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Batch Distillation

Batch distillation is used when small amounts of products with varying compositions are needed. It has several advantages over continuous distillation for producing pharmaceuticals and other specialty chemicals where high purity and cleanliness are required. The key differences from continuous distillation are that there is no continuous feed or product withdrawal, and material balances are performed over the entire operating period rather than as flow rates. The additional Rayleigh equation is derived to provide a third equation to solve batch distillation problems using material balances.
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0% found this document useful (0 votes)
36 views33 pages

Batch Distillation

Batch distillation is used when small amounts of products with varying compositions are needed. It has several advantages over continuous distillation for producing pharmaceuticals and other specialty chemicals where high purity and cleanliness are required. The key differences from continuous distillation are that there is no continuous feed or product withdrawal, and material balances are performed over the entire operating period rather than as flow rates. The additional Rayleigh equation is derived to provide a third equation to solve batch distillation problems using material balances.
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© © All Rights Reserved
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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withdrawn from the column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

1
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 (Lo / 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

2
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

3
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

4
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

5
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

6
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

7
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

8
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

9
Overall:
F = Wfinal + Dtotal (7.1)
where
F = the total amount of feed fed into
the distillation column for the
entire operating period
Wfinal = 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)
Dtotal = the total amount of the distillate
withdrawn from the distillation
column (in some textbooks, the
notation Dfinal may be used)

10
Species balance (for a more volatile compo-
nent: MVC):
x F F = x w , finalWfinal + x D , avgDtotal

(7.2)
where
xF = mole fraction of a more volatile
species in the feed
x w , final = the mole fraction of an MVC of the

remaining liquid in the re-boiler


x D , avg = an average concentration of an

MVC in the distillate


(in some textbooks the notation
x D , final may be used)

11
Normally, F and x F are specified (or given in
the problem statement), and the value of either
x w , final or x D , avg is also specified (or given)

Thus, there are 3 unknowns for the binary-


mixture batch distillation system:
 Wfinal
 Dtotal
 either x D , avg or x w , final

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

12
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,
x DdD , is equal to the decreasing rate of
species i the liquid in the still pot
-d (Wx w )

13
Thus, the following equations can be formu-
lated:
dD = -dW (7.3)
x DdD = -d (Wx w ) (7.4)

Note that it is assumed that, at any instant


of time, the concentration or the composition of
the distillate (x D ) is constant

Combining Eq. 7.3 with Eq. 7.4 and re-arran-


ging gives
-x DdW = -d (Wx w )

-x DdW = -Wdx w - x wdW


(7.5)

14
Re-arranging Eq. 7.5 and integrating the resul-
ting equation yields
Wdx w = x DdW - x wdW
Wdx w = (x D - x w )dW
dx w dW
=
(x D - x w ) W

W =Wfinal x w =x w , final
dW dx w
ò W
= ò xD - xw
W =F x w =x F

which results in
x w , final
æW ö dx w
ln ççç final ÷÷÷ = ò (7.6a)
çè F ÷ø xF
xD - xw

or
æW ö xF
dx w
ln ççç final ÷÷÷ = - ò (7.6b)
çè F ÷ø x w , final
xD - xw

15
In order to perform an integration of the right
hand side (RHS) of Eq. 7.6 (a & b), x D must be
a function of x w :
x D = y = f (x w )

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,


y = xD

16
and x D and x w can be related to each other using
an equilibrium curve or equilibrium equation

Accordingly, Eq. 7.6b can be re-written as


follows
æW ö xF
dx
xF
dx
ln ççç final ÷÷÷ = - ò =- ò
çè F ÷ø x w , final
y -x x
f (x ) - x
w , final

(7.7)
Note that y = f (x ) = x D and x = x w

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 x F to x w , final ),

determine the value of y (or x D ) from the


equilibrium curve/equation

17
1
3) Plot (Y-axis) against x (X-axis) or
y -x
fit it to an equation
4) Graphically determine the area under the
curve from x F to x w , final or perform the

integration analytically or numerically


from x F to x w , final ; the graphical integra-

tion is as illustrated below

(from “Separation Process Engineering” by Wankat, 2007)

18
After the numerical value of the integration
is obtained, the value of Wfinal (i.e. the amount of
liquid remained in the still pot) can be obtained
from manipulating Eq. 7.7 as follows
æ xF ö
çç dx ÷÷÷
Wfinal = F exp çç- ò ÷÷
çç xw , final y - x
è ø÷
(7.8a)
or
Wfinal = F exp (-area under the curve)
(7.8b)

Finally, the value of the average distillate con-


centration, x D ,avg , and the total amount of the

distillate, Dtotal , can be obtained by solving Eqs.


7.1 and 7.2:

19
F = Wfinal + Dtotal (7.1)
x F F = x w , finalWfinal + x D , avgDtotal

(7.2)
simultaneously, which results in
x F F - x w , finalWfinal
x D,avg =
F -Wfinal
(7.9)
and
Dtotal = F -Wfinal (7.10)

In the case that the equilibrium relationship


between y (x D ) and x (x w ) is given as
ax
y=
1 + (a - 1) x
the RHS of Eq. 7.7 can be integrated analytical-
ly as follows

20
æW ö xF
dx
ln ççç final ÷÷÷ = - ò
çè F ÷ø x w , final
y -x
é ù
1 ê x w , final (1 - x F )ú
= ln ê ú
(
(a - 1) êê x F 1 - x w, final úú
ë
) û
é ù
ê (1 - x F ) ú
+ ln ê ú
ê
(
ê 1 - x w , final ú
ë
ú
û
)
(7.11)

For the problem that the value of x D is speci-


fied, and the value of x w , final is to be determined,

a trial & error technique must be employed as


follows
1) Make a first (1st) guess for the value of
x w , final and calculate the value of the inte-

gration of Eq. 7.8a or determine the area


21
under the curve for Eq. 7.8b, according
to the guessed value of x w , final

2) Then, the value of Wfinal can be calculated


from Eq. 7.8 (either a or b)
3) Use the value of Wfinal obtained from 2
and the guessed value of x w , final made in 1,

combined with the given values of F and


x F , to compute the values of Dcalc and
x D, calc using the following equations:

Dcalc = F -Wfinal (7.12)


and
x F F - x w , finalWfinal
x D, calc =
Dcalc
(7.13)

22
4) Compare the value of x D, calc obtained

from 3 with the given value of x D : if


x D, calc = x D , the trial & error procedure is

finished; however, if x D, calc ¹ x D , the new

trial & error has to be repeated, until we


obtain the guessed value of x w , final that

makes x D, calc = x D

The following Example illustrates the employ-


ment of the trial & error technique to solve the
batch distillation problem

23
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 (x D ) is
89.2 mol% MeOH

24
Determine:
a) the total amount of the distillate collected
(D )
total

b) the amount of material (liquid or waste)


remained in the pot after the distillation
has ended (Wfinal ) and its corresponding

(
concentration x w , final )

It is given that
 F = 50 moles
 x F = 0.80
 x D, avg = 0.892

The equilibrium (y - x ) data of MeOH is as


summarised in the following Table

25
Methanol liquid (x MeOH ) Methanol vapour (y MeOH )
(mol%) (mol%)
0 0
2.0 13.4
4.0 23.0
6.0 30.4
8.0 36.5
10.0 41.8
15.0 51.7
20.0 57.9
30.0 66.5
40.0 72.9
50.0 77.9
60.0 82.5
70.0 87.0
80.0 91.5
90.0 95.8
95.0 97.9
100.0 100.0

26
In this Example, the unknowns are
 Dtotal
 Wfinal
 x w , final

Since x w , final , one of the integral boundaries, is

NOT known, a trial & error technique must be


xF
dx
employed to compute the integral ò y -x
x w , final

To start the calculations, the 1st guess with


x w , final of 0.70 is used

27
From the given equilibrium data, the value of
1
for each value of x can be summarised in
y -x
the following Table (note that interpolations are
1
needed to obtain the values of y and when
y -x
the values of x are, e.g., 0.75, 0.65):
1
x y y–x
y -x
0.80 0.915 0.115 8.69
0.75 0.895 0.145 6.89
0.70 0.871 0.171 5.85
0.65 0.845 0.195 5.13
0.60 0.825 0.225 4.44
0.50 0.780 0.280 3.57

28
Plotting a graph between x (X-axis) and
1
(Y-axis) using the data in the Table on the
y -x
previous Page, from x w , final = 0.70 (the dashed

lines) to x F = 0.80, yields the following graph

(from “Separation Process Engineering” by Wankat, 2007)

29
0.80
dx
From the resulting graph, ò is, in fact,
0.70
y -x
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 Wfinal (i.e. the liquid remained in


the still pot) can then be calculated, using Eq.
7.8b, as follows
Wfinal = F exp (-area under the curve)
= (50) exp (-0.7044)

Wfinal = 24.72 mol

30
Thus, the total amount of the distillate can
be computed using from Eq. 7.12 as follows
Dcalc = F -Wfinal
= 50 - 24.72

Dcalc = 25.28

The value of x D , calc can be calculated using Eq.

7.13 as follows
x F F - x w , finalWfinal
x D, calc =
Dcalc
é(0.80)(50)ù - é(0.70)(24.72)ù
ê úû êë úû

(25.28)
x D, calc = 0.898

However, the desired value of x D or x D, avg is

0.892 – the calculated x D value is too high!

31
Thus, a new guess of x w , final is needed

With the new guess of x w , final of 0.60, we obtain

the following (by performing similar calculations


as above):
 area under the curve from x w , final = 0.60 to

x F = 0.80 is 1.2084
 Wfinal = 50 exp (-1.2084) = 14.93
 Dcalc = F -Wfinal = 50 - 14.93 = 35.07
 x D, calc = 0.885 (too low!)

Hence, we need to make a new (the 3rd) guess


for x w , final

32
With the 3rd guess of x w , final 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
 Wfinal = 18.94
 Dcalc = 31.06
 x D, calc = 0.891 (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)

33

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