactor Continuous StIrred Tank Reactor
Design orientation Vertical
Production 100,000 MT Butyl Acetate / year
Physical Condition
Volume of reactor, m3 63
Diameter of reactor, m 3
Height of reactor, m 9
Type of insulator Mixture of Magnesia and Asbestos
Types of jacket Half Pipe Jackets
Reaction
Type of reaction Transesterferication process
Raw materials Butanol,methyl acetate and methanol
Order of reaction Second order
Residence time, min 70
Type of catalyst Amberlyst 15
Volume of catalyst, m 3 19
Weight of catalyst, kg 5550
129
SECTION 2: CHEMICAL DESIGN OF DISTILLATION COLUMN 1 (T100)
5.2 INTRODUCTION
Distillation is probably the most widely used separation process in the chemical and
allied industries, its application to get purification of product. Distillation Column
function to separatethe feed stream which is the product from the second reactorinto
desired purified product. Both the top and bottom product of distillation column 1 are
fed to two separate distillation columns for further distillation to obtain the purified
product of butyl acetate.
The design of a distillation column can be divided in the following steps (

Coulson and Richardson, page 493):
1. Specify the degree of separation required: set specification.

2. Select the operating conditions: batch or continuous; operating pressure.
3. Select the type of contacting device: plate or packing.
4. Determine the stage and reflux requirements: the number of equilibrium
stages.
5. Size of the column: diameter, number of real plates.
6. Design the column internals, plates, distributors, and packing support.
7. Mechanical design: vessel and internal fittings.
5.2.1 DESIGN OF SIEVE PLATE COLUMNS
The most important part to be considered when designing plates is the efficiencies
of plates. It is important to get better fractionation and get the desired purity while
compatible with the operating temperature and pressure. Another important
consideration is to fix the number of plates before completing the design.
Tower diameters may range from 300 mm (1 ft) to more than 9 m (30 ft) and
the number of plates from a few to about a hundred. Plate spacing may vary from
150 mm or less to 1 or 2 m (Mccabe,2001).
a) Light Key (LK)
130
Before designing the distillation column, it is desired to determine the light key and
heavy key components. Light key is actually the most volatile component whose
concentration is to be controlled in bottom product. (Coulson and Richardson:
page 516). For this distillation column, methyl acetate is chosen as a light key
mainly because it is high in boiling point and volatility value. Choosing methyl
acetate as a light key can be described as the perfect solution in producing the
purified product.
b) Heavy Key (HK)
Heavy key is the least volatile component whose concentration is to be controlled

in overhead product. Therefore, methanol is chosen as a heavy key.
c) Estimation of the number of stages
To estimate number of stages, condenser and reboiler temperature, and procedures

are required for calculating dew and bubble points. By definition, a saturated liquid is
at its bubble point (any rise in temperature will cause a bubble vapor to form), and a
saturated vapor is at its dew point (any drop in temperature will cause a drop of
liquid to form). Dew point and Bubble point can be described by equation shown
below:
Bubble point:  yi   kixi  1.0

Dew point :  xi   yi / ki  1.0
d) Overall column efficiency
Overall column is depending by relative volatility of light key component and molar
average viscosity of feed by determines average column temperature. To determine
column efficiencies, it have 2 correlation which Eduljee (1958) correlation and
O’Connell’s correlation. For Eduljee (1958) correlation, the equation shown below:
E0  51  32.5 log(  a a )
Where,  a = average relative volatility of the light key
 a = the molar average liquid viscosity, mNs/m 2
131
A quick estimate of the overall column efficiency can be obtained from correlation
given by O’ Connell (1946) based on graph. (Coulson and Richarson: page 550)
e) Approximate column sizing
i) Plate spacing
Overall height of column depends on the plate spacing. Plate spacing ranges
from 0.5 to 1.0 m is normally used. Its spacing depends on column diameter
and operating condition. For this particular distillation column, plate spacing
used is 0.5m.
ii) Plate Contactors

Sieve plate is the simplest type of cross flow plate. The vapor passes up
through perforating on the plates, and the liquid is retained on the plate by
the vapor flow. The perforating are usually small holes, but larger holes and
slots are used. The sieve plate is used because it bears the lowest cost.
f) Pressure drop
In order to design distillation column, pressure drop should be determinedto ensure

that the plate will operate properly without flooding. Two major sources of pressure
drop are vapor flow through the holes (on orifice loss) and the static head of liquid
on the plate.
The total pressure drop calculated for the flow of vapor through the dry plate (the dry
plate drop, h d: the head of clear liquid on the plate (h w + how), and a term to account
for other minor sources of pressure loss, the so-called residual loss, hr. The total
plate pressure drop:
ht  hd  hw  how  hr
g) Weir length
With segmental down comers the length of the weir fixes the area of the down
comer. A good initial value to use is 0.77, which equivalent to a down comer area of
12 %.
132
h) Weir height
The height of the weir determines the volume of liquid on the plate and is an
important factor in determining the plate efficiency. A high weir will increase the
plate efficiency but resulting a higher plate pressure drop.
i) Flooding
Flooding velocity can be estimated from the correlation given by Fair (1961):
 L  V
U f  Ki
V
Where, U f =flooding vapor velocity, m/s, based on the net column
Cross-sectional area
Ki = a constant obtain from graph.
j) Weeping
The lower limit of the operating range occurs when liquid leakage through the plate’s
hole becomes excessive. This is known as weep point. The vapor velocity at the
weep point is the minimum value for stable operation. The hole area must be
chosen so that at the lowest operating rate the vapor flow velocity is still well above
the weep point.
Minimum vapor velocity through the holes based on the holes area can be
calculated using Eduljee (1959) equation:
K 2  0.9(25.4  d h )
U h (min) 
(  v )1 / 2
Where, U h =minimum vapor velocity through the holes based on the holes area
d h = hole diameter, mm
K 2 = a constant, dependent on the depth of clear liquid on the plate,
Obtain from figure 11.30 (Sinnott, 2000; Appendix B, p. B-4)
133
k) Weir liquid crest
The height of the liquid crest over the weir can be estimated using the Francis weir
formula. For a segmental down comer this can be written as:
2/3
 Lw 
how = 750 
  l (l w ) 
Where, lW = weir length
Lw = liquid flow rate, kg/s
 L =liquid density
l) Entrainment
In operating, some liquid droplets will be entrained and carried up the column by
vapor flow, and this will reduce the actual operating efficiency.
CALCULATION OF CHEMICAL DESIGN OF DISTILLATION COLUMN
5.2.2 Composition of Component Inlet and Outlet Streams
Table 5.4 : Composition of Component Inlet and Outlet Streams

Comp Feed distillate/top bottom
molar flow mole frac molar flow mole frac molar flow mole frac
Methyl 34.6936 0.068 34.58637 0.1339 0.0005
acetate 0.126
Butanol 4.28568 0.0084 0 0 4.28 0.017
Butyl 100.7645 0.1975 0 0 0.4
acetate 101
Methanol 370.45622 0.7261 223.71363 0.8661 147 0.5824
total 510.2 1 258.3 1 251.9 1
134
5.2.3 To calculate bubble and dew point
Using Antoine equation to find vapor pressure (P 0)

B
LogP 0  A 
(T  C )
Table 5.5: Antoine coefficient’s for every component

Comp A B C
Methyl acetate 16.1295 2601.92 -56.15
Butanol 17.216 3137.02 -94.43
Butyl acetate 16.1836 3151.09 -69.15
Methanol 18.5875 3626.55 -34.29
Ki = P0
P
5.2.4 Dew temperature (Top column)
x  y i i / k i  1.0
Temperature = 368.12 K Operating pressure =304 kPa
Table 5.6 : Calculation to determine dew point

Component yi = xi Pi* (mmHg) Pi* (kPa) Ki=(Pio/P) yi/Ki
Methyl 0.1339 7326.57 976.79 0.9302 1.0749
acetate
Butanol 0 379.42 50.58 0.0481 2.08 x 10-5
Butyl acetate 0 83.01 11.06 0.0105 9.49 x 10-5
Methanol 0.8661 7789.02 1038.45 0.9890 1.075056
Total 1 1.0001269
y i / k i value close to 1.0, therefore this temperature is accepted.

So, dew temperature is 368.12 K.
135
Sample calculation for butyl acetate component
3151.09
𝐿𝑜𝑔 𝑃0 = 16.1836 −
368.12 − 69.15
= 5.6438
𝑃0 = 𝐸𝑥𝑝 5.6438
= 282.5343 mmHg
Convert to kPa:
𝑃0 = 282.5343 0.13324
= 3.84967 kPa
37.64390145𝑘𝑃𝑎
𝐾𝑖 =
90𝑘𝑃𝑎
= 0.12383
Assume Xi = Y i = 0
𝑌𝑖 0
So, =
𝐾𝑖 0.04277
=0
5.2.5 Bubble point (Bottom Column)
y i  k x
i i  1.0
Temperature = 392.54 K Operating pressure = 403.5 Kpa
Table 5.7: Calculation to determine Bubble Point

Component yi = xi Pi* (mmHg) Pi*(kPa) Ki(Pi*/P) xiKi
Methyl 0.0005 4423.296695 589.289279 1.46044431 0.000730222
acetate
Butanol 0.017 806.681431 107.469327 0.266342818 0.004527828
Butyl 0.4 626.1763432 83.42171714 0.206745272 0.082698109
acetate
Methanol 0.5824 4743.388097 631.9331359 1.566129209 0.912113651
Total 1.00006981
k xi i value is close to 1.0, therefore this temperature is accepted.
So, bubble temperature is 392.54 K.
136
Bubble temperature:
3151.09
𝐿𝑜𝑔 𝑃0 = 16.1836 −
392.54 − 69.15
= 6.4397
𝑃0 = 𝐸𝑥𝑝 6.4397
= 626.1763 mmHg
Convert to kPa:
𝑃0 = 626.1763 0.13324
= 83.42171714 kPa
83.42171714 𝑘𝑃𝑎
𝐾𝑖 =
403.5 𝑘𝑃𝑎
= 0.2067
Assume Xi = Yi = 0.4
So, KiXi = (0.2067)(0.4)
= 0.0827
5.2.6 Relative volatility
The relative volatility of two components can be expressed as the ratio of their K value. The
determination of relative volatility, α of the components can be determined as the ratio
between K values of light key component to heavy key component.
The relative volatility of two components can be expressed as the ratio of their K
value:
Ki
i j 
Kj
Where, Ki = light components
Kj = heavy components
137
Table 5.7: Relative volatility value for every component
comp Bottom Top Average
α α α
methyl 0.9998581 1.345762084 1.172810092
acetate
butanol 0.170064396 0.139463513 0.154763954
butyl 0.132010354 0.124899257 0.128454806
acetate
methanol 1 1 1

At bottom:
0.206745272
𝛼𝑖 =
1.566129209
= 0.132010354
At top:
0.123828623
𝛼𝑖 =
0.991428022
= 0.124899257
For average:
0.132010354 + 0.124899257
𝛼𝑖 =
2
= 0.128454806
5.2.7 Calculation to find q, the Thermal Condition at Feed
  Hfs  Hf
q=

 = the molar of the latent heat of vaporization
Hfs = the molar enthalpy of the feed at its boiling point
Hf = the molar enthalpy of the feed
138
Temperature = 343K Pressure = 1.5 bar
Table 5.8: A,B,C,D constant for heat capacity calculation

0
Comp a b c d CP
Methyl 16.5500 0.2245 -0.00004 0.000000029144 23651.3565

acetate
Butanol 3.2660 0.4180 -0.00022 0.00000004685 30003.1452
Butyl 13.6200 0.5489 -0.00023 -0.0000000007913 44121.3770
acetate
Methanol 21.1520 0.0709 0.00003 -0.00000002852 14405.7385
5.2.8 Specific heat capacity, Cp0:
CP 0 = aT + (1/2)bT2 + (1/3)cT3 + (1/4)dT4
CP 0 (Methyl acetate) = 16.5500+[ (0.2245/2) (T)2 ] + [(-0.00004/3)( (T)3)

[(0.000000029144/4) (T)4]
= 16.5500 (411) +[ (0.2245/2) (411)2 ] + [(-0.00004/3)(
(T)3)
+( 0.000000029144/4) (411)4]
= 23651.3565 kJ/kmol
CP 0 (Butanol) = 3.2660T +[ (0.4180/2) (T)2 ] +[ (-0.00022/3) (T)3 ]

+ [ (0.00000004685/4) (T)4 ]
= 30003.1452 kJ/kmol
CP 0 (Butyl acetate) = 13.6200T +[ (0.5489/2) (T)2 ] +[ (-0.00023/3) (T)3 ]

+[ (-0.0000000007913/4) (T)4 ]
= 44121.3770 kJ/kmol
CP 0 (Methanol) = 21.1520T +[ (0.0709/2) (T)2 ] +[ (0.00003/3) (T)3 ]

+[ (-0.00000002852/4) (T)4 ]
= 14405.7385 kJ/kmol
Latent heat equation due to Haggenmacher (1946) is derived from the Antoine
vapor pressure equation:
139
8.32BT 2 z
Lv =
( T  C) 2
Where
Lv = latent heat at the required temperature, kJ/kmol
T = temperature, K
B, C = coefficients in the Antoine equation
z= Zgas–Z liquid (where z is the compressibility constant),
0.5
 P 
from equation: z  1  r 3 
 Tr 
Pr = reduced pressure
Tr = reduced temperature
Feed composition:
Table 5.9 : Calculation for q-line for every component
Component TC (K) z PC (bar) Pr Tr CP
Methyl acetate 506.8000 0.9416 46.9000 0.0549 0.7855 23651.3565
Butanol 562.9000 0.9139 44.2000 0.0583 0.7072 30003.1452
Butyl acetate 579.0000 0.8647 31.4000 0.0820 0.6876 44121.3770
Methanol
512.6000 0.9655 81.0000 0.0318 0.7766 14405.7385
Comp Mol.Fraction MW Tbp (K) Lv

Methyl acetate 0.068 74.08 329.9 27628.78385
Butanol 0.0084 74.123 390.7 40994.99463
Butyl acetate 0.1975 116.16 399 33200.96514
Methanol 0.7261 32.042 337.6 34880.78311
Feed at temperature 343 K :
Mean molecular weight = (0.068 X 74.08) + (0.0084 X 74.123)

+ (0.1975 X 116.16) + (0.7261 X 32.042)
= 51.8674 kg/kmol
140
.
Mean boiling point = (0.068 X 329.9) + (0.0084 X 390.7)
+ (0.1975 X 399) + (0.7261 X 337.6)
= 349.6489 K
Specific heat, C P = (0.068 X 23651.3565) + (0.0084 X

30003.1452)
+ (0.1975 X 44121.3770) + (0.7261 X
34880.78311)
= 21034.2974 kJ/kmol
Latent heat,  = (0.068 X 27628.78385) + (0.0084 X

40994.99463)
+ (0.1975 X 33200.96514) + (0.7261 X
34880.78311)
= 34107.2425 kJ/kmol
Hfs = 2.31*51.8674 kg/kmol*(349.6489 -273)

= 10105.7400 kJ/kmol
Hf = 2.31*51.8674 kg/kmol*(298.1 -273)

= 14988.6843 kJ/kmol
Therefore,
  Hfs  Hf
q= = 0.8298

141
5.2.9 Calculate the reflux ratio (R).
Reflux ratio can be calculating using Underwood equation:

 i x i ,d
 i  
= Rm + 1
Where,
i = the relative volatility of component i with respect to some
reference component, usually the heavy key
Rm = the minimum reflux ratio
Xi,d = concentration of component i in the tops at minimum reflux
And  is the root of the equation:

x,
 ii i f = 1 – q
xi,f = the concentration of component I in the feed, and q depends

on
the condition of the feed
x,
 ii i f = 1 – q
where q = 0.8298
1-q = 1- 0.8298 = 0.1702
Table 5.10: Calculation value of θ
(αi - θ)  i xi , f
Component 
x i ,f αi  i x i ,f Let θ = 0.16642 i 
Methyl acetate 0.068 1.172810092 0.079751086 1.006394944 0.0792443

Butanol 0.0084 0.154763954 0.001300017 -0.011651194 -0.1115780
Butyl acetate 0.1975 0.128454806 0.025369824 -0.037960343 -0.6683244
Methanol 0.7261 1 0.7261 0.833584852 0.8710571
Total 1 0.1703990
0.1703990 is close to 1 – q = 0.1702
142
Therefore  = 0.16642
Table 5.11: Calculation value of Rm+1
comp Average x,d α xd (θ = 7459.909)

α α xd/(α – θ)
Methyl
acetate 0.1339 1.172810092 0.157039271 0.156041395
Butanol 0 0.154763954 0 0
Butyl
acetate 0 0.128454806 0 0
Methanol 0.8661 1 0.8661 1.039006405
Total 1 1.195047801 -1.01892x10-8
Hence,
The minimum reflux ratio
Rm + 1 = 1.195047801
Rm = 0.195047801
For optimum reflux ratio, the value will lie between 1.2 to 1.5 times reflux ratio
(Coulson and Rcharson: page 496).
So, Reflux ratio (R) = 1.3 x 0.195047801
= 0.253562141
From Erbar – Maddox correlation, (Appendices 1).:

Nm
= 0.9
N
Minimum number of stages can be calculated using Fenske Equation:
x  x 
log LK d  HK b
Nm   x HK   x LK 
log  LK
0.1339 0.5824
𝐿𝑜𝑔 ( )( )
𝑁𝑚 = 0.8661 0.0005
𝐿𝑜𝑔(1.172810092)
Nm = 32.58037
143
Therefore for ideal stages, N = Nm /(0.9)
N = 32.58037/ (0.4)
N = 36.2004111stage (approximately 7 stages)
5.2.10 Overall column efficiency
given by O’Connell (1946). (APPENDICES 2)
E0  51  32.5 log(  a a )
 a = the molar average liquid viscosity, mNs/m 2

Temperature = 368 K (top column)
= 392 K (bottom column)
Average temperature = (368 + 392) K = 391 K
Viscosity of components at average temperature, 381 K:
Log ( a ) = [VISA] * [(1 / T) – (1/VISB)]
Where, VISA, VISB = correlation constant
144
Table 5.12: Calculation value of average viscosity
Comp VISA VISB µ Mol. Frac.
Methyl acetate 408.62 224.03 -0.745799115 0.179556398
Butanol 984.54 341.42 -0.285931481 0.517688502
Butyl acetate 537.58 272.3 -0.555802724 0.278097622
Methanol 555.3 260.64 -0.665353358 0.216095957
Component xi µi xi*µi
Methyl acetate 0.068 0.179556398 0.012051752
Butanol 0.0084 0.517688502 0.004214164
Butyl acetate 0.1975 0.278097622 0.053990658
Methanol 0.7261 0.216095957 0.154152968
Total 1 0.224409542
From the previous calculation, relative volatility of light key(methanol) is:

 a = 1.172810092
Therefore, overall column efficiency, E o = 80 %
The minimum number of stages is 2.46, and overall column efficiency is 50 %. Ideal
stages is 7. So for The actual stages:
=N–1
Eo
= 36.2004111-1
0.8
= 43.75stages . Approximately (44 stages)
5.2.11 Calculation to Determine Feed Point
An estimate can be made by using the Fenske equation to calculate the number of
stages in the rectifying and stripping section separately, but this requires an
estimate of the feed-point temperature. An alternative approach is to use the
empirical equation given by Kirkbride (1944):
145
 x  x b,LK 
2
N   B  f ,HK   
Log  r  = 0.206 log
 Ns   D  x f ,LK  x
 d,HK

 
 
Where, Nr = number of stages above the feed, including any

partial condenser
Ns = number of stages below the feed, including the
reboiler
x f ,HK = concentration of the heavy key in the feed
x f ,LK = concentration of the light key in the feed
x d,HK = concentration of the heavy key in the top

product
x b,LK = concentration of the light key if in the bottom
product
B = molar flow of bottom product
D = molar flow of top product
  
2

N 
Log  r  = 0.206 log  251.9  0.7261  0.0005   =-1.1118
 Ns   223.71363  0.068  0.8661 
 
 
 Nr 
  = 2.07730
 Ns 
Where actual number of stages is 44,

Nr  Ns = 44
0.07730Ns+ Ns= 44
Nr =14.30
Ns=29.7
Therefore, the feed is at stages 15 from the top column.
5.2.12 Pressure drop
Pressure at top column = 304 kPa
146
Pressure at bottom column =403.5 kPa
Total pressure drop in the column is = (403.5-304) kPa
= 99.5 kPa
5.2.13 Calculation for density and relative molar mass (RMM)
Table 5.13 : Liquid density, Relative Molar Mass for every component
Top (D) Bottom (B) Liquid

Molecular Feed Mol. Mol. Mol. Density
Comp Weight,MW Frac.,xF Frac.,xD Frac.,xB (kg/m3)
Methyl acetate 74.08 0.068 0.1339 0.0005 934
Butanol 74.123 0.0084 0 0.017 810
Butyl acetatel 116.16 0.1975 0 0.4 898
Methanol 32.042 0.7261 0.8661 0.5824 719
Total 1 1 1 3361
Comp RMM feed RMM Dis RMM Bot

Methyl acetate 5.03744 9.919312 0.03704
Butanol 0.6226332 0 1.260091
Butyl acetatel 22.9416 0 46.464
Methanol 23.2656962 27.7515762 18.6612608
Total 51.8673694 37.6708882 66.4223918
5.2.14 Calculation for Relative Molar Mass (RMM)
RMM of Feed = 0.068 (74.08) + 0.0084 (74.123) + 0.1975

(116.16)
+ 0.7261 (32.042)
= 51.8673694 kg / kmol
RMM of Top Product = 0.1339 (74.08) + 0 (74.123) + 0 (116.16)
+ 0.8661 (32.042)
= 37.6708882 kg / kmol
RMM of Bottom Product = 0.0005 (74.08) +0.017 (74.123)+ 0.4 (116.16)
+ 0.5824 (32.042)
= 66.4223918 kg / kmol
147
5.2.15 Calculation for density
1. Bottom product
Liquid density,  L = x B ,i i
= 0.0005(934) + 0.017(810) + 0.4(898) + 0.5824(719)
= 792.1826 kg / m3
MW TSTP POP
Vapor density,  V = V x x
TOP PSTP
STP
= (66.4223918/ 22.4) kg/m3(393 / 370.03)K(4.035/1.0) bar

= 8.321279 kg / m 3
2. Top product
Liquid density,  L = x B ,i i
= 0.1339(934) + 0 (810) + 0 (898) + 0.8661(719)
= 747.7885 kg / m 3
MW TSTP POP
Vapor density,  V = V x x
TOP PSTP
STP
= (37.6708882 / 22.4) kg/m3 (273 / 368) K (3.04/ 1.0) bar

= 3.79268 kg/m 3
5.2.16 Surface tension (  )
 Pch (  L  V ) 
4
   x10–12
 M 
Where,  = surface tension, MJ/m2 or (dyne/cm)

Pch = Sugden’sparachor at Coulson and Rcharson(page335)
V  Vapor density, kg/m3
 l = Liquid density, kg/m 3
M = relative molecular weight
148
For mixture,
 m   1 x1   2 x 2 .....
Where,  m = surface tension mixture
 1 2 = surface tension for mixture

x1 x 2 = component mol fraction
5.2.17 Calculation for parachor (Pch)
Table 5.14: Calculation value of Pch contribution

Mol. Frac
Mol. Frac. Bottom
Comp top column,xD column,x,B Pch Contribution
Methyl acetate 0.1339 0.0005 174
Butanol 0 0.017 224.4
Butyl acetatel 0 0.4 294
Methanol 0.8661 0.5824 248.2
Pch at Top column = x D ,i Pch, i

= 0.1339(174) + 0(224.4) + 0(294) + 0.8661(248.2)
= 238.26462
Pch at Bottom column = x B ,i Pch, i
= 0.0005(174) + 0.017(224.4) + 0.4(294) + 0.5824(248.2)
= 266.05248
Therefore, surface tension at bottom column,

266.05248 792.1826−8.321279 4
𝜍=[ ] x 10-12
66.4223918
 = 97.1785684 N/mm2
Surface tension for Top column,
238.26462 717.7885 −3.79268 4

𝜍=[ ] x 10-12
37.6708882
 = 490.3427292 N/mm2
149
By getting the value for surface tension at top and bottom column, calculation for
liquid vapor flow factor are shown below:
LW V
FLV 
VW L
Where, LW =liquid mass flow rate, kg/s
VW =vapor mass flow rate, kg/s
574.775 8.321279
𝐹𝐿𝑉 𝑏𝑜𝑡𝑡𝑜𝑚 =
322.875 792.1826
= 0.18245
64.575 3.79268
𝐹𝐿𝑉 𝑡𝑜𝑝 =
322.875 747.7885
= 0.01788
By taking plate spacing as 0.5 m for bottom and for top, (Appendices 3)
base K1 =0.038
top K1 = 0.09
So, correction for surface tension is,

0.2
490.3427292
𝑇𝑜𝑝 𝐾1 = × 0.09 = 0.170661854
20
0.2
97.1785684
𝐵𝑎𝑠𝑒 𝐾1 = × 0.12 = 0.052130577
20
792.1826 − 8.432279
𝐵𝑎𝑠𝑒 𝑢𝑓 = 0.052130577 = 0.505961067 𝑚 𝑠
8.432279
747.7885 − 3.79268
𝑇𝑜𝑝 𝑢𝑓 = 0.170661854 = 2.390681169 𝑚 𝑠
3.79268
design for 85% flooding at maximum flow rate
150
𝐵𝑎𝑠𝑒 𝑢𝑣 = 0.505961067 × 0.85 = 0.430066907 𝑚 𝑠

𝑇𝑜𝑝 𝑢𝑣 = 2.390681169 × 0.85 = 2.032078994 𝑚 𝑠
5.2.18 Maximum volumetric flow-rate

Vm ( RMM )
Maximum volumetric flow-rate =
V
1. Above the feed point
Vapor flow rate will be:
Vn  D( R  1)
= 258.3 kmol/h (0.25 + 1)
= 322.875 kmol/h
Liquid down flow will be:
Vn = Ln  D
Ln = Vn  D
= (322.875-258.3) kmol/h
= 64.575 kmol/h
2. Below the feed point

Liquid flow rate will be:
Lm = Ln  F
= (64.575 + 510.2) kmol/h
= 574.775 kmol/h

Vm = Lm  W
= (574.775 – 251.9) kmol/h
= 322.875 kmol/h
Therefore, Maximum volumetric flow rate,
66.4223918 ×322 .875 3

𝐵𝑎𝑠𝑒 = = 0.717946666 𝑚 𝑠
8.321279 𝑋 3600
(37.6708882 ×322 .875 ) 3
𝑇𝑜𝑝 = = 0.893660991 𝑚 𝑠
3.79268 𝑋 3600
volumetricflowrate
Net area required for both bottom and top column:
floodingvelocity
151
0.717946666 71591
𝐵𝑎𝑠𝑒 = = 1.418976108 𝑚2
0.430066907
0.893660991
𝑇𝑜𝑝 = = 0.373810194 𝑚 2
2.032078994
As first trial take downcomer area as 12% of total.
Column cross-sectioned area,
1.418976108
𝐵𝑎𝑠𝑒 = = 1.61247285 𝑚2
0.88
0.373810194
𝑇𝑜𝑝 = = 0.424784311 𝑚 2
0.88
Column diameter
1.61247285×4
𝐵𝑎𝑠𝑒 = = 1.433215106 𝑚
𝜋
0.424784311×4
𝑇𝑜𝑝 = =0.735613017 𝑚
𝜋
So, the same column diameter for above and below feed is 1.45 m.
152
5.2.19Liquid Flow Pattern
Maximum volumetric liquid flow rate,
574.775 × 66.4223918 3
= = 0.013408471 𝑚 𝑠
3600 × 792.1826
The plate diameter is inside the range of Figure 2.1.5 from Appendix A, so it is clear
that a single pass plate can be used.(Coulson and Rchardson: page 569)
5.2.20 Provisional Plate Design
Column diameter, Dc = 1.948327548 m

Column area, Ac = 1.61247285 m2
Downcomer area, Ad = 0.12 x 1.61247285 = 0.193496742 m2
Net area, An = Ac –Ad = 1.61247285 – 0.193496742 = 1.418976108
m2
Active area, Aa =Ac – 2Ad = 1.61247285 – 2(0.193496742) =
2
1.225479366 m
Hole area, Ah take 10% Aa as first trial = 0.1x 1.225479366 = 0.122547937 m2
Weir length (from Figure 11.31 from Appendix A)

Ad/Ac =0.12
Iw/Dc =0.77
Iw = 1.500212212 m
Take,
Weir height = 50mm
Hole diameter = 5mm
Plate thickness = 5mm
Area of 1 hole,
d h 2 𝜋 (0.005 )2
Alh = = = 1.9625x10-5 m 2
4 4
153
Number of holes per plate,
Ah 0.122547937
Nh  = = 6244.480845 (approximately 6245 holes)
Alh 1.9625x10−5
2. Check weeping (Enough vapor to prevent liquid flow through hole)

LW ( RMM )
Maximum liquid rate =
3600s
574.775 × 66.4223918 𝑘𝑔
= = 10.6219571 𝑠
3600
Minimum liquid rate = 0.7 x 10.6219571kg/s (at 70% turn-down ratio)

=7.435369969 kg/s
5.2.21 Weir liquid crest
The height of the liquid crest over the weir can be estimated using the Francis weir
formula. For a segmental down comer this can be written as:
2/3
 Lw 
how = 750 
  l (l w ) 
2
10.6219571 3
𝑀𝑎𝑥𝑖𝑚𝑢𝑚 𝑕𝑜𝑤 = 750 = 32.30072684 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑
792.1826 × 1.500212212
2
7.435369969 3
𝑀𝑖𝑛𝑖𝑚𝑢𝑚 𝑕𝑜𝑤 = 750 = 25.4650376 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑
792.1826 × 1.500212212
At minimum rate, clear liquid depth,

how  hw = (0.025465038 + 0.05) m liquid = 0.075465038 m liquid
From the figure 11.30 [weep-point correlation (Eduljee, 1959)],
When how  hw = 0.075465038 m
K 2 = 35 from (Appendices 5)
154
5.2.22 Weep point
The lower limit of the operating range occurs when liquid leakage through the plate
holes becomes excessive is known as weep point. The vapor velocity at the weep
point is the minimum value for stable operation. Minimum vapor velocity through the
holes based on the holes area can be calculated using Eduljee (1959) equation:
K 2  0.9(25.4  d h )
U h (min) 
(  v )1 / 2
Obtain from figure 2.5 (Sinnott, 2000; Appendix B, p. B-4)
K 2  0.9(25.4  d h )
U h (min) 
(  v )1 / 2
35 − 0.9(25.4 − 0.005)
=
8.3212790.5
= 4.210024172 m/s
Actual minimum vapor velocity,

= minimum vapor rate
Ah
0.8 ×0.717946666
=
0.122547937
= 4.686797256 m/s
So, minimum operating rate will be below the weep point.
155
5.2.23 Plate pressure drop
a) Dry plate drop
The pressure drop through the dry plate can be estimated using expression derived
for flow through orifices:
2
U  
hd  51 h  v
 Co   L
Where, U h = velocity through the holes
C o = orifice coefficient
volumetricflowrate
Uh =
holearea , Ah
0.717946666
𝑈h = = 5.85849657 𝑚 𝑠
0.122547937
For plate thickness/hole diameter:

𝐴𝑕 0.122547937
= 100% = 10%
𝐴𝑝 1.225479366
So, orifice coefficient value can be obtained from figure 2.6 (Sinnott, 2000; Appendix
B, p. B-5) Coulson and Richardson: page 576
C o = 0.84
Therefore, dry plate drop:
1.225479366 2 8.321279
𝑕𝑑 = 51 × × = 26.0584611 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑
0.84 792.1826
b) Residual head
Residual head can be calculate using Hunt et al (1955) equation:
12.5 x10 3
hr 
L
12500
𝑕𝑟 = = 15.7791903 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑
792.1826
156
c) Total drop
The total plate drop is:
ht  hd  (hw  how )  hr
𝑕𝑡 = 26.0584611 + 75.465038 + 15.7791903 = 117.302689 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑
5.2.24 Downcomer Liquid Back-up
The downcomer area and plate spacing must be such that level of the liquid. The
froth in the downcomer is well below the top of the outlet weir on the plate above.
The liquid level that risers above the outlet weir will causes the column flood.
a) Downcomer pressure loss
𝑇𝑎𝑘𝑒 𝑕𝑎𝑝 = 𝑕𝑤 − 10 = 40 𝑚𝑚
Where, hap is the height of the bottom edge of the apron above the plate.
𝐴𝑟𝑒𝑎 𝑢𝑛𝑑𝑒𝑟 𝑎𝑝𝑟𝑜𝑛, 𝐴𝑎𝑝 = 1.500212212 40 × 10−3 = 0.060008488 𝑚2
As this is less than Ad =0.08262 m2, thus equation can be used to calculate the head
loss in down comer:
2
 L 
hdc  166 wd 
  L Am 
Where, hdc = head loss in down comer, mm
Lwd = liquid flow rate in down, kg/s
Am = either the down comer area Ad or the clearance area

under the downcomer Aap ; whichever is the smaller
2
10.6219571
𝑕𝑑𝑐 = 166 × = 8.287836986 𝑚𝑚
792.1826 × 0.060008488
Then take hdc = 8.287836986 mm.
157
b) Back-up in downcomer,
𝑕𝑏𝑐 = 50 + 32.30072684 + 117.302689 + 8.287836986 = 207.8912528 𝑚𝑚
After rounding off, take value hbc = 0.208 m.
For plate spacing 0.5m,

0.208 < ½(plate spacing + weir height)
0.208< 0.275
So, this plate spacing is acceptable.
c) Check residue 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 at least 3
seconds is recommended.
Ac hb c  L
tr 
Lwd
0.5 × 0.20789 × 792.1826

𝑡𝑟 = = 7.752235848 𝑠
10.6219571
This value is larger than 3, then it is satisfactory
5.2.25 Check entrainment

Entrainment can be estimated from the correlation given by Fair (1961). The
percentage flooding is given by:
% flooding = U n actual velocity (based on net area)
Uf
0.893660991
𝑈𝑕 = = 0.300310504 𝑚 𝑠
1.418976108
158
0.505961067
𝑝𝑒𝑟𝑐𝑒𝑛𝑡 𝑓𝑙𝑜𝑜𝑑𝑖𝑛𝑔 = × 100% = 80.33769776%
0.629792839
From figure 11.29 (Appendices 4):

 value = 0.039
 value is below 0.1, so column diameter which is proposed earlier is
acceptable.
5.2.26 Perforated area
From figure 2.8 (Sinnott, 2000; Appendix B, p. B-7)

𝑙𝑤 1.500212212
At 𝐷𝑐 = 1.948327548 = 0.77
Therefore,  c = 870
Angle subtended at plate edge by unperforated strips,
= (180 –87) = 930
a) Mean length, unperforated edge strips,
= (Dc –0.05) x  x
93
180
= (1.948327548 – 50 x10-3) m x  x
93
= 3.079720059 𝑚
180
b) Area of unperforated edge strips,

= (50 x 10-3) m x (3.079720059 m)
= 0.153986003 m2
c) Mean length of calming zone,
𝑀𝑒𝑎𝑛 𝑙𝑒𝑛𝑔𝑡𝑕 𝑜𝑓 𝑐𝑎𝑙𝑚𝑖𝑛𝑔 𝑧𝑜𝑛𝑒, 𝑎𝑝𝑝𝑟𝑜𝑥.
= 𝑤𝑒𝑖𝑟 𝑙𝑒𝑛𝑔𝑡𝑕 + 𝑤𝑖𝑑𝑡𝑕 𝑜𝑓 𝑢𝑛𝑝𝑒𝑟𝑓𝑜𝑟𝑎𝑡𝑒𝑑 𝑠𝑡𝑟𝑖𝑝
= 1.500212212 + 0.05
= 1.550212212 m
d) Area of calming zones,
= 2 x 0.05 (lw – 2 x 50x10-3) m 2
= 2 x 0.05 (1.500212212 – 2 x 50x10-3) m 2
= 0.140021221 m2
e) Total area available for perforation, Ap:
Ap= Active area – (Area of unperforated edge + Area of calming zones)
= 1.225479366 m2 – (0.153986003 + 0.140021221) m2
= 0.931472142 m2
159
𝐴𝑕 0.122547937
𝐴𝑝 = 0.931472142 = 0.131563716
From figure 2.9 (Sinnott, 2000; Appendix B, p. B-8):

lp
= 2.58 (satisfactory, range normally within 2.5 to 4.0)
dh
5.2.27 Summary for Chemical Design
Table 5.15: Summary of the Chemical Process Design

ITEMS Top Bottom
Column Diameter 1.433215 m 0.73561 m
Column Height 22 m 22 m
Column Area 1.6125 m2 0.4248 m2
Number of Plates 44 44
Tray Spacing 0.5 m 0.5 m
Plate Thickness 5mm 5mm
Down comer Area 0.193496742m 2 0.193496742m 2
Net Area 1.418976108m 2 1.418976108 m2
Active Area 1.225479366 m2 1.225479366 m2
Hole Area 0.122547937m 2 0.122547937m 2
Number of Holes 6245 units 6245 units
Weir Length 1.500 m 1.500 m
Weir Height 50mm 50mm
Resident Times 5.555s 5.555s
Minimum Reflux Ratio 0.195047801 0.195047801
Reflux Ratio 0.253562141 0.253562141
Column Efficiencies 80% 80%
q line 0.1702 0.1702
Feed Tray 15 from top 15 from top
160
SECTION 3: DESIGN OF BUTYL ACETATE DISTILLATION COLUMN (T101)
5.3 INTRODUCTION
Distillation is a mode of separation in the chemical industry where liquid or vapor mixture of
two or more substances is separated. These substances are separated into its component
fractions of desired purity by the application and removal of heat. Distillation principle is
base on the fact that vapor of a boiling mixture will be richer in components that have lower
boiling points or higher relative volatility. Hence when this vapor is condense, the
condensate will contain more volatile components and the original mixture will contain
components which are less volatile.
Distillation is the most widely used separation process in the chemical industry as its
application ranges from rectification of alcohol which had been practiced since antiquity to
the fractional of crude oil. Some of the characteristic of distillation are it is designed to
achieve efficient separation, is one of the most common separation technique, it consumes
large amount of energy (in terms of cooling and heating) and it contributes to more than 50%
of plant operation cost. Separation via distillation depends on the differences in volatility
between components. The greater the relative volatilities, the easier the separation process on
which is in accordance to the specification.
Since the relative volatilities are far apart, therefore distillation is the ideal means of
separation as it is common mode of separation and the design is common. However
distillation can be categorized as many types depending on the design which are specifically
for that particular separation where it is depending on the complexity of the design.
Generally the initial way of classifying the type of distillation is either in batch or continuous
operation which is explained in Table 1.0
Table 5.16: Difference between Batch and Continuous Column

Batch Column Continuous Column
 Batch operation is highly dependent on  Continuous column implies a
how the feed is introduced on which is continuous process where the feed
batch wise. introduced to the column is not
 The column is fed with a batch feed and interrupted unless the problem arises
the separation takes place. due to column or surrounding process
 When the separation is complete, the units.
next batch of feed is introduced.  This column is able to handle high
 Residence time is very important throughputs.
parameter to be control.
161
Since the designed plant is to be operated continuously, therefore it implies that the
distillation column (T-101) is running continuously. A further classification of the
continuous type of column would depend on either it is a binary (feed consist of two
components) or multi-component (feed consist of more than two components) column. Since
the feed effluent are two component mixture (methanol and methyl acetate), the distillation
column is a binary column. Since this column operates for binary system, Lewis Sorell
methods is selected to measure the number of stages required.
5.3.1 PRINCIPLES OF DISTILLATION
In the major design equipment of discussion, the separation is focused on separating liquid-
vapor mixtures and this is achievable by utilizing the difference in relative volatilities
between the components. In simplification, as the relative volatilities between components
are greater, the easier the separation. The separation of homogenous mixture requires the
creation or addition of another phase by repeated vaporization and condensation distillation.
The general arrangement in relation to distillation is as shown in Figure 1.1.
Figure 5.2: Basic Distillation Column
162
Since vapor consists of the lower boiling point components, it is considered as the
light key which flows to the top of the column and liquid flows to the bottom as it is heavy.
This counter current flow will cause interaction between vapor and liquid which is further
enhanced by contactors which are generally trays or packing.
The contactors will increase the interaction between vapor and liquid which
increases the efficiency in separation. A portion of the condensate from the condenser is
returned to the top of the column to provide liquid flow above the feed point which is known
as reflux and another portion of liquid from the bottom of the column is vaporized by the
reboiler and is returned in order to provide the vapor flow. The section below the feed is
known as the stripping section where the more volatile components are stripped from the
liquid and the section above the feed is known as the enrichment or rectifying section where
the concentration of the more volatile components is increased.
However there are cases where it is required by the process to strip a volatile
component from a relatively non-volatile mixture where rectification section is omitted. This
column is known as the stripping column. Some operation would have the top product as in
vapor where only a small required amount of liquid is condensed to provide the reflux flow
to the column and this condenser are known as the partial condenser. If the liquid is totally
condensed, the liquid returning to the column will have the same composition as the top
product.
5.3.2 TYPES OF SEPARATION PROCESS
There are many others separation processes available in the industry. Table 1.2 below
describes the common separation units and its functions.
163
Table 5.17: Common Separation Units in Industry
Type of Separation Explanation
Absorption  2 contacting phases are a gas and a liquid.
 Solutes are absorbed from gas phase into liquid phase.
 Involving molecular and turbulent diffusion or mass transfer of
solute through a stagnant non-diffusing gas into a stagnant
liquid.
 The reverse of absorption is called stripping or desorption.
Distillation  Involving a volatile vapor phase and a liquid phase that
vaporizes.
 Vapor consists of the more volatile component.
Liquid-liquid Extraction  2 phases are liquids where solutes are removed from one liquid
phase to another liquid phase.
Leaching  A fluid is used to extract a solute from solid.
Membrane Processing  Separation of molecules by the use of membrane.
 Membrane is a relatively thin, solid membrane controls the rate
of movement of molecules between 2 phases
Crystallization  Soluble solute in a solution is removed from solution by
changing the conditions (temperature or concentration).
 This will encourage solubility of one or more solute
components are exceeded and crystallization happens out as a
solid phase.
Adsorption  One or more components of a liquid or gas stream are adsorbed
on the surface or in the pores of a solid absorbent.
Advantages and Disadvantages of Distillation
Table 5.18 enlists the advantages and disadvantages of distillation. This indirectly are the
criteria that are considered in selecting distillation.
Table 5.18: The Advantage and Disadvantage of Distillation

Advantages Disadvantages
 Able to handle a wide range of  Incapability to separate low molecular weight
throughput. Other alternative to (MW) materials as these is distilled at high
distillation is capable of pressure to increase their condensing temperature.
handling low throughput. Refrigeration is required for condensing low MW
materials.
 Able to handle wide range of  Incapability to separate high MW heat sensitive

feed concentration. Other materials. High MW is often heat sensitive and is
alternative can handle only usually distilled under vacuum to reduce their
relatively pure feed. boiling temperature.
 Able to produce high product  Inability to separate of components with low

purity. concentration.
164
 Incapable to separate according to classes of
components as it separates according to boiling
points.
 In capability to separate mixture with low relative

volatility or exhibit azeotropic behaviour.
 Incapability of separation of a volatile (non-

condensable) liquid from an in volatile
component (condensable).
Based on above table, it is cleared that the capability of distillation is limited but
nevertheless it is still the best as the basic advantage still supersedes the disadvantage. Since
the advantage is similar to the characteristic of this process, distillation had been selected as
the ideal mode of separation for this purpose. Based on all the consideration above,
distillation column is the preferred mode of separation for the production of product
5.3.3 DISTILLATION CONTACTORS
a) CONTACTORS
In order for separation to occur the internal flows are important. The interaction between
liquid and vapor will enhance the separation process (mass transfer). In other words, if the
interaction (intimate contact) between these flows is increase the separation will be better.
Hence the rate to increase these interaction forces research to be conducted in this area and
generally the two common type of contactors used are plate and packing. Table 1.4 shows
the advantages and disadvantages of using plates versus packing column.
Table 5.19: Difference between Plate and Packed Column

Contactor Advantage Disadvantage
Plate  Designed to handle wider range of liquid and gas flow
rates.
 Plate efficiency can be predicted more certainty than HETP
or HTU for packing.
 Designed with more assurance than packing.
 Good liquid distribution can be maintained throughout a
plate column under all operating condition particularly in
large columns.
 Easier to make provision for cooling
 Easier to make provision for withdrawal of side streams.
 Easier to make provision for cleaning if the liquid causes
fouling (man way can be installed)
165
Packing  More cost effective for dealing with corrosive liquids.  Not suitable
 Liquid hold up is lower than plate (important when for very low
inventory of toxic or flammable liquids need to be keep as liquid rates.
small as possible).  Expensive
 Suitable for handling foaming systems.
 Pressure drop per equilibrium stage (HETP) is lower and
should be considered for vacuum columns.
 Suitable for small columns (diameter less than 0.6m) where
it is cost effective.
Based on Table 1.4, plate column is more economical choice instead of a packing column
due to the column is large and it is not economically feasible to have packing for such high
throughput.
b) Plate Contactors
The terminology of plates or trays is used interchangeably. Cross flow plates are the most
common type of plate contactor used for distillation. The definition of cross flow illustrates
that the liquid flows across the plate and the vapor up through the plate. Figure 1.2, shows
the typical layout of a cross flow plate. The liquid that is flowing is transferred in a cascade
formation from plate to plate by gravity through vertical channels known as “down comers”.
Normally a pool of liquid is retained on top of the plate by an outlet weir. The weir
is design in such that the hold up will be at a suitable height. Vapor being lighter will flow
up the column by passing through the liquid via the openings on each tray. This area which
is allowed for the passage of vapor on each tray is known as the active tray area. As the hot
vapor passes through the liquid heat is being transferred to the liquid. This interaction will
cause some vapor to condense adding to the liquid and the condensate now is richer in the
less volatile component than the vapor.
The same principle but opposite in application is experienced by the liquid where
heat input from the vapor will cause the liquid on the tray to boil generating more vapor.
Vapor will move to the next higher tray where it is richer in more volatile components. This
process happens continuously in each tray and causes the separation between low boiling
point and higher boiling point components.
166
Figure 5.3 Typical Cross Flow Plate (Sieve Tray)

Table 5.20 classifies the various types of plate or tray design. The one shown here is the
common type of plates used in the chemical industry.
Table 5.20: Types of Plates Common in Industry

Type Explanation Illustration
Sieve Plates  Simplest type of cross flow plate.
(Perforated Plate)  Vapor passes up through perforations in the
plate and liquid is retained on the plate by
vapor flow (by the kinetic energy of the
vapor).
 No positive vapor liquid seal.
 Low flow rates liquid will “weep” through the
holes reducing plate efficiency.
 Vapor area of holes varies between 5 to 15%
of the tray area.
Bubble-Cap Plates  Vapor passes through short pipes known as

risers or chimney covered with cap with a
serrated edge or slots.
 The significant feature of the bubble cap plate
is that the use of risers ensures that the level of
liquid is maintained on the tray at all vapor
flow-rates.
 Vapor rises through the opening in the plate
into the bubble caps.
 The cap is mounted so that the space between
riser and cap allow the passage of vapor.
167
Valve Plates  It is sieve plates with large diameter holes
(Floating Cap covered by movable flaps which lift as vapor
Plates) flow increases.
 Area for vapor flow varies with flow rate.
 Vapor flows lift the cap thus creating a flow is
for the passage of vapor.
 The vapor is directed to flow horizontally into
the liquid providing better mixing.
 It is able to operate efficiently at lower flow
rates than sieve plates (valve closing at low
vapor rates)
Table 5.21: Performance of Three Plates

Factors Discussion
Cost  Bubble cap more expensive than sieve or valve.
 Relative cost dependent on the material of construction used (for
mild steel the ratio bubble cap: valve: sieve – 3.0: 1.5: 1.0)
Capacity  Little difference in capacity rating.
 Diameter required for given flow rate (sieve, valve, bubble cap)
Operating range  Range of vapor and liquid rates over which the plate will operate
satisfactory.
 Flexibility is required to allow changes in production rate and start-
up and shut down conditions.
 Bubble cap has positive liquid seal and can operate efficiently at
very low vapor rates.
 Good design sieve plates can operate from 50 to 129 % of design
capacity.
 Valve can give flexibility than sieve at a lower cost.
Efficiency  According to Murphree efficiency, the three types of plate is
virtually the same when operating over their design flow range.
Pressure drop  Pressure drop is important design consideration when involving
vacuum columns.
 Sieve plates will give the lowest pressure drop followed by valves
with bubble cap having the highest.
In selecting the ideal plate to be used for which process there are various factors that should
be considered in selection. Table 5.21 discusses the performance of the three mentioned type
of plates according to the cost, capacity, operating range, efficiency and pressure drop Sieve
plates are the cheapest and satisfactory for most application. The valve plates could be
considered if the specified turn-down ratio cannot meet with sieve plate and the bubble caps
should be used when very low vapor rates are handled and positive liquid seal is essential at
168
all flow rates. Hence in this preliminary design a sieve plate should be sufficient to provide a
good performance with respect to cost and efficiency.
5.3.4 THEORY OF CHEMICAL ENGINEERING DESIGN OF BUTYL ACETATE

DISTILLATION COLUMN
a) Introduction
Distillation is the most widely applied separation process in the chemical and allied
industries. Distillation also used in separation technology the various components of a liquid
solution, which depends upon distribution of these various components between a vapor and
a liquid phase. All components are present in both phases. The vapor phase is created from
the liquid phase by vaporization at the boiling point. The basic requirement for the separation
of components by distillation is the composition of the vapor is different from the
composition of the liquid which it is equilibrium at the boiling point of the liquid.
The design of a distillation column can be divided in the following steps:

8. Specify the degree of separation required: set specification.
9. Select the operating conditions: batch or continuous; operating pressure.
10. Select the type of contacting device: plate or packing.
11. Determine the stage and reflux requirements: the number of equilibrium stages.
12. Size of the column: diameter, number of real plates.
13. Design the column internals, plates, distributors, and packing support.
14. Mechanical design: vessel and internal fittings.
b) Estimate number of stages

To estimate number of stages, condenser and reboiler temperature, and procedures are
required for calculating dew and bubble points. By definition, a saturated liquid is at its
bubble point (any rise in temperature will cause a bubble vapor to form), and a saturated
vapor is at its dew point (any drop in temperature will cause a drop of liquid to form). Dew
point and bubble point can be calculated from knowledge of the vapor-liquid equilibrium for
the system. In term of equilibrium constants, the bubble point is defined by the equation:
Bubble point:  yi   kixi  1.0

Dew point :  xi   yi / ki  1.0
169
5.3.5 PRODUCT SPECIFICATION
a) Mass Balance at Distillation Column (T-101)
Stream 15
Stream 13A
E-3
Stream 16
Figure 5.4: Distillation Column (T-101)
Table 5.22: Stream Summary of Mass Balance Distillation Column (T-101)

No of Stream 13A 15 16
Flowrate (kmol/h) 144.8900 33.1368 111.7532
Total Flowrate
(kmol/h) 144.8900 144.8900
Composition
(mol %)
Methyl acetate 0.1727 0.8203 0.1706
Butyl acetate - - -
Methanol 0.8273 0.1797 0.8294
Butanol - - -
Total 1.0000 1.0000 1.0
170
5.3.6 CALCULATION OF CHEMICAL DESIGN OF DISTILLATION COLUMN
a) To calculate bubble and dew point

Using Antoine equation to find vapor pressure (P 0)
B
LogP 0  A 
(T  C )
Where
P - vapor pressure in mmHg
A, B, C, D, E – Constants obtained from Chemical Engineering, volume six, Page
766-785)
T – Temperature in degree celcius
Table 1.8: The Antoine constant values for each component

Comp A B C
Methyl acetate 7.06524 1157.630 219.726
Methanol 7.87863 1473.11 230
Sources: (Chemical Engineering, volume six, Page 766-785)
Ki = P0
b) Dew temperature (Top column) x   y

i i / k i  1.0
Temperature = 64.1°C Operating pressure =1064.175 mm Hg

Comp yi = xd Pi (mm Hg) ki ∑xi=∑yi/ki
Methyl acetate 0.8203 969.57 0.9111 0.9003
Methanol 0.1797 737.83 0.6933 0.2592
Total 1.160

So, dew temperature is 64.1°C
171
c) Bubble point (Bottom Column) y i  k x

i i  1.0
Temperature = 80.92 °C Operating pressure = 1406.3657mm Hg
Comp xw = xi Pi (mm Hg) ki yi =kixi

Methyl acetate 0.1706 1639.7011 1.1659 0.1989
Methanol 0.8294 1382.6847 0.9832 0.8154
Total 1.014
k x i i value is close to 1.0, therefore this temperature is accepted.
So, bubble temperature is 80.92°C
1.6.1.3 Bubble point of the feed y i  k x

i i  1.0
Temperature = 64.10 °C Operating pressure = 1500mm Hg
Comp xf = xi Pi (mm Hg) ki yi = ki xi

Methyl acetate 0.1727 969.5699 1.1970 0.2067
Methanol 0.8273 740.8930 0.9147 0.7567
Total 0.9634
So, bubble temperature is 64.10°C
d) To find q line
  H fs  H f
q=

 = the molar of the latent heat of vaporization
Hfs = the molar enthalpy of the feed at its boiling point
Hf = the molar enthalpy of the feed
Temperature = 193 K
172
Table 5.23: The constant values for each component
CP
Comp (kJ/kmol.K)
A b C d
Methyl acetate 16.550 2.245x10-1 -4.341x10-5 2.914x10-8
Methanol 21.152 7.092x10-2 2.587x10-5 -2.851x10-8
Specific heat capacity, Cp0:
CP 0 = a + bT + cT2 + dT3
C P 0 (Methanol) = 21.152 + 7.092E-02 (337.1) + (2.587E-05) (337.1)2 – 2.851E-08

(337.1)3
= 46.9068KJ/kmol.K
Latent heat equation due to Haggenmacher (1946) is derived from the Antoine vapor
pressure equation:
8.32 BT 2 z
Lv =
(T  C ) 2
Where Lv = latent heat at the required temperature, kJ/kmol

T = temperature, K
B, C= coefficients in the Antoine equation
z = Zgas – Z liquid (where z is the compressibility constant), calculated
from the equation :
0.5
 P 
z  1  r 3 
 Tr 
Pr = reduced pressure
Tr = reduced temperature
173
Feed composition:
Comp TC (K) z

P0 (bar) PC (bar) CP Pr Tr
Methyl acetate 506.8 0.9230 1.2927 46.9 88.4123 0.02132 0.6509
Methanol 512.6 0.9568 0.9878 81.0 46.9068 0.01235 0.6586
Comp Mol. Frac MW Tbp (K) Lv

Methyl acetate 0.1727 74.08 329.9 7.5963
Methanol 0.8273 32.042 337.6 7.8745
Feed:
Mean molecular weight = 0.1727(74.08) + 0.8273(32.042)

= 39.3020 kg/kmol
Mean boiling point = 0.1727(329.9) + 0.8273(337.6)

= 336.27 K
Specific heat, C P = 0.1727(88.4123) + 0.8273(46.9068)

= 54.0748 J/mol.K
Latent heat,  =0.1727(7.59629) + 0.8273(7.874463)

=7.8264 J/mol
H fs = C P T
= 54.0748 J/g.K (39.3020 kg/kmol) (336.27 – 273)K

= 134.46KJ/kmol
Hf = C P T
= 54.0748 J/g.K (39.3020 kg/kmol) (337.1 – 273)K

=136.23 KJ/kmol
Therefore,
  H fs  H f
q= = 0.7491 < 0 (feed in liquid phase)

174
5.3.6 Relative volatility
The vapor-liquid equilibria for a mixture are described by distribution coefficients or K

factors, where K for each component is the ratio of mole fractions in the vapor and liquid
phases at equilibrium. If Raoult’s law and Dalton’s law hold, values of Ki can be calculated
from the vapor pressure and the total pressure of the system. The K factors are strongly
temperature dependent because of the change in vapor pressure, but the relative values of K
for two components change only moderately with temperature. The relative volatility of two
components can be expressed as the ratio of their K values:
Ki
i j 
Kj
0.9481
 =0.8871 (at top column)
1.0688
1.1659
 =1.1858 (at bottom column)
0.9832
0.871  1.1858
 =1.0365 (at average)
2
5.3.7 Overall column efficiency
The overall column efficiency can be calculated by O’Connel (1946) where it is correlated
with the product of the relative volatility of the light key component and the molar average
viscosity of the feed, estimated at the average column temperature. It had been found that it
give reliable estimates of the overall column efficiency for hydrocarbon systems and can be
used to make approximate estimate of the efficiency for other systems. This method does not
account of the plate design parameters and includes only two physical property variables.
Eduljee (1958) expressed the O’Connel correlation in the form of
E0  51  32.5 log(  a a )
 a = the molar average liquid viscosity, mNs/m2
175
Temperature = 363.19 K (top column)
= 353.92 K (bottom column)
Average temperature =358.56 K
Viscosity of components at average temperature, 358.56 K:
Log ( a ) = [VISA] * [(1 / T) – (1/VISB)]
Where, VISA, VISB = correlation constant
Table 5.24: The constant values for each component
Comp VISA VISB Viscosity Mol. Frac.

Methyl acetate 408.62 224.03 0.6843 0.1727
Methanol 555.30 260.64 0.5818 0.8273
Mean average viscosity =(0.1727 x 0.6843)+(0.8273x0.5818)

= 0.5995
From the previous calculation, relative volatility is:
 a = 1.0365
E0  51  32.5 log(  a a )
Therefore, overall column efficiency, E o = 57.72 %
The minimum number of stages is 9 ( according to Lewis Sorell), and overall column
efficiency is 57.72 %.
Lewis Sorell Method
176
Consider reboiler and condenser as a stage, therefore, number of real stages is:
E 0 = number of ideal stages

number of real stages
(9  1)
Number of real stages = = 13.86 (approximately 14 stages)
0.5772
a) Calculation to Determine Feed Point
An estimate can be made by using the Fenske equation to calculate the

number of stages in the rectifying and stripping section separately, but this
requires an estimate of the feed-point temperature. An alternative approach
is to use the empirical equation given by Kirkbride (1944):
177
N   x  x b,LK 
2
Log  r  = 0.206 log  B  f ,HK   
 Ns   D  x f ,LK  x
 d,HK

 
 
Where, Nr = number of stages above the feed, including

any
partial condenser
Ns = number of stages below the feed, including
the
reboiler
product
x b,LK = concentration of the light key if in the
bottom
product
N   33.1368 0.8273  0.1706 

2

Log  r  = 0.206 log  


  
 Ns   111.7532  0.1727  0.1797 
 
 
 Nr 
  = 1.0635
 Ns 
Nr  Ns = 14
2.7518Ns + Ns = 14
Nr = 7.2154
Ns =6.785
Therefore, the feed is at stages 7 from the bottom column.
178
b) Pressure drop
Pressure at top column = 141.9 kPa
Pressure at bottom column =187.5 kPa
Total pressure drop in the column is = (187.5-141.9) kPa
= 45.6 kPa
i. Calculation for density and relative molar mass (RMM)
Comp Molecular Feed Top (D) Bottom (B) Liquid

Weight,MW Mol. Frac.,xF Mol. Frac.,xD Mol. Frac.,xB Density (kg/m3)
Methyl acetate 74.080 0.1727 0.8203 0.1706 934
Methanol 32.042 0.8273 0.1797 0.8294 791
ii. Calculation for Relative Molar Mass (RMM)
RMM of Feed = (0.1727x74.080) +(0.8273x32.042)

= 39.3020 kg / kmol
RMM of Top Product = (0.8203x74.080) +(0.1797x32.042)
= 66.5258 kg / kmol
RMM of Bottom Product = (0.1706x74.080) +(0.8294x32.042)
= 39.2137kg / kmol
iii. Calculation for density
a) Bottom product
Liquid density, L = x B ,i i
= 0.17066(934) + 0.8294(791)
=815.3958 kg / m3
Vapor density,  V =  x B ,i  i
= 0.17066(4.7205) + 0.8294(2.042)
= 2.4990 kg / m3
b) Top product
179
Liquid density,  L =  x B ,i  i
= 0.8203(934) + 0.1797(791)
= 908.3029 kg / m3
Vapor density,  V =  x B ,i  i
= 0.8203(3.4812) + 0.1797(1.5057)
=3.1262 kg / m3
5.3.8 Column diameter
The principal factor that determines the column diameter is the vapor flow rate. The equation
given below, which is based on the well-known Souders and Brown equation, Lowenstein
(1961), can be used to estimate the maximum allowable superficial vapor velocity, and hence
the column area and diameter:
1/ 2
 (  L  V 
uv  (0.171l  0.27lt  0.047) 
2

 V 
t
Where, u v = maximum allowable vapor velocity, based on the gross (total)

Column cross-sectional area, m/s
l t =plate spacing, (range 0.5 – 1.0)
The column diameter can be calculated using equation:
4Vw
Dc =
 v u v
Where, Vw = the maximum vapor rate, kg/s
 (815.3958  3.1262) 
1/ 2
uv  (0.171(0.500)  0.27(0.500)  0.047)  

 3.1262
uV = 0.7375 m/s
Therefore, column diameter is:
4(1.317)
Dc = = 0.8528 m
 (3.1262)(0.7375)
180
Dc = 0.8528 x 1.5
= 1.2792 m
For safety reason, the approximate diameter was increased 50% more than the calculated
value, as it deals with vapour, which is in high pressure.
5.3.9 Column area
Column area can be calculated using equation:

D 2 =  (1.2792m) 2 =1.2852 m2
Area 
4 4
5.3.10 Surface tension ( )
 Pch (  L  V )  x10 –12

4
  
 M 
Where,  = surface tension, MJ/m2 or (dyne/cm)

Pch = Sugden’s parachor
V  Vapor density, kg/m3
 l = Liquid density, kg/m3
For mixture,
 m   1 x1   2 x 2 .....
Where,  m = surface tension mixture
 1 2 = surface tension for mixture
x1 x 2 = component mol fraction
Calculation for parachor (Pch

Comp Mol. Frac. Mol. Frac. Pch
top column,xD Bottom column,x,B Contribution
Methyl acetate 0.8203 0.1706
177.00
Methanol 0.1797 0.8294
87.400
Pch at Top column = x D ,i Pch, i
181
= (0.8203x177) +(0.1797x87.4)
= 160.90
Pch at Bottom column = x B ,i Pch, i
= (0.1706x177) + (0.8294x87.4)
= 102.86
Therefore, surface tension at top column,
4
160.90(815.3958  3.1262)kg / m 3 
   x10
–12
 66.5258 
 = 14.90 N/m
Surface tension for Bottom column,

4
102.68(815.3958  3.1262)kg / m 3 
   x10
–12
 39.2137 
 = 20.46 N/m
5.3.11 Flooding velocity

Flooding velocity can be estimated from the correlation given by Fair (1961):
 L  V
U f  Ki
V
Where, U f = flooding vapor velocity, m/s, based on the net column

cross-sectional area
K i = a constant obtain from figure 2.2 (Sinnott, 2000;pg 459)
The liquid-vapor flow factor, FLV in figure 2.2 is given by:
LW V
FLV 
VW L
Where, LW =liquid mass flow rate, kg/s
VW =vapor mass flow rate, kg/s
1.3856kg / s 3.1262
FLV 
1.3169kg / s 815.3958
FLV = 0.06515
From the figure 11.27, pg459 value of Ki = 0.092
182
908.3029  3.1262
Top U f = 0.092 = 1.5654 m/s
3.1262
815.3958  2.4990
Bottom U f = 0.092 = 1.6592 m/s
2.4990
For design, a value of 80 to 85 per cent of the flooding velocity should be used.
Bottom U f = 1.6592m/s (0.85) = 1.4104m/s
Top U f =1.5654 m/s (0.85) = 1.3306m/s
5.3.12 Maximum volumetric flow-rate

Vm ( RMM )
Maximum volumetric flow-rate =
V
a) Above the feed point
Vn  D( R  1)
= 33.1368 kmol/h (4.65 + 1)
= 187.2224 kmol/h
Liquid down flow will be:
Vn = Ln  D
Ln = Vn  D
= (187.2224 – 33.1368) kmol/h
= 154.0861 kmol/h
b) Below the feed point

Liquid flow rate will be:
Lm = Ln  F
= (154.0861 – 144.8900) kmol/h
= 9.1961 kmol/h

Vm = Lm  W
= (111.7532–9.1961) kmol/h
183
= 102.5571 kmol/h
Therefore, maximum volumetric flow rate:
Vm ( RMM ) 102.5571(39.2137)
Bottom = = = 0.4470 m3/s
V 2.4990
Vm ( RMM ) 102.5571(66.5258)
Top = = = 0.6062 m3/s
V 3.1262
Net area required = volumetricflowrate

floodingvelocity
0.4470
Bottom = = 0.3170 m2
1.4101
0.6062
Top = =0.4556 m2
1.3306
As first trial, take down comer area as 12 % of total column cross-sectional area:
0.3170
Bottom = = 0.4216 m2
0.88
0.4556
Top = = 0.5177 m2
0.88
Liquid flow pattern,

L ( RMM )
Maximum volumetric liquid rate =
L
111.7532kmol / h(39.2137)kg / kmol

=
3
815.3958kg / m
= 1.4929x10-3 m3/s
The choice of plate type (reverse, single pass or multiple pass) will depend on the liquid flow
rate and column diameter. An initial selection can be made using Figure 11.28 (Sinnott,
volume6; page 460) which has been adapted from a similar figure given by Huang and
Hodson. From the figure, it show that cross-flow (single pass) plate can be used.
184
5.3.12 Provisional plate design
Column diameter, DC = 1.2792 m
Column area, AC = 1.2852 m2
Down comer area, Ad = 0.12 x 1.2852 m2 (at 12%)
= 0.1542 m2
Net area, An = AC  Ad
= 1.2852 – 0.1542
= 1.131 m2
Active area, Aa = AC  2 Ad
= 1.2852 – (2 x0.1542)
= 0.9768 m2
Hole area,Ah = 0.09768 m2 (take 10% of Aa as first trial)
a) Weir Length
Ad 0.1542
x 100% = x 100% = 12%
AC 1.2852
From figure 11.31, (Sinnott, 2000;pg464)
IW = 0.76 x 1.2792m = 0.9722m
Take weir height , hw = 50mm

Hole diameter,dh = 5mm
Area of 1 hole,
d h 2  (0.005) 2
Alh = = =1.963 x 10-5 m2
4 4
Number of holes per plate,

Ah 0.09768
Nh  = =4976.05holes (approximately 4976 holes)
Alh 1.963x105
185
b) Check weeping (Enough vapor to prevent liquid flow through hole)
LW ( RMM )
Maximum liquid rate =
3600s
111.7532kmol / h(39.2137kg / kmol)
=
3600s
= 1.2173 kg/s
Minimum liquid rate = 0.7 x 1.2173 kg/s (at 70% turn-down ratio)
= 0.8521 kg/s
c) Weir liquid crest
The height of the liquid crest over the weir can be estimated using the Francis weir formula.
For a segmental down comer this can be written as:
2/3
 Lw 
how = 750 
  l (l w ) 
2/3
 1.2173kg / s 
Maximum how = 750 3
 =9.98 mm liquid
 815.3958kg / m (0.9722m) 
2/3
 0.8521kg / s 
Minimum how = 750 3
 =7.87 mm liquid
 815.3958kg / m (0.9722m) 

how  hw = (7.87 + 50) mm liquid = 57.87 mm liquid
From the figure 11.30 [weep-point correlation (Eduljee, 1959)],
When how  hw =57.87
K 2 = 30.5
d) Weep point
The lower limit of the operating range occurs when liquid leakage through the plate’s hole
becomes excessive. This is known as weep point. The vapor velocity at the weep point is the
minimum value for stable operation. The hole area must be chosen so that at the lowest
operating rate the vapor flow velocity is still well above the weep point.
186
Minimum vapor velocity through the holes based on the holes area can be calculated using
Eduljee (1959) equation:
K 2  0.9(25.4  d h )
U h (min) 
(  v )1 / 2
Obtain from figure 11.30 (Chemical Engineering, Coulson,
Richardson and R.K.Sinnot ,volume 6)
K 2  0.9(25.4  d h )
U h (min) 
(  v )1 / 2
= 30.5  0.9(25.4  5)
(3.121)
= 3.8898m/s
Actual minimum vapor velocity,

= minimum vapor rate
Ah
3
= 0.7(0.4470m 2 / s)
0.09768m
=3.2033 m/s
So, minimum operating rate will be below the weep point.
5.3.13 Plate pressure drop
a) Dry plate drop

The pressure drop through the dry plate can be estimated using expression derived for flow
through orifices:
2
U  
hd  51 h  v
 Co   L
Where, U h = velocity through the holes
187
C o = orifice coefficient
volumetric flowrate
Uh =
holearea , Ah
0.6062m 3 / s
Uh = = 6.2060 m/s
0.09768m 2
For plate thickness/hole diameter:
Ah 0.09768m 2
 x100% = 10
Aa 0.9768m 2
So, orifice coefficient value can be obtain from figure 11.34 (Sinnott, volume6, page467)
For plate thickness/hole diameter =1, therefore,
C o = 0.83
Therefore, dry plate drop:
2
 6.2060m / s  3.1262kg / m 3
hd  51  3 = 10.9316 mm liquid
 0.83  815.3958kg / m
b) Residual head
Residual head can be calculate using Hunt et al (1955) equation:
12.5 x10 3
hr 
L
12.5 x10 3 =15.3300 mm liquid
hr 
815.3958
c) Total drop
The total plate drop is:
ht  hd  (hw  how )  hr
ht  10.93  (57.87)  15.33
ht  84.13 mm liquid
188
5.3.14 Down comer liquid back-up
Down comer pressure loss:
hap  hw  10mm
hap  50mm  10mm = 40 mm
Area under apron,

Aap  hap (l w ) = 40 x 10-3 m (0.9722m) =0.039 m2
Where Aap is the clearance area under down comer.
As this is less than Ad = 0.1542 m2, thus equation can be used to calculate the head loss in
down comer:
2
 L 
hdc  166 wd 
  L Am 
Where, hdc = head loss in down comer, mm
Lwd = liquid flow rate in down, kg/s
Am = either the down comer area Ad or the clearance area under the
down comer Aap ; whichever is the smaller
2
 1.3856 
hdc  166  = 1.8983mm
 (815.3958)(0.039) 
= say it as 2mm
Back-up in the down comer, ( hb ),
hbc  hw  how  ht  hdc
hdc  (50 +7.87 + 84.13 + 2)
hdc  144 mm liquid or 0.144 m

Check,
1
0.144 m < (plate spacing + weir height)
2
1
0.144m < (0.5  0.05)m = 0.275 m
2
So, tray spacing is acceptable, (to avoid flooding)
189
5.2.15 Check entrainment
Entrainment can be estimated from the correlation given by Fair (1961). The percentage
flooding is given by:
% flooding = U n actual velocity (based on net area)
Uf
Uf 3
Un = = 0.4470m 2 / s = 0.3952 m/s
An 1.131m
0.3952m / s
% flooding = x100 = 53.59 %
0.7375m / s
From figure 11.29 (Sinnott, volume6; page 461):
 value = 0.026
 value is below 0.1, so column diameter which is proposed earlier is acceptable.
5.3.16 Perforated area
From figure 11.32 (Sinnott, volume6;page 465 )

lw
At  0.76
Dc
Therefore,  c = 990
Angle subtended at plate edge by unperforated strips,

= (180 –99) = 810
Mean length, unperforated edge strips,
= (Dc –0.05) x x 81
180
= (1.2792 – 50 x10-3) m x x 81
180
= 1.7377 m
Area of unperforated edge strips,

= (50 x 10-3)m x (1.7377 m)
= 0.08689 m2
190
Area of calming zones,

= 2 x 0.05 (lw – 2 x 50x10-3) m2
= 2 x 0.05 (0.9722 – 2 x 50x10-3) m2
= 0.08722 m2
Total area available for perforation, Ap :
Ap = Active area – (Area of unperforated edge + Area of calming zones)
= 0.9768 m2 – (0.08689 + 0.08722) m2
= 0.8027 m2
Ah 0.09768
= = 0.1217
Ap 0.8027
From figure 11.33 (Sinnott, volume6; page 466):

lp
= 2.750 (satisfactory, range normally within 2.5 to 4.0)
dh
191
Table 5.25 : Summary of the Chemical Design
Overall Efficiency, Eo 0.5772

Plate spacing, It 0.5 m
Column diameter 1.2792 m
Column Thickness 12 mm
Column area 1.2852 m2
Surface tension, σ
Surface tension at top, σ 14.90 N/m
Surface tension at bottom, σ 20.46 N/m
Flooding velocity, Uf
Flooding velocity at top 1.3306 m/s
Flooding velocity at bottom 1.4104 m/s
Down comer area, Ad 0.1542 m2
Net area, An 1.131 m2
Active area, Aa 0.9768 m2

Hole area,Ah 0.09768 m2
Column diameter, DC 1.2792 m
Column area, AC 1.2852 m2

Weir Length 0.9722 m
weir height , hw 50 mm
Hole diameter, dh 5 mm
Plate thickness 5 mm
Area of 1 hole 1.963 x 10-5 m2
Number of holes per plate 4976 holes
Check weeping
Maximum liquid rate 1.2173 kg/s
Minimum liquid rate 0.8521 kg/s
Weir liquid crest
Maximum 9.98 mm liquid
Minimum 7.87 mm liquid
weep-point correlation 30.5
Actual minimum vapor velocity 3.2033 m/s
Residual head 15.3300 mm liquid
Total drop 84.13 mm liquid
Mean length, unperforated edge strips 1.7377 m
Area of unperforated edge strips 0.08689 m2
Area of calming zones 0.08722 m2
Total area available for perforation, Ap 0.8027 m2
192
SECTION 4: DESIGN EQUIPMENT FOR DISTILLATION COLUMN (T102)
5.4 INTRODUCTION
Distillation is a mode of separation in the chemical industry where liquid or vapor

mixture of two or more substances is separated. These substances are separated into
its component fractions of desired purity by the application and removal of heat.
Distillation principle is base on the fact that vapor of a boiling mixture will be richer
in components that have lower boiling points or higher relative volatility. Hence
when this vapor is condense, the condensate will contain more volatile components
and the original mixture will contain components which are less volatile.
Distillation is the most widely used separation process in the chemical
industry as its application ranges from rectification of alcohol which had been
practiced since antiquity to the fractional of crude oil. Some of the characteristic of
distillation are it is designed to achieve efficient separation, is one of the most
common separation technique, it consumes large amount of energy (in terms of
cooling and heating) and it contributes to more than 50% of plant operation cost.
Separation via distillation depends on the differences in volatility between
components. The greater the relative volatilities, the easier the separation process on
which is in accordance to the specification.
Since the relative volatilities are far apart, therefore distillation is the ideal
means of separation as it is common mode of separation and the design is common.
However distillation can be categorized as many types depending on the design
which are specifically for that particular separation where it is depending on the
complexity of the design.
Since the designed plant is to be operated continuously, therefore it implies that the
Distillatio column (T-102) is running continuously. A further classification of the
continuous type of column would depend on either it is a binary (feed consist of two
components) or multi-component (feed consist of more than two components)
column.
193
5.4.1 FACTORS AFFECTING DISTILLATION COLUMN OPERATION
The performance of a distillation column is determined by many factors, for example
a) Feed Condition
The state of the feed mixture and feed composition affects the operating lines and
hence the number of stages required for separation. It also affects the location of feed tray.
During operation, if the deviations from design specifications are excessive, than the column
may no longer be able to handle the separation task. To overcome the problems associated
with the feed, some column are design to have multiple feeds points when the feed is
expected to containing varying amounts components.
b) Internal liquid and fluid flow conditions
As the reflux ratio is increased, the gradient of operating line for the rectification
section moves towards a maximum value of 1. Physically, means that more and more liquid
that is rich in the more volatile components are being recycled back into the column.
Separation then becomes better and thus fewer trays are needed to achieve the same degree
of separation. Minimum trays are required under total reflux conditions, for example there is
no withdrawal of distillate. On the other hand, as reflux is decreased, the operating line for
the rectification section moves towards the equilibrium line. The pinch between operating
and Equilibrium lines becomes more pronounced and more and more trays are required. This
is easy to verify using Fenske Equation method. The limiting condition occurs at minimum
reflux ratios, when an infinite number of trays will be required to effect separation. Most
columns are designed to operate between 1.2 to 1.5 times the minimum reflux ratios because
that is approximately the region of minimum operating costs (more reflux means higher
reboiler duty).
194
c) Column diameter
Most of the above factors that affect column operation are due to vapor flow
conditions: Either excessive or too lows. Vapor flows velocity is dependent on column
diameter. Determines the minimum vapor flow required while flooding determines the
maximum vapor flow to allowed, hence column capacity. Thus, if the column diameter is not
sized properly, the column will not perform well. Not only will operational problems occur,
the desired separation duties may not be achieved.
d) State of trays (packing)
The actual number of trays required for a particular separation duty is determined by
the efficiency of the plate, and the packing if packing is used. Thus, any factors that cause a
decrease in tray efficiency will also change the performance of the column. Tray efficiencies
are affected by fouling, wear and tear and corrosion and the rates at which these occur
depends on the properties of the liquids being processed. Thus appropriate materials should
be specified for tray construction.
e) Weather conditions
Most distillation columns are open to the atmosphere. Although many of the
columns are insulated, changing weather conditions can still affect column operation.
Thus the re-boiler must be appropriately sized to ensure that enough vapour can be
generated during cold and windy spells and that it can be turned down sufficiently
during hot seasons. The same applied to condensers. These are some of the more
important factors that can cause poor distillation column performance. Other factors
include changing operating conditions and throughputs, brought about by changes in
upstream conditions and changes in the demand for the products. All these factors,
including the associated control systems, should be considered at the design stages
because once a column is built and installed, nothing much can be done to rectify the
situation without incurring significant costs.
195
5.4.2 SAFETY FACTOR
Safety factors represent the amount of overdesign that would be used to

account for not only the changes in the operating performance with time, but also the
uncertainties in the design process.The role of the principle piece of equipment in the
overall operation must be considered along with the consequences of underdesign.
Fouling, which may occur during operation, should never be overlooked when design
safety factor is determined. Potential increases in capacity requirements are
sometimes used as an excuse for applying large safety factors. This practice,
however, can result in so much overdesign that the process or equipment never has
an opportunity to prove its economic value.
In general design work, the magnitudes of safety factors are dictated by

economic or market consideration, the accuracy of the design data and calculations,
potential changes in the operating performance, background information available on
the overall process, and the amount of conversation used in developing the individual
components of the design. Each safety factor must be chosen on the basis of the
existing conditions, and the chemical engineer should not hesitate to use a safety
factor of zero if the situations warrant it.
196
5.4.3 CALCULATION OF CHEMICAL DESIGN OF DISTILLATION
COLUMN
a) Composition of Component Inlet and Outlet Streams
Component Flow rate (kmol/hr) Mole Fraction

Methanol 134.8616 0.5388
Methyl Acetate 1.10132 0.0044
Feed (S26) Butanol 32.8644 0.1313

Butyl Acetate 81.4727 0.3255
Total 250.3000 1.0000

Methanol 118.5200 0.8000
Methyl Acetate 0.1037 0.0007
Top (S17) Butanol 12.4298 0.0839

Total 148.1500 1.0000

Methanol - -
Methyl Acetate - -
Bottom (S18) Butanol 2.043 0.0200

Total 102.1500 1.0000
197
b) Calculation of Bubble and Dew Point
To estimate the stage, and the condenser and reboiler temperatures, procedures are required
for calculating dew and bubble points. By definition, a saturated liquid is at its bubble point
(any rise in temperature will cause a bubble of vapour to form), and a saturated vapour is at
its dew point (any drop in temperature will cause a drop of liquid to form). It can be
calculated in terms of equilibrium constant, K. Dew point and bubble point can be calculated
from knowledge of the vapor-liquid equilibrium for the system. In term of equilibrium
constants, the bubble point is defined by the equation.
Using Antoine equation to find vapor pressure (P o)

AnTB
ln P 0  AnTA 
(T  AnTC )
Where;
A, B and C = Antoine constant
Po = Vapor pressure at T (mmHg)
T = Operating Temperature (K)
P = Operating Presure (kPa)
Table 5.25: List of constants in the Antoine equation

Component AnT A AnT B AnT C
Methanol
16.1295 2601.92 -56.15
Methyl Acetate
18.5875 3626.55 -34.29
Butanol
17.216 3137.02 -94.43
Butyl Acetate
16.1836 3151.09 -69.15
P0
Ki 
P
198
c) Calculation of Dew Temperature
x  y
i i / k i  1.0
Temperature = 395 K Operating Pressure, P =304 kPa
Table 5.26: Calculation of composition, xi to determine dew temperature

Component yi = xi Pi* Pi* (kPa) Ki(Pio/P) yi/Ki
(mmHg)
Methyl Acetate
0.0007 4678.918 623.7933186 2.051952 0.000341
Methanol
0.8 5082.602 677.6124669 2.228988 0.358907
Butanol
0.0839 879.2742 117.224835 0.385608 0.217578
Butyl Acetate
0.1258 674.0001 89.85768782 0.295584 0.425597
Total
1.002424
So, dew temperature is 395 K.
d) Calculation of Bubble Temperature
 y  k x
i i i  1.0
Temperature = 460.13 K Operating Pressure, P =456 kPa
199
Table 5.27: Calculation of composition, yi to determine bubble temperature
Component yi = xi Pi* Pi*(kPa) Ki(Pi*/P) xiKi
(mmHg)
Methyl Acetate
0 16135.63 2151.202114 4.717548 0
Methanol
0 23653.66 3153.506296 6.915584 0
Butanol
0.02 5641.334 752.1026588 1.649348 0.032987
Butyl Acetate
0.98 3374.944 449.9475485 0.986727 0.966993
Total
0.999979
So, bubble temperature is 457 K.
e) Calculation of Bubble Point of the Feed
 y  k x
i i i  1.0
Temperature = 402 K Operating Pressure, P =506.6 kPa
Table 5.28: Calculation of composition, yi to determine bubble temperature

Component yi = xi Pi* Pi*(kPa) Ki(Pi*/P) xiKi
(mmHg)
Methyl Acetate
0.0044 5465.651 728.6806 1.438375 0.006329
Methanol
0.5388 6154.707 820.5456 1.619711 0.8727
Butanol
0.1313 1115.023 148.6549 0.293437 0.038528
Butyl Acetate
0.3255 826.0067 110.1232 0.217377 0.070756
Total
0.988314
The k xi i value is close to 1.0, therefore this temperature is accepted.
So, bubble temperature is at 402 K.
200
5.4.4 Relative Volatility
Before a binary distillation column can be designed, a decision must be made as to the two
key components between which it is desired to make the separation. The light key
component is the one to be kept out of the bottom stream according to some specification.
The heavy key component is the one to be kept out of the top stream according to some
specification. In general form, the greater relative volatilities is the easier way for separation
to take place. The relative volatility of two components can be expressed as the ratio of their
K value. The determination of relative volatility, α of the components can be determined as
the ratio between K values of light key component to heavy key component.
The relative volatility of two components can be expressed as the ratio of their K
value:
Ki
i j 
Kj

αmethanol = 2.2290/ 0.2956 = 7.5410
Table 5.29: Value of relative volatility at the top and bottom column
Component αBottom αTop αAverage
Methyl Acetate
4.7810 6.9420 5.8615
Methanol
7.0086 7.5410 7.2748
Butanol
1.6715 1.3046 1.4880
Butyl Acetate
1 1 1
201
5.4.5 Calculate the minimum reflux ratio (R m).
Using the Underwood (1948), equation 11.60 (Coulson & Richardson’s), vol.6 page
525.
 x i ,d
  ii   = Rm + 1
 = the relative volatility of component with respect to reference

component, usually the heavy component.
Rm = minimum reflux ratio
X,d = concentration of component in the tops at minimum reflux.
And  is the root of the equation:

x,
 ii i f = 1 – q
xi,f = the concentration of component I in the feed, and q depends on

the condition of the feed
x,
 ii i f = 1 – q
where q = 1.0 , it assume that the process at feed stream is liquid

state
1-q=1-1
=0
202
Table 5.30: Calculation value of θ
Component Bottom Top Average x,f α xf (θ = 2.8)
α α α  i xi , d

i 
Methyl Acetate
4.7810 6.9420 5.8615 0.0044 0.02579 0.008424
Methanol
7.0086 7.5410 7.2748 0.5388 3.9197 0.8759
Butanol
1.6715 1.3046 1.4880 0.1313 0.1954 -0.1489
Butyl Acetate
1 1 1 0.3255 0.3255 -0.1808
Total 1.000
0.5546
 x i ,d
θ = 2.5 acceptable because this value will approximately   ii   = 0.
Table 5.31: Calculation value of R m

 i x i ,d
Component xd α xd α
 i  
Methyl Acetate
0.0007 5.8615 0.004103 0.001340
Methanol
0.8 7.2748 5.8198 1.3006
Butanol
0.0839 1.4880 0.1248 -0.09516
Butyl Acetate
0.1258 1 0.1258 -0.06989
Total 1.0000
1.1369
Hence,
The minimum reflux ratio
Rm + 1 = 1.1369
Rm = 0.1369
Rm 0.1369
= = 0.12039
R m  1 1  0.1369
Specimen calculation, for R= 2.0

R 2
= = 0.66667
(R  1) 3
203
From Erbar – Maddox correlation, Figure 11.11 from Coulson & Richardson’s, vol.6
page 524 :
Nm
= 0.85
N
By taking value of R varies from 2 until 5, here the table that shows relation between
R and N. When R increase, the value of N also increase.
Table 5.32: Relation R and N

R 1 2 3 4 5
R/(R+1) 0.5 0.666667 0.75 0.8 0.833333
Nm / N 0.75 0.85 0.91 0.94 0.95
N 13.92 12.28 11.47 11.11 10.99
But the number of stages can be calculated by using equation Fenske Equation.
Minimum number of stages can be calculated using Fenske Equation:

x  x 
log LK d  HK b
Nm   x HK   x LK 
log  LK
0.0839 0.98
𝐿𝑜𝑔 ( )( )
𝑁𝑚 = 0.1258 0.02
log 1.3963
Nm = 10.44 stages
Therefore, N = N m (0.83)
N = 10.44 (0.85)
N = 12.28
From Table 5.32, there are slightly different in N when the value of R increases. By
taking the value of R=2, the value of N is 12.28 rounding off 11.47 to 12.28, and
finally the number of stages excluding boiler is 12. With value of R=2, the number of
stages is fit with value of N by using Fenske Equation.
204
Calculation of stages also can be determined by using method trial and error nature
of stage by stages calculation states at Appendix. The total top and bottom
calculation stage is 12.
5.4.6 Overall Column Efficiency
given by O’Connell (1946);
E0  51  32.5 log(  a  a )
Where, a = average relative volatility of the light key

a = the molar average liquid viscosity, mNs/m 2
Temperature = 395 K (top column)

= 460.13 K (bottom column)
Average temperature = (395+ 460.13) K = 427.57 K

Viscosity of components at average temperature, 427.57 K:
Log ( a ) = [VISA] * [(1 / T) – (1/VISB)]
Table 5.33: List of constant in the liquid viscosity equation and value of viscosity
Component VISA VISB μ
Methyl Acetate 408.62 224.03 0.1354
Methanol 555.3 260.64 0.1473
Butanol 984.54 341.12 0.2609
Butyl Acetate 537.58 272.30 0.1919
Log (µ) = (408.62) x[ (1/427.57)-(1/224.03)]

Log (µ) = -0.8683
µ = 0.1354
For feed composition, molar average viscosity ,
205
Table 5.34: Summary calculation of viscosity and composition
Component xi µi xi*µi
Methyl Acetate 0.1354 5.9576 x 10-4
0.0044
Methanol 0.1473 0.07937
0.5388
Butanol 0.2609 0.03426
0.1313
0.3255
Total 0.1767mNs/m2
αF x µT = 1.3963 x 0.1767
= 0.2467
From Figure 2.4.12 from Appendix

Eo = 63%
By taking safety margin 1.5, the new E0 is

Eo = 0.63/1.5 x 100% = 42%
The number of ideal stages is 12, so the number of real stages is

12
=
0.42
= 28.5714
= 29 stages
5.4.7 Calculation to Determine Feed Point
An estimate can be made by using the Fenske equation to calculate the number of
stages in the rectifying and stripping section separately, but this requires an estimate
of the feed-point temperature. An alternative approach is to use the empirical
equation given by Kirkbride (1944):
 Nr   x  x b,LK 
2
Log   = 0.206 log  B  f ,HK   
 Ns   D  x f ,LK  x
 d,HK

 
 
206
Where, Nr = number of stages above the feed, including any
partial condenser
Ns = number of stages below the feed, including the
reboiler
product
x b,LK = concentration of the light key if in the bottom
product
N   102.15 0.5388  0.02 

2

Log  r  = 0.206 log  


   =0.6776
 Ns   148.15  0.0044  0.98 
 
 
 Nr 
  = 2.7518
 Ns 
Nr  Ns = 29
2.7518Ns + Ns = 29
Nr = 21.2704
Ns =7.7296
Therefore, the feed is at stages 8 from the bottom column.
207
5.4.8 Calculation to Design the Plate
Maximum feed rate = 1.6294 x 10 4 kg/hr

By taking 70% of the maximum flow rate at feed,
Minimum Feed rate = 0.7 x 1.6294 x 10 4
= 11711 kg/hr
Number of ideal stages = 12

Reflux ratio = 2
MW feed = 65.1
Feed, kmol/h = 250.3 kmol/h
A mass balance on F gives:

Top product, D(kmol/h) = 148.15 kmol/h
Vapour rate, V (kmol/h) = 444.45 kmol/h
An overall mass balance gives:
Bottom product, B(kmol/h) = 102.15 kmol/h
Slope of the bottom operating line, Lm'/Vm' = 1.23
and Vm' = Lm' - B, from which:
Vapour flow below feed, Vm' (kmol/h) = 444.45 kmol/h

Liquid flow below feed, Lm'(kmol/h) = 546.6 kmol/h
208
5.4.9 Pressure Drop
Pt = (ρl) x g x ht x number of real stages (N)

Assume pressure drop 200 mm liquid per plate
( ρl ) at bottom column =0.98 (898) + 0.02(810)
= 896.24 kg/m3
g = 9.81m2/s
ht = 200 x 10-3 m
N = 29
Hence, pt = 896.24 x 9.81 x 200 x 10 -3 x 29
= 50994.26 N/m2 or Pa
Top pressure 3 bar = 300 x 10 3 pa
Estimated bottom pressure = 300 x 10 3 + 50994.26
= 350994.26 Pa
= 3.51 bar
5.4.10 Calculation For Density And Relative Molar Mass
Table 5.35: Properties of Methyl Acetate, Methanol, Butanol and Butyl Acetate
Component Molecular Feed Top product Bot. product Liquid

weight Mol fraction Mol fraction Mol fraction density
(kg/m3)
Methyl 74.08 0.0044 0.0007 - 934.0

Acetate
Methanol 32.04 0.5388 - 791.0

0.8
Butanol 74.12 0.1313 0.02 810.0

0.0839
Butyl Acetate 116.16 0.3255 0.98 898.0

0.1258
209
a) Calculation for relative molar mass
Feed = 0.0044 (74.08) + 0.5388 (32.04) + 0.1313 (74.12) +

0.3255(116.16)
= 65.1311 kg/kmol
Top product = 0.0007 (74.08) + 0.8 (32.04)+ 0.0839(74.12)+
0.1258(116.16)
= 46.5155 kg/kmol
Bottom product = 0.98 (116.16) + 0.02(74.12)
= 115.3192 kg/kmol
b) Calculation for density ( ρ)
Bottom product:
Liquid density (ρL) = 0.98 (898) + 0.02(810)
= 896.24 kg/m3
Vapour density (ρv) = (116.16 / 22.4) (273 / 460.13) (1.51 / 1.00)
= 4.646 kg/m3
Top product:
Liquid density (ρL) = 0.0007 (934) + 0.8(791) + 0.0839(810) + 0.1258(898)
= 814.3812 kg/m3
Vapour density (ρv) = (74.12 / 22.4) (273 / 395) (1.0 / 1.0)
= 2.2869 kg/m3
5.4.11 Calculation Surface Tension (Σ)
Using Sugden (1924), equation 8.23 (Coulson & Richardson’s) vol.6 page 334
σ = [ {Pch (ρL – ρv)} / M ]4 x 10-12
Where,
σ = surface tension, MJ/ m2
Pch = Sugden’s parachor
ρL = liquid density
ρv = Vapour density
210
For mixture
σm = σ1 x1 + σ2 x2
Table 5.36: The Sudgen’s Parachor

Component Formula Pch Top product Bot. product
contribution Mol fraction Mol fraction
C3H6O2 197 -
Methyl Acetate
0.0007
CH3OH 87.4 -
Methanol
0.8
C4H10O 204.4 0.02
Butanol
0.0839
C6H12O2 314 0.98
Butyl Acetate
0.1258
Pch at top = 0.0007 (197) + 0.8(87.4) + 0.0839(204.4) + 0.1258(314)

= 126.7083
Pch at bottom = 0.98 (314) + 0.02 (204.4)
= 311.8080
Hence,
Surface tension at top Column,
σm = {[126.7083 (814.3812 - 2.2869)] / 46.5155} 4 x 10-12
= 23.95 dyne /cm or 23.95 x 10 -3 N/m
Surface tension at bottom column,

σm = {[311.8080 (896.24 -4.646)] / 115.3192} 4 x 10-12
= 33.78 dyne / cm or 33.78 x 10 -3 N/m
5.4.12 Column Diameter
𝐿𝑚 ,𝑛 ρ𝑙 0.5
F LV =
𝑉𝑚 ,𝑛 ρ𝑣
Where, FLV is a liquid flow factor.

546 ,6 2.2869 0.5
FLV (Top) =
444 .45 814 .3812
211
= 0.065
Where, 0.065 is the distillate operating line.
296.3 4.646 0.5
FLV (Bottom) =
444 .45 896.24
= 0.048
Where, 0.048 is the bottom operating line.
Assume initially 0.5m of tray spacing, to know that flooding occurred or not.
From figure 11.27 (Coulson & Richardson’s, Vol. 6 page 567) we get the value of K i.
(Please refer APPENDIX A-1)
Hence,
Bottom Ki = 0.094 x 10-1
Top Ki = 0.088 x 10-1
Take hole active area 10 %,

Bottom Ki = 0.094 x 10-1 x 1.0 = 0.094
Top Ki = 0.088 x 10-1 x 1.0 = 0.088
Correction for surface tension,
σ 0.2
= 𝐾𝑖
0.02
Which, liquid surface tension is 0.02 N/m

33.78 x 10−3 0.2
Bottom Ki = x 0.094= 0.1044
0.02
23.95 x 10−3 0.2

Top Ki = x 0.088= 0.09123
0.02
Flooding velocity,
ρ𝑙 −ρ𝑣
𝑈𝑓 = 𝐾𝑖
ρ𝑣
896.24 − 4.646
𝐵𝑜𝑡𝑡𝑜𝑚 𝑈𝑓 = 0.1044 = 1.4463 𝑚 𝑠
4.646
814.3812 − 2.2869
𝑇𝑜𝑝 𝑈𝑓 = 0.09123 = 1.7192 𝑚 𝑠
2.2869
212
The flooding percentage was assumed to be 80%, this is based on flooding velocity
for design, a value of 70 % to 90 %.
Bottom Uf = 1.4463 m/s x 0.8 = 1.1570 m/s
Top Uf = 1.7192 m/s x 0.8 = 1.3754 m/s
Maximum volumetric flow rate,
𝑉𝑚 × 𝑅𝑀𝑀
Bottom =
ρv
RMM = Relative molecular mass

444 .45× 115.3192
Bottom = = 3.0644 m3/s
4.646×3600
𝑉𝑛 × 𝑅𝑀𝑀
Top =
ρv
444 .45× 46.5155

= = 2.5111 m3/s
2.2869×3600
Net area required = Volumetric flow rate / flooding velocity

Bottom = 3.0644 / 1.1570 = 2.6486 m2
Top = 2.5111 / 1.3754 = 1.8257 m2
As first trial, take downcomer area as 10% of total column cross sectional area
Bottom = 2.6486 / 0.90 = 2.3837 m2
Top = 1.8257 / 0.90 = 1.6432 m2
Column Diameter
𝜋𝐷 2
Hence, Column cross sectional area, A =
4
2.3837 ×4 0.5
Bottom = = 1.74 m
𝜋
1.6432 ×4 0.5
Top = = 1.45m
𝜋
For the design take the whole diameter as 1.5 m.
5.4.13 Provisional Plate Design
Column diameter Dc = 1.5 m

Column area Ac = 1.7671 m2
Downcomer area Ad = 0.12 x 1.7671 (at 12%) = 0.21205 m2
213
Net area An = Ac – Ad = 1.7671 – 0.21205 = 1.5550 m2
Active area Aa = Ac – 2Ad
= 1.7671 – 2(0.21205) = 1.343 m2
Hole area Ah = 0.1343 m2 (take 10% of Aa as first trial)
Weir length
(Ad / Ac) x 100% = 0.21205 / 1.7671 x 100% = 12%
(From figure 11.31, Coulson & Richardson’s, vol. 6 page 572),
Iw = 0.76 x Dc
= 0.76 x 1.5
= 1.14m
Take weir height, hw = 50mm
Hole diameter, dh = 5mm
5.4.14 Evaluation Design
a) Check weeping (enough vapour to prevent liquid flow through hole).

546.6 × 46.5155
𝑀𝑎𝑥 𝑙𝑖𝑞𝑢𝑖𝑑 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 , 𝐿𝑤 =
3600
= 7.0626 kg/s
Minimum Liquid rate = 0.7 x 7.0626 kg/s (70% turn down ratio)
= 4.9438 kg/s.
b) Weir Liquid crest
how = 750 (Lw / (ρL x I w) 2/3

Where, Iw = weir length
ρL = Liquid density
Maximum, how = 750 {7.0626/ (814.3812 x 1.14)} 2/3

= 29.01 mm liquid
Minimum, how = 750 {4.9438 / (814.3812 x 1.14)} 2/3
214
= 22.87 mm liquid
how + hw = 22.87 + 50 = 72.87 mm liquid.
From figure 11.30, Coulson & Richardson’s, vol. 6, page 571)

When, how + hw = 72.87 mm liquid

k2 = 30.5
c) Weep point
The purpose to calculate this weep point is to know the lower limit of the operating
range occurs when liquid leakage through the plate holes becomes excessive.
Minimum vapour velocity through the holes based on the holes area.
𝐾2 − 0.9(25.4 − 𝑑𝑕 )
𝑈𝑕 min =
𝜌𝑣 0.5
30.5 − 0.9(25.4 − 5)
𝑈𝑕 min =
2.2869 0.5
= 5.3085 m/s
Actual minimum Vapour velocity,

= minimum vapour rate / Ah
= (0.7 x 2.5111) / 0.1343
= 13.09 m/s
So, minimum operating rate will above weep point.
d) Plate pressure drop

Dry plate drop ( hd)
Maximum vapour velocity through holes
Uh (Max.) = volumetric flow rate / hole area (Ah)
= 2.5111 / 0.1343
= 18.70 m/s
215
From figure 11.34, (Coulson & Richardson’s), Vol 6 page 576.
For the thickness / hole diameter =1
Ah / Ap = Ah / Aa = 0.1343/ 1.1343
= 0.1
So, (Orifice coefficient) Co = 0.84
𝑈𝑕 2 𝜌𝑣
hd =51
𝐶𝑂 𝜌𝑙
18.7 2 2.2869
= 51
0.84 815 .3812
= 70.98 mm liquid
12.5×103
Residual head ( hr) =
𝜌𝐿
12.5×103
=
814 .3812
= 15.35 mm liquid
Pressure drop per plate ( ht) = hd + (hw+how) + hr
= 70.98 + (50+22.87) + 15.35
= 159.2 mm liquid
Note: 200 mm liquid was assumed to calculate the bottom pressure. The calculation
could be repeated but the small change in physical properties will have effect on the
plate design. Hence, 159.2 mm liquid per plate is considered acceptable.
e) Down comer liquid back–up

Downcomer pressure loss.
Take hap = hw - 10mm
= 50 - 100 = 40 mm
Area under apron, Aap = hap x I w

= 40 x 10-3 x 1.14 m2
= 0.0456 m2
Where, Aap is the clearance area under downcomer.
216
As this less than Ad = 0.21206 m2
𝐿𝑊 2
hdc = 166
𝜌 𝐿 𝐴𝑚
Where, hdc = head loss in downcomer, mm

Lwd = liquid flow-rate in downcomer, kg/s
Am = either the downcomer area Ad / the clearance area
under the downcomer
Aap, whichever is the smaller.

7.0626 2
Hdc = 166
814 .3812 ×0.0456
= 6.0042 mm.
Back up in the downcomer, (hb),
Hbc = hw + how + hf + hdc
= 50 + 22.87+ 159.2 + 6.0042
=238.0742 mm liquid @ 0.238 m.
Check,
0.238 ‹ 1/2 (plate spacing + weir height)
‹ 1/2 (0.5 + 0.05) m
‹ 0.275 m
So, tray spacing is acceptable, (to avoid flooding).
f) Residence time, t
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 at least 3 seconds is recommended.
Check residence time:
A d ×h bc ×ρl
tr =
L wd
0.21206 ×0.238×814.3812
=
7.0626
= 5.82 s.
tr is greater than 3.0s which recommended so t r here is satisfactory.
217
g) Check Entrainment.
𝑈𝑓 (max )
Actual velocity, Uv =
𝐴 𝑛 (𝑛𝑒𝑡 𝑎𝑟𝑒𝑎 )
2.5111
=
1.5550
= 1.61 m/s
𝑈𝑛 𝑎𝑐𝑡𝑢𝑎𝑙 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦 (based on area )

% Flooding, =
𝑈𝑓
1.61
=
2.041
= 79%
Flv (bottom) = 0.048
From figure 11.29 (Coulson & Richardson’s), Vol.6 page 570
Ψ value = 0.054
Ψ value is below 0.1, so the column diameter, which is proposed earlier, is
acceptable.
5.4.15 Trial Layout

Use cartridge type construction.
Allow 50 mm unperforated
50 mm wide calming zone.
50 mm
Iw=1.14
θ
Dc
= 1.5m
50 mm
Figure 1.3: Trial layout of plate
218
a) Perforated area:
From figure 11.32 (Coulson & Richardson’s), Vol.6 page 573.

At Iw / D c = 1.14 / 1.5
= 0.76
θc = 980
Angle subtended at plate edge by unperforated strips

= 180 – 98
= 820
b) Mean length, unperforated edge strips
82
= (1.5 – 50 × 10−3 ) × 𝜋 ×
180
= 2.075 m
c) Area of unperforated edge strips,
= 50 x 10-3 x 2.075 m
= 0.1038 m2
d) Area of Claming zone,
= 2 x 50 x 10-3 (1.5 - 50 x 10-3) sin (98/2)

= 0.1094 m2
e) Total area available for perforation, Ap:
Ap = Active area - (area of unperforated edge + area of calming)

= 1.343 - (0.1038 + 0.1094)
= 1.1298 m2
Ah / Ap , = 0.1343 / 1.1298
= 0.119
From figure 11.33, (Coulson & Richardson’s) vol.6 page 574.
219
Ip / dh, = 2.73
Satisfactory, range normally within 2.5 – 4.0
f) Number of holes:
Area of one hole = 1.964 x 10-5 (with diameter 5mm)
Number of holes = 0.1343 / 1.964 x 10 -5
= 6838 holes
5.4.16 Plate Specification
50 mm
Iw=1.14m Dc =1.5m
50 mm
Figure 1.4: Plate specification
Plate no. = 1 (from bottom column)
Plate ID = 1.5
Hole size diameter = 5 mm
Hole pitch = 12.5 x10-3
Active holes = 6838
Turn down ratio = 70% at max.Liquid
Plate Material = stainless
Downcomer material = stainless
Plate spacing = 0.5 m
Plate thickness = 5 mm
Plate pressure drop = 159.2 mm liquid.
220
SECTION 5: DESIGN FOR HEAT EXCHANGER
5.5 INTRODUCTION
In petrochemical industries, many streams in the plant may need to be
heated or cooled to the target temperature as it is desired to preheat the
feedstock, meet the operating temperature in the reactor which is of the
essence to drives the reaction to produce product, cool down the stream’s
temperature to ambient temperature for storage purpose and heating duty in
the reboiler for continuous operation in the distillation column. Of all these
purpose, there is one industrial equipment which can accomplish that duty;
heat exchanger.
The principal of heat exchanger is basically transferring or ‘exchanging’
heat between hot and cold fluids involved where the desired outlet
temperature can be achieved. In fact, heat exchanger duty is consistent with
the second law of thermodynamic which clearly states that heat can only be
transferred from hot to cold medium. In another word, heat exchanger is a
heat-transfer devise used for transfer of internal thermal energy between two
of more fluids available at different temperatures (Kuppan, 2000).
There are several types of heat exchanger being used commercially
according to the nature of the process. General types of heat exchanger that
are in interest of the designer are:
1. Shell and Tube exchanger
2. Plate Heat Exchanger
3. Air-Cooled Heat Exchanger
4. Teflon Heat Exchanger
Arguably, the most selected type of heat exchanger being utilised in the
industry is shell and tube heat exchanger. Its long and satisfied service
period, suitability to operate in any operating temperature and pressure, can
be engineered in a wide range of materials and reliable plus its abundance
standards and specifications and mechanically uncomplicated makes it
attractive to be used (Rose, 2009 & Sinnott, 2005).
221
i. Process Description
It is desired to preheat the stream into the first reactor with heater or heat
exchanger in order to initiate the transesterification reaction between methyl
acetate and butanol in Continuous Stirred Tank Reactor (CSTR) which
produce butyl acetate and methanol. The cool stream entering the heater is
consists of mixture of n-butanol, methyl acetate and methanol and the
heating medium is saturated steam, which ranged from 180 oC to 217oC
(Optimal Chemical Malaysia). In a counter-current flow, temperature cross
can be avoided when the cool stream temperature outlet is higher than the
hot stream outlet stream (Ludwig, 2000). The cold stream need to be heated
from 26.61oC to 110oC at 6.3 atm while saturated steam entering the
exchanger at 180oC at 10 atm and leaving at 55oC .
55oC
26.61oC 110oC
E-100
180oC CSTR- CSTR-

100 101
Figure 5.5 : Selected process stream
222
5.5.1 Comparison and Selection of Heat Exchanger
Below are the comparison between heat exchanger types and its advantages
and disadvantages.
Table 5.37 Comparison of types of heat exchanger
Type Advantages Disadvantages
a) Shell and Tube Heat i) Mechanically i) Design is fixed and
uncomplicated, easy to cannot be altered if
Exchanger
design changes in process is
ii) Satisfying service required
period and can be ii) Low heat transfer
constructed from wide coefficient
range of materials iii) Occupying large area
iii) Suitable for any in the shell diameter sense
operating temperature and iv) Tube and shell-side
pressure process velocity is limited to certain
iv) Abundance in standard value to avoid flow-
and specifications induced vibration and
v) Cleaning of fouled fluid corrosion
by mechanical and
chemical process
b) Plate Heat Exchanger i) High heat transfer i) Not suitable for pressure
coefficient more than 30 bar.
ii) Operate in true counter- ii) Selection of suitable
current flow gasket is critical.
iii) Ability to work in a iii) The maximum
minimum temperature operating temperature is
difference limited to 250oC due to the
iv) Corrugated surface performance of the
inside helps to create a available gasket materials.
turbulent, thus increase
heat transfer coefficient
v) Easier to maintain,
attractive when the
material cost is high
vi) Fouling tends to be
significantly less, flexible
and suitable for highly
viscous materials
c) Air-cooled Heat i) Suitable when the i) Produce environmental
cooling water is insufficient noise from the fan used
Exchanger
or expensive ii) Problems in air flow
ii) Use for cooling and control
condensing.
iii) Environmental-friendly
and without great ongoing
cost.
e) Teflon Heat Exchanger i) Operate at higher pressure
drop
ii) Suited for relatively clean
fluids.
iii) Removable tube bundles
223
So, based on the above comparison, it is obvious that shell and tube
heat exchanger has the upper hand than other types of heat exchanger and
is attractive to be used to preheat the stream’s temperature into the reactor in
the selected transesterification process of methyl acetate to produce butyl
acetate. It has a relatively long and satisfied service period and reliable,
mechanically simple, flexible in any temperature and pressure and material in
construction and intuitively suitable for the required duty to be performed.
Here, a few types of shell and tube heat exchangers being discussed
and comparison is made between those types of shell and tube shell
exchangers in order to select the best types of shell and tube exchanger.
Types of Shell and Tube Heat Exchanger and its Advantages and
Disadvantages
Table 5.38 : Comparison of shell and tube heat exchanger
Type Advantages Disadvantages

1) Fixed Tube Sheet ● Best used for condenser ● Temperature difference
● Both tubesheet fixed to at extreme of about 200oF
shell due to thermal expansion
2) Floating Head ● Suit for high ● Internal gaskets offer
temperature differential danger of leaking.
about 200oF extremes ● Corrosiveness of fluids
● Suitable for dirty fluids on shell-side floating parts.
requiring cleaning of ● Usually confined to
inside as well as outside horizontal units.
of shell.
● Tube bundle is
removable as well as back
cover for maintenance.
3) U-Tube ● Bundle is removable ● Bend must be carefully
● Allow high temperature made; otherwise it may
differentials, which might cause mechanical damage
require provision for or danger of rupture.
expansion in fixed tube ● Tube side velocities can
units. cause erosion of inside of
● Easily cleaned on both bends.
tube side and shell side. ● Fluid must be clean; free
of suspended particles.
4) Kettle ● Tube bundle is ● For horizontal
removable. installation.
● Suitable for boiling fluid ● Physically large for other
on shell side as refrigerant application.
or process fluid being
vaporized, and also
chilling or cooling of tube-
side fluid in refrigerant
224
evaporation on shell-side.
5) Double Pipe ● Relatively small transfer ● Services suitable for
area service, or in banks finned tube only.
for larger applications. ● Piping-up a large
● Suited for high pressure number often requires cost
in tube > 400 psig. and space.
● Each tube has its own
shell forming annular
space for shell-side fluid.
6) Pipe Coil ● Suitable for condensing, ● Transfer coefficient is
or relatively low heat loads low and requires relatively
on sensible transfer. large space if heat load is
high.
7) Open Tube Sections ● Tubes require no shell, ● Transfer coefficient is
(Water cooled) only end headers, usually low.
long, water sprays over ● Takes up less space
surface, sheds scales on than pipe coil.
outside tubes by
expansion and
contraction.
● Suitable for condensing,
or relatively low heat loads
on sensible transfer.
8) Open Tube Section (air ● No shell required, only ● Transfer coefficient is
cooled); Plain or Finned headers similar to water low, if natural convection
Tubes units circulation, but is improved
● Suitable for condensing, with forced air flow across
high-level heat transfer. tubes.
The selected type of shell and tube exchanger is internal floating head with
clamp ring shell and tube heat exchanger because it is easy to clean and
replace tubes if required, not limited to clean fluids as in U-tube type, and
reduce the need for clearance which is require to expand shell, thus large
shell diameter which is expensive.
225
Figure 5.6 : Floating-head shell and tube heat exchanger. Extracted from BS
3274 : 1960
5.5.2 CONSIDERATION IN DETERMINING THE LOCATION OF FLUIDS

R.K Sinnott (2005) stressed that it is imperative to select the right
location of the fluids, either in shell or tube. There are 6 factors that need to
apply in selecting the fluid in shell and tube:
1) Corrosion
The more corrosive component should be located to the tube-side as it will
reduce the cost of metal component.
2) Fouling
The fluid with greatest tendency to foul the heat transfer surfaces should be
located in the tube as it will give better control over design fluid velocity and
226
higher allowable velocity in the tubes will reduce fouling. In addition tube is
easy to clean.
3) Operating Pressure
Higher pressure stream should be located to the tube -side. High pressure
tube is relatively less expensive than higher pressure shell.
4) Pressure Drop
For the same pressure drop, higher heat transfer coefficient will be achieved
on the tube-side compare to the shell-side, and fluid with the lowest allowable
pressure drop should be allocated to the tube side.
5) Viscosity
A higher heat transfer coefficient will be obtained by allocating the more
viscous material to the shell-side, providing the flow is turbulent. If turbulent
flow cannot be achieved in the shell, it is better to place the fluid in the tube
as tube heat-transfer coefficient can be predicted with more certainty.
6) Stream Flowrate
Fluid with low flowrate is generally allocated to the shell-side which will give
the most economical design.
7) Temperature
Higher temperature fluid in the tubes will reduce the overall cost. At moderate
temperature, it is appropriate to locate the hotter fluid in the tubes which will
reduce shell surface temperature and hence the need for lagging to reduce
heat loss, or for safety reason.
Based on the above statements, a table which analyze the suitable fluid to be
located either in tube or shell side is constructed. Table 1.3 shows the
results:
227
Table 5.39 Comparison of suitability of streams at tube and shell side
Properties Stream Steam

a) Corrosion Corrosive due to the Saturated steam is being
presence of corrosive used, so it is corrosive.
substance, OH-.
b) Fouling Yes Yes
c) Operating Pressure High pressure (6.2 atm) Relatively low pressure
d) Pressure Drop 35 kN/m 2 35 kN/m 2
e) Viscosity More viscous Less viscous
f) Flowrate Higher (2.708 x 104 kg/hr) Lower (186.26 kg/hr)
g) Temperature Lower mean temperature Relatively higher caloric
(68.31oC) temperature
It is obvious that the stream, which consists of mixture of methyl acetate, 1-

butanol and methanol, should be located in the tube side. As it is more
fouling, locating the stream in the tube-side will give a better control over fluid
velocity where higher velocity will minimize fouling and also it is easy to
clean. Moreover, a higher pressure of stream means that it is suitable to be
located in the tube, thus reduce the cost of design and higher heat-transfer
coefficient is achieved in the tube-side which is enough for effective heat
transfer from hot fluid to the cool fluid.
5.5.3 CHEMICAL DESIGN

a) Determination of Outlet Hot Stream Temperature
Basically, the process stream inlet and outlet temperature and flowrate
(cold stream) consisting of mixture of n-butanol, methanol and methyl acetate
are already known, but the problem arise as the outlet temperature of hot
stream and its flowrate are unknown. The inlet steam temperature is at
180oC, 10 atm. To determine the unknown temperature and flowrate, Based
on After Murty method to determine outlet temperature of hot stream for 1-2
pass:
T1  t1
T2  T1   T1  t1 
  t 2  t1  
1   
  2  T  t   
  1 1 
where T 1 = hot stream inlet temperature

T2 = hot stream outlet temperature
t1 = cold stream inlet
228
 
 
 180  26.61 
 180  26.61  26.61
So, T2  
 110  26.61  
 1    
    
  2 180 26.61 
= 83.87oC
Based on the obtained temperature, the log mean temperature difference is

calculated by the previous equation.
LMTD =
180  110  83.87  26.61
 180  110 
ln  
 83.8.617  26 
= 63.41oC
and
180  83.87 110  26.61
R S
110  26.61 180  26.61
= 1.15 = 0.54
Apparently, the value of R and S are not suit to the 1-2 shell to tube pass
correction factor chart. So, the tube pass is changed to 4 tube pass. R.K
Sinnott explains that the economical heat exchanger should have the value
of Ft not less than 0.75, by taking this value and S value previously R value
can be determined. From Figure 12.20 (Sinnott, 2005), R value is 1.5. Then;
180  T2
R  1.5 
110  26.61
T2  54.9
≈ 55oC
At this temperature, steam will partially condense.
229
b) LOGARITHMATIC MEAN TEMPERATURE DIFFERENCE (LMTD)
Basically, the factor that drives heat transfer between streams of fluids is
the temperature difference. There must be a markedly temperature difference
between hot fluid and cold fluid. For over surface area, heat transfer duty can
be calculated by the equation:
Q  UATm
where Q = heat transferred per unit time
U = overall heat transfer coefficient, W/m2oC
A = heat transfer area, m 2
ΔTlm = mean temperature difference, oC
Mean temperature difference can be calculated from the difference in fluid

temperature at the inlet and outlet heat exchanger. Generally, the well-known
method called log mean temperature difference (LMTD) is applied to
calculate this mean temperature difference. Again, LMTD is the temperature
driving force that is significance in heat transfer over a surface area of the
tubes. It is applicable to sensible heat transfer in true counter-current and co-
current flow. For counter-current flow, LMTD is calculated by:
T1  t 2   T2  t1 
Tm 
T t 
ln  1 2 
 T2  t1 
where ΔTm = log mean temperature difference (LMTD)

T1 = hot fluid inlet temperature
T2 = hot fluid outlet temperature
t1 = cold fluid inlet temperature
t2 = cold fluid outlet temperature
In real situation, the fluid flow might not achieved true co-current or
counter-current flow. Several literature reported that a mixture of co-current,
counter-current and cross flow simultaneously occur in the heat exchanger
thus the correction factor must be applied to the LMTD calculation.
230
Correction factor (F) is being investigated by using correction chart based on
the shell-to-tube pass (R.K Sinnott, pg 657-658) with the following correlation
is calculated:
T1  T2  t  t 
R S 2 1
t 2  t1  T1  t1 
The assumptions being made when applying this correction factor (F t) are as
follow:
1. A constant heat transfer coefficient in each pass

2. Equal heat transfer area in each pass
3. No leakage occur between shell passes
The temperature of shell-side fluid in any pass is constant across any cross-
section It is observed that the temperature change of the hot stream (steam)
is quite large and condensed at fixed temperature at constant pressure.
Based on this characteristic, the log mean temperature difference (LMTD)
can be calculated by:
t 2  t1
Tm 
 T t 
ln  sat 1 
 Tsat  t 2 
where T sat = saturation temperature of the vapour, oC
t1 = inlet cold stream temperature, oC
t2 = outlet cold stream temperature, oC
110  26.61
Tm 
 180  26.61 
ln  
 180  110 
= 106.30 oC
Take the correction factor (Ft) = 0.75 as one side experience partial
condensation, then :
Tm  106.30oC x 0.75
231
= 79.73oC
Below are the thermophysical properties of each streams involved in the

system:
Table 5.40 : Thermophysical properties of streams
Properties Inlet Mean Outlet

1) Stream
Temperature (oC) 26.61 68.31 110
Cp (kJ/kmol. K) 116.8 132.99 149.18
Thermal 0.1678 0.1531 0.1343
conductivity
(W/m. K)
Density (kg/m 3) 831.88 819.16 806.43
Viscosity (Ns/m 2) 7.22 x 10-4 5.08 x 10-4 2.94 x 10-4
Pressure (kPa) 6.3 6.3 6.3
2) Steam
Temperature (oC) 180 61.22* 55
Cp (kJ/kmol. K) 46.008 42.53 40.27
Thermal 0.2953 0.6540 0.6482
conductivity (W/m.
K)
Density (kg/m 3) 5.154 982.53 985.65
Viscosity (Ns/m 2) 8.2398 x 10-5 4.71 x 10-4 5.13 x 10-4
Pressure (kPa) 10 0.2110 0.15752
For the steam stream, the average temperature is calculated by caloric

temperature because there is a significant difference between inlet and outlet
properties. At 55oC, steam is partially condensed and at this temperature, the
pressure of steam is 0.15752 kPa (NBS/NRC Steam Table). Heat required to
increase temperature of stream from 26.61oC to 110oC:
2.708 10 4 kg
= hr   2.5868 kJ 383  299.61
 kgK 
3600s 
= 1622.6430 kW
By taking the value for overall coefficient of steam and organic solvents
(Sinnott, 2005):
Uo, ass = 500 – 1000 W/m.oC.
For initial calculation, U = 500 W/m.oC is taken. Mass flowrate of the stream
entering the exchanger is 2.708 x 10 4 kg/hr.
232
5.4.4 Initial Calculation
i. Area Required
1622.6430  103W
Area required =
500 W 2  79.73K
m K
= 40.7034 m2
ii. Tube-Side Analysis

By using 19.05 mm outside diameter, 17.83 mm inside diameter, 5 m
long tubes on a square 23.81 mm pitch. By allowing for tube-sheet thickness,
length of tube will be reduced by 25 mm. (Sinnott, 2005). [Thickness of
stainless steel as stated in BS 3274 for 19.05 mm outside diameter is 1.2192
mm]
Do Di
L
Figure 5.7 : Tube dimensional
L = 5 m – 0.025 m
= 4.975 m
Area of one tube = πDoL

= π (19.05 x 10-3) (4.975)
= 0.2962
233
a) Number of Tubes
40.7034m 2
Number of tubes =
0.2962m 2
= 137.42
≈ 137
137
For 4 tube passes =
4
= 34.25 or 34 tubes/pass
π
Tube cross-sectional area = D2𝑖
4
π
= (17.83 ×10-3 )2
4
= 2.4969 x 10-4 m2
Area per pass = 34 x (2.4969 x 10-4)

= 8.4895 x 10-3 m2
b) Tube Side Velocity

   4 kg 
   2.708  10 
1
Volumetric flowrate =   hr 
 kg   3600s 
 819.33 3   
 m   
= 9.1809 x 10-3 m3/s
m3
9.1809  10 3
Tube side velocity = s
8.4895  10 3 m 2
= 1.0814 m/s
c) Shell Diameter
To find bundle diameter (assembly of tubes, baffles, tube sheets, spacers and
tie rods and longitudinal baffles):
234
1
Nt n1
Db = do
K1
where N t = number of tubes

D b = bundle diameter, mm
do = tube outside diameter, mm
From Table 12.4 (Sinnott, 2005), for square tube pattern and for 4 tube-side
pass:
Square pitch, pt = 1.25do
K1 = 0.158
n1 = 2.263
1
137 2.263
So, D b = 19.05
0.158
= 378.6166 mm or 0.3786 m
From Figure 12.10 (Sinnott, 2005), the shell-bundle clearance is 56 mm.

So, shell inside diameter, D s = 378.6166 mm + 56 mm
= 434.6166 mm
d) Tube-Side Heat Transfer Coefficient
Di
Reynolds Number =

=
819.161.08140.01783
5.08  10 4
= 31091.58
Cp
Prandtl Number, Pr =
kf
=
132.99 10 5.08 10 
3 4
0.1531
= 441.27
L
Ratio of length to diameter =
Do
235
4.975
=
0.01905
= 261.15
From Figure 12.23 (Sinnott, 2005), the heat transfer factor j h = 3.6 x 10-3
Heat transfer coefficient on tube-side can be determined by the equation below:
0.14
hi d i   
 j f Re Pr 0.33  
kf  w 
where μ = fluid viscosity at the bulk fluid temperature, Ns/m 2

μ w = fluid viscosity at the wall, Ns/m2
Re = Reynolds number
Pr = Prandtl number
di = tube internal diameter, m
kf = fluid thermal conductivity, W/moC
With no viscosity correction,

j f Re Pr 0.33 k f
hi =
di
=
3.6  10 31091.58441.27 0.1531
3 0.33
0.01783
= 7170.0402 W/m K
iii. Shell-Side Analysis

a) Area of Shell
E.E Ludwig suggests that for steam oil free that condensed, its film heat
transfer coefficient, (h s) is approximately 1500 Btu / ft oF or 8517 W/m K.
Assume no need for clearance. So, baffles spacing = shell internal diameter.
Area of shell, As =
 pt  d o Ds lb
pt
where pt = tube pitch
do = outside diameter of tube
Ds = diameter of shell
236
lb = baffle spacing
As =
23.81  19.05  434.6166  434.6166
23.81
= 37762.4512 mm2 or 0.03776 m2
b) Shell-Side Velocity
Ws
Shell side mass velocity, G s =
As
where W s = fluid flowrate on the shell-side, kg / s
As = area of shell, m2
 kg  1 
 2204.4960  
Gs = 
hr  3600s 
0.03776m 2
= 16.2172 kg / m2.s
Gs
Linear velocity, us =

16.2172
=
5.154
= 3.1465 m /s
For square pitch tube:
Shell equivalent diameter, d e =

1.27 2
do

pt  0.785d o2 
=
1.27
19.05
 
23.812  0.785 19.052 
= 18.8025 mm or 0.0188 m
Gs d e us de 
Reynolds number = =
 
237
=
16.21720.0188
8.24  10 5
= 3700.0408
c) Pressure Drop of Tube-Side
To find pressure drop at the tube side,
  L   
m
 u 2
Ps  N p 8 j f     2.5 t
  Di   w   2
Where N p = number of tubes passes

jf = friction factor
Ut = tube-side velocity, m/s
L = length of one tube, m
µ w = viscosity at tube wall, Ns/m 2
ρ = density of fluid, kg/m3
From Figure 12.24, jf = 3.8 x 10-3.Neglecting viscosity coefficient;

  819.161.0814
 
 4.975 
2
Ps  48 3.8 10 3    2.5
  0.01783   2
= 43.9293479.9735
= 21084.90 Pa or 21.0849 kPa
Pressure drop of the tube side is within the minimum pressure drop required,
which is 0.8 bar (Sinnott, 2005). So, the heat exchanger will perform
satisfactorily.
d) Pressure Drop of Shell-Side
238
For calculation of pressure drop at the shell side which experience total
condensing, R.K Sinnott suggest that the value is 50% of that pressure value
obtained from the single phase calculation based on inlet stream properties.
D  L   s2   0.14 
Ps  8 j f  s    
 w 
 de  lb  2  
where Ds = shell internal diameter, mm
D e = equivalent diameter, mm
lb = baffle spacing
vs = shell-side velocity, m/s
jf = friction factor
µ w = viscosity at wall, Ns/m 2
Take baffle cut of 30% for steam at shell side (J.E. Edwards, 1998). The shell-
side friction factor taken from Figure 12.30 (Sinnott, 2005) is 5.5 x 10 -2.
 434.6166  4.975  5.1543.1465 

 
2
Ps  8 5.5 10 2    
 18.8025  0.4346  2 
= 2970.4118 Pa or 2.9704 kPa
Pressure drop is within range and it is quite low. So, pressure drop at shell-side
can taken to be negligible.
e) Overall Heat Transfer Coefficient
The overall heat transfer coefficient is the calculation of reciprocal of total

thermal resistances that occur in heat transfer that is due to the fouling on the
surface, selected material resistance and modes of heat transfer such as
conduction or convection. It is given as:
d 
d o ln  o 
1 1
 
1
  di   do  1  do  1
U o ho hod 2k w d i hid d i hi
239
where Uo = overall heat transfer coefficient, W / m2oC
ho = outside fluid film coefficient, W/m2oC
hi = inside fluid film coefficient, W/m2oC
hod = outside dirt coefficient, W/m2oC
hid = inside dirt coefficient, W/m2oC
kw = thermal conductivity of tube wall material, W/moC
di = tube inside diameter, m
do = tube outside diameter, m
For this process, the outside dirt coefficient for steam condensate is taken by
4000 W/m2oC and for inside dirt coefficient with organic liquids it is about 5000
W/m2oC. The metal resistance for stainless steel Type 316 is 16.2 W/m K at
100oC (R.K Sinnott, 2005 and AK Steel, 2007).
Then, based on the previous calculation,
 0.01905 
0.01905 ln  
1

1

1
  0.01783  0.01905
 
1

0.01905

1
U o 8517 1500 2  16.2 0.01783 5000 0.01783 7170.04
= 1.1857 x 10-3
U o = 843.3837 W/m2oC
5.5.5 Calculation of Second Iteration
The overall heat transfer coefficient obtained is well above the estimated
one and within the range, so the heat exchanger design has adequate area to
perform the duty. Second iteration is made by taking the obtained overall heat
transfer coefficient (Uo) with tube specifications of 25.4 mm outside diameter,
23.37 mm inside diameter and 2.032 mm thickness (BS 3274) with 4 m long.
i. Area Required
1622.6430  103W
Area required =
843.3837 W 2  79.73K
m K
= 24.1310 m2
240
ii. Tube-Side Analysis

Net tube length = 4 m – 0.025 m
= 3.975 m
Area of one tube = πDoL
= π (25.4 x 10-3) (3.975)
= 0.3172 m2
24.1310m 2
Number of tubes =
0.3172m 2
= 76.08
≈ 76
76
For 4 tube passes =
4
= 19 tubes/pass
π
Tube cross-sectional area = D2𝑖
4
π
= (23.37×10-3 )2
4
= 4.2895 x 10-4 m2
Area per pass = 19 x (4.2895 x 10-4)

= 8.1501 x 10-3 m2
   4 kg 
   2.708  10 
1
Volumetric flowrate =   hr 
 kg   3600s 
 819.33 3   
 m   
= 9.1809 x 10-3 m3/s
m3
9.1809  10 3
So, tube side velocity = s
3
8.1501  10 m 2
= 1.1265 m/s
241
1
76 2.263
Bundle diameter, Db = 25.40
0.158
= 389.0947 mm or 0.3891 m
So, shell inside diameter, D s = 389.0947 mm + 56 mm

= 445.0947 mm
Di
Reynolds Number =

=
819.161.12650.02337
5.08 10 4
= 42451.69
Cp
Prandtl Number, Pr =
kf
=
132.99 10 5.08 10 
3 4
0.1531
= 441.27
L
Ratio of length to diameter =
Do
3.975
=
0.02540
= 156.50
From Figure 12.23 (Sinnott, 2005), the heat transfer factor j h = 3.4 x 10-3
With no viscosity correction,
j f Re Pr 0.33 k f
hi =
di
=
3.4  10 42451.69441.27 0.1531
3 0.33
0.02337
= 7054.1198 W/m K
iii. Shell-Side Analysis
242
Again the steam heat transfer coefficient is estimated at1500 Btu / ft oF or 8517
W/m K and assume for no clearance between baffles and shell.
As =
31.75  25.40  445.0947  445.0947
31.75
= 36502.0270 mm2 or 0.03650 m2
 kg  1 
 2204.4960  
Shell side mass velocity, Gs = 
hr  3600s 
0.03650m 2
= 16.7770 kg / m2.s
Gs
Linear velocity, us =

16.7770
=
5.154
= 3.2551 m /s
For square pitch tube:
Shell equivalent diameter, d e =

1.27 2
do

pt  0.785d o2 
=
1.27
25.40
 
31.752  0.785 25.40 2 
= 25.0806 mm or 0.02508 m
Gs d e us de 
Reynolds number = =
 
=
16.77700.02508
8.24  10 5
= 5106.40
243
iv. Pressure Drop for Tube-Side
From Figure 12.24 (Sinnott, 2005), heat transfer friction factor on tube side is
3.3x10-3:
  819.161.1265
  0.302337
.975 
2
Ps  48 3.3 10 3   2.5
    2
= 27.9615519.7579
= 14533.2105 Pa or 14.5332 kPa
Pressure drop of the tube side is within the minimum pressure drop required.
So, the heat exchanger will perform satisfactorily.
v. Pressure Drop For Shell-Side

Take the value of pressure drop as 50% of that pressure value obtained from
the single phase calculation based on inlet stream properties and baffle cut of
30%. The shell-side friction factor taken from Figure 12.30 (Sinnott, 2005) is 5 x
10-2.
 445.0947  3.975  5.1543.2551 

 
2
Ps  8 5 10 2
  
 25.0806  0.4451  2 

= 1731.0041 Pa or 1.7310 kPa
Pressure drop is within range and it is quite low. So, pressure drop at shell-side
is taken to be negligible.
vi. Overall Heat Transfer Coefficient
With the same value of resistances, the overall heat transfer coefficient (U o) is
calculated:
 0.02540 
0.02540 ln  
1

1

1
  0.02337  0.02540
 
1

0.02540

1
U o 8517 1500 2  16.2 0.02330 5000 0.02330 7054.1198
244
-3
= 1.2220 x 10
U o = 818.3306 W/m2 K
The obtained overall heat transfer coefficient (U o) shows that the value is
consistent and below that of the previous calculation. So, the design of heat
exchanger is satisfactory. Table 1.5 shows the final design specifications of
floating head shell and tube heat exchanger.
Table 5.41 : Final design specification
Specification Value
Overall heat Transfer Coefficient 818.3306 W/m2 oC
Heat transfer area available 24.1310 m2
Number of tubes 76
Tube-side velocity 1.1265 m/s
Shell-side velocity 3.2251 m/s
Pressure drop at tube-side 14.5332 kPa
Pressure drop at shell-side 1.7310 kPa
245

Chapter 5 - Chemical DSGN

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Chapter 5 - Chemical DSGN

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Production of 100,000 Tonnes Per Year of Butyl Acetate

SECTION 1 DESIGN OF CONTINUOUS STIRRED TANK REACTOR (CSTR-100)

a. The composition is constant. To maintain its composition of the products, the

c. To maintain high conversion. The amount of the product is quite huge

d) No temperature change in the reaction.

CHEMICAL ENGINEERING DESIGN

5.1.1 Determination of Reaction Rate

CH3COOCH3 (l) + CH3(CH2)3OH (l) ↔ CH3COO(CH2)3CH3 (l) + CH3OH (l)

kF= 1.246 × 105e-71960/RT

Component Volumetric Mole Flowrate Concentration

T=The reactor temperature is 383 K

5.1.2 Determination of The Reactor Volume

Hence the radius, ractual  V 6 

 1.25 m (round up to1.5)

Vdesign volume  3.142 * 1.5 * 9  63m 3

The calculation of reactor residence time, shown below [Levenspiel, 1999]:

Hence, the reactor residence time,   70 min

where v o is the inlet volumetric flow rate

5.1.4 Rate of Change

From the mass balance equation:

d(ρV)/dt = mass in – mass out (unit mass /time)

Rate change of component = input – output + generation – consumption (unit

V d(CA)/dt = F0 CA– Fi CA– Vr1 + Vr2

Since the volume is constant;

We used Euler Algorithm to solve the mathematical model ,

Table 5.2 The change of concentration profile of each components in reactor

Methyl Acetate Butanol Methanol Butyl Acetate

5.1.5 Determining the Weight of Catalyst

The bulk density,

The volume of catalyst,

The weight of the catalyst,

5.1.6 The Volume of Cooling Water

Based on the simulation result;

Where heat capacity of water Cp = 4.181 kJ/kg.K

The design of a distillation column can be divided in the following steps (

1. Specify the degree of separation required: set specification.

5.2.1 DESIGN OF SIEVE PLATE COLUMNS

a) Light Key (LK)

b) Heavy Key (HK)

Heavy key is the least volatile component whose concentration is to be controlled

c) Estimation of the number of stages

To estimate number of stages, condenser and reboiler temperature, and procedures

Bubble point:  yi   kixi  1.0

d) Overall column efficiency

Where,  a = average relative volatility of the light key

 a = the molar average liquid viscosity, mNs/m 2

e) Approximate column sizing

ii) Plate Contactors

In order to design distillation column, pressure drop should be determinedto ensure

CALCULATION OF CHEMICAL DESIGN OF DISTILLATION COLUMN

5.2.2 Composition of Component Inlet and Outlet Streams

Table 5.4 : Composition of Component Inlet and Outlet Streams

Using Antoine equation to find vapor pressure (P 0)

Table 5.5: Antoine coefficient’s for every component

5.2.4 Dew temperature (Top column)

Table 5.6 : Calculation to determine dew point

y i / k i value close to 1.0, therefore this temperature is accepted.

5.2.5 Bubble point (Bottom Column)

Table 5.7: Calculation to determine Bubble Point

k xi i value is close to 1.0, therefore this temperature is accepted.

So, bubble temperature is 392.54 K.

Sample calculation for butyl acetate component

5.2.7 Calculation to find q, the Thermal Condition at Feed

Hfs = 2.3151.8674 kg/kmol(349.6489 -273)

Hf = 2.3151.8674 kg/kmol(298.1 -273)