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Distillation Processes

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 95
DISTILLATION PROCESSES

Chapter Three

DISTILLATION PROCESSES

INTRODUCTION
One of the major operations in the process industries is the separation of liquid mixtures
into their various components. Distillation is the most widely used method of achieving
separation and this is the key operation in any crude oil process refinery. In an attempt to
achieve the demand for purer products, coupled with the need for greater efficiency,
refinery operators have promoted continued research into the techniques of distillation
Richardson et al. (2003). In this chapter the fundamental principles, relationships,
equations and methods of distillation and calculation of the number of stages required for
both binary and multi-component systems are presented. Basic problems of design
associated with physical, chemical properties and hydraulic phenomenon inside the unit
are considered; incorporating the column internal configurations. The composition of the
vapour in equilibrium with a liquid of given composition is determined experimentally
using an equilibrium still.

3.1 Equations for Simple Distillation

According to the phase rule, a two-phase, two-component system has two degrees of
freedom.
F =C–P+2 (3.1)
The equation of simple distillation is:

F xF dx
In  (3.2)
W xw y *  x

where F = Feed (the initial amount of the mixture being distilled).

W = Bottom product (the residue of the liquid in the still or column after
distillation)
96  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

y* and x = equilibrium concentrations of the low-boiling component (the low

boiler) in the vapour and in the liquid, respectively.
xF = content of the low boiler in the feed
xw = content of the low boiler in the bottom
The average composition of the distilled liquid (overhead product) is;
FXF  Wx w
xD  (3.3)
F W

When the relative volatility  is constant,

x
y  (3.4)
1    1x
Substituting Equation (3.4) into Eq. (3.2) we obtain:

 F 1  x 1 - x w   1 - x w  (3.5)
In    In    In  
W
    1 x
 w 1  x    1- x 

For binary system following Raoult’s law:

 y
 
(3.6)
  
x a Pa

 y Pb
 
 x b

where Pi = partial pressure of component i

When a liquid mixture is distilled with steam (or an inert gas), the consumption of the
steam is calculated by the equation:
M W Ptot  P  (3.7)
Gw  G
MP

where Gw = amount of the steam carried off with the vapour of the liquid being
distilled, kg
G = amount of the liquid being distilled, kg
Mw and M = molar masses of the water and the liquid being distilled,
respectively.
P = pressure of the saturated vapour of the liquid being distilled at the
temperature of distillation
 97
DISTILLATION PROCESSES

Ptot = total pressure of the mixture of vapour and steam

 = coefficient taking into account the incomplete saturation of the steam with
the vapour of the substance being distilled (in approximate calculations it
is assumed that  = 0.7 to 0.8)
3.2.1 Methods of Distillation – Two Component Mixtures
For a binary mixture with a normal y-x curve, the vapour is always richer in the
more volatile component than the liquid from which it is formed. The three main
methods used in distillation practice which depend on this basic factor are:
- Differential distillation
- Flash or equilibrium distillation
- Rectification.

Of these, rectification is the most important, and it differs from the other two
methods. This is because part of the vapour is condensed and returned as liquid to
the still, where as in the other methods, all the vapour is either removed or is
condensed as product.

3.2.2 Differential Distillation

The simplest example of batch distillation is a single stage, differential
distillation, starting with a still pot, initially full, heated at a constant rate. In this
process, the vapour formed on boiling the liquid is removed at once from the
system. Since this vapour is richer in the more volatile component than the liquid,
it follows that the liquid remaining becomes steadily weaker in this component,
with the result that the composition of the product progressively alters. Thus,
while the vapour formed over a short period is in equilibrium with the liquid, the
total vapour formed is not in equilibrium with the residual liquid. At the end of
the process the liquid which has not been vaporized is removed as the bottom
product. Rayleigh (1902) first proposed the analysis and other researchers have
since presented reliable and sustainable concepts.
Let us consider S as the number of moles of material in the still, x is the mole
fraction of component A and an amount dS, containing a mole fraction y of A, is
vaporized, then a material balance on component A gives:
ydS = d(Sx)
= Sdx + xdS
98  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

dS dx
 
S x

So S xo yx

S dx

x
In  (3.8)
So xo yx

The integral on the right-hand side of Equation (3.8) may be solved graphically if
the equilibrium relationship between y and x is available. Direct integration may
also be possible. Thus, if over the range considered, the equilibrium relationship
is a straight line of the form; y = mx + C, then:

S  1   m -1x  C  (3.9)
In   In  
So  m 1 m 1xo  C

or S   y  x 
 m 1

So  yo  xo 

m1
and  yx   S  (3.10)
    
 yo  xo   So 

This process consists of only a single stage, and so a complete separation becomes
impossible unless the relative volatility is infinite. Application is restricted to
conditions where a preliminary separation is to be followed by a more rigorous
distillation, where high purities of product are not required, or where the mixture
is easily separated.
3.2.3 Flash or Equilibrium Distillation
Flash or equilibrium distillation consists of vaporizing a definite fraction of the
liquid feed in such a way that the vapour evolved is in equilibrium with the
residual liquid. The feed is pumped through a fired heater and enters the still
through a valve where the pressure is controlled (usually reduced). The still is a
separator in which the liquid and vapour produced by the reduction in pressure
have sufficient time to reach equilibrium. The vapour is removed from the top of
the separator and is condensed, while the liquid leaves from the bottom.
In considering a pipe still where crude oil was pumped in at 167oC at about
900 kN/m2, pressure and would leave at 247 oC and 400 kN/m2, it was observed
that 15 % could vaporize in the process. The vapour and liquid streams may
contain many components in such an application.
 99
DISTILLATION PROCESSES

This process may be analysed simply for a binary mixture of components A and B
as follows:
If F = moles per unit time of feed of mole fraction, x of A
V = moles per unit time of vapour formed with y, the mole fraction of A
S = moles per unit of liquid with x the mole fraction of A

Then an overall mass balance gives;

F = V+S (3.11)
and for the more volatile component:
Fxy = Vy + Sx (3.12)

V  xf  x 
  
F  y  x 

or y = F F 
x f  x  1 (3.13)
V V 

This Equation (3.13) represents a straight line of slope:

F V S
  
V V

Passing through the point (xf, y)

In practice, the quantity vaporized is not fixed directly, but it depends upon the
enthalpy of the incoming feed and the enthalpies of the vapour and liquid leaving
the separator (Coulson and Richardson, 2002). F or a given feed condition, the
fraction vaporized may be increased by lowering the pressure in the separator.
3.2.4 Rectification
The essential merit of rectification is that it enables a vapour to be obtained that is
substantially richer in the more volatile component than is the liquid left in the
still. This is achieved by an arrangement known as a fractionating column which
enables successive vaporization and condensation to be accomplished in one unit.
100  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

Gv = GR + GD

Water

y GF, xF GD, xD

Steam

Condensate

Gw , Xw

Figure 3.1: Diagram of Rectification Column

The material balance equations of a continuous rectification column

(Figure 3.1) are:

GF  GD  GW (3.14)
 101
DISTILLATION PROCESSES

GF XF  GDxD  Gwxw (3.15)

where GF, GD, Gw = mass or molar consumption of the feed,

overhead product, (distillate) and bottom product respectively.
xF , xD, xw = mass or mole fractions of the low boiler in the feed,
overhead and bottom product respectively.
Equations (3.14) and (3.15) hold for a rectification column heated with indirect
steam. When aqueous mixtures are being rectified with direct (live) steam, the
equation of the material balance and the operating line of the bottom part of the
column change Seader and Henley, (2006) Fig. 3.2.
Material balance of the column for direct steam:
F+V=1+W (3.16)
Where F, V, W = feed, top products, bottom product respectively
FxF = xD + Wxw (3.17)
when W = F + R, we obtain

x D  Rxw (3.18)
F 
xF  xw

xD  RxF
W (3.19)
xF  xw

V = R+1 material balance at the top of the column (Fig. 3.2) (3.20)

Indirect Steam
The equations of the operating lines of a rectification column are:
(a) for the top section of the column (same as for indirect steam)
R x (3.21)
y x D
R 1 R 1

(b) for the bottom section of the column

102  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

RF RF (3.22)

y  x  xw
R 1 R 1
In Equations (3.21) and (3.22)

GF GW Gv
F ; W ; V
GD GD GD

where GF, GD, Gw and GV are the molar rates of flow of the feed, overhead product
(distillate) the bottom product, and the supplied steam, respectively, kmol/s.
The operating line from the top section of the column is the same as when a column is
heated with indirect steam.

Figure 3.2: Rectification column whose still is supplied with direct steam

The operating line for the bottom section of the column intersects the axis of abscissa at
x = xw. Both operating lines intersect at x = xF.
Theoretically it is assumed that in a rectification column, unlike in the absorption
column, the total molar rates of flow of the vapour and liquid are constant along the
 103
DISTILLATION PROCESSES

height of the column. Hence, the molar rates and concentrations are used in Equations
(3.21 and 3.22).
In the top section of the column above the inlet of the liquid feed mixture, the molar rate
of flow of the liquid is constant along the height of the column equals GR, and the
bottom section of the column, equals (GR + GF), (Figure 3.2).
The molar rate of flow of the vapour is constant along the height of the column; Gv is
identical in its top and bottom sections. In Equations 3.21 and 3.22, y and x are the non-
equilibrium concentrations (mole fractions) of the low boiling component in the vapour
and the liquid in a given column cross section respectively: they vary along the height of
the column. For plate columns, y is the mole fraction of the low boiling component in
the vapour entering the plate from below: x is the mole fraction of the low boiling
component in the liquid flowing down from this plate:
G R is the reflux ratio; (3.23)
R 
GD

GF x  x w is the relative (per kmole of overhead product) molar rate of

f   D
GD xF  xw
flow of the feed when using relative rates of flow, the equations of the material
balance of a column becomes,
f=1+w (3.24)
In analyzing the operation on each tray it is important to note that the vapour rising to it,
and the reflux flowing down to it, are not in equilibrium, and adequate rates of mass and
heat transfer are essential for the proper functioning of the tray Kister and Olsson,
(2011)
However, on each tray the system tends to reach equilibrium because of the following:
(a) Some of the less volatile component condenses from the rising vapour into the
liquid thus increasing the concentration of the more volatile component in the
vapour.
(b) Some of the more volatile component is vaporized from the liquid on the tray thus
decreasing the concentration of the more volatile component in the liquid.
It is worthy of note to point out that the number of molecules passing in each direction
from vapour to liquid and in reverse is approximately the same since the heat given out
by one mole of the vapour on descending is approximately equal to the heat required to
vaporize one mole of the liquid.
104  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

3.3 The Minimum Reflux Ratio, Rmin

The ratio of the top overflow to the quantity of product is denoted by R and it enables the
equation of the operating line to be expressed in a simple form as shown in Equations
(3.21, 3.22, and 3.23).
If no product is withdrawn from the still, that is GD = 0, in Figure 3.1, then the column is
said to be operating under conditions of total reflux Coulson and Richardson, (2003)
The determination of the cost of distillation column (United States Dollar) depends on the
specifications of its height, H; diameter, D; and the shell thickness, t (Kumar, 1981).
0.58

CostDist  26896.7 DHt 

                                                                                                   (3.25)
 16387

The diameter is calculated from the knowledge of the reflux ratio, R.

The minimum reflux ratio, Rmin in a continuous rectification column when the
equilibrium curve has no points of inflection (hollows) is determined by the equation:
xD  yF (3.26)
R min 
yF  xF

where yF = mole fraction of the low boiling component in the vapour in equilibrium with
the feed liquid.
[All others are as earlier defined]
The operating (actual) reflux ratio is:

R  R min (3.27)

where   1 is the excess reflux coefficient

In practice, the operating reflux ratio of rectification columns is determined by the

equation:
R = 1.3Rmin + 0.3 (3.28)
The quantity Rmin can be obtained graphically; as shown in the example at the end of this
chapter.
 105
DISTILLATION PROCESSES

The consumption of heat in the reboiler of a continuous rectification column is

determined from the heat balance equation for a column with a reflux condenser (Figure
3.1):
Q b + G FH F = Qr,C + GDHD + GwHw + Q1 (3.29)
where Qb = amount of heat received by the boiling liquid from the condensing
heating steam in the reboiler w.
Qr,c = amount of heat taken away by the cooling water from the vapour
condensing in the reflux condenser, w.
Q1 = heat losses of the column to the surroundings, w
G F, G D , G w = mass rates of flow of the feed, overhead, and bottom products, kg/s
H F, H D , H w = corresponding specific enthalpies, J/kg

Introducing specific heat capacities into equation 3.29 we have;

Qb = Qr,c + GDCDtD + GwCwtw - GFCFtF + Q1 (3.30)
where CD, Cw, CF = specific heat capacities, J/kg.K
tD, tw, tF = corresponding temperatures, K

The amount of heat given up to the cooling water in the reflux condenser is:
Qr,C = GD (1+R)LD (3.31)
LD = specific heat of condensation of vapour in the reflux condenser, J/kg
R = reflux ratio.
3.4 The diameter of a plate rectification column is determined by the equation:
1

 QV 
2

D   (3.32)

 0 . 785 v 

where QV = volumetric rate of flow of the vapour through the column, m3/s
v = velocity of the vapour related to the total cross-sectional area of
the column, m/s
106  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

The permissible optimal velocity of the vapour in the column is calculated by the
formula:
1
   V  (3.33)
2

v  C  ld 
 V 

where C = coefficient depending on the design of the plates, the distance between the
plates, the operating pressure in the column, and the load on the column with respect to
the liquid.
 ld, and  v = densities of the liquid and the vapour, respectively kg/m3
When  ld >>  v, we have
1

v  C  ld


2
(3.34)

 V 

The dependence of the coefficient C on the distance between the plates for rectification
columns that operate under atmospheric pressure and with medium loads with respect to
the liquid are shown in Figure 3.3.

C 0.10 C

0.08

0.06 B

0.04

0.02

A
0
100 200 300 400 500 600 700

h, mm
Figure 3.3: Values of coefficient C; A B-bubble-cap plates with round caps C- sieve plate
 107
DISTILLATION PROCESSES

3.5 The height of a plate rectification column (the distance Zpl between
the top and bottom plates) is determined by the equation:
Zpl = (n-1)h (3.35)
where n = number of plates in the column
h = distance between the plate, mm

3.6 Number of theoretical plates-stages of concentration change

The required number of plates, n, is determined graphically using kinetic laws – the
equation of mass transfer and the relationships for calculating the individual mass transfer
coefficients (or the number of transfer units) in the vapour and liquid phases on a plate as
shown in Equations (2.64) and (2.67).
In approximate calculations, a theoretically less substantiated but simpler method of
determining the number of plates is used. It employs the so called overall plate efficiency
(Column efficiency) :

n 
nth (3.36)


where nth is the number of theoretical plates-stages of concentration change which is

found by graphical construction between the equilibrium and the operating lines in a y-x
diagram see Figure 3.4
108  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

Fig. 3.4: Vapour-Liquid Equilibrium diagram for determination of number of stages.

 109
DISTILLATION PROCESSES

Fig. 3.5: Vapour-Liquid Equilibrium diagram for determination of plate efficiency

The value of the overall plate efficiency, , which considers the actual conditions of mass
exchange on the plates depends on many variables (the design and dimensions of the
plates, hydrodynamic factors, the physicochemical properties of the vapour and liquid).
The values of  are determined according to plant data.
On plates with a cross flow of the vapour and liquid an increase in the length of the path
of the liquid over a plate that is in the time spent by the liquid on the plate, results in
improved mass exchange and the value of the overall efficiency  increases.
110  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

The simplest way to gain efficiency is to increase the number of trays within a given
section by reducing the spacing between trays. For instance, a 4- for – 3 tray revamp (e.
g., replacing 18 trays on 24- in. spacings with 24 trays on 18-in. spacing) increases the
number of theoretical stages (NTS) of a section by 33 %. Since capacity decreases with
lower tray spacing, higher performance (i.e., higher-capacity) trays are usually needed to
handle the capacity while delivering the same tray efficiency per tray, Mark and Daniel
(2012).
The value of overall plate efficiency for a typical Refinery, obtained from Fig. 3.5 is 93.9
%. Ujile and Amagbo, (2013) The efficiency values obtained for plates 1, 2, 3 and
perhaps plate 4 shows that the column requires adequate maintenance of the plates. There
may be other sections of the plant that require thorough investigation for proper
performance.

3.7 Determination of Plate efficiency

When determining the overall efficiency for columns having large diameter (with the
length l of the path traveling by the liquid exceeding 0.9 m), it is recommended (Mark
and Daniel, 2012) to add the correction  to the values obtained from experimental data.

t = n(1+) (3.37)

The dependence of the correction  on the length (of the path of the liquid along a plate is
given in Figure 3.6 
0.30 

0.25 

0.20 
  ∆
0.15 

0.10 

0.05 

0 
1  2  3  4 5

l, m 
Figure 3.6: Dependence of the correction,  on the length l of the path of the liquid along a plate
 111
DISTILLATION PROCESSES

3.8 Murphree Efficiency

Murphree efficiency of a separate plate is defined by the following relation:

EmE 
y  yn1 
n (3.38)
y  yn1
*
n

where y = concentration of vapour above plate n

yn+1 = concentration of vapour entering from plate below n
y*n = concentration of vapour in equilibrium with liquid leaving plate n
If the liquid on the plate is completely miscible then y*n is the mole fraction of the low
boiling component in the vapour in equilibrium with the liquid on the plate.
The diameter and height of a packed rectification column are determined in the same way
as for packed absorption column (see Chapter 2).
The diameter of a packed column is calculated by Eq. 2.53. The fictitious velocity of the
vapour at the flooding point Vfl, when  lq   V is obtained by Equation 2.54 but with
a different value of the constant C. In practice C = -0.125 for rectification column.
The fictitious velocity of the vapour in packed rectification columns operating in
conditions of the beginning of suspension is determined by Eq. 2.54.
The depth of the packed section hp for the film conditions of column operation is found
separately for the top and for the bottom sections of the column by the equation:
G dy (3.39)
 y *
y
hp   hoy n oy
2

k w Ac y * y
1

This is similar to Eq. 2.65.

In Equation 3.39
G = molar rate of flow of the vapour constant along the height of the column,
kmol/sec

Ky = overall mass transfer coefficient, kmol/m2.S(y=1)

112  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

D 2
AC = = cross sectional area of the column, m2
4
 = dimensionless coefficient of packing wetting.
y* and y = equilibrium and operating mole fractions of the low boiling component in the
vapour.
The equivalent depth of the packing heq (at the point of inversion) for packed rectification
columns operating in emulsifying conditions can be determined by the equation:
t
0 .2 log (3.40)
  ld 
0 . 35
h eq G    mG
 5 . 2 Re 0 .2
 
L  V
v
d eq  G
1 m
L

where deq = 4V free = equivalent diameter of the column



4V  v
Rev =
 v

G = ratio of the flow rates of the vapour and the liquid for the top section of a column
L

G = R 1,
L R

and for the bottom section

G = R  1
L R  F 

m = slope of the equilibrium line.

The depth of the packed section hp is found by using Equation 2.66.
 113
DISTILLATION PROCESSES

Examples
Example 3.1: Calculate the composition of the equilibrium vapour phase at 60 OC for a
liquid mixture consisting of 40 mole percent of benzene and 60 mole percent of toluene,
considering that the given mixture is obeys the Raoult’s law. Also find the composition
of a liquid mixture of benzene and toluene that boils at 90 OC under a pressure of 760 mm
Hg.
Solution: We determine the saturated vapour pressures of benzene and toluene at 60 OC
from nomograph (temperature dependence of saturated vapour pressure of organic liquids
immiscible with water); for benzene pbo = 385 mmHg, for toluene pt = 140 mmHg.
We determine the partial pressures of the benzene and toluene by the relation:
pb = pboxb = 385  0.4 = 154 mmHg
pt = ptoxt = 140(1-0.4) = 84 mmHg
the total pressure is: p = pb + pt =154 + 84 = 238 mmHg
We determine the composition of the vapour phase by applying Eq.(3.1):
pb 154
yb = =  0.648
p 238

Thus, the equilibrium vapour contains 64.8 mole % of benzene and 35.2 mole % of
toluene. To find the composition of the liquid boiling under a pressure of 760 mmHg at
90 OC, we write the equation:
p = pbxb + ptxt
or 760 = 1013xb + 408 (1-xb)
xb = 58.3 % and xt = 41.7 %
Note: The 1013 and 408 are the saturated vapour pressures of pure benzene and toluene
respectively at 90 OC, mmHg.
Example 3.2: In designing bubble-cap rectification column, the plate spacing was taken
equal to 300 mm. Vapour flows through the column at a rate of 3200 m3/h. The density of
the vapour is 1.25 kg/m3 (the density and rate of flow are given for standard conditions).
The density of the liquid is 430 kg/m3. Determine the required diameter of the column if
the absolute pressure in it is 1.2 atm and the mean temperature is – 40 OC.
114  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

Solution: To determine the diameter of the column, we have to find the permissible
operating velocity of the vapour in it.
The density of the vapour in the operating conditions is:
 OTO p 1.25  273  1.2 kg/m3
v    1.75
Tp O 233  1

By Eq. (3.34), we have:

v = C  lq = 0.032 430
 0.502 m/s
v 1.75

where C = 0.032 was obtained from Fig. 3.3

the volumetric rate of flow of the vapour in the column in operating conditions is:

Qv = QV , OTpO

3200 1 233
 0.632 m3/s
TO p  3600 273 1.2  3600

The required cross-sectional area of the column could be obtained from the relation:

Ac = QV 0.632 1.26
  m2
v 0.502

and the diameter of the column is:

D= AC 1.26 1.267 m
 
0.785 0.785

From catalogue of column apparatuses, one can adopt D = 1200 mm.

Example 3.3: A simple still is used to distill 1000 kg of a mixture containing 60 mass
percent of ethyl alcohol and 40 mass percent of water. After distillation, the bottom
product contains 5 mass percent of the alcohol. Determine the composition of the
overhead product, its mass, and the mass of the bottom product. The data on the
equilibrium compositions are given in Table 3.1, where x1 stands for the mass fraction of
the ethyl alcohol in the liquid, and y* for the mass fraction of the ethyl alcohol in the
equilibrium vapour. Find the consumption of heating steam (pabs = 2 atm) for the
distillation process. Assume that the losses of heat to the surroundings are 10 % of the
usefully consumed amount of heat. It has been found from a diagram of t against x and y
that the temperature of the beginning of distillation when the boiling mixture contains 60
% (mass) of alcohol, is 81 OC and the temperature at the end of distillation when the
boiling mixture contains 5 % (mass) of alcohol, is 95 OC. The moisture content of the
heating steam is 5 %.
 115
DISTILLATION PROCESSES

TABLE 3.1
x1 y* y*-x1 1 x1 y* y*-x1 1
y  x1
*
y  x1
*

0.025 0.225 0.200 5.00 0.45 0.754 0.304 3.29

0.05 0.360 0.310 3.22 0.50 0.767 0.267 3.74

0.10 0.516 0.416 2.40 0.55 0.778 0.228 4.38
0.15 0.600 0.450 2.22 0.60 0.789 0.189 5.29
0.20 0.655 0.455 2.20 0.65 0.800 0.150 6.66
0.25 0.690 0.440 2.27 0.70 0.810 0.110 9.09
0.30 0.710 0.410 2.44 0.75 0.835 0.085 11.75
0.35 0.728 0.378 2.64 0.80 0.855 0.055 18.20
0.40 0.740 0.340 2.94
Solution:
A We apply Eq. 3.2:
F xF dx
In 
W x w y * x

It is impossible to perform integration analytically because the analytical form of the

relationship between y* and x1 is not known. The integral can then be solved graphically.
To carry out this, we plot a graph showing how 1/(y*- x1) depends on x1 for the alcohol-
water mixture.

The area under the curve determines the solution to the problem.
Let us use the scale 1 mm = 0.02 along the axis of abscissas and 1 mm = 0.2 along the
axis of ordinates. Hence 1 mm2 = 0.02 x 0.2 = 0.004.
116  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

The value of the integral within the limits x1 = 0.6 to x2 = 0.05 as shown in Fig.3.7. This
area equals 403 mm2.
Therefore, 0.6
dx1 = 403 x 0.004 = 1.612*

0.05

y  x1

Consequently,

In F = 2.3 log F = 1.612, and F/W = 5.01

W W

From the initial conditions, F = 1000 kg. Hence, W = 1000 = 200 kg

5.01

The mass of the overhead product is:

D = F – W = 1000 – 200 = 800 kg.
The amount of the alcohol in the bottom product after distillation is:
Gw = W xw = 200 x 0.05 = 10 kg.
The amount of alcohol withdrawn with the overhead product becomes:
GD = F xf – GW = 1000 x 0.6 – 10 =590 kg.
The mass per cent of the alcohol in the overhead product is:

XD = GD
 100 = 73.7 %
D

B The consumption of the heating steam is determined as follows:

Mean distillation temperature is: 81  95 = 88 oC

2

The consumption of heat for heating the feed from 81 to 88 oC is:

Q1 = (1000 x 0.6 x 3.35 x 103 + 1000 x 0.4 x 4.19 x 103) (88-81) = 25800 x103 J
where 3.35 x 103 and 4.19 x 103 J/kg.K are the specific heat capacities of
alcohol and water respectively.
The specific heats of vaporization of alcohol and water are 855 x 103 and 2290 x 103 J/kg,
respectively, and the consumption of heat for vaporization at 88 oC is:
Q2 = 590 x 855 x 103 + (800 -590) 2290 x 103 = 985000 x 103 J
 117
DISTILLATION PROCESSES

The consumption of heat for heating the bottom product fro 88 to 95 oC is:
Q3 = (200 x 0.05 x3.35 x 10 3 + 200 x0.95 x 4.19 x 10 3 ) (95 – 88) = 5700 x 10 3 J
The total consumption of heat with losses is:
Q = (25800 + 985000 + 5700) 10 3 x 1.1 = 1120 x 10 3 KJ
The consumption of the heating steam is:

1120000 x10 3
Gst = = 535 kg where 2208 x 10 3 J/kg is the specific heat of
2208 x10 3 x0.95
condensation of steam at p abs = 2 at.
Example 3.4: In designing a bubble cap rectification column, the plate spacing was taken
equal to 300 mm. Vapour flows through the column at a rate of 3200 m3/h. The density of
the vapour is 1.25 kg/m3 (the density and the rate of flow are given for standard
conditions). The density of the liquid is 430 kg/m3. Determine the required diameter of
the column if the absolute pressure in it is 1.2 atm, and the mean temperature is – 40 oC.
Solution: To determine the diameter of the column, we must find the permissible
operating velocity of the vapour in it. The density of the vapour in the operating
conditions is:

ρv =  oTo P  1.25  273  1.2 = 1.75 kg/m3

TP 233  1

from Eq. (3.34), we have;

v=C  lq = 0.0315 430 = 0.495 m/s

v 1.75

where C = 0.0315 was obtained from Fig. 3.3.

The volumetric rate of flow of the vapour in the column in operating conditions is:

Qv = QV , oT  po 3200  233 = 0.632 m3/s


To  p  3600 273  1.2  3600

The required cross sectional area of the column is:

Ac = Qv = 0.632 = 1.28 m2
v 0.495

and the diameter of the column is:

118  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

D= AC = 1.28 = 1.275 m
0.785 0.785

Example 3.5: A mixture of ethyl alcohol and water containing 25 mole % of the alcohol
is fractionated in a continuous rectification column under atmospheric pressure. The
required concentration of the overhead product is 80 mole %, and the permissible alcohol
content in the bottom product is not over 0.1 mole %. The still of the column is supplied
with direct steam. Determine the operating reflux ratio and the relative molar rates of
flow of feed, the direct steam supplied and the bottom product per kmol of overhead
product.

Solution: Fig. 3.2 shown below gives a diagram of the material streams (the relative
molar rates of flow) in a rectification column whose still is supplied with direct steam.
From the equations of the material balance of the column, we have,
F+V=1+W
FxF = xD + W xW
when W = F + R, we obtain;
 119
DISTILLATION PROCESSES

Fig 3.2 for Example 3.5

x D  RxW
F
x F  xW

x D  Rx F
W
x F  xW

V = R + 1 (material balance at the top of the column)

The equations of the operating lines are:
For the top section of the column

R x
y x D
R 1 R 1
For the bottom section of the column

RF RF
y x xW
R 1 R 1
We determine the operating reflux by Equation (3.28):
R = 1.3 Rmin + 0.3
The equilibrium curve constructed according to the given data has a depression as shown
in Figure 3.8.

Fig 3.8 to Example 3.5

120  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

To determine Rmin, we draw tangent AB to the equilibrium curve from point A. Tangent
AB intercepts a segment equal to 37.5 on the ordinate axis. Hence,

xD 0.8  0.375
 0.375 and R min   1.13
R min  1 0.375

becomes R = 1.3 x 1.13 + 0.3 = 1.77

The segment intercepted by the operating line of the top section of the column on the
ordinate axis at R = 1.77 is:

xD 0. 8
  0.289
R  1 1.77  1
The relative molar rates of flow could be obtained from the formula

x D  RxW 80  1.77  0.1

F   3.21
x F  xW 25  0.1

x D  Rx F 80  1.77  25
W   4.98
x F  xW 24.9

V = R + 1 = 1.77 + 1 = 2.77
Checking of the material balance:
F+V=1+W
3.21 + 2.77 = 1 + 4.98
The rate of flow of the direct steam supplied to the column should be checked according
to the heat balance of the column (Equations 3.29 and 3.30).
 121
DISTILLATION PROCESSES

REFERENCES
1. Coulson, J.M and Richardson, J. F. (2002): Chemical Engineering vol 2
Butterworth- Heinemann.
2. Frank, O. (1977): Distillation design, Chem. Eng. Albany, 84, 14 March 1977
3. Kister, H. Z. and Olsson, M. (2011): ‘Don’t Let Baffle Tray Flood Baffle You’,
AIChE CEP Journal p. 22 July, 2011
4. Kumar, A. (1981): ‘Chemical Process Synthesis and Engineering Design’. Tata
McGraw Hill Publishing Company Limited, New Delhi
5. Mark, P. and Daniel, R. S. (2012): Be smart about column design, AIChE CEP
Journal p. 37 Nov. 2012
6. Perry, R. H., Green, D. W. and Maloney, J. O.(1997): Perry’s Chemical
Engineers’ Handbook, 7th Edition, McHGraw –Hill Book Company, New York.
7. Rayleigh, L. (1902): On the Distillation of Binary Mixtures, Phil Mag. 4 (vi) No
23, 521
8. Richardson, J. F., Harker, J. H. and Backhurst, J. R. (2003): Coulson & Richardson
Chemical Engineering, Particle Technology& Separation Processes, vol. Fifth
Edition, Butterworth- Heinemann
9. Seader, J. D and Henley, E. J. (2006): Separation Processes Principles. 2nd Edition.
Wiley & Sons Inc.
122  CHEMICAL ENGINEERING UNIT OPERATIONS, SYNTHESIS AND BASIC DESIGN CALCULATIONS

10. Ujile, A. A. and Amagbo, L. G. (2013): Determination of Plate Efficiency of

Rectification Column in Refinery Operations. International Journal of
Engineering and Technology, Volume 3 No. 8, August, 2013.

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