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Chapter 7:
Batch Distillation
In the previous chapters, we have learned the
distillation operation in the continuous mode,
meaning that
 the feed(s) is(are) fed continuously into
the distillation column
 the distillation products [e.g., distillate,
bottom, side stream(s)] are continuously
withdrawn from the column
In the continuous operation, after the column
has been operated for a certain period of time,
the system reaches a steady state
2
At steady state, the properties of the system,
such as
 the feed flow rate
 the flow rates of, e.g., the distillate and
the bottom
 the feed composition
 the compositions of the distillate and the
bottom
 reflux ratio ( )/o
L D
 system’s pressure
are constant
With these characteristics, a continuous dis-
tillation is the thermodynamically and economi-
cally efficient method for producing large
amounts of material of constant composition
3
However, when small amounts of products of
varying compositions are required, a batch dis-
tillation provides several advantages over the
continuous distillation (the details of the batch
distillation will be discussed later in this chapter)
Batch distillation is versatile and commonly
employed for producing biochemical, biomedical,
and/or pharmaceutical products, in which the
production amounts are small but a very high
purity and/or an ultra clean product is needed
The equipment for batch distillation can be
arranged in a wide variety of configurations
4
In a simple batch distillation (Figure 7.1), va-
pour (i.e. the product) is withdrawn from the top
of the re-boiler (which is also called the “still
pot”) continuously, and by doing so, the liquid
level in the still pot is decreasing continuously
Figure 7.1: A simple batch distillation
(from “Separation Process Engineering” by Wankat, 2007)
Note that the distillation system shown in Fig-
ure 7.1 is similar to the flash distillation
5
However, there are a number of differences
between the batch distillation (e.g., Figure 7.1)
and the flash distillation: i.e.
 in the flash distillation, feed is continuous-
ly fed into the column, whereas there is
no continuous feed input into the still
pot for the batch distillation
 in the flash distillation, the products (i.e.
vapour and liquid products) are withdrawn
continuously from the system, whereas, for
the batch distillation, the remaining liquid
in the still pot is drained out of the pot
(or the re-boiler) only at the end of the
distillation
6
Another configuration of batch distillation is
a constant-level batch distillation, which is
similar to the simple batch distillation, as illus-
trated in Figure 7.1; however, in this configura-
tion, the liquid (i.e. the feed) is continuously
fed into the still pot (or the re-boiler) to keep the
liquid level in the pot constant
The more complex batch distillation (than
the simple and the constant-level batch distilla-
tion) is the multi-stage batch distillation
In this distillation system, a staged or packed
distillation column is placed on top of the re-
boiler (or the still pot), as shown in Figure 7.2
7
Figure 7.2: A multi-stage batch distillation
(from “Separation Process Engineering” by Wankat, 2007)
In the usual operation of the multi-stage dis-
tillation system, the distillate is withdrawn con-
tinuously from the system, until the distillation
is ended
8
Another way of operating the multi-stage
batch distillation is that the system is operated
such that there is no distillate withdrawn from
the column (or system), thus resulting in a con-
tinuous change in the concentration or com-
position of liquid in the pot (or the re-boiler)
Additionally, when a pure bottom product is
required, an inverted batch distillation is em-
ployed
In this technique (i.e. the inverted batch dis-
tillation), the bottom product or the liquid in
the re-boiler is withdrawn continuously while
the distillate is withdrawn only at the end of
the distillation
9
7.1 Binary-mixture Batch Distillation: Rayleigh
Equation
The material balances for the batch distillation
are different from those for continuous distillation
In the batch distillation, the main focus is
at the total amounts of input(s) [i.e. feed(s)] and
outputs (e.g., distillate or bottom) collected at
the end of the distillation, rather than the rates
of such inputs and outputs
The material balances around the batch dis-
tillation system for the entire operating time are
as follows
10
Overall:
final total
F W D= + (7.1)
where
F = the total amount of feed fed into
the distillation column for the
entire operating period
final
W = the final amount of liquid in the
re-boiler (the notation W is used
because the remaining liquid in the
still pot is normally a waste)
total
D = the total amount of the distillate
withdrawn from the distillation
column (in some textbooks, the
notation final
D may be used)
11
Species balance (for a more volatile compo-
nent: MVC):
,final final ,avg totalF w D
x F x W x D= +
(7.2)
where
F
x = mole fraction of a more volatile
species in the feed
,finalw
x = the mole fraction of an MVC of the
remaining liquid in the re-boiler
,avgD
x = an average concentration of an
MVC in the distillate
(in some textbooks the notation
,finalD
x may be used)
12
Normally, F and F
x are specified (or given in
the problem statement), and the value of either
,finalw
x or ,avgD
x is also specified (or given)
Thus, there are 3 unknowns for the binary-
mixture batch distillation system:
 final
W
 total
D
 either ,avgD
x or ,finalw
x
Problematically, however, by just performing
material balances, we have only 2 equations (i.e.
Eqs. 7.1 and 7.2)
Hence, another or additional equation is re-
quired
13
The additional equation for solving batch
distillation problems is commonly known as
the Rayleigh equation
To derive this equation, Lord Rayleigh (1902)
employed the facts that (see Figure 7.1), at any
instant of time,
1) the rate of the distillate flowing out of
the batch distillation system, dD, is equal
to the decreasing rate of the liquid in the
still pot, dW-
2) the rate of species i in the distillate flow-
ing out of the batch distillation system,
D
x dD, is equal to the decreasing rate of
species i the liquid in the still pot
( )w
d Wx-
14
Thus, the following equations can be formu-
lated:
dD dW= - (7.3)
( )D w
x dD d Wx= - (7.4)
Note that it is assumed that, at any instant
of time, the concentration or the composition of
the distillate ( )D
x is constant
Combining Eq. 7.3 with Eq. 7.4 and re-arran-
ging gives
( )D w
x dW d Wx- = -
D w w
x dW Wdx x dW- = - -
(7.5)
15
Re-arranging Eq. 7.5 and integrating the resul-
ting equation yields
w D w
Wdx x dW x dW= -
( )w D w
Wdx x x dW= -
( )
w
D w
dx dW
Wx x
=
-
,final
final
w w
w F
x xW W
w
D wW F x x
dxdW
W x x
==
= =
=
-ò ò
which results in
,final
final
ln
w
F
x
w
D wx
W dx
F x x
æ ö
÷ç ÷ =ç ÷ç ÷ç -è ø
ò (7.6a)
or
,final
final
ln
F
w
x
w
D wx
W dx
F x x
æ ö
÷ç ÷ = -ç ÷ç ÷ç -è ø
ò (7.6b)
16
In order to perform an integration of the right
hand side (RHS) of Eq. 7.6 (a & b), D
x must be
a function of w
x :
( )D w
x y f x= =
For a simple batch distillation shown in Fig-
ure 7.1, it is reasonable to assume that the vapour
that comes out of the top of the still pot (or the
re-boiler) [note that the amount of the vapour is
equal to that of the distillate] is in equilibrium
with the liquid ( )W in the re-boiler
Thus, if the total condenser is used,
D
y x=
17
and D
x and w
x can be related to each other using
an equilibrium curve or equilibrium equation
Accordingly, Eq. 7.6b can be re-written as
follows
( ),final ,final
final
ln
F F
w w
x x
x x
W dx dx
F y x f x x
æ ö
÷ç ÷ = - = -ç ÷ç ÷ç - -è ø
ò ò
(7.7)
Note that ( ) D
y f x x= = and w
x x=
The integration of the RHS of Eq. 7.7 can be
done sequentially (ตามขั้นตอน) as follows
1) Plot an equilibrium curve
2) At each value of x (from F
x to ,finalw
x ),
determine the value of y (or D
x ) from the
equilibrium curve/equation
18
3) Plot
1
y x-
(Y-axis) against x (X-axis) or
fit it to an equation
4) Graphically determine the area under the
curve from F
x to ,finalw
x or perform the
integration analytically or numerically
from F
x to ,finalw
x ; the graphical integra-
tion is as illustrated below
(from “Separation Process Engineering” by Wankat, 2007)
19
After the numerical value of the integration
is obtained, the value of final
W (i.e. the amount of
liquid remained in the still pot) can be obtained
from manipulating Eq. 7.7 as follows
,final
final
exp
F
w
x
x
dx
W F
y x
æ ö
÷ç ÷ç ÷= -ç ÷ç ÷-ç ÷÷çè ø
ò
(7.8a)
or
( )final
exp area under the curveW F= -
(7.8b)
Finally, the value of the average distillate con-
centration, ,D avg
x , and the total amount of the
distillate, total
D , can be obtained by solving Eqs.
7.1 and 7.2:
20
final total
F W D= + (7.1)
,final final ,avg totalF w D
x F x W x D= +
(7.2)
simultaneously, which results in
,final final
,
final
F w
D avg
x F x W
x
F W
-
=
-
(7.9)
and
total final
D F W= - (7.10)
In the case that the equilibrium relationship
between y ( )D
x and x ( )w
x is given as
( )1 1
x
y
x
a
a
=
+ -
the RHS of Eq. 7.7 can be integrated analytical-
ly as follows
21
( )
( )
( )
( )
( )
,final
final
,final
,final
,final
ln
11
ln
1 1
1
ln
1
F
w
x
x
w F
F w
F
w
W dx
F y x
x x
x x
x
x
a
æ ö
÷ç ÷ = -ç ÷ç ÷ç -è ø
é ù
-ê ú
ê ú=
ê ú- -ê ú
ë û
é ù
ê ú-
ê ú+
ê ú
-ê ú
ë û
ò
(7.11)
For the problem that the value of D
x is speci-
fied, and the value of ,finalw
x is to be determined,
a trial & error technique must be employed as
follows
1) Make a first (1st
) guess for the value of
,finalw
x and calculate the value of the inte-
gration of Eq. 7.8a or determine the area
22
under the curve for Eq. 7.8b, according
to the guessed value of ,finalw
x
2) Then, the value of final
W can be calculated
from Eq. 7.8 (either a or b)
3) Use the value of final
W obtained from 2
and the guessed value of ,finalw
x made in 1,
combined with the given values of F and
F
x , to compute the values of calc
D and
,calcD
x using the following equations:
calc final
D F W= - (7.12)
and
,final final
,calc
calc
F w
D
x F x W
x
D
-
=
(7.13)
23
4) Compare the value of ,calcD
x obtained
from 3 with the given value of D
x : if
,calcD D
x x= , the trial & error procedure is
finished; however, if ,calcD D
x x¹ , the new
trial & error has to be repeated, until we
obtain the guessed value of ,finalw
x that
makes ,calcD D
x x=
The following Example illustrates the employ-
ment of the trial & error technique to solve the
batch distillation problem
24
Example Use the given equilibrium data of me-
thanol (MeOH) and water for solving the simple
batch distillation problem with the following
description:
A single-equilibrium-stage (or a simple) batch
still pot is used to separate MeOH from water
The feed with the total amount of 50 moles
of an 80 mol% MeOH is charged into the still
pot operated at 1 atm
The desired distillate concentration ( )D
x is
89.2 mol% MeOH
25
Determine:
a) the total amount of the distillate collected
( )total
D
b) the amount of material (liquid or waste)
remained in the pot after the distillation
has ended ( )final
W and its corresponding
concentration ( ),finalw
x
It is given that
 F = 50 moles
 F
x = 0.80
 ,avgD
x = 0.892
The equilibrium ( )y x- data of MeOH is as
summarised in the following Table
26
Methanol liquid ( )MeOH
x
(mol%)
Methanol vapour ( )MeOH
y
(mol%)
0
2.0
4.0
6.0
8.0
10.0
15.0
20.0
30.0
40.0
50.0
60.0
70.0
80.0
90.0
95.0
100.0
0
13.4
23.0
30.4
36.5
41.8
51.7
57.9
66.5
72.9
77.9
82.5
87.0
91.5
95.8
97.9
100.0
27
In this Example, the unknowns are
 total
D
 final
W
 ,finalw
x
Since ,finalw
x , one of the integral boundaries, is
NOT known, a trial & error technique must be
employed to compute the integral
,final
F
w
x
x
dx
y x-ò
To start the calculations, the 1st
guess with
,finalw
x of 0.70 is used
28
From the given equilibrium data, the value of
1
y x-
for each value of x can be summarised in
the following Table (note that interpolations are
needed to obtain the values of y and
1
y x-
when
the values of x are, e.g., 0.75, 0.65):
x y y – x
-
1
y x
0.80
0.75
0.70
0.65
0.60
0.50
0.915
0.895
0.871
0.845
0.825
0.780
0.115
0.145
0.171
0.195
0.225
0.280
8.69
6.89
5.85
5.13
4.44
3.57
29
Plotting a graph between x (X-axis) and
1
y x-
(Y-axis) using the data in the Table on the
previous Page, from ,final
0.70w
x = (the dashed
lines) to F
x = 0.80, yields the following graph
(from “Separation Process Engineering” by Wankat, 2007)
30
From the resulting graph,
0.80
0.70
dx
y x-ò is, in fact,
the area under the curve from x = 0.70 to x =
0.80
For this Example, the area under the curve
is found to be 0.7044
The value of final
W (i.e. the liquid remained in
the still pot) can then be calculated, using Eq.
7.8b, as follows
( )
( ) ( )
final
exp area under the curve
50 exp 0.7044
W F= -
= -
final
24.72 molW =
31
Thus, the total amount of the distillate can
be computed using from Eq. 7.12 as follows
calc final
50 24.72
D F W= -
= -
calc
25.28D =
The value of ,calcD
x can be calculated using Eq.
7.13 as follows
( )( ) ( )( )
( )
,final final
,calc
calc
0.80 50 0.70 24.72
25.28
F w
D
x F x W
x
D
-
=
é ù é ù-ê ú ê úë û ë û=
,calc
0.898D
x =
However, the desired value of D
x or ,avgD
x is
0.892 – the calculated D
x value is too high!
32
Thus, a new guess of ,finalw
x is needed
With the new guess of ,finalw
x of 0.60, we obtain
the following (by performing similar calculations
as above):
 area under the curve from ,final
0.60w
x = to
0.80F
x = is 1.2084
 ( )final
50exp 1.2084 14.93W = - =
 calc final
50 14.93 35.07D F W= - = - =
 ,calc
0.885D
x = (too low!)
Hence, we need to make a new (the 3rd
) guess
for ,finalw
x
33
With the 3rd
guess of ,finalw
x of 0.65, we obtain
the following (try doing the detailed calculations
yourself):
 area under the curve (from x = 0.65 to
x = 0.80) = 0.9710
 final
18.94W =
 calc
31.06D =
 ,calc
0.891D
x = (O.K. – close enough!)
7.2 Constant-level Batch Distillation
The recent Example is the simple batch distil-
lation problem in which the amount of liquid in
the still pot is decreasing as the distillation pro-
ceeds (while the distillate is being collected)
34
In a constant-level batch distillation, which is
another configuration of a batch distillation, a
solvent (or the feed) is added to the re-boiler (or
the still pot) to keep the level of the liquid in
the pot constant
Note that, during the addition of the solvent,
the total number of moles of all species in the
still pot is kept constant
The total mole balance is
Accumulation
In Out
in the still pot
é ù
ê úé ù é ù- =ê ú ê ú ê úë û ë û
ê úë û
(7.14)
35
Since, in this kind of batch distillation, the
total number of moles is constant, Eq. 7.14 be-
comes
In Out 0é ù é ù- =ê ú ê úë û ë û (7.15)
Also, since this is a constant-level batch dis-
tillation, the amount of solvent evaporated ( )dV-
must be equal to the amount of solvent added to
the still pot ( )dS+ — note that the solvent added
into the still pot is called “the second solvent”
dV dS- = (7.16)
(or dV dS= - )
Performing a species (or component) balance
on the evaporated solvent (called “the original
solvent”) gives
36
( )
( )
w
w
ydV d Wx
ydV d Wx
- = -
=
[note that, at any instant of time, the concentra-
tion of the vapour evaporated from the liquid ( )y
is constant; thus, it is drawn from the differenti-
ation)
w w
ydV Wdx x dW= + (7.17)
but W is kept constant
Thus, Eq. 7.17 becomes
w
ydV Wdx= (7.18)
Substituting Eq. 7.16 into Eq. 7.18 yields
w
ydS Wdx- = (7.19)
37
Re-arranging Eq. 7.19 and integrating the
resulting equation gives
,final
,initial
w
w
w
w
x
w
x
ydS Wdx
dxdS
W y
dxdS
W y
- =
= -
= -ò ò
,initial
,final
w
w
x
w
x
dxS
W y
= ò (7.20)
In this kind of batch distillation, the vapour
phase and the liquid phase in the system (i.e. the
still pot) are assumed to be in equilibrium with
each other
38
Hence, the value of y (the concentration of
the vapour phase) can be related to the value of
w
x (the concentration of the liquid phase in the
still pot) using either equilibrium curve or equa-
tion
If the relationship between y and w
x can be
expressed in the following form:
( )1 1
w
w
x
y
x
a
a
=
+ -
(7.21)
the integral of the RHS of Eq. 7.20 is
( ), initial
, initial , final
, final
1 1
ln w
w w
w
xS
x x
W x
a
a a
é ù -ê ú= + -ê ú
ê úë û
(7.22)
39
Alternatively, the graphical solution (for the
value of
S
W
) to this kind of problem can be ob-
tained as follows
For each value of w
x , the value of y can be
read from the equilibrium curve, and the graph
between w
x (X-axis) and
1
y
(Y-axis) is plotted
The area under the curve from , finalw
x to
, initialw
x is, in fact,
S
W
Generally, the value of W is given; thus, Eq.
7.20 (or 7.22) is normally used to compute the
value of S (i.e. the amount of solvent required to
keep the liquid level in the still pot constant)
40
7.3 Batch Steam Distillation
In the batch steam distillation, steam is purged
directly into the still pot, as shown in Figure 7.3
Figure 7.3: A batch steam distillation
(from “Separation Process Engineering” by Wankat, 2007)
Normally, the direct addition of steam into
the still pot is done for the system that is NOT
miscible (ละลาย) with water
41
Like the steam distillation in the continuous
operation, the principal purpose of adding
steam directly into the still pot is to keep the
temperature of the system below the boiling
point of water, while eliminating the need of a
heat transfer device (as steam can provide heat/
energy to the system)
By solving Eqs 7.1:
final total
F W D= + (7.1)
and 7.2:
,final final ,avg totalF w D
x F x W x D= +
(7.2)
simultaneously, we obtain the following equation:
42
final
,final
D F
D w
x x
W F
x x
æ ö
÷-ç ÷ç= ÷ç ÷ç ÷- ÷çè ø
(7.23)
Since the more volatile component (e.g., the
volatile organic components: VOCs) is much
more volatile than water, its concentration
( ). . D
ie x in the vapour phase can be considered
pure (i.e. the distillate contains only the VOCs,
or D
x for the VOCs is 1.0)
Thus, Eq. 7.23 becomes
final
,final
1
1
F
w
x
W F
x
æ ö
÷-ç ÷ç= ÷ç ÷ç ÷- ÷çè ø
(7.24)
43
The amount of the distillate, D, can, thus, be
calculated using the following equation:
final
D F W= - (7.25)
The amount of water in the separating tank
( )w
n (see Figure 7.3), which is, in fact, the
amount of steam condensed at the condenser, can
be computed using the following equation:
*
total VOC in the remaining liquid VOC
*
0 VOC in the remaining liquid VOC
D
w org
P x P
n dn
x P
-
= ò
(7.26)
The total amount of steam required is w
n plus
with the amount of steam that is condensed and
remained in the still pot (note that this steam is
used to heat up the feed and vaporise the VOCs)
44
( ) ( )steam steamtotal used to heat up the feedw
n n n= +
(7.27)
7.4 Multi-stage Batch Distillation
If very high purity of a product (either distil-
late or bottom) is needed, a multi-stage column
is added to the batch distillation system, as illu-
strated in Figure 7.2 (Page 7)
The complexity with the multi-stage equili-
brium is attributed to the fact that D
x and w
x
are no longer in equilibrium with each other as
per the case of the simple batch distillation
45
In other words, the relationship between D
x
and w
x can no longer be expressed using the equi-
librium curve or equation
Accordingly, the Rayleigh equation (i.e. Eq.
7.6a or 7.6b), cannot be integrated until the rela-
tionship between D
x and w
x is established
Generally, this relationship between D
x and
w
x for the multi-stage distillation can be obtained
by performing stage-by-stage calculations
The following is how to formulate the rela-
tionship between D
x and w
x for the multi-stage
distillation system
46
Performing material and energy balances for
Figure 7.2 from stage j to the top of the column,
with the assumption that the accumulation at any
where except the re-boiler is negligible, yields
1j j
V L D+
= + (7.28)
1 1j j j j D
y V x L x D+ +
= + (7.29)
1 1C j j j j D
Q V H L h Dh+ +
+ = + (7.30)
In order to simplify the calculations, CMO is
assumed, and the operating equation of the multi-
stage batch distillation can be written, by re-
arranging Eq. 7.29, as follows
1
1j j D
L L
y x x
V V+
æ ö
÷ç= + - ÷ç ÷ç ÷è ø
(7.31)
47
However, the difficulty of using Eq. 7.31 in
the batch distillation is that either D
x or
L
V
is
varying during the operation, thus resulting in
the fact that the operating line will continuously
be changing (or it is not constant) throughout
the operation
Normally, the batch distillation operation can
be divided into 2 modes:
 Constant reflux ratio
L
D
æ ö
÷ç ÷ç ÷ç ÷è ø
 Constant distillate concentration ( )D
x
The following is the details of each mode
48
7.4.1 Constant reflux ratio
One of the most common multi-stage batch
distillation modes is the operation in which the
reflux ratio
æ ö
÷ç ÷ç ÷ç ÷è ø
L
D
is kept constant throughout the
distillation
In this kind of operation, the concentration
of the distillate ( )D
x is varied (changed), while
the values of L and V are kept constant (by
fixing the reflux ratio)
49
Accordingly, we obtain the operating lines
with the same slope (i.e. the same
L
V
) but various
Y-intercepts; note that the points where y x= =
D
x are also varied
In other words, in this kind of distillation op-
eration (i.e. batch distillation), there are several
operating lines, which is in contrast to the case of
continuous distillation, in which there is only one
operating line
After an appropriate number of operating
lines are plotted for each value of D
x , we step off
stages (for a given number of equilibrium stages)
to find the value of w
x for each D
x
50
Once w
x value for each value of D
x is obtained,
we can perform the integration for the Rayleigh
equation (Eq. 7.6), and the values of
 final
W
 total
D
 ,avgD
x
will subsequently be obtained
Note, once again, that if the value of ,avgD
x is
specified, the trial & error technique is to be
employed to calculate the value of ,finalw
x
Let’s examine the following Example, which
illustrates how to solve the constant reflux ratio
distillation problem
51
Example The 50-mol feed comprising 32% EtOH
and 68% water is to be distilled in the multi-stage
batch distillation with the additional 2 equili-
brium stages on top of the re-boiler (still pot)
Reflux is returned to the column as a satu-
rated liquid with the constant reflux ratio
L
D
æ ö
÷ç ÷ç ÷ç ÷è ø
of
2/3
It is desired that the solvent remained in the
still pot has the concentration of EtOH of 4.5
mol%
Determine the average distillate composition
( ),avgD
x , the final amount (in moles) of liquid in
the still pot ( )final
W , and the total amount of the
distillate collected ( )total
D
The operation is at 1 atm
52
The schematic diagram of the batch distilla-
tion in this Example is as shown below
(from “Separation Process Engineering” by Wankat, 2007)
Since the operation is at 1 atm, the equili-
brium curve of EtOH can be obtained from the
x y- equilibrium data of the EtOH-water mixture
at 1 atm
53
A value of D
x is selected (specified), and the
corresponding value of w
x for each selected value
of D
x (or for each operating line) for the number
of stages of 3 (why “3”?) is obtained, as shown
in the following McCabe-Thiele diagram
(from “Separation Process Engineering” by Wankat, 2007)
54
From each pair of D
x and w
x , the value of
1
D w
x x-
is calculated
Eventually, a graph between
1
D w
x x-
and w
x
is plotted from ,final
0.045w
x = (4.5%) to F
x =
0.32 (32%), as shown on the next Page, and the
area under the curve is found to be 0.608
Hence,
( )
( ) ( )
final
exp area under the curve
50 exp 0.608
W F= -
= -
final
27.21W =
and
total final
50 27.21 22.79D F W= - = - =
55
(from “Separation Process Engineering” by Wankat, 2007)
The value of ,avgD
x can, thus, be calculated as
follows
( )( ) ( )( )
( )
,final final
,avg
total
0.32 50 0.045 27.21
22.79
F w
D
x F x W
x
D
-
=
é ù é ù-ê ú ê úë û ë û=
,avg
0.648D
x =
56
7.4.2 Variable reflux ratio (Constant D
x )
In this batch distillation mode, the distillation
is carried out such that the value of D
x is fixed,
while the reflux ratio
L
D
æ ö
÷ç ÷ç ÷ç ÷è ø
is varied
As the reflux ratio is varied, the slope of the
operating line keeps changing as illustrated in
Figure 7.4
Note that the point where the operating line
intersects with the y = x line at D
x is fixed (as
the value of D
x is kept constant)
Similar to the constant reflux ratio batch dis-
tillation (but not exactly the same), to solve this
57
problem, we step off stages (for a given number
of equilibrium stages) from the point where y = x
D
x= for each operating line, and the correspond-
ing value of w
x is obtained; then, the graph bet-
ween
1
D w
x x-
and w
x is plotted
Figure 7.4: The batch distillation with varying
reflux ratio
(from “Separation Process Engineering” by Wankat, 2007)
58
7.5 Operating Time for Batch Distillation
The overall operating time for batch distilla-
tion includes the operating time and the down
time:
batch operating down
t t t= + (7.32)
The actual operating time for batch distilla-
tion ( )operating
t can be computed using the following
equation:
total
operating
D
t
D
=  (7.33)
where D = the flow rate of the distillate
The value of D cannot be set arbitrarily
(อย่างไรก็ได้ or ตามใจชอบ), as the column must be
59
designed to accommodate a limited amount of
vapour flow rate ( )max
V , to avoid the flooding
phenomenon
The maximum distillate flow rate ( )max
D can
be computed as follows
max
max
1
V
D
L
D
=
+
 (7.34)
Normally, the optimal or operating value of
D is 0.75 max
D
The down time ( )down
t includes
1) the time required for dumping (draining
out) the remaining bottom product
2) the clean-up time (to clean up the column)
60
3) the loading time for the next batch
4) the heat-up time until the reflux starts to
appear
Note that ehe energy requirements for a con-
denser and a re-boiler can be calculated from the
energy balance equations around the condenser
and the whole system, respectively
If the reflux is a saturated liquid,
( )1 1 1C D
Q V H h V l= - - = - (7.35)
where l is the latent heat of vaporisation
The energy balance around the entire system
yields the heating load ( )R
Q as follows
R C D
Q Q Dh= - + (7.36)

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batch distillation, multi stage batch distillation

  • 1. 1 Chapter 7: Batch Distillation In the previous chapters, we have learned the distillation operation in the continuous mode, meaning that  the feed(s) is(are) fed continuously into the distillation column  the distillation products [e.g., distillate, bottom, side stream(s)] are continuously withdrawn from the column In the continuous operation, after the column has been operated for a certain period of time, the system reaches a steady state
  • 2. 2 At steady state, the properties of the system, such as  the feed flow rate  the flow rates of, e.g., the distillate and the bottom  the feed composition  the compositions of the distillate and the bottom  reflux ratio ( )/o L D  system’s pressure are constant With these characteristics, a continuous dis- tillation is the thermodynamically and economi- cally efficient method for producing large amounts of material of constant composition
  • 3. 3 However, when small amounts of products of varying compositions are required, a batch dis- tillation provides several advantages over the continuous distillation (the details of the batch distillation will be discussed later in this chapter) Batch distillation is versatile and commonly employed for producing biochemical, biomedical, and/or pharmaceutical products, in which the production amounts are small but a very high purity and/or an ultra clean product is needed The equipment for batch distillation can be arranged in a wide variety of configurations
  • 4. 4 In a simple batch distillation (Figure 7.1), va- pour (i.e. the product) is withdrawn from the top of the re-boiler (which is also called the “still pot”) continuously, and by doing so, the liquid level in the still pot is decreasing continuously Figure 7.1: A simple batch distillation (from “Separation Process Engineering” by Wankat, 2007) Note that the distillation system shown in Fig- ure 7.1 is similar to the flash distillation
  • 5. 5 However, there are a number of differences between the batch distillation (e.g., Figure 7.1) and the flash distillation: i.e.  in the flash distillation, feed is continuous- ly fed into the column, whereas there is no continuous feed input into the still pot for the batch distillation  in the flash distillation, the products (i.e. vapour and liquid products) are withdrawn continuously from the system, whereas, for the batch distillation, the remaining liquid in the still pot is drained out of the pot (or the re-boiler) only at the end of the distillation
  • 6. 6 Another configuration of batch distillation is a constant-level batch distillation, which is similar to the simple batch distillation, as illus- trated in Figure 7.1; however, in this configura- tion, the liquid (i.e. the feed) is continuously fed into the still pot (or the re-boiler) to keep the liquid level in the pot constant The more complex batch distillation (than the simple and the constant-level batch distilla- tion) is the multi-stage batch distillation In this distillation system, a staged or packed distillation column is placed on top of the re- boiler (or the still pot), as shown in Figure 7.2
  • 7. 7 Figure 7.2: A multi-stage batch distillation (from “Separation Process Engineering” by Wankat, 2007) In the usual operation of the multi-stage dis- tillation system, the distillate is withdrawn con- tinuously from the system, until the distillation is ended
  • 8. 8 Another way of operating the multi-stage batch distillation is that the system is operated such that there is no distillate withdrawn from the column (or system), thus resulting in a con- tinuous change in the concentration or com- position of liquid in the pot (or the re-boiler) Additionally, when a pure bottom product is required, an inverted batch distillation is em- ployed In this technique (i.e. the inverted batch dis- tillation), the bottom product or the liquid in the re-boiler is withdrawn continuously while the distillate is withdrawn only at the end of the distillation
  • 9. 9 7.1 Binary-mixture Batch Distillation: Rayleigh Equation The material balances for the batch distillation are different from those for continuous distillation In the batch distillation, the main focus is at the total amounts of input(s) [i.e. feed(s)] and outputs (e.g., distillate or bottom) collected at the end of the distillation, rather than the rates of such inputs and outputs The material balances around the batch dis- tillation system for the entire operating time are as follows
  • 10. 10 Overall: final total F W D= + (7.1) where F = the total amount of feed fed into the distillation column for the entire operating period final W = the final amount of liquid in the re-boiler (the notation W is used because the remaining liquid in the still pot is normally a waste) total D = the total amount of the distillate withdrawn from the distillation column (in some textbooks, the notation final D may be used)
  • 11. 11 Species balance (for a more volatile compo- nent: MVC): ,final final ,avg totalF w D x F x W x D= + (7.2) where F x = mole fraction of a more volatile species in the feed ,finalw x = the mole fraction of an MVC of the remaining liquid in the re-boiler ,avgD x = an average concentration of an MVC in the distillate (in some textbooks the notation ,finalD x may be used)
  • 12. 12 Normally, F and F x are specified (or given in the problem statement), and the value of either ,finalw x or ,avgD x is also specified (or given) Thus, there are 3 unknowns for the binary- mixture batch distillation system:  final W  total D  either ,avgD x or ,finalw x Problematically, however, by just performing material balances, we have only 2 equations (i.e. Eqs. 7.1 and 7.2) Hence, another or additional equation is re- quired
  • 13. 13 The additional equation for solving batch distillation problems is commonly known as the Rayleigh equation To derive this equation, Lord Rayleigh (1902) employed the facts that (see Figure 7.1), at any instant of time, 1) the rate of the distillate flowing out of the batch distillation system, dD, is equal to the decreasing rate of the liquid in the still pot, dW- 2) the rate of species i in the distillate flow- ing out of the batch distillation system, D x dD, is equal to the decreasing rate of species i the liquid in the still pot ( )w d Wx-
  • 14. 14 Thus, the following equations can be formu- lated: dD dW= - (7.3) ( )D w x dD d Wx= - (7.4) Note that it is assumed that, at any instant of time, the concentration or the composition of the distillate ( )D x is constant Combining Eq. 7.3 with Eq. 7.4 and re-arran- ging gives ( )D w x dW d Wx- = - D w w x dW Wdx x dW- = - - (7.5)
  • 15. 15 Re-arranging Eq. 7.5 and integrating the resul- ting equation yields w D w Wdx x dW x dW= - ( )w D w Wdx x x dW= - ( ) w D w dx dW Wx x = - ,final final w w w F x xW W w D wW F x x dxdW W x x == = = = -ò ò which results in ,final final ln w F x w D wx W dx F x x æ ö ÷ç ÷ =ç ÷ç ÷ç -è ø ò (7.6a) or ,final final ln F w x w D wx W dx F x x æ ö ÷ç ÷ = -ç ÷ç ÷ç -è ø ò (7.6b)
  • 16. 16 In order to perform an integration of the right hand side (RHS) of Eq. 7.6 (a & b), D x must be a function of w x : ( )D w x y f x= = For a simple batch distillation shown in Fig- ure 7.1, it is reasonable to assume that the vapour that comes out of the top of the still pot (or the re-boiler) [note that the amount of the vapour is equal to that of the distillate] is in equilibrium with the liquid ( )W in the re-boiler Thus, if the total condenser is used, D y x=
  • 17. 17 and D x and w x can be related to each other using an equilibrium curve or equilibrium equation Accordingly, Eq. 7.6b can be re-written as follows ( ),final ,final final ln F F w w x x x x W dx dx F y x f x x æ ö ÷ç ÷ = - = -ç ÷ç ÷ç - -è ø ò ò (7.7) Note that ( ) D y f x x= = and w x x= The integration of the RHS of Eq. 7.7 can be done sequentially (ตามขั้นตอน) as follows 1) Plot an equilibrium curve 2) At each value of x (from F x to ,finalw x ), determine the value of y (or D x ) from the equilibrium curve/equation
  • 18. 18 3) Plot 1 y x- (Y-axis) against x (X-axis) or fit it to an equation 4) Graphically determine the area under the curve from F x to ,finalw x or perform the integration analytically or numerically from F x to ,finalw x ; the graphical integra- tion is as illustrated below (from “Separation Process Engineering” by Wankat, 2007)
  • 19. 19 After the numerical value of the integration is obtained, the value of final W (i.e. the amount of liquid remained in the still pot) can be obtained from manipulating Eq. 7.7 as follows ,final final exp F w x x dx W F y x æ ö ÷ç ÷ç ÷= -ç ÷ç ÷-ç ÷÷çè ø ò (7.8a) or ( )final exp area under the curveW F= - (7.8b) Finally, the value of the average distillate con- centration, ,D avg x , and the total amount of the distillate, total D , can be obtained by solving Eqs. 7.1 and 7.2:
  • 20. 20 final total F W D= + (7.1) ,final final ,avg totalF w D x F x W x D= + (7.2) simultaneously, which results in ,final final , final F w D avg x F x W x F W - = - (7.9) and total final D F W= - (7.10) In the case that the equilibrium relationship between y ( )D x and x ( )w x is given as ( )1 1 x y x a a = + - the RHS of Eq. 7.7 can be integrated analytical- ly as follows
  • 21. 21 ( ) ( ) ( ) ( ) ( ) ,final final ,final ,final ,final ln 11 ln 1 1 1 ln 1 F w x x w F F w F w W dx F y x x x x x x x a æ ö ÷ç ÷ = -ç ÷ç ÷ç -è ø é ù -ê ú ê ú= ê ú- -ê ú ë û é ù ê ú- ê ú+ ê ú -ê ú ë û ò (7.11) For the problem that the value of D x is speci- fied, and the value of ,finalw x is to be determined, a trial & error technique must be employed as follows 1) Make a first (1st ) guess for the value of ,finalw x and calculate the value of the inte- gration of Eq. 7.8a or determine the area
  • 22. 22 under the curve for Eq. 7.8b, according to the guessed value of ,finalw x 2) Then, the value of final W can be calculated from Eq. 7.8 (either a or b) 3) Use the value of final W obtained from 2 and the guessed value of ,finalw x made in 1, combined with the given values of F and F x , to compute the values of calc D and ,calcD x using the following equations: calc final D F W= - (7.12) and ,final final ,calc calc F w D x F x W x D - = (7.13)
  • 23. 23 4) Compare the value of ,calcD x obtained from 3 with the given value of D x : if ,calcD D x x= , the trial & error procedure is finished; however, if ,calcD D x x¹ , the new trial & error has to be repeated, until we obtain the guessed value of ,finalw x that makes ,calcD D x x= The following Example illustrates the employ- ment of the trial & error technique to solve the batch distillation problem
  • 24. 24 Example Use the given equilibrium data of me- thanol (MeOH) and water for solving the simple batch distillation problem with the following description: A single-equilibrium-stage (or a simple) batch still pot is used to separate MeOH from water The feed with the total amount of 50 moles of an 80 mol% MeOH is charged into the still pot operated at 1 atm The desired distillate concentration ( )D x is 89.2 mol% MeOH
  • 25. 25 Determine: a) the total amount of the distillate collected ( )total D b) the amount of material (liquid or waste) remained in the pot after the distillation has ended ( )final W and its corresponding concentration ( ),finalw x It is given that  F = 50 moles  F x = 0.80  ,avgD x = 0.892 The equilibrium ( )y x- data of MeOH is as summarised in the following Table
  • 26. 26 Methanol liquid ( )MeOH x (mol%) Methanol vapour ( )MeOH y (mol%) 0 2.0 4.0 6.0 8.0 10.0 15.0 20.0 30.0 40.0 50.0 60.0 70.0 80.0 90.0 95.0 100.0 0 13.4 23.0 30.4 36.5 41.8 51.7 57.9 66.5 72.9 77.9 82.5 87.0 91.5 95.8 97.9 100.0
  • 27. 27 In this Example, the unknowns are  total D  final W  ,finalw x Since ,finalw x , one of the integral boundaries, is NOT known, a trial & error technique must be employed to compute the integral ,final F w x x dx y x-ò To start the calculations, the 1st guess with ,finalw x of 0.70 is used
  • 28. 28 From the given equilibrium data, the value of 1 y x- for each value of x can be summarised in the following Table (note that interpolations are needed to obtain the values of y and 1 y x- when the values of x are, e.g., 0.75, 0.65): x y y – x - 1 y x 0.80 0.75 0.70 0.65 0.60 0.50 0.915 0.895 0.871 0.845 0.825 0.780 0.115 0.145 0.171 0.195 0.225 0.280 8.69 6.89 5.85 5.13 4.44 3.57
  • 29. 29 Plotting a graph between x (X-axis) and 1 y x- (Y-axis) using the data in the Table on the previous Page, from ,final 0.70w x = (the dashed lines) to F x = 0.80, yields the following graph (from “Separation Process Engineering” by Wankat, 2007)
  • 30. 30 From the resulting graph, 0.80 0.70 dx y x-ò is, in fact, the area under the curve from x = 0.70 to x = 0.80 For this Example, the area under the curve is found to be 0.7044 The value of final W (i.e. the liquid remained in the still pot) can then be calculated, using Eq. 7.8b, as follows ( ) ( ) ( ) final exp area under the curve 50 exp 0.7044 W F= - = - final 24.72 molW =
  • 31. 31 Thus, the total amount of the distillate can be computed using from Eq. 7.12 as follows calc final 50 24.72 D F W= - = - calc 25.28D = The value of ,calcD x can be calculated using Eq. 7.13 as follows ( )( ) ( )( ) ( ) ,final final ,calc calc 0.80 50 0.70 24.72 25.28 F w D x F x W x D - = é ù é ù-ê ú ê úë û ë û= ,calc 0.898D x = However, the desired value of D x or ,avgD x is 0.892 – the calculated D x value is too high!
  • 32. 32 Thus, a new guess of ,finalw x is needed With the new guess of ,finalw x of 0.60, we obtain the following (by performing similar calculations as above):  area under the curve from ,final 0.60w x = to 0.80F x = is 1.2084  ( )final 50exp 1.2084 14.93W = - =  calc final 50 14.93 35.07D F W= - = - =  ,calc 0.885D x = (too low!) Hence, we need to make a new (the 3rd ) guess for ,finalw x
  • 33. 33 With the 3rd guess of ,finalw x of 0.65, we obtain the following (try doing the detailed calculations yourself):  area under the curve (from x = 0.65 to x = 0.80) = 0.9710  final 18.94W =  calc 31.06D =  ,calc 0.891D x = (O.K. – close enough!) 7.2 Constant-level Batch Distillation The recent Example is the simple batch distil- lation problem in which the amount of liquid in the still pot is decreasing as the distillation pro- ceeds (while the distillate is being collected)
  • 34. 34 In a constant-level batch distillation, which is another configuration of a batch distillation, a solvent (or the feed) is added to the re-boiler (or the still pot) to keep the level of the liquid in the pot constant Note that, during the addition of the solvent, the total number of moles of all species in the still pot is kept constant The total mole balance is Accumulation In Out in the still pot é ù ê úé ù é ù- =ê ú ê ú ê úë û ë û ê úë û (7.14)
  • 35. 35 Since, in this kind of batch distillation, the total number of moles is constant, Eq. 7.14 be- comes In Out 0é ù é ù- =ê ú ê úë û ë û (7.15) Also, since this is a constant-level batch dis- tillation, the amount of solvent evaporated ( )dV- must be equal to the amount of solvent added to the still pot ( )dS+ — note that the solvent added into the still pot is called “the second solvent” dV dS- = (7.16) (or dV dS= - ) Performing a species (or component) balance on the evaporated solvent (called “the original solvent”) gives
  • 36. 36 ( ) ( ) w w ydV d Wx ydV d Wx - = - = [note that, at any instant of time, the concentra- tion of the vapour evaporated from the liquid ( )y is constant; thus, it is drawn from the differenti- ation) w w ydV Wdx x dW= + (7.17) but W is kept constant Thus, Eq. 7.17 becomes w ydV Wdx= (7.18) Substituting Eq. 7.16 into Eq. 7.18 yields w ydS Wdx- = (7.19)
  • 37. 37 Re-arranging Eq. 7.19 and integrating the resulting equation gives ,final ,initial w w w w x w x ydS Wdx dxdS W y dxdS W y - = = - = -ò ò ,initial ,final w w x w x dxS W y = ò (7.20) In this kind of batch distillation, the vapour phase and the liquid phase in the system (i.e. the still pot) are assumed to be in equilibrium with each other
  • 38. 38 Hence, the value of y (the concentration of the vapour phase) can be related to the value of w x (the concentration of the liquid phase in the still pot) using either equilibrium curve or equa- tion If the relationship between y and w x can be expressed in the following form: ( )1 1 w w x y x a a = + - (7.21) the integral of the RHS of Eq. 7.20 is ( ), initial , initial , final , final 1 1 ln w w w w xS x x W x a a a é ù -ê ú= + -ê ú ê úë û (7.22)
  • 39. 39 Alternatively, the graphical solution (for the value of S W ) to this kind of problem can be ob- tained as follows For each value of w x , the value of y can be read from the equilibrium curve, and the graph between w x (X-axis) and 1 y (Y-axis) is plotted The area under the curve from , finalw x to , initialw x is, in fact, S W Generally, the value of W is given; thus, Eq. 7.20 (or 7.22) is normally used to compute the value of S (i.e. the amount of solvent required to keep the liquid level in the still pot constant)
  • 40. 40 7.3 Batch Steam Distillation In the batch steam distillation, steam is purged directly into the still pot, as shown in Figure 7.3 Figure 7.3: A batch steam distillation (from “Separation Process Engineering” by Wankat, 2007) Normally, the direct addition of steam into the still pot is done for the system that is NOT miscible (ละลาย) with water
  • 41. 41 Like the steam distillation in the continuous operation, the principal purpose of adding steam directly into the still pot is to keep the temperature of the system below the boiling point of water, while eliminating the need of a heat transfer device (as steam can provide heat/ energy to the system) By solving Eqs 7.1: final total F W D= + (7.1) and 7.2: ,final final ,avg totalF w D x F x W x D= + (7.2) simultaneously, we obtain the following equation:
  • 42. 42 final ,final D F D w x x W F x x æ ö ÷-ç ÷ç= ÷ç ÷ç ÷- ÷çè ø (7.23) Since the more volatile component (e.g., the volatile organic components: VOCs) is much more volatile than water, its concentration ( ). . D ie x in the vapour phase can be considered pure (i.e. the distillate contains only the VOCs, or D x for the VOCs is 1.0) Thus, Eq. 7.23 becomes final ,final 1 1 F w x W F x æ ö ÷-ç ÷ç= ÷ç ÷ç ÷- ÷çè ø (7.24)
  • 43. 43 The amount of the distillate, D, can, thus, be calculated using the following equation: final D F W= - (7.25) The amount of water in the separating tank ( )w n (see Figure 7.3), which is, in fact, the amount of steam condensed at the condenser, can be computed using the following equation: * total VOC in the remaining liquid VOC * 0 VOC in the remaining liquid VOC D w org P x P n dn x P - = ò (7.26) The total amount of steam required is w n plus with the amount of steam that is condensed and remained in the still pot (note that this steam is used to heat up the feed and vaporise the VOCs)
  • 44. 44 ( ) ( )steam steamtotal used to heat up the feedw n n n= + (7.27) 7.4 Multi-stage Batch Distillation If very high purity of a product (either distil- late or bottom) is needed, a multi-stage column is added to the batch distillation system, as illu- strated in Figure 7.2 (Page 7) The complexity with the multi-stage equili- brium is attributed to the fact that D x and w x are no longer in equilibrium with each other as per the case of the simple batch distillation
  • 45. 45 In other words, the relationship between D x and w x can no longer be expressed using the equi- librium curve or equation Accordingly, the Rayleigh equation (i.e. Eq. 7.6a or 7.6b), cannot be integrated until the rela- tionship between D x and w x is established Generally, this relationship between D x and w x for the multi-stage distillation can be obtained by performing stage-by-stage calculations The following is how to formulate the rela- tionship between D x and w x for the multi-stage distillation system
  • 46. 46 Performing material and energy balances for Figure 7.2 from stage j to the top of the column, with the assumption that the accumulation at any where except the re-boiler is negligible, yields 1j j V L D+ = + (7.28) 1 1j j j j D y V x L x D+ + = + (7.29) 1 1C j j j j D Q V H L h Dh+ + + = + (7.30) In order to simplify the calculations, CMO is assumed, and the operating equation of the multi- stage batch distillation can be written, by re- arranging Eq. 7.29, as follows 1 1j j D L L y x x V V+ æ ö ÷ç= + - ÷ç ÷ç ÷è ø (7.31)
  • 47. 47 However, the difficulty of using Eq. 7.31 in the batch distillation is that either D x or L V is varying during the operation, thus resulting in the fact that the operating line will continuously be changing (or it is not constant) throughout the operation Normally, the batch distillation operation can be divided into 2 modes:  Constant reflux ratio L D æ ö ÷ç ÷ç ÷ç ÷è ø  Constant distillate concentration ( )D x The following is the details of each mode
  • 48. 48 7.4.1 Constant reflux ratio One of the most common multi-stage batch distillation modes is the operation in which the reflux ratio æ ö ÷ç ÷ç ÷ç ÷è ø L D is kept constant throughout the distillation In this kind of operation, the concentration of the distillate ( )D x is varied (changed), while the values of L and V are kept constant (by fixing the reflux ratio)
  • 49. 49 Accordingly, we obtain the operating lines with the same slope (i.e. the same L V ) but various Y-intercepts; note that the points where y x= = D x are also varied In other words, in this kind of distillation op- eration (i.e. batch distillation), there are several operating lines, which is in contrast to the case of continuous distillation, in which there is only one operating line After an appropriate number of operating lines are plotted for each value of D x , we step off stages (for a given number of equilibrium stages) to find the value of w x for each D x
  • 50. 50 Once w x value for each value of D x is obtained, we can perform the integration for the Rayleigh equation (Eq. 7.6), and the values of  final W  total D  ,avgD x will subsequently be obtained Note, once again, that if the value of ,avgD x is specified, the trial & error technique is to be employed to calculate the value of ,finalw x Let’s examine the following Example, which illustrates how to solve the constant reflux ratio distillation problem
  • 51. 51 Example The 50-mol feed comprising 32% EtOH and 68% water is to be distilled in the multi-stage batch distillation with the additional 2 equili- brium stages on top of the re-boiler (still pot) Reflux is returned to the column as a satu- rated liquid with the constant reflux ratio L D æ ö ÷ç ÷ç ÷ç ÷è ø of 2/3 It is desired that the solvent remained in the still pot has the concentration of EtOH of 4.5 mol% Determine the average distillate composition ( ),avgD x , the final amount (in moles) of liquid in the still pot ( )final W , and the total amount of the distillate collected ( )total D The operation is at 1 atm
  • 52. 52 The schematic diagram of the batch distilla- tion in this Example is as shown below (from “Separation Process Engineering” by Wankat, 2007) Since the operation is at 1 atm, the equili- brium curve of EtOH can be obtained from the x y- equilibrium data of the EtOH-water mixture at 1 atm
  • 53. 53 A value of D x is selected (specified), and the corresponding value of w x for each selected value of D x (or for each operating line) for the number of stages of 3 (why “3”?) is obtained, as shown in the following McCabe-Thiele diagram (from “Separation Process Engineering” by Wankat, 2007)
  • 54. 54 From each pair of D x and w x , the value of 1 D w x x- is calculated Eventually, a graph between 1 D w x x- and w x is plotted from ,final 0.045w x = (4.5%) to F x = 0.32 (32%), as shown on the next Page, and the area under the curve is found to be 0.608 Hence, ( ) ( ) ( ) final exp area under the curve 50 exp 0.608 W F= - = - final 27.21W = and total final 50 27.21 22.79D F W= - = - =
  • 55. 55 (from “Separation Process Engineering” by Wankat, 2007) The value of ,avgD x can, thus, be calculated as follows ( )( ) ( )( ) ( ) ,final final ,avg total 0.32 50 0.045 27.21 22.79 F w D x F x W x D - = é ù é ù-ê ú ê úë û ë û= ,avg 0.648D x =
  • 56. 56 7.4.2 Variable reflux ratio (Constant D x ) In this batch distillation mode, the distillation is carried out such that the value of D x is fixed, while the reflux ratio L D æ ö ÷ç ÷ç ÷ç ÷è ø is varied As the reflux ratio is varied, the slope of the operating line keeps changing as illustrated in Figure 7.4 Note that the point where the operating line intersects with the y = x line at D x is fixed (as the value of D x is kept constant) Similar to the constant reflux ratio batch dis- tillation (but not exactly the same), to solve this
  • 57. 57 problem, we step off stages (for a given number of equilibrium stages) from the point where y = x D x= for each operating line, and the correspond- ing value of w x is obtained; then, the graph bet- ween 1 D w x x- and w x is plotted Figure 7.4: The batch distillation with varying reflux ratio (from “Separation Process Engineering” by Wankat, 2007)
  • 58. 58 7.5 Operating Time for Batch Distillation The overall operating time for batch distilla- tion includes the operating time and the down time: batch operating down t t t= + (7.32) The actual operating time for batch distilla- tion ( )operating t can be computed using the following equation: total operating D t D =  (7.33) where D = the flow rate of the distillate The value of D cannot be set arbitrarily (อย่างไรก็ได้ or ตามใจชอบ), as the column must be
  • 59. 59 designed to accommodate a limited amount of vapour flow rate ( )max V , to avoid the flooding phenomenon The maximum distillate flow rate ( )max D can be computed as follows max max 1 V D L D = +  (7.34) Normally, the optimal or operating value of D is 0.75 max D The down time ( )down t includes 1) the time required for dumping (draining out) the remaining bottom product 2) the clean-up time (to clean up the column)
  • 60. 60 3) the loading time for the next batch 4) the heat-up time until the reflux starts to appear Note that ehe energy requirements for a con- denser and a re-boiler can be calculated from the energy balance equations around the condenser and the whole system, respectively If the reflux is a saturated liquid, ( )1 1 1C D Q V H h V l= - - = - (7.35) where l is the latent heat of vaporisation The energy balance around the entire system yields the heating load ( )R Q as follows R C D Q Q Dh= - + (7.36)