Computers them. Eagng Vol. 19, Suppl., pp.

S597-S602,1995
Pergamon Copyright @ 1995 Elsevier Science Ltd
009%1354(95)00125-S Printed in Great Britain. All rights reserved
0098-1354/95 $9.50 t 0.00

Design and Operation of a Batch Distillation Column with a

Middle Vessel

George A. Meski Manfred Morari *

Chemical Engineering 210-41

California Institute of Technology
Pasa,dena, CA 91125, U.S.A.

Abstract

The paper examines a new type of a batch distillation column which is built up from two
separation sections and a vessel in between. The behavior of the column is analyzed using
the infinite separation and the minimum reflux models. A comparison of a batch rectifier,
a batch stripper and a column with a middle vessel showed that the latter always performs
better than conventional design. Using the minimum reflux model it is shown that operation
at the steady state is the optimal control policy for the column with a middle vessel in the
case of a binary separation.

KEYWORDS

Distillation; batch distillation; minimum reflux; infinite sepa.ra.tion; distillation design.

INTRODUCTION
In the 1970s Devyatikh [l] proposed a new batch distillation design - a column built up from
two separation sections and a. middle vessel in between (Fig. 1). A mixture to be separated
is loaded into the middle vessel and the products are simultaneously withdrawn from the top
and the bottom of the column. Assuming negligible vapor and liquid holdups in both sections
compared to the liquid holdup of the middle vessel, the separation process in the column under
consideration is described by :

dxmv D+B
-=,-(znz,-&q,-&“B); :=-D-B (1)
dt

In (1) 2~ and XB are functions of z,,, and the operating parameters and, in general, in order to
find them one has to solve two systems of algcbra.ic equa.tions describing the upper

V”‘“Y(Zj+r) - L”“x~ - D.z.D = 0,j = 1, . . . . (mu- 1)

and the lower section:

LlOxJ._ 1 - V’“y(xj) - BxB = 0,j = (r/w + l), . . . . N

*Author to whom all correspondence should be acltlresscd: phone (818)395-4186, fax (818)568-8743, e-mail:
MMQIMC.CALTECFI.EDU
s597
S598 European Symposium on Computer Aided Process Engineering-S

a)
0 1 x

b)
0 X“ 1 x

cl
0 1 X
Fig. 2: Binary nonazeotropic mixture. a - batch

with a middle ves- rectifier; b - column with a middle vessel; c -

sel batch stripper.

It was shown [2] that the model of the column with a middle vessel has three independent
operating parameters, for example, R - reflux ratio, S- reboil ratio and q - ratio between vapor
flows in the upper and lower section (instea.d of V“p/V’” one ca.n use L“P/L’O, L”P/V’” , etc).
In this paper we discuss the behavior of batch distillation using two limiting models known as
infinite separation and minimum reflux conditions.
Infinite separation model assumes that the number of trays in each section is infinite and the
internal flows L”P, P’, LIO,V’” are infinitely large compared to the product flows D and B.
Minimurn refluz conditions assume infinite number of trays in both sections and finite internal
flows. This model allows to determine the lowest amount of energy necessary for separation of
the mixtures and was examined in [2] for mixtures with constant relative volatilities.

INFINITE SEPARATION

It is well known [3],[4] that the composition profiles in sections of distillation columns operating
at infinite reflux can be approximated by residue curves and for the upper (lower) section of any
batch distillation column they always contain the lightest (heaviest) pure component or azeotrope
in the corresponding distillation region.
Let the mole fraction of the light component represent the composition of the mixture, then for
nonazeotropic binary mixtures equation (1) becomes

0, X,, =o
dx,,
-= GW - &, 0 < x,, < 1, 7- = -I??(;
RT-f (2)
dr
( 0, .x,, = 1

We compare the behavior of the column with conventional batch distillation. The phase portraits
of the batch rectifier and the batch stripper have two steady states corresponding to pure light
and heavy components and differ only by their orienta.tion(Fig 2a,c). The reboiler composition
of the batch rectifier goes to the hea.vy component and the composition of the condenser of the
batch stripper goes to the light component. The situation is different for a column with a middle
vessel (Fig 2b). It has one a.dditional unstable steady state in the interior of the phase space
with the coordinate xg,, = & which depends only on the ratio between the distillate and the
bottom flows.
Consider now ternary mixtures. The mol fra.ct,ions of the heavy and light components are used
 Eurooean SvmDosium on CommuterAided Process Enkneerine-5 S599

W
sa
I

L L2i 4

S3 L 1 H

L H
s1 I

b)

H
Fig. 3: Three com~ouent nonazeotropic mixture. Fig. 4: Thr& component -aseotripic mixture.

a - Composition of the reboiler of a batch strip residue curve diagram; b -evolution of the middle

per; b - composition of the middle vessel; c - vessel composition.

composition of the condenser of a batch rectifier.

as independent va,riables to represent the composition. If the middle vessel contains all three
components then the distillate is always the pure light component and the bottom product is the
pure heavy component. Equation (1) becomes:

-dxmv = x,, -
dr
Figure 3 shows the phase portraits of conventional batch columns and the column with a middle
vessel. One can notice that the existence of the operational parameter D/B makes the separation
process in the column more flexible compared to conventional batch where the reboiler (condenser)
composition always changes uniformly going in the direction where the temperature increases
(decreases). For a column with a middle vessel choosing an a.ppropriate parameter D/B the
composition of the middle vessel can reach any point in the composition triangle.
Based on the ideal case it is not difficult to extend the analysis to azeotropic mixtures. Every
distillation region of an azeotropic mixture is similar to an ideal mixture. Figure 4 shows the
evolution of the middle vessel in the separation of a ternary mixture with one binary azeotrope.

MINIMUM R.EFLUX CONDITIONS

As was shown in [‘2]for the sha.rp separation of binary nonazeotropic mixtures, when pure heavy
and light component are withdrawn as the products, the phase portrait of the system at minimum
reflux conditions is qualita,tively the same a,s the infinite sepa.ration - additional unstable steady
states exist on the binary edges of the composition space. The difference between the two is that
the minimum reflus model determines composition points such that, when the evolution brings
the composition of the middle vessel beyond these points, the rcflux and reboil ratio have to be
SO0 European Symposium on Computer Aided Process Engineering-S

changed to insure pure components in the products.

Operating strategy for a column with a middle vessel

The optimal control problem for the column with a middle vessel can be solved in the case
when both products are pure components throughout the separation process. Let us consider the
separation of Ho kmol of a binary mixture with the initial mole fraction of the light component
being z” into the pure heavy and light components. Distillate and bottom product flow rates me
the optimization variables. The vapor flow rates in the upper and lower sections are assumed
to be the same and equal to V during the process. Then zg = 0, XD = 1 and equation (1)
describing the separation process in a column with a middle vessel becomes

* = ~qQp(xmv(t)- ~*I, xmm= &, (4

g = -D(t) - B(t), H(0) = Ho
Let us solve the maximum product problem [5], that is, determine the optimal policy which
produces the maximum amount of pure products in a fixed amount of time:

J = t:l(D(t) + B(Q)& + sup (5)

I
D(t) and B(t) must satisfy the following conditions Vi:

0 I o(t) I &L(t)
(6)
{ 0 I B(t) 5 an(t)
Qn(t) aad &n(t) are the maximum values of product flows necessary to obtain pure light com-
ponent in the distillate and pure heavy component in the bottom product when the mol fraction
of the light component in the middle vessel is x ,,(t). A simple analysis shows that the functions
D(t) = ~m(%v(t))), B(t) = &(%v(Q) are the only solution of the problem (5) with equality
and inequality constraints (4) and (6).
For mixtures with no inflection points on the curve Y(X), &(t*,,) and Z&,(X,,,) can be calculated
from the equations of the operating line in the upper and lower sections

Substitution of D(t) and B(t) from (7) in (4) yields: * = 0. Finally we obtain the solution of
(5) with conditions (4) and (6):

D(t) = D&$,) = const

B(t) = B,(z;o) = consi! (8)

The optimal strategy is to operate the column with a middle vessel at the steady state with the
middle vessel composition equal to the composition of the initial charge. Clearly, under the above
assumptions, the solution of the ma.ximum product problem is also the solution of the minimum
time problem, to produce a required quantity of products in the shortest possible time.

Comparison with conventional batch

We compare the sepa.ration of the sa,me a,mount of a bina.ry mixture at minimum reflux conditions
in three columns: batch rectifier, batch stripper and a column with a middle vessel. In order to
equalize energy consumption the boil-up rate in ea.& of the three columns is assumed to be the
same. The composition of the distilla.te and the bottom product is specified.
The new column operates at the stea.dy state unclcr constant distillate and bottom flows, the only
variable that changes with time is the holdup of the middle vessel. For batch rectifier and batch
stripper the boil-up is consiclcred to be constant throughout the process; the product flows must
be decrea.sed with time in ordrr 1.0 keep t,hc conlposit,ion of the products consta.nt.
 European Symposium on Computer Aided Process Engineering-S s601

Fig. 5: Relative separation time a8 a function of

initial composition. Purity specifications 0.995

Fig. 5 shows the results of a compa.rison of the different batch processes for the separation
of mixtures with constant relative volatilities (Y. The relrlive separation time T, = Taep/Tsep.mv
shows how much faster or slower the separation is compared to the separation of the same amount
of the initial mixture in the column with a. middle vessel.
One can notice that:
1) Separation in a column with a. middle vessel requires alwa.ys less time than in a batch stripper
or batch rectifier.
2) For the batch stripper and the batch rectifier the separation time goes through a maximum.
That reflects a trade-off between two factors - the amount of impurity which must be removed
from the initial charge in order to meet the specifications and the product flow rate. For the batch
rectifier, for example, the closer the composition of the initial mixture is to the specification, the
smaller is the amount of the light component that needs to be removed from the reboiler. On
the other hand, a small composition of the light component in the initial charge requires a bigger
reflux and a smaller distillate flow (recall, tha.t the va.por flow was assumed to be constant during
the whole process).
3) Separation in the batch rectifier requires less time than in the batch stripper for almost all
initial compositions of the mixture. Only in the region of low mol fraction of the light component
a batch stripper performs better than a batch rectifier. The nonsymmetrical behavior of the
batch rectifier and batch stripper ca.n be explained following [6] as the result of the nonsymmetry
of the binary vapor - liquid equilibria.

CONCLUSION
The behavior of a column with a. middle vessel wa.s compa.red with conventiona.l batch distillation
using infinite separation and minimum reflux mod&. It was shown that the column has additional
unstable steady states compared to conventiol1a.l batch distillation. For mixtures with constant
relative volatilities the steady sta.tes are on the binary edges, for nonideal azeotropic mixtures,
they also appear on the sepa.ratrices of the distillation regions.
A comparison of the ba.tch rectifier, ba.tch stripper and a column with a middle vessel showed that
the latter performs always better than the conventional designs. Separation of binary mixtures
in a batch stripper, in general, requires more time (energy) tl1a.n in a ba.tch rectifier which stems
from the nonsymmetry of the bina.ry va.por-liquid equilibria..
s602 European Symposium on Computer Aided Process Engineering-5

The optimal control problem for the column with a middle vessel was solved in the case of a
binary separation when both products a.re pure components throughout the separation process
using the minimum reflux model. It was shown that operation at the steady state with the steady
state equal to the initial composition is the only solution of the problem.

Acknowledgments: We gratefully acknowledge partial financial support from the Department

of Energy and through the Petroleum Research Fund administered by the American Chemical
Society .

Notations
D - distillate flow rate, kmol/hr.
B - bottom product flow rate, kmol/hr.
H - holdup of the middle vessel, kmol.
x - liquid mol fraction.
y - vapor mol fraction.
subscripts and superscripts:
lo - corresponding to the lower section.
rnv - corresponding to the middle vessel.
up - corresponding to the upper section.

References
[l] G.G. Devyatikh, M.F. Churba.nov Methods of high purification. Znanie, 1976, USSR

[2] A.G. Davidyan, V.N. Kiva, G.A.Meski, M.Morari Batch distillation in a column with a
middle vessel. Chem. Eng. Scietzce, in print,1994.

[3] F.B. Petlyuk, L.A. Serafimov Multicomponent distillation. Theory and methods of calcula-
tion. (in Russian), Moscow, Iilrinzia., 273 p., 1983.

[4] N. Bekiaris, G.A. Meski, C.M. Radu, M. Mora.ri Multiple steady states in homogeneous
azeotropic distillation. Ind. E71g. Chenl. Res., 32:2023-38, 1993.

[5] Eva Sorensen Studies on optimal opera.tion and control of batch distillation columns Dr.
Ing. thesis, University of Trondheim, The Norwegian Institure of Technology, July 1994.

[6] H. Hasebe, B.B. Abdul Aziz, I. Hashimoto, T.Wata.na.be Optimal design and operation of
complex batch distillation column Interaction between process design and process control.
Preprints of the IFAC Workshop, London, UK. 7-S September 1992, Edited by J.D. Perkins.