92

Chem. Eng. Technol. I0 (1987) 92-98

h
h,
level of manometer oil above (or below) the datumline
level of start position for oil manometer in Griffin per-
meameter (1 1.1 cm)
level of stop position (coarse powders) (7.2 cm)
level of stop position (fine poweders) (4.5 cm)
integrals
Kozeny constant (aspect factor) (k =5)
variable in Carman-Amell equation
length of powder bed
equivalent length of oil manometer tubing (Blaine Apparatus)
( = K/ a =16cm)
mass of gas
mean relative molecular mass of air (M =29)
mean gas pressure in the bed
pressure at bed outlet
atmospheric pressure (101.325 kN/m2; 76 cm Hg)
pressure drop across the bed
universal gas constant (8.314 kJ /mol K)
powder surface area as given by the Carman-Kozeny equation
powder surface area as given by the slip term
powder surface area as given by the Carman-Amell equation
absolute temperature
time
gas velocity (= 7)
gas volume
inlet volume of Blaine apparatus to datumline (76 cm')
inlet volume of Griffin permeameter to datumline (100 cm3)
1 dV
dV
dt
cp
-
volume flow rate of the gas
atmospheric pressure measured in cm of manometer oil
(P,/p,g =1202 cm)
viscosity of air (186 x l o-' Ns/m2)
density of manometer oil (860 kg/m3)
E bed porosity
11
Pf
References
B. S. I. Drafr Standard Methods for the Determination of Specific Sur-
face of Powders. Part 2: Air Permeability Methods (revision of BS
4359: Part 2: (1971). Document 81/70580, March 1981.
Allen, T., Particle Size Measurement, 3. Ed., Chapman and Hall,
London-Methuen-New York 1981.
Carman, P.C., Amell, J .C., Can. J. Res. 26 (1948) p. 128.
Harris, C.C., Powder Technol. 17 (1977) pp. 235-252.
Shultz, N.F., Int. J. Min. Proc. I (1974) No. 1, pp. 65-80.
Allen, T., Powder Technol. 33(1982) pp. 195-200.
Chirlin, G.R., Soc. Pet. Eng. J. (J une 1985) pp. 358 - 362.
Koplik, J ., Lasseter, T.J ., Soc. Pet. Eng. J. (Feb. 1985) pp. 89 - 100.
Hirasaki, G.J ., Lawson, J .B., Soc. Pet. Eng. J. (April 1985) pp.
Brower, K.R., Morrow, N.R., Soc. Pet. Eng. J. (April 1985) pp.
Bentsen, R.G., SOC. Pet. Eng. J. (Oct. 1985) pp. 765-779.
Vairogs, J ., et al., J . Pet. Technol. (Sept. 1971) pp. 1161 - 1167.
Thomas, R.D., Ward, D.C., J .Pet. Technol. (Feb. 1972) pp.
176 - 190.
191 -201.
120- 124.
Distillation Columns with Vertical Partitions
Gerd Kaibel *
Distillation columns with vertical partitions can separate a feed mixture into 3 or 4 pure fractions.
Compared to other column arrangements, their investment costs and energy consumption are low-
er. Production columns show good results and are easily controlled. Conventional distillation
columns produce only 2 pure product streams at the top and at the bottom of the column. Side
products are contaminated by light or heavy components, depending on the location of the side
stream in the rectifying or stripping section. This disadvantage is set aside by using a distillation
column with a vertical partition. The internal separation wall prevents lateral mixing of liquid
and vapour in the central part of the column, forming there separate feed and outlet sections.
In the presence of a vertical partition, 3 or 4 pure fractions can be obtained in a single distillation
step. This is particularly advantageous when heat sensitive components are to be separated. On
account of good thermodynamic properties, the energy consumption is 20 to 35% lower than that
of other distillation arrangements. The control behaviour is similar or better than that of conven-
tional distillation columns.
1 Column Arrangements
With respect to investment costs, batchwise distillation provides
the best method of separating a multicomponent mixture. The
components are distilled overhead according to their relative
*
Dipl.-Ing. G. Kaibel, BASF AG, D-6700 LudwigshafedRh.
0930-7516/87/0204-0092 $02.50/0
volatilities. Therefore, batchwise distillation is the most com-
mon mode of operation in production plants of small capacities.
Larger capacities require continuous operation. In this case
(n - 1) distillation columns are required for the separation of a
feed mixture containing n components. This necessitates a con-
siderable effort when mixtures consisting of several compo-
nents are to be separated.
Chem. Eng. Techno]. 10 (1987) 92-98
93
Fig. 1 shows examples of separation schemes for a 4-component
mixture. The top diagram represents a distillation arrangement,
corresponding to the direct sequence.
In order to reduce investment costs, an arrangement consisting
of a main column with attached side columns can be employed.
As shown by the centre diagram in Fig. 1, each side stream
results in the saving of either a reboiler or a condenser.
However, the number of distillation columns is not reduced.
To reduce also the number of distillation columns, the side
columns can be omitted as shown in the bottom diagram. In the
present example, the remaining distillation column has 2 simple
side outlets.
This type of distillation column has a serious disadvantage, i.e.
it merely produces pure overhead and bottom products while the
side products are contaminated. In the rectifying section of the
column, the side product is always contaminated by small
amounts of volatiles, since they must be transported past the
side outlet. The amount of contamination by volatiles can be
reduced by withdrawal of liquid normally applied in the rectify-
ing section. According to the vapour/liquid equilibrium, the li-
quid phase contains a smaller amount of volatiles than the
vapour phase. Absolute purity of the side product cannot,
however, be achieved.
A similar situation prevails in the stripping section of the distil-
lation column. There, the side product is discharged as vapour.
With the exception of salt residues, absolute purity of the side
product cannot be achieved either.
1
D
C
h- - B, ( A )
Fig. 1. Separation of a 4-component mixture.
Fig. 2. Thermally coupled
tillation columns.
dis-
An increased heating load provides a further possibility of in-
creasing the purity of side products. On account of increased li-
quid and vapour streams, lower concentrations of light and
heavy fractions result in the centre of the distillation column.
Such improved product quality requires higher energy costs
which are not always economically viable. Moreover, even very
high energy consumption cannot achieve absolutely pure side
products.
The disadvantage of contaminated side products can be avoided
when side columns are employed which are connected to the
main column at their top as well as their bottom ends (Fig. 2).
Such arrangements of distillation columns are well known. An
early description was given by Brugma in 1936 [ 11. He present-
ed the example of an arrangement of 3 distillation columns
which could separate an 8-component mixture into pure
products (Fig. 3).
An important advantage of these column arrangements is their
low energy consumption. There are some recent publications on
the subject [2-61. Some numerical results have also been
presented [7 - 101.
Fig. 3. Arrangement of
L!&
Brugma for separation of an 8-component
94
B
Chem. Eng. Technol. 10 (1987) 92 - 98
However, so far, there is no indication of application on indus-
trial scale. The reasons probably lie in the difficult numerical
calculation of the complex column arrangements and a lack of
experience with respect to the control behaviour.
2 Distillation Column with Vertical Partition
The complex column arrangement, consisting of a main column
with a side column, connected to the main column at both ends,
can besimplified by employing a single distillation column with
a vertical partition. This type of column has an internal separa-
tion wall in thecentre part of the column which prevents a later-
al mixing of liquid and vapour streams (Fig. 4). Thus, the centre
of the column forms two separate parts, i.e. a feed and a dis-
charge section. Application of such distillation columns not
only reduces thenumber of condensers and reboilers but also
requires fewer distillation columns.
This type of column was described by Wright in 1946 [ 1 11. Like
the arrangement of Brugma, such a distillation column appar-
ently has not been applied on industrial scale.
The simplest example of application of a distillation column
with a vertical partition is the separation of a 3-component mix-
ture. The vertical partition, which in the simplest case consists
of a metal sheet, forms two separate parts in the centre section
of the column, above and below the inlet and the outlet.
The feed enters the feed section of the column. The medium
boiling component leaves the feed section upwards via its rec-
tifying section as well as downwards via its stripping section.
The way by which the medium boiling component is distilled
from the feed section is optional. Important is only that no heavy
components should be distilled from the upper end of the feed
section and no light components should leave the feed section
at its lower end. This can be ensured by appropriate dimension-
ing of the feed section with respect to the number of theoretical
trays and sufficiently large liquid and vapour streams.
If there are no heavy components at the upper end of the vertical
partition and no light components at the lower end, a pure medi-
Fig. 4. Distillation column with
vertical partition.
um boiling component can be obtained from the discharge sec-
tion. The location of the side stream can be at the same height
of the distillation column as the feed. Depending on the separa-
tion task, the optimum position of the side stream could also be
higher or lower than the feed position. The correct positions of
the feed and of the side stream are found by calculation.
In contrast to a conventional side stream distillation column, in
the case of distillation column with a vertical partition, it is im-
material whether the side product is withdrawn as liquid or as
vapour. With respect to investment costs, a liquid side stream
is normally preferred, thus eliminating the need for a condenser
for the side stream.
As shown by Fig. 5, the same column arrangement also permits
the separation in a single column of a 4-component mixture into
4 pure fractions. In this case, the light and medium boiling com-
ponents A and B are distilled upwards while the heavy and
medium boiling components D and C are distilled downwards.
In this way, a separation of the medium boiling components into
two pure fractions is achieved in the outlet section.
The basic principle of vertical partitions can be extended. The
addition of further partitions in theory permits the separation of
feed streams into any number of pure fractions (Fig. 5). In prac-
tice, the number of fractions is naturally limited. An increasing
number of components requires more theoretical trays and, with
respect to the height of the column, imposes limitations on the
pressure drop and produces undesirably high bottom temper-
atures.
Normally, only one partition is used. Fig. 6 shows that even this
simple construction considerably reduces the number of distilla-
tion columns.
B
C
A
B
C
D
E
F
Fig. 5. Columns with vertical
H partitions.
Chem. Eng. Technol. 10 (1987) 92-98
(J 1 I 1203kmol/h
__
krnal/
1
0 999kmol /h
Q4 0 . 4 7 1 kW
\
95
Nc ol . =Ncomp. - 1
Fig. 6. Number of columns as a function of thenumber of components.
The number of theoretical trays of a column with a vertical par-
tition corresponds to a conventional column with a side outlet.
It is smaller than in the case of a main column with a side
column or two separate distillation columns when the total num-
bers of theoretical trays are compared. Also with respect to
energy consumption, a distillation column with a vertical par-
tition shows advantages over conventional distillation arrange-
ments.
3 Comparison of Distillation Arrangements
In the following, the separation performance of a distillation
column with a vertical partition is compared with other column
arrangements. The separation of an equimolar 3-component
mixture of n-hexane, n-heptane and n-octane at atmospheric
pressure serves as an example. This system exhibits an almost
ideal separation behaviour. All compared distillation columns
have the same number of theoretical trays, namely 50. The
overhead fraction n-hexane and the bottom fraction n-octane are
always withdrawn with the same purity of 99.9 %. Thus, a com-
parison of the performance of individual systems can be carried
out with the aid of only 2 values, i.e. the total energy require-
ment for heating and the purity of the n-heptane fraction.
Fig. 7 shows the separation of this 3-component mixture in a
distillation column with a liquid side outlet in the rectifying sec-
tion. The locations of the feed inlet and the side outlet were op-
timized. The purity of n-heptane fraction is 83%.
A likewise optimized distillation column with a vapour side out-
let in the stripping section and identical heating duty gives
almost the same purity of n-heptane. In this case, the pre-
50
45
40
35
30
25
20
15
10
5
1
0 20 40 60 80 1
Concentrati on (mol-%)
70 l E90 1 5 130
Temperat ure (OC)
Fig. 7. Comparison of column arrangements; column with liquid side outlet.
dominant impurity is n-octane, while n-hexane is the main con-
taminant in the presence of a liquid side outlet in the rectifying
section.
Even an optimized arrangement of a main and a side column
with only one connection cannot effet any major improvements
if the total energy supply remains the same. The purity of the
medium boiling component is increased by no more than 1 %.
A variation in the distribution of the total heating energy affects
only the ratio of impurities in n-hexane and n-octane.
The performance of a distillation column with a vertical parti-
tion between the 20th and the 40th theoretical tray is shown in
Fig. 8. At the same heating duty and the same total number of
theoretical trays, the purity of the medium boiling component
heptane increases from 83 % to 99 % .
In this case, the locations of the feed and the side outlet are at
the same height in the column. This arrangement is, as a rule,
reasonable with respect to investment costs and results in a sim-
pler construction.
Depending on relative volatilities of the components, a further
optimization with regard to energy consumption may be achie-
ved when the feed and the side outlet are at different heights in
the column. In the present example, the feed inlet would be low-
er than the side outlet and the purity of the medium boiling com-
ponent would be further increased.
Another process variant is a distillation in two separate co-
lumns. Each column has 50 theoretical trays. If an optimized
96 Chem. Eng. Technol. 10 (1987) 92-98
50
45
40
35
30
25
20
1s
10
5
1
0 20 40 60 80 100
Concentrati on Imol -%) Temperat ure (" Cl
Fig. 8. Comparison of column arrangements; column with vertical par-
tition.
0. 997kmol / h 1010kmol / h
(1, =25.228kW
(1, =26.360 k W'
(1,=51.500kW
3kmoVh
Fig. 9. Comparison of column arrangements; two separate columns.
50
45
40
35
30
25
20
15
10
5
1
Theor .st age
20 40 60
Concentrati on (mol -* Temperat ure (OCI
Fig. 10. Comparison of column arrangements; column with liquid side
outlet.
Table 1. Heuristic Rules for Separation Sequence.
I . Favour the easiest separation
2. Favour equimolar separation
3. Remove the most abundant components
4. Favour the direct sequence
arrangement of these columns produces the same purity of 99 %
for n-heptane as the column with a vertical partition shown in
Fig.8, the total heating duty is increased by 27.5% (Fig.9).
Finally, Fig. 10 shows an optimized side outlet column, without
a vertical partition, which also produces 99% pure n-heptane.
It can be seen that such high purities of the side product cannot
be obtained economically in a single distillation column unless
a vertical partition is provided. The heating duty is higher than
that of the distillation column with a vertical partition by a factor
of 17.
4 Thermodynamic Evaluation
Let us now examine the reason for the low energy demand of
a distillation column with a vertical partition as compared to
conventional column arrangements.
First, heuristic rules, which are commonly used for the se-
quencing of distillation columns, are considered. Table 1 lists
the most important ones. Two main rules stipulate:
Chem. Eng. Technol. 10 (1987) 92-98 97
- favour the easiest separation of the components and
- strive for a uniform separation of the feed stream into over-
head and bottom products.
These rules are based on different parameters, physical proper-
ties of the components and their mass distributions, and, for this
reason, frequently cannot be simultaneously maintained.
When thermodynamic aspects are considered, the apparent con-
tradiction of the heuristic rules can be set aside. Instead of the
simplest separation of components whose boiling points im-
mediately follow one another, the overall easiest possible sepa-
ration of the most and the least volatile components should be
selected. This results in a general separation structure, shown
in Fig. 11 for an example of the separation of a 4-component
mixture.
It can be seen that only the easiest possible separations are al-
ways carried out. This means that, in the first separation steps,
product mixtures are obtained. Only the last step yields pure
products.
This general arrangement is particularly advantageous with
respect to thermodynamics. The thermodynamic process of dis-
tillative separation consists in the removal of the entropy of mix-
ing of the feed stream by exergy (heating in the reboiler at a high
temperature and cooling in the condenser at a low temperature).
This means that, in the distillation process, additional mixing
must be avoided as far as possible by an appropriate design of
the distillation column. The undesirable additional mixing
would result in excess entropy to be removed and would require
more exergy or more energy for the separation.
Hints for an appropriate design and operation of a distillation
column can be obtained from an exergetic analysis of distillative
separation. When the most important sources of exergy losses
are strictly avoided, the general arrangement for the separation,
shown in Fig. 11, is obtained.
The distillation column with a vertical partition in the centre
section of the distillation column can be regarded as a consistent
- B
- c
P
I D
apparative simplification of this thermodynamically advanta-
geous separation scheme. The parallel columns are combined
into one single column. The important feature of minimization
of the entropy of mixing at the feed plate is preserved.
In conventional distillation arrangements, the medium boiling
components are forced in only one direction, either to the top
or to the bottom of the distillation column. In this way, the con-
centration of the medium boiling components in the region of
the feed tray is increased to values in excess of the feed concen-
tration. This leads to a considerable increase in the entropy of
mixing at the feed inlet. In some cases, the additional mixing
entropy at the inlet amounts to 30% of that to be removed from
the feed by distillation.
On the other hand, the distillation column with a vertical parti-
tion permits the medium boiling components to distill both to
the upper and lower ends of the partition and to recombine in
the outlet section. Excessive concentrations in the region of the
feed plate can thus be avoided (see Fig. 8).
In the simplest case, the distillation column with a vertical parti-
tion is operated without an intermediate reboiler or condenser.
Compared to the general scheme, this means that only the re-
boiler and condenser of the last column are used while the heat
exchangers of the preceding columns are eliminated. These co-
lumns are supplied by partial liquid and vapour flows from the
subsequent columns.
The advantage of apparative simplification, on the other hand,
implies the thermodynamic disadvantage that the intermediate
input and removal of heat at smaller temperature differences
cannot be effected. This leads to exergy losses. In addition, the
possibilities of heat transfer to other units are reduced. Thus,
in every case, a compromise must be made between lower in-
vestment costs and heat integration.
5 Control Behaviour
The control behaviour of a distillation column with a vertical
partition corresponds to that of a conventional side outlet
column. The usual control strategies can be applied.
With regard to control of the side outflow, the column with ver-
tical partition has advantages because, in the outlet section,
there are no resultant light and heavy component streams. In this
case, disturbances exert a smaller influence on the temperature
profile in the outlet section. Temperature measurements of the
outflow in the outlet section are less affected and the control ob-
jective is better achieved.
As a rule, no special measures are required for the distribution
of vapour flow at the lower end of the partition since a rough
distribution is determined by the cross-section portions of the
feed and discharge sections.
Simulation calculations show an astonishingly low sensitivity of
this distillation column to variations in vapour distribution. In
most cases, the distribution ratios can be varied from 2: 1 to 1 :2 Fig. 11. General structure.
98 Chem. Eng. Technol. 10 (1987) 92-98
with only minor disadvantages with respect to energy consump-
tion and separation performance. The reason for this is that this
variation affects only the mass ratio of the medium boiling com-
ponent which is distilled from the feed section to the outlet sec-
tion via the upper or the lower end of the vertical partition. The
purity of the outflow is not directly affected.
Variations in the distribution ratio of the liquid at the upper end
of the vertical partition exert a larger influence. It is appropriate
to set the optimum ratio, which can be found by simulation cal-
culations, at least roughly in the range of about f 20 % . A fixed
ratio is sufficient. Control of the distribution ratio of the liquid
is not necessary. In general, the outlet section is supplied with
more liquid than the feed section.
The distribution of the liquid at the upper end of the vertical par-
tition can also compensate for any undesirably large deviations
in the vapour distribution ratio.
6 Applications
Distillation columns with vertical partitions are capable of
separating a feed mixture into 3 or 4 pure fractions. This is ad-
vantageous especially for heat sensitive components. These can
be separated from their higher and lower boiling impurities at
a lower thermal stress. In this way, better product qualities were
obtained in production columns.
The control behaviour proved similar or better than that in con-
ventional distillation columns.
Investment costs are lower than for alternative column arrange-
ments and less space is required.
Because of advantageous thermodynamic properties, the energy
consumption is low. Typical energy savings, compared to alter-
native distillation arrangements, are 20 to 35 %. When inter-
mediate heaters or coolers are applied, the columns provide
favourable conditions for heat integration.
Received: 8. August 1986 [CET 101
References
[l ] US Patent 2 295 256 (1942).
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(MOSCOW) NO. 11, pp. 65 - 68.
[4] Miiller, W., Wiss. Z. Tech. Hochsch. Chem. Carl Schorlemmer
Leuna-Merseburg 14 (1972) No. 1, pp. 60-65.
[5] Stupin, W., Lockhart, F., Chem. Eng Prog. 68 (1972) No. 10, pp.
[6] Miiller, W., Chem. Tech. 26Leipzig (1974) No. 1, pp. 16-20.
[7] Wozny, G., J ohannisbauer, W., J eromin, L., Ger. Chem. Eng 9
(1986) NO. 6, pp. 353-361.
[8] Elaahl, A., Luyben, W., Znd. Eng Chem., Process Des. Dev. (1983)
NO. 22, pp. 80-86.
[9] Cheng, H., Luyben, W., Znd. Eng Chem., Process Des. Dev. (1985)
NO. 24, pp. 707 - 713.
[lo] Alatigi, I., Luyben, W., Znd. Eng Chem., Process Des. Dev. (1985)
NO. 24, pp. 500-506.
[l l ] US Patent 2 471 134 (1949).
71 -72.