Factors Controlling Efficiency and Capacity of

Sieve-Pla te Extraction Towers

CYRUS PYLE, A. P. COLEURN', AND H. R . D U F F E Y ~
E N Q l N E E R l N G RESEARCH LABORATORY-EN5lNEERING DEPARTMENT,
E. I . D U P O N T DE N E M O U R S e COMPANY, INC., WILMINOTON. DEL.

T h e factors influencing the efficiency and capacity of

sieve-plate extraction towers have been stud ed in a small
glass extraction tower, using the system ethyl ether-
acetic acid-water. It has been found t h a t a t normal oper-
ating rates there i s little effect of hole size, within limits,
on efficiency whereas a higher percentage of free area i s
more advantageous than a lower percentage. Higher
capacities are obtained when settling time of the two
phases is rapid, and when down pipes are flush with the
surface of the plate from which they drop.

I N T H E manufacture of cellulose acetate. one of the most feed entered the column through the center supporting post
I important steps in $he process is the recokery of acetic acid and was fed to the top plate. The down pipes (or riser pipes) rose
1 inch above the plate to which they were attached, and extended
from aqueous mixtures containing about 25% acid by weight. to within 1 inch of the plate below. The spaces between plates
Most manufacturers carry out the initial phase of the recovery by and column wall were sealed by means of rubber tubing held in
the uroces of liauid-liauid extraction. When large volumes of place by copper expansion rings. Rubber gaskets were used be-
liquid must be iandled continuously and when k g h recovery ~ $ & ~in$ the$ ~ top
g ~ section
~ ~ ~ o fofl tthe::kt dcolumn ~ r ~ ~ ~ $ f$
d " , " to~ assist $ ~2 e:
,
efficiencies are desired, it is believed that plate-type towers are in breaking emul-
most satisfactory, and sieve-plate towers in particular seem to sions of extract which were hard to separate. This separator was
have marked advantages ( 4 ) . Although sieve extractors have not employed in all r u m
been used for many years, designs for these extractors appear to Connections were arranged for sampling the feed ether, feed
acid saturated with ether, exit ether, and exit water. Ther-
have been evolved from experience and judgment, without benefit mometer wells were provided for determining the temperatures
of detailed experimental investigation. Because of the increasing of feed ether, feed acid, exit ether. and exit water.
utility of extraction processes, Five setsof interchangeable
a study of the factors con- plates were used, three sets
having a constant hole size
trolling the efficiency and (0.110 inch) and varyingper-
capacity of sieve-plate extrac- EXIT ETHER centage of hole area (1.77 to
tors was inaugurated. This
study was undertsken several
years ago on a plant actually COPPER-
PLATE
-(I 5.05%) and two other sets
having a varying hole size
(0.0635 to 0.2010 inch) with
a constant hole area (3.34%).
recovering acetic acid by ex- The details of the plate con-
traction. The system ethyl struction are given in Table
ether-acetic acid-water was T I E ROD-
I. The drilled area of the
plate amounted to 75.9% of
chosen for test purposes be- RINOS
the column area. For the
cause all feed streams were runs in which the plate spac-
conveniently available. ing was 2.5 inches, the down
pipes were shortened by 2
inches, so that the space be-
EXPERIMENTAL STUDY tween the top of the plate
below and the bottom of the
Apparatus. Details of con- down pipe was approximately
struction of the experimental the same as for the 4.62-
inch plate spacing ( 1 inch).
extraction column are shown
in Figure 1. PLATES Equilibrium Data. This
study was undertaken pri-
The ether entered the col- marily to find out how to de-
umn through twelve 0.25- sign plant columns. The
inch holes in the bottom of
a distributing ring and aased feed mixture is not one of two
through about 5 incles of pure components, acid and
water phase before reachin water, but does contain other
the bottom plate. The acii materials which probably
1 Present address, University of
F E E D E T H E R __f \ ' E X I T WATER influence the distribution
Delaware, Newark, Del. coefficient. For this reason
8 Preaent address, Chemicals F E E D ACID
Department, The Quaker Oats
distribution coefficients were
Company, Chicago, 111. Figure 1. Semiworks Glass Extraction Column measured on the liquids
1042
June 1950 INDUSTRIAL AND ENGINEERING CHEMISTRY 1043
e
Table 1. Plate Speclfloations

0 110-inoh holes on i/,-inch centers -

(4 plates per set and 20 plates total)
a

--
No 1 e l
No' 2 0'110-inch holes on Wis-inch canters = -I
No: 3 0:llO-inch holes on 'a/:r-inch centers a
No 4 0 201-inch holes on '/:*-inch centers
No: 5 0.'0635-inch holes on 9/ta-inch centers = 2
c
W

actually employed. The standard method of expressing

.s
0

0
acetic acid concentrations at the plant was as grams of acetic
*
2
acid per 100 ml. of solution. This standard was adhered to *
u
for this study and the distribution coefficients expressed as
ui
grams of acetic acid per 100 ml. of water phase divided by grams al
of acetic acid per 100 ml. of ether phase at 20" C. are shown in
Table 11. Although these coefficients are lower than reported in
the literature for pure components, they n-ere used as a basis for
the equilibrium data, because they were obtained under condi- 0 4 8 12 eo z4
OMS. ACETIC ACID/ IOOCC. W l T t R LAYER
tions presumably similar to those encountered a t the plant. Had
the more recently obtained equilibrium data of Major and Figure 2. Typioal Extractiorr Diagram
Swenson (6)been employed, the calculated plate efficiencieswould Plate ef?lciency, EOB, 0.28
have been slightly higher than those reported herein. Run 24A

The results of this study are shown graphically in Figures 3 to

Table II. Equilibrium Data a t 20" C. 8 and the experimental data are included 88 Table 111. The
Distribution Coefficient results may logically be divided into plate efficiency measure-
G. Acetic Acid/lOO G. Acetic Acid/lbO G . ACid/1m MI*Ether LiYer
M1. Ether Layer MI. Water Layer G. Aoid/100 Ml. Water Layer ments and capacity measurements.
0.225 0.5 0.450
0.460 1.o 0.459
0.954 2.0 0.477 EFFICIENCY TESTS
2.035 4.0 0.509
3.245 6.0 0.541 Reproducibility. The first three runs were carried out in
4.590 8.0 0.574
6.10 10.0 0.610 duplicate in order to determine how nearly reproducible the re-
7.80 k2.0 0.649
9.65 14.0 0.689 sults were. I t was observed that the difference between the
11.78 16.0 0.737
14-20 18.0 0,788 efficiencies at the two lower rates was less than 1%,whereas the
16.9 20.0 0.846 difference between the efficiencies a t the high rates waa 2%. I t
20.0 22.0 0.911
is believed that,all efficiencies could be reproduced with a differ-
ence of about 2% in the check run in each case.
Effect of Per Cent Free Area. These testa were made on
Method of Calculation. The two most promising methods plates having 0.110-inch holes, I-inch overflow pipes, and 4.62-
for calculation of plate efficiencies in extraction appear to be: inch plate spacing. The results are shown in Figure 3. The
use of the triangular diagram as described by Hunter and Nash ( 6 ) efficiencies are all near 30%, but there is a tendency at high rates
and the absorption process method described by Sherwood (7). for the plate with the high percentage of free area to give higher
Careful study of both methods led to the choice of a combination efficiencies. It is believed that a minimum depth of 0.25 inch of
of the two as suitable for the purpose.
The method actually used in the calculation of the results of the
experimental runs was as follows:
The absorption method was used with the concentrations
plotted in grama of acetic acid per 100 ml. of ether layer us. grams
of acetic acid per 100 ml. of water layer, as shown in Figure 2.
Curvature of the operating line was determined by converting E.. Htt
terminal compositions to weight percentage, with use of the tri-
angular phase diagram] constructed in the same units, for com-
putation of various points on the operating line. Material bal-
ances based on uantitiea of acetic acid in and out of the system
were computed ?or most of the runs. In nearly all cases the inlet
quantity checked the amount leaving within 10%. Where ma- L
terial balances were obviously in error, the runs were not em- 2 s
plo ed for construction of the graphs. 5i
$he plate efficiency was determined by the Baker-Stockhardt e;
( I ) procedure of drawing on the equilibrium diagram a series of Y
t C
*
curves, each representing a definite percentage of the driving force ti'
and by stepping off four plates between the operating line and the
several "percentage" curves until the experimentally observed 'S
:a
separation was obtained by four ste s (when four plates were em- gg9oo mo sac 400 wo wo
ployed in the test). In each case afTowance was made for extrac-
CTMCR RATC, O A L . / l M R - ) ~ S o . IT.)
tion taking place between the distributor ring and the bottom
plate. The proper correction had previously been measured as a
unction of ether flow rate, and was found to be 60% of a theoreti- Flgure 3. Effeot of Per Cent Free Area
cal plate at an ether rate of 550 gallons/(hour)(sq. foot) and 43% G8llcns of ether par p8llon of feed acid, 8pproxi-
of a theoretical plate a t the lower ether rates. A graph illustrating rnably 2.4
PI8te spacln 4 62 Inches
run 24A is shown as Figure 2. Hole size, 0.RO inch
1044 INDUSTRIAL A N D ENGINEERING CHEMISTRY Vol. 42, No. 6

V t . 0
? k Y
m - m

0 0 0

., .. . . . , .. ,. .. .. .. .. .. .. .. .. .. .. ..
lune 19% I N D U S T R I A L A N D E N G I N E E R I N G CHEMISTRY
ether below the plate is desirable to ensure good distribution of the
ether and that the maximum depth of ether below the plate
should be 0.75 to 1 inch in order to avoid too great a reduction in
the depth of water layer through which the ether passes.
Effect of Hole Size. Using plates with 3.34% free area,
there was little effect of hole size on plate efficiency between the
limits 0.0635 and 0.201 inch, although the smaller holes (which
gave a greater depth of ether below the plate) show a higher
efficiency (Figure 4). It is possible that with the 0.201-inch holes,
the drops were not as large as 0.2 inch in diameter, inasmuch as
the effect of water and ether flow may be such as to reduce the
sise of the drops.
<I I I I I / I / I I ! I ! ! / ! I ! ! ! !! ! I
P
f ao
Y
W Y
m .
$5 * to 13 inches as found by Colburn and Welsh (8). The water
a -
=P
;:
YO
I
=B
'100 PO0 BOO 400 600
STWLR RATE. ~ A b , / l W R . l ~ 8 0FTI
.
Figure 4. Effect of Hole SIze
OIllon8 of ether per g8llon of feed rold, 8pproxl-
mately 2.4
Plate epaoln 4.62 Inches
F m area, 3.&%
Because a large number of small holes is required to give the
dame percentage of free area and these holes are more easily
clogged, it is not desirable to use holes that are too small in diam-
eter,
Effect of Plate Spacing. The effect of plate spacing on plate
efficiency is shown in Figure 5. While the plate efficiency in-
creases with increasing plate spacing, the separating effect per
foot of height decreases, so that a somewhat taller tower would be
required for larger plate spacings. The economic plate spacing is
obtained by balancing the increased cost of shell, pumping, and
building, if one is employed, against the reduced cost of the platee.
Although no calculations have been made, it seems probable that
the economic plate spacing for this mixture would be between 4
and 8 inches. For large-diameter towers the necessary clearance
between the bottom of the down pipe and the plate below fixes
the minimum plate spacing a t about 5 inches. In such towers it
would probably be desirable to have a somewhat larger plate
spacing, say 7 or 8 inches.
For a plate column, plotting (1 -Eo#)against depth of water
layer above the plate on semilog paper should give a straight
line if the effectiveness of contact is proportional to depth.
Figure 6 shows that an approximately straight line is obtained.
This indicates that the water layer on the plate is mixed. Visual
observation also indicated that there was considerable mixing of
the water layer on the plate. For large-diameter columns with
small plate spacings and with cross flow of the continuous layer,
each unit must act as a cross-flow plate rather than as a counter-
current scrubber. As in distillation, some increase in plate
efficiency will be obtained because of the varying liquid composi-
tion across the plate. For low plate efficiencies, however, this
increase is relatively small.
Effect of Ratio of Ether to Acid Flow Rates. The effect of
ratio of ether to acid on plate efficiency is shown in Figure 7. It
will be noted that the efficiency decreases as the ratio of ether to
1045
acid increases. This decrease is believed to be largely due to the
greater effect of water film resistance at higher values of mWE/Ww
Thus, there are resistances to mass transfer in both the ether and
water layers. Analogously to distillation, as employed by Gkr-
ster, Colburn, Bonnott, and Carmody (a),the plate efficiency can
be related to the separate film resistances as follows:
where Nb = number of transfer units in ether phase alone, N W =
number of transfer units in water phase alone and m = dCe/dCa.
Although the values of Ne and N W are not independent of the
flow rates, WE and Ww, they can often be so considered as a first
approximation. When EOE< 0.1, the left-hand side of the above
equation can be approximated closely by the term, ~ / E o EBe- .
cause the data in Figure 7 are plotted according to Equation l, it
is possible to obtain from the intercept and slope of a straight
line rough values gf N E = 0.55 and Nw = 2.5. For a vertical
path of travel of the ether drops through the water layer of about
4 inches, the value of HE becomes 7.3 inches, which compares
with values of height of a transfer unit, for the discontinuous
phase for isobutyl alcohol in water in a packed column, of from 7
layer flows horizontally a distance of approximately 8 inches, so
the value of Hw (horizontal) is about 3.2 inches, which appears
reasonable.
More precise values of the separate film resistanges would have
600
to be determined individually by some technique like that used by
Colburn and Welsh (4).
80
70
# 60
0
2 so
i
40
W
0
E
W
30
*
i 10
0,
0 P 4 6 e IO I0 H I6 IO 00 ee
RATE SPACINO, IN
Figure 5. Effect of Plate Spacing
G8llOnl of ether per g8iion of feed acid, approrl-
mately 2.4
Hole8, 0,110 Inch on 0.6-inch centers
Fmearea 3.34%
Ether rat:, 560 gsllonr/(hour) (sq. foot)
Effect of Feed Concentration. The high feed-acid concen-
trations of about 25% gave better efficiencies, around 0.30, than
low feed concentration of about 0.5% acetic acid, where the frac-
tional efficiency was around 0.20. However, a small increase in
efficiency with increasing concentration for this system would be
predicted on the basis of Equation 1. For very dilute solutions of
acetic acid, rn is 0.45, whereas the average value for higher con-
centration is about 1.1. Inasmuch as WE/WWis held approxi-
mately constant at 2.38, the value of mWE/Ww is about 1.07 for
dilute solutions and 2.62 for the more concentrated solutions.
Reference to Figure 7 indicates that the plate efficiency corre-
sponding to mWE/Ww = 1.07 would be expected to be about 0.36.
The explanation of the very low efficiencies observed is not
readily apparent. They may be due to systematic errors in
analysis, to errors in equilibrium data, or to factors that influence
drop size, such as interfacial tension. Continued investigation in
the field of extraction, however, has led to the postulation of
another theory. It has been observed that better plate efficiencies
are obtained with those systems which exhibit a fair degree of
 1046 I N D U S T R I A L A N D E N G I N E E R I N G CHEMISTRY Vol. 42, No. 6

mutual solubility between phases. Extracting out of water into 50 ml. of ether were shaken in a 100-ml. stoppered graduate. The
hydrocarbons such aa benzene usually results in poor efficiencies time of separation of the ether and water layers bas measured
even with plate arrangements similar to those used for this study. with a stop watch. A settling time of about 30 seconds or less is
As the concentration of acid in the feed solution is decreased, the considered satisfactory.
mutual phaae solubility diminishes and the interfacial tension in- For an ether-acid ratio of 2.4 gallons of ether per gallon of feed
creases, which may be the cause of the results observed. acid, the maximum capacities obtained are shown in Table IV.
In the first three cases, with feed acid of satisfactory settling
characteristics, the capacity was limited by a build-up of ether
1.0
0.9
below the bottom plate. In the last two, with feed acid of un-
ae satisfactory settling characteristics, an emulsion of ether and
0. T water was carried out with the extract. As shown in Table IV, an
0.6 emulsion separating section (Figure 1) above the top plate as-
0.5 sisted in breaking extract emulsions, which were hard to separate,
3 a4 in several runs.
-
I When the column is operated properly, the controlling ether-
water interface is held in the space above the top plate. The loca-
tion of the interfaces below each plate is determined by the
ether flow rate. .4n overflow pipe extending above the plate from
which it drops is not necessary and decreases the capacity of the
column. Down pipes should be cut off flush with the top of the
plate but should extend sufficiently far below the plate to be
sealed in the aqueous layer.
It was observed on operating this tower that a layer of ether
DEPTH OF WATER LbYER, IH. builds up under each plate. The depth of this layer IS a function
Figure 6. Effect of Depth of Water Layer of ether flow rate. The pressure loss of the disperse phase in
Gdbns of ether per gallon of feed acid, approxi-
passing through the holes of a sieve-plate extraction column may
mately 2.4 be calculated by the orifice equation. The orifice constant, C, is a
Holes, 0.110 inch on 0.5-inch centers function of Reynolds number, as shown in Figure 8. In this form
Free area 3 34%
Ether rat;, 660 gaiions/(hour) (sq. foot)

Effect of Dispersing Water through Holes. Several runs

Table IV. Capacity of Sieve-Plate Column
(17A, HA, 19A) were made with the plates inverted and levels
Distance
maintained 80 that the feed acid ran down through the holes, and between
the ether paased up through the riser pipes. It was concluded that Top of
Emulsion Overflow Max.
this method of operation was about equivalent to the use of five Separating Pipe and Ether
% Settling Section Next Plate Rate,
plates, and efficiencies were computed on that basis. When Free Time, above Above, Gal./(Hr.)
efficiencieswere calculated on the basis of change of solute concen- Area Sec. Top Plate 1nche.j (Sq. Ft.) j
tration in the ether phase, these runs gave efficiencies only about 1.77 26 Yes 1.62 385
1.77 31 No 3.62 550
60% as great as those obtained when ether was run through the 3.34 27 Yes 3.62 690
3.34 88 N O 3.62 199
holes. Because, however, the feed acid was the dispersed phase 3.34 78 Yes 3.62 317
for these particular runs, efficiencies were also calculated on the
basis of change in solute concentration in feed acid or water phase.
These efficiencies were about 75% higher than when calculated on
the basis of change in concentration of ether phase. I t was ob-
served that when the feed acid or water phase was dispersed, it ran
through the holes in streams while the ether went through in the
form of droplets. As a general rule, the phase that gives the
largest surface area should be run through the holes. This will
ordinarily be the phase having the greater volumetric flow rate.
Effect of Height of Overflow Pipe. In Runs 29 and 30, an
overflow pipe extending 3 inches above the plate was used with a
4.62-inch plate spacing. These results should be compared with
runs 8 and 9. Although the efficiency is slightly higher for the tall
down pipe, the capacity is considerably reduced. The effect of
down-pipe height on efficiency should be negligible for a plate
3 feet or more in diameter utilizing cross flow.

CAPACITY MEASUREMENTS
Capacity. The capacity of a sieve-plate column may be
limited by the pressure drop required to pass the liquids or by the 0 I 2 3 4
time required for separating the emulsion of the two phases. In
the fist caae, the disperse phase accumulates in the column until
it finally overflows with the continuous phase. When the emul- rn
sion does not completely separate, some of each phase is carried
out with the other. Various impurities often contained in the
feed sometimes influence the settling time of the two phases. A Figure 7. Effect of mWE/Ww
simple qualitative test for ease of separation was made for each Holes, 0,110 inch on 0. inch centen
Plate spacing 4.62 In&
run as follows. Forty milliliters of feed acid, 10 ml.of water, and Ether rate, 3r7 gaiions/(hour)(sq. foot)
June 1950 INDUSTRIAL A N D ENGINEERING CHEMISTRY 1047

(Equation a). The calculated and experimental results are com-

pared in Table V.
The pressure loss through the holes was taken aa equivalent to
the average head of ether under the plate minus the head of
ether equivalent to the pressure loss through the downpipe.
Figure 8 shows a plot of the orifice coefficients va. Reynolds
number. The solid line gives the best correlation of the data as
measured. The Reynolds numbers shown range between 80 and
3000 and thus cover the viscous flow region and the transition
region, as well as the turbulent flow region. For this range, the
uncertainty in orifice coefficients is fairly large, and hence ade-
40 too 1000 4000 quate factors of safety should be used in calculating the capacity
REYWOLOS NUMBER Re *
8
of a dieve-plate column for extraction.

ACKNOWLEDGMENT

The authors wish to take this opportunity to acknowledge the

6 S . O d *re% IhE3%%1.. able assistance and advice of the technical and engineering staffs
of the Du Pont Rayon Department plant at Waynesboro, Va.,
Figure 8. Variation of Orlfloe Coefficient with
Reynolds Number during this study.

NOMENCLATURE
C also corrects for the pressure drop to overcome the surface ten-
sion between the droplet and the periphery of the hole. The equa- c = concentration of solute
tion that gives the inches of continuous phase displaced in order C = orifice coefficient
to provide the pressure drop through the holes is d = differential operator
D = orifice diameter, feet
E = fractional plate efficiency
g = acceleration due to gravity, 32.2 feet/(sec.)(sec.)
hw 5 depth of continuous phase displaced by dicontinuous
phase to supply pressure loss through down pipe, inches
The pressure loss of the continuous phase in passing through the h(p = depth of continuous phase displaced by discontinuous
down pipes may be calculated by assuming that it is due to one phase to supply pressure loss through sieve plate, inches
expansion and one contraction. For cases where the down-pipe H = height of a transfer unit, inches
area is less than 5% of the column cross section, the combined m = slope of equilibrium line, dcE/dcw
expansion and contraction losses are approximately 1.6 velocity N = number of transfer units
heads. The equation that gives the inches of continuous phase S = cross-sectional area of column, sq. feet
displaced in order to provide the pressure drop through the down SA = erosbsectional area of holes, sq. feet
pipe is as follows:

0.28 2 u% (3)
Uh -
Ud = velocity of continuous phase through down pipe, feet/sec.
velocity of discontinuous phase through the holes, feet/sec
W = rate of flow, volumetric units
hw = 1 2 ( g ) ( y ) p = liquid density, lb./cu. foot
Ap = difference in density between heavy phase and light phase,
The total depth of the discontinyous phase required to produce
+
the desired flow of liquids is then hw hw. This depth should be
Ib./cu. foot
~r = viscosity of liquid, Ib./(sec.)(foot)
large enough so that there will be no tendency for channeling of
the two phases, but not so great that it will seriously reduce the Subscripts
height of continuous phase through which the discontinuous
phase rises. It is possible to operate an extraction column so that d refers to down pipe
the general column interface is near the top of the column, near E designates ether phase (usually &continuous phase)
the bottom, or in between, or to make either phase the discon- h refers to holes in sieve plate
tinuous one. In general, if the drop sizes obtained are of about OE = over-all ether concentration basis
equal diameter, the phase having the largest volume should be OW = over-all water concentration basis
dispersed so that the maximum interfacial area will be exposed. W designates water phase, usually continuous phase
The interfacial level should then be adjusted so that the con-
tinuous phase will occupy as much of the column as is practicable. LITERATURE CITED
The data on head of ether below the plate for runs 20, 21, 22,
(1) Baker, T.,and Stockhardt, J. S., IND.ENQ.CHEM.,22, 376-7
and 24 (ether flow rate constant, varying water flow) were used to (1930).
check the calculation of the pressure lossthrough the down pipes (2)Colburn, A. P.,and Welsh, D. G., Tram. Am. Inst. Chem. Engm.,
38, 178-202 (1942).
(3) Gerater, J. A,, Colburn, A. P., Bonnett, W. F., and Carmody.
T. W., Chem. Eng. Progrese, 45,716-24 (1949).
Table V. Head of Ether below Plate (4) Harrington, P. J. (to Standard Oil Development Co.), U. S.
Patent 1,943,822(Jan. 16, 1934); Reissue 21,725 (Feb. 25,
W8br Depth Ether below Plate 1941).
~ ~ l , / D~ :{&her
Rat0 througt 80wn
to Su PI Pressure
Pipe, Loas
Inch ( 5 ) Hunter, T. G., and Naah, A. W., J . SOC.Chem. Id.,
53, 95-102T
bekw Plate, Calcd. Experi- (1934).
Run Inch by eq. mental (6) Major, C. J., and Swenson, 0. J., IND.ENQ.CHEM.,38, 834-6
(1946).
(7) Sherwood, T. K.,Absorption and Extraction, New York,
McGraw-Hill Book Co.,1937.
RECEIVED
November 30, 1949.