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PERFORMANCE.

OF PACKED
COLUMNS

I. Total, Static, and Operating Holdups


H. L. Shulman, C. F. Ullrich, and N. Wells
Clarkson College of Technology, Potsdam, New York

Total and static holdups have been measured for %-, and 1-in. ceramic Berl
saddles, %-, I-, and I%-in. ceramic Raschig rings, and I-in. carbon Raschig rings
with air rates from 100 to 1,000 lbJ(hr.1 (sq. ft.) and water rates from 1,ooO
to 10,000 lb./(hr.) (sq. ft.).
The holdup measurements and motion picture observations of the flow of dye
solutions through packings provide an explanation for the great differences observed
when gas-phase mass transfer rates are measured by absorption and vaporization
methods. If the effective interfacial area for vaporization is assumed to be pro-
portional to total holdup and the area for absorption is assumed proportional to
operating holdup, the ratio of the two mass transfer rates should be equal to the
ratio of the two holdups.
The departure from equality of the two ratios can be explained by the observation
that the static holdup is displaced slowly, resulting in additional effective area for
absorption over that expected from the operating holdup alone.

In recent years investigations of literature(8,ll). The total holdup, 19,ZZ) have measured or estimated
mass, heat, and momentum trans- h,, defined as the total liquid in the liquid holdups, and two extensive
fer in fluid-soild systems have in- packing under operating conditions, studies have been reported by
dicated that the free space, or void is expressed as cubic feet of liquid .
Elgin and coworkers ( 3 , l l ) Un-
fraction, E , is an important variable per cubic foot of packing. The fortunately the previous investi-
in the correlation of data(l,.4,5, static holdup, h,, as used in this gations have dealt with operating
6,10,12). To apply these findings work is defined as the liquid in the holdups almost exclusively and no
t o an analysis of more complex packing which does not drain from investigation has been reported of
systems such as those occurring in the packing when the liquid supply the t h r e e types of liquid holdup in
packed absorption and distillation to the column is discontinued and packings for which extensive mass
columns, one must know the total is also expressed as cubic feet of transfer data are available, namely,
liquid holdup to determine the void liquid per cubic foot of packing. Raschig rings and Berl saddles.
fraction available for gas flow un- The operating holdup, h,, defined The object of the present work
der operating conditions. A knowl- as the difference between the total is the determination of the three
edge of liquid holdups is also of and static holdups, represents the types of liquid holdup f o r 0.5-, LO-,
interest in the study of batch dis- liquid which will drain from the and 1.5-in. unglazed white porcelain
tillation and effective interfacial packing and is also a measure of Raschig rings, 0.5-, and 1.0-in. un-
areas for diffusional operations em- the liquid flowing through the pack- glazed white porcelain Berl sad-
ploying packed columns. ing when the column is in opera- dles, and 1.0-in. carbon Raschig
Three different types of liquid tion. The relation between the three rings. These data will be used to
holdup have been discussed in the holdups is given by explain the differences observed in
gas-phase mass transfer rates when
Additional tabular material may be obtained
from the Photoduplication Service, American
ht = h, + h,. vaporization and absorption tech-
Documentation Institute, Library of Congress, niques are used. In P a r t I1 of this
Washington 25 D.C., as document 4565 for
$1.25 for micrdfilm or photoprints. Several investigators (2,9,13,15, paper the data will be applied to

Vol. 1, No. 2 A.1.Ch.E. Journal Page 247


TABLEl.-CHARACTERISTICS O F PACKING USED FOR HOLDUPMEASUREMENTS
Type Raschig rings Berl saddles Raschig rings
Manufacturer (U. S. Stoneware Co.) (Maurice A. Knight Co.) (National Carbon Co )
Material Unglazed white porcelain Unglazed white porcelain Carbon
Nominal size, in.. ................ 0.5 1.0 1.5 0.5 1.0 1.o
Void fraction, dry.. .............. 0.605 0.726 0.715 0.660 0.695 0.700
Specificgravity, dry.. ............ 2.38 2.41 2.36 2.36 2.44 1.57
Pieces/cu. f t .................... 10,900 1,370 430 15,000 1,810 1,470
Surface area, sq. ft./cu. it.. . . . . . . . 116 58.5 40.9 133 62.6 62.7
Surface area/piece, sq. ft.. . . . . . . 0.0 1063 0.0427 0.0952 0.00888 0.0346 0.0427
Diameter of equivalent sphere, ft.. 0.0582 0.1167 0.1740 0.0532 0.1050 0.1167

the problem of separating t h e volu- and DeGouff(l8) except for minor packing, consisted of eight arms ex-
metric mass t r a n s f e r coefficients modifications, which will be discussed. tending radially from a special fitting
(k,a and k,a) into their com- A water tank and pump were in- and was 9 in. in diameter. I t had a
stalled to permit adjustmefit of water total of 160 0.1-in. holes evenly spaced
ponents, t h e effective interfacial temperature and recycling of water. in three rows on four alternate arms
area, a, and t h e mass t r a n s f e r Two calibrated rotameters were in- and in a single row on the remaining
coefficients, kG and kL. stalled to replace the orifice meters arms. Several holes were plugged with
previously used to meter the air. The solder as the result of tests made to
EQUIPMENT 10-in.-diam. by 36-in. packed glass col- ensure uniform distribution of liquid
umn was arranged so that it might be for the liquid rates employed.
The equipment used for these weighed with its contents while in
studies, shown schematically in Fig- operation. This was done by sup- PROCEDURE
ure 1, is the same as that described in porting the column by means of four Preliminary tests made possible
detail in a recent paper by Shulman 0.25-in. steel rods connected at the the establishment of a procedure
top by a yoke and at the bottom by which gave reproducible data even
a steel ring on which the glass col- when the column was emptied and
umn and the four legs of the packing repacked. When the column was
support plate rested. In operation the packed with dry packing and the

DIAGRAM
FIG.1. SCHEMATIC OF
1 SCALE
glass column was suspended in air
except for a few inches a t the bot-
tom which were immersed in a water
seal. The column and its contents
were counterbalanced by weights on
a pan connected t o the yoke a t the
top of the column by the lever arm
and knife edges obtained from a
platform scale. The pan of weights
rested in turn on the pan of a 20-kg.-
capacity platform scale which could
water rate was set at a fixed value,
the total holdup was found to in-
crease with time until a constaxt
equilibrium value was reached. The
same equilibrium value could he
reached in a much shorter time by
supplying water a t a very high rate
for a short time, to wet the packing
thoroughly, and then running a t the
desired rate. Figure 2 shows the total
holdup for 1.0-in. Berl saddles as a
APPARATUS. be read to within 1 g. The weighing function of time when the two meth-
system was capable of detecting a ods are employed. The effect of time
change in weight of the column of is even more noticeable with the
0.10, , , I , , , , , , , , I , ] , a s little a s 3 g., and it was therefore smaller packings, which have greater
possible to determine holdups to holdups. The buildup with time is
within 1% under the poorest con- believed to be due t o the gradual
ditions, Le., static-holdup determina- accumulation of water in pockets at
tions of the larger packings. The points of contact, inside rings, or on
column was open at me top to the portions of the surface which are not
atmosphere, and so a draft gauge continually covered by flowing liquid.
employed for reading the pressure at The splashing of liquid as i t falls
the base of the column measured the from one piece of packing t o another
pressure drop across the packing. and the random motion of the mov-
- 0 D
. (PO 110 1.0 300
The weighings were corrected for ing liquid over the surface of the
m.
TWE.
the buoyancy effect of the portion of packing not only causes this gradual
FIG. 2. TOTALHOLDUPVS. TIME AT the column in the water seal and for accumulation, until an equilibrium
L = 3 , 5 0 0 FOR 1.O-IN. BERL SADDLES. the upward thrust due to the pres- value is reached, but also results In
sure drop across the column, which a slow turnover of the liquid in what
was operated at all times with 28 might otherwise be stagnant pockets.
in. of packing using water a t 1 9 O to Observations based upon motion pic-
25°C. and saturated air of approxi- ture studies of the flow of dye solu-
mately the same temperature to pre- tions in packings will be discussed
vent vaporization of water. later in connection with the interpre-
The water distributor, which was tation of mass transfer data.
supported independently of the col- The total holdup was found to vary
umn approximately 1 / 2 in. above the with the density of the packed bed

TABLE2.-vARIATION OF HOLDUPWITH PACKING DENSITY


Packing: 1.0-in. porcelain Raschig rings
1.0 IN. PORCELAIN BERL 8100LES Liquid rate, lb./(hr.) (sq. ft.) 3,500 3,500 3,500 3,500 3.500 3,500
Gas rate, lb./(hr.) (sq. ft.) 0 0 300 300 600 6Ol.l
O b lb 20 20 20 a! : Void fraction, dry 0.726 0.709 0.726 0.709 0.726 0.709
TIME, YUI.
Pieces/cu. ft., N 1,370 1,460 1,370 1,460 1,370 1,460
FIG.3. STATICHOLDUPvs. DRAINAGE h,, cu. ft./cu. ft. 0.0539 0.0567 0.0543 0.0574 0.0592 0.0724
TIME. ( h , i N )x lo6 3.94 3.88 3.96 3.93 4.32 4.96

Page 248 A.1.Ch.E. Journal June, 1955


i t I
o.a*o nbw. Lnmm-m

FIG.4. TOTALHOLDUP
I N 0.5- FIG.5. TOTALHOLDUP
I N 1.0- FIG.6. TOTALHOLDUP I N 1.5- FIG.7. TOTALHOLDUPI N 0.5-
IN. RASCHIGRINGS. IN. RASCHIGRINGS. I N . RASCHIGRINGS. IN. BERLSADDLES.

when the column was repacked sev-


eral times with the same packing.
For this reason the holdups reported
apply only t o packing with the char-
acteristics listed in Table 1. The
data in Table 2 show t h a t the total
holdups are approximately propor-
09 17rrrl_l
tional to the number of pieces of
packing per cubic foot for a given
packing. This observation provides
the simplest correction for packing
densities other than those listed in
Table 1.
To determine the static holdup, h,,
the water supply was cut off after
equilibrium conditions were reached,
the column was permitted to drain,
and a record of column weight vs.
time was made. Figure 3 illustrates
several drainage curves. It will he
0 01
100
I I I I I 7 l l
500
0 . O A S I A T C , LOllHRllSO FIB
1,000 u
0 01 100 Q . ON RITE. L B ~ I H R ~ ~ ~ ~ F T I

noticed that different packings re- FIG.8. TOTALHOLDUPI N 1.0- FIG.9. TOTALHOLDUPI N 1.0-
quire different lengths of time to IN. BERL SADDLES. IN. CARBON RINGS.
drain t o fairly constant weight.
On the basis of these preliminary
tests the following procedure was
adopted to ensure obtaining repro- brium was reached and data for a the static holdup, as will be shown
ducible data. The air was saturated drainage curve were recorded. It was later. At low liquid rates the total
and cooled to the temperature of the soon found that static holdup was
water in the tank. The weight of the holdup is almost independent of
independent of liquid and gas rates gas rate up to the loading point,
column and the dry packing was ob- when this procedure was employed,
tained and the packing was thorough- and so i t was not necessary to in-
but for higher liquid rates, espe-
ly wetted by setting the water rate vestigate the two ranges so thmough- cially for the smaller packings, and
up t o over 10,000 lb./ (hr.) (sq.ft.) for ly as for total holdup. for gas rates a t approximately the
a minimum of 1 hr. The water rate loading point the effect of gas rate
was then decreased to the rate to be in- cannot be ignored. This sudden in-
vestigated and the air rate was set at EXPERIMENTAL RESULTS crease in holdup as gas rate in-
100 1b.i (hr.) (sq.ft.) When the plat- Total Holdup. The data obtained creases causes the break in the
form scale indicated constant weight from the total‘ holdup measure- pressure-drop curve which has been
f o r more than 3 min. the readings of ments are plotted in Figures 4 t o taken as the definition of the load-
weight, pressure drop, and tempera- 9 f o r the six packings studied. The
ture were taken and the air rate was ing point. It is interesting t o note
increased to the next higher value. experimental points are shown, and t h a t the total holdups for 1.0-in
For each packing a series of runs was additional lines, obtained by in- carbon rings are greater than those
made in this fashion a t constant liquid terpolation, extrapolation, and cross f o r porcelain rings of the same
rates with increasing gas rates. The plotting, have been added t o make size. This difference is accounted
highest liquid rate, 10,000 lb./ (hr.) the plots more useful f o r estimat- for by the differences in static
(sq.ft.), was used first, and the gas ing total holdups in t h e ranges of holdup for the two packings; thus
rate was increased up to 1,000 lb./ gas and liquid rates covered. The the operating holdups are of the
(hr.) (sq.ft.) or the flooding point, loading-point line on each plot was same magnitude. Apparently the
whichever was reached first. The obtained from the data of Tillson
lowest liquid rate employed was 1,000 nature of the surfaces causes a
Ib./ (hr.) (sq.ft.) because i t was felt (21) f o r the same packing. The greater accumulation of semistag-
that good liquid distribution could shapes of the curves are quite simi- nant water in carbon than in por-
not be ensured a t lower rates. lar to those obtained by Elgin and celain; therefore the total and
F o r the static holdup tests a simi- Weiss ( 3 ) for operating holdups. static holdups reported here prob-
lar procedure was followed, but the This is t o be expected because the ably do not apply t o surfaces other
water supply was cut off when equili- two holdups differ by a constant, than ceramics similar to unglazed

Vol. 1, No. 2 A.1.Ch.E. Journal Page 249


TABLE3.-cONSTANTS FOR EMPIRICAL EQUATIONS
FOR TOTALAND STATIC HOLDUPS I' ':'"I I I I 1
Type of packing
material
Raschig rings
Porcelain Carbon
Saddles
Porcelain Equation
0.06 I- '\

CY 225x10-6 7.90X10-6 2.5OXlOJ 2


Y 0.965 0.706 0.965 3
6 0.00104 0.00250 0.00032 4
e 0.376 0.376 0.376 3
x 1.21 1.21 1.56 4
D,, 1.5-in. packing, ft. 0.174 0.178 0.155 2,3,4
D,, 2.0-in. packing, ft. 0.238 0.235 ...... 2,3,4

porcelain. The operating holdups, The lines on Figure 10 may be


however, seem to be independent used to estimate the static holdups
of the nature of the surface. of packings which have not been
For purposes of estimating the studied, or the following equation I \BERL SAODLES I
total holdups of rings and saddles f o r the lines may be used.
0.04 0.1
1 \ I
0 1
I
larger than those investigated in D,, EQUIVALENT DIAMETER, FT.
this study the following empirical -A
equations are recommended below
ha = 6Dp (4) FIG.10. STATIC
HOLDUP
OF PACKINGS.
the loading point: The constants, 6 and 1, are given
in Table 3.
The static holdup, which is a times. Thus Furnas and Bellinger
measure of the accumulated semi- ( 9 ) drained for 3 min., Jesser and
stagnant liquid, may play an im- Elgin(l1) for 10 min., and the
portant, but hitherto unknown, role authors f o r each packing to a con-
in the interpretation of mass trans- stant weight.
f e r studies in packing. It can easily Serious errors may be made in
be seen that this semistagnant estimating operating holdups by
The constants, a, y, and 0, are given liquid may be as effective as mov- using the methods presented by
in Table 3. These equations fit t h e ing liquid f o r vaporization work, previous investigators and adopted
experimental data very well up to but relatively ineffective for ab- by various texts and handbooks
loading and have been found use- sorption o r desorption operations. presenting these data. In the past
ful for estimating the holdups f o r A more detailed analysis of this it has been assumed that operating
2.0-in. rings and 1.5-in. saddles. problem is given in another section holdup is independent of gas rate
of this paper. up to the flooding point and so
Static Holdup. The experimental operating holdups were in many
data for the static holdups, sum- Operating Holdup. The operating cases measured a t zero gas rate.
marized in Table 4, show the hold- holdup is determined by taking the These data are then plotted as
ups to be independent of varying difference between the total and straight lines with logarithmic co-
gas and liquid rates. In Figure 10 the static holdups, as indicated by ordinates and extrapolated to very
the average value of static holdup Equation (1). The operating hold- high liquid rates approaching 100,-
f o r each packing is plotted vs. the ups derived from the present 000 Ib./ (hr.) (sq.ft.) in some cases.
equivalent diameter, D,. Although studies are in fair agreement with From Figures 4 t o 9 i t may be
an insufficient number of packings those obtained by previous investi- seen such a procedure would give
of each type have been studied to gators. The differences may be due erroneous operating holdups f o r all
give a good correlation of the data, to the use of different materials of but very low gas rates. It is recom-
it is evident that the static holdup construction of the packing, slight- mended that by means of Figures
is a function of the material of ly different packing dimensions, 4 to 10 and Equation (1) operat-
construction, the shape of the pack- differences in methods of packing ing holdups be determined at the
ing, and the size of the packing. the column, and different drainage actual gas and liquid rates em-
ployed.
TABLE4.-sUMMARY O F STATIC HOLDUP DATA
Static holdup, hs, cu. ft./cu. ft. APPLICATIONS TO MASS
Type of packing Raschig rings Berl saddles Raschig rings TRANSFER
material Unglazed porcelain Unglazed porcelain Carbon The primary reason f o r obtain-
Nominal size, in. 0.5 1.o 1.5 0.5 1.o 1.0 ing the holdup data was a desire
L G to determine the void fraction in
10,Ooo 0 0.0322 0.0150 0.00884 0.0315 0.0108 0.0358 packings under operating condi-
6,000 0 0.0328 0.0149 0.00895 0.0315 0.0110 0.0357 tions in order to separate the mass
3.500 0 0.0326 0.0150 0.00895 0.0319 0.0110 0.0359 transfer coefficients, kG and k,,
2,000 0 0.0326 0.0149 0.00899 0.0318 0.0111 0.3539
from the volumetric transfer coeffi-
1,000 0 0.0324 0.0148 0.00893 0.0318 0.0110 0.0359 cients, k,a and kLa. This work is
3,500 300 ..... ..... 0.00896 0.0318 reported in Part 11 and will not
3,500 300 ..... 0.0152 be discussed here.
3,500 600 ..... ..... 0.00867 Figure 2 emphasizes a fact
3,500 600 ..... 0.0151 which has been reported occasional-
6,000 200 0.0325
ly by investigators on the basis of
6,000 300 ..... ..... ...... ..... 0.0111 0.0359 their experience: i t is desirable to
Average h, 0.0325 0.0150 0.00890 0.0317 0.0110 0.0358 wet a packing thoroughly before

Page 250 A.1.Ch.E. Journal June, 1953


attempting to determine mass arranged so t h a t a concentrated the moving liquid.
transfer coefficients or the equiva- dye solution might be injected into This same line of reasoning can
lent. This is particularly important the water line several inches be- be extended to predict, in part, the
when small packings a r e employed fore the liquid distributor. With behavior of packed columns used
a t low liquid rates because i t the equipment in operation at a for absorption followed by a n irre-
may take several hours of opera- fixed liquid rate the dye solution versible chemical reaction such a s
tion under such conditions before was injected a t a continuous rate the absorption of ammonia in acid
the equilibrium total holdup is f o r a short period of time and then or of sulfur dioxide and chlorine
reached. Failure to observe this cut off. By use of 1.5-in. Raschig in alkali solutions. For example, if
precaution undoubtedly acoouats rings, i t was possible to observe ammonia is absorbed in water or
for widely scattered data, which the displacement of clear water by very dilute acid, the effective area
are difficult to interpret and im- dye solution and then the displace- will be that of the moving liquid.
possible t o reproduce. If in addi- ment of dye solution by clear water As the acid Concentration is in-
tion, poor liquid distribution and through the glass column. It was creased, the semistagnant liquid,
end effects a r e added to the usual found that a considerable portion even with its slow turnover, will
analytical problems i t is easy t o of the water was not displaced im- have an increasing capacity t o ab-
understand why the literature coil- mediately; is., there was no sharp sorb ammonia and at high enough
tains a considerable number of in- line of demarcation between water acid concentrations this liquid may
vestigations, the results of which and dye solution as dye was added be as effective as the moving liquid.
may never be fully explained. or when the dye was cut off. In- Thus one would predict a plot of
The results of the holdup studies, stead there were pockets of what k,a vs. acid concentration which
presented in Figures 4 to 10, may might be described as semistag- would have the k,a value f o r water
offer an explanation of several nant liquid and splashing, and the absorption at zero acid concentra-
mass transfer anomalies which random motion of liquid over the tion, and then k,a would increase
have arisen in recent years. The packing surface deposited o r re- as acid concentration increased
first is concerned with the dif- moved dye from these areas by until the limiting value correspond-
ferences observed when gas-phase means of a slow and random dilu- ing to the k& to be expected f o r
mass transfer coefficients, k,a, a r e tion process. Thus when dye was vaporization, corrected for dif-
determined by vaporization and injected for about 20 see. some of fusivity, was reached. It should be
absorption methods. Excellent dis- the pockets picked up dye, which noted t h a t this explanation pro-
cussions of this problem a r e pro- was not completely washed out by vides the two extreme values of
vided by Pigford and Colburn (21) the following clear water until as k,a but cannot, by itself, predict
and Sherwood and Pigford(l7). much as 5 min. had passed. The t h e shape of the intermediate por-
These authors point out that the water in these pockets corresponds tion of the curve because the rda-
most reliable data for &a, obtained to the static holdup, and the rate tive rates of chemical reaction and
by vaporization and absorption at which water enters or leaves diffusion must be taken into ac-
measurements, are in disagreement these areas can be judged quali- count as well as the changing ef-
by as much as 300% and no simple tatively from Figure 2, which fective area. For the same reason,
explanation is available to account shows the buildup of total holdup any theory of absorption and
for such large differences. One pos- when dry packing is used. It can chemical reaction in packed col-
sibility suggested by these authors be concluded t h a t there exists in umns which does not take account
is that the ammonia absorption t h e packing a quantity of water, of the variable effective area could
data, which a r e believed to be re- with a corresponding interfacial not predict quantitatively the effect
liable, should be interpreted as area, the composition of which of concentrations. It should be
though a chemical reaction takes would change rather slowly even noted that the concentration of the
place when ammonia dissolves in if the composition of the liquid solute in t h e gas phase will in-.
water and the reaction rate is slow entering the column changed rapid- fluence the effectiveness of the
enough to cause an abnormally ly. semistagnant liquid. The greater
high liquid-phase resistance. This If a packed column is used f o r this concentration, the lower the
suggestion was based on the work vaporization, the effective inter- effectiveness because the acid in
of Vivian and Whitney(Z3 and 24) facial area consists of the surface the pockets will be neutralized at
on the absorption of chlorine and area of the moving liquid as well a faster rate than a t lower concen-
sulfur dioxide where a mechanism as of the water in the semistagnant trations. As both acid concentra-
of this sort seemed to explain the pockets. If the column is used f o r tion in the liquid and solute con-
data; however, the same authors absorption the semistagnant poc- centration in the gas must be con-
compared the gas-phase mass trans- kets tend to become saturated in a sidered when a reaction occurs with
fer coefficients obtained from the short time, their surface area be- or without a changing effective
sulfur dioxide work with those comes ineffective, and so the ef- area, it may be possible t o take
obtained by ammonia absorption fective interfacial area is substan- into account the effect of these
and found them to be in reason- tially that of the moving liquid concentrations on both the rates
able agreement, and so it is rather alone. Of course, the observed vol- and areas at the same time. Sher-
unlikely that the chemical reac- umetric mass transfer coefficients, wood and Pigford(l7') provide an
tion mechanism can explain such k,a, f o r the two cases will be dif- excellent discussion of simultaneous
large differences as have been ob- ferent because the effective areas absorption and chemical reaction.
served. a r e different. This explanation can To test the explanations offered,
An explanation for this mass be tested quantitatively if the ef- as suggested, it was necessary to
transfer problem can be offered on fective area for vaporization is search the literature for reliable
the basis of observations of the assumed t o be proportional to the mass transfer data obtained with
flow of dye solutions through total holdup, ht, and that for ab- the Raschig rings and Berl saddles
packed columns. The equipment sorption proportional to t h e operat- f o r which holdup data a r e availa-
used for the holdup studies was ing holdup, h,, which represents ble. Unfortunately, there is a very

Vol. 1, No. 2 A.1.Ch.E. Journal Page 251


30
I I l I l l 1 scattering of the original data and
result in an inconclusive test of
the proposed explanation.
Pigure 11 is a plot of the ratio
(k+x),,ap/(k,a) aba vs. the holdup
ratio hJh0 where (kGa),, is the
value obtained from the vaporiza-
tion measurements and absorption
runs with high acid concentrations
and (k,a),b, is the corresponding 'L
00 .GI0 "OIYLLIT"

4.F '
10
W h o
'
PO
I
3.0
I value for ammonia absorption in
water a t the same gas and liquid
rate, as obtained by Fellinger (7).
FIG. 12. AMMONIA ABSORPTION
SULFURIC
ACID.
IN

FIG.11. (kGa),,aD/
(kGu)absVS. k,lh,. The ammonia and water data were
corrected to a common basis by Another packed-column mass
correcting f o r gas diffusivity t o transfer anomaly which may be
limited amount of data suitable for the 213 power, employing the values
this purpose. An excellent set of explained eventually with holdup
of 0.236 (cm.sq.) / (see.) for am- data is the reason for the different
data given by Fellinger(7') for monia and 0.256 (cmsq.) I (see.)
ammonia absorption in water can effects of gas diffusivity obtained
for water a t 25°C. and 1 atm. It when vaporization and absorption
be corrected f o r liquid-phase re- can be seen t h a t the points fad1 in
sistance by means of the Sherwood techniques are employed. A large
a band which is relatively narrow amount of mass transfer data ob-
and Holloway (16) correlation and when one considers that the magni-
for gas diffusivity to the 213 power tained with aQ sorts of materials
tude of some of the ratios repre- and techniques indicates that the
to provide k,a for absorption for sents otherwise unexplainable dif-
a11 the comparisons desired. Re- gas-phase mass transfer rates
ferences of well over 200%. The should be proportional to gas dif-
liable vaporization data are diffi- best line through the points can be
cult to obtain because end effects fusivity raised to the 213 power.
represented by However, two seemingly reliable
are extremely important when the
short packing heights required are sets of data obtained by vaporiza-
employed. Surosky and Dodge(Z0) tion techniques by Surosky and
give water-vaporization data f o r Dodge(20) and Mehta and Parekh
1.0-in. carbon rings which have The broken lines on the diagram as reported by Sherwood and Hollo-
been corrected for end effects. Sher- 15% above and below the best line way(l6) indicate the power to be
indicate the magnitude of the 0.15 to 0.17, The vaporization tech-
wood and Holloway (16 ) report
agreement of most of the points. nique assumes that the effective
water vaporization data for 1.5-in.
The average deviation from the interfaaial area is the same when
ceramic rings for which end effects
line given by Equation (7) is 2 different liquids wet the packing.
are estimated to be 35 to 40%. An 8%. The inequality of the two
equation was given for the uncor- In view of the fact that static hold-
rected data by Pigford and Colburn ratios may be caused by the failure ups are a function of surface
of the effective areas to be directly properties such as interfacial ten-
(14) which is equivalent to proportional to the holdups as as- sions, as illustrated by the dif-
sumed, a different proportionality ferences obtained with carbon and
for the two areas, surface tempera- porcelain, one would expect Iiquids
ture variations making one area with different physical and chemi-
Applying a correction of 37.5% less effective than the other, and cal properties to wet solid surfaces
based on the investigators' esti- the possibility that the slow, but differently. At the present time this
mate of end effects results in the finite, turnover of the semistag- explanation cannot be tested ; how-
corrected equation nant liquid makes some of its area ever, work underway to study the
effective for absorption with water effects of surface tension, viscosity,
work. The departure from equality and the nature of solid surface on
is not great, however, and i t seems holdups may provide the required
This equation as well as the cor- a s if Equation (7) can be used data.
rected experimental data can be empirically with Fellinger's data
used for the comparisons. Some and the holdups to predict mass SUMMARY
data for the absorption of ammonia transfer rates for vaporization and Total, static, and operating hold-
in sulfuric acid by use of 1.0-in. absorption with concentrated ab- ups, obtained for six ring and sad-
carbon rings were obtained by sorbents. dle packings, are represented by
Doherty and Johnson and reported A test of the ability of Equakion Figures 4 to 10 and Equation (1).
by Sherwood and Holloway ( 1 6 ) . (7) to predict the limiting values Equations (21, (31, and (4) may
The experimental points of the of kGa for a kGa vs. acid concen- be used to estimate holdups up to
f o u r sources mentioned were used tration plot is shown in Figure 12. loading conditions for rings and
if the combination of liquid and The acid-absorption KGa data are saddles larger than those investi-
gas rates fell in the regions in- plotted, and Fellinger's water-ab- gated. Total holdups are approxi-
vestigated in the holdup work re- sorption value of k,a as well as mately proportional to the number
ported in Figures 4 to 9. It was the k,a obtained by multiplying i t o f pieces of packing per cubic foot.
felt t h a t excessive extrapolation of by 0.85 (h,/h,) are shown as limit- Static holdups are independent of
the holdup curves was not justified ing values. It can be seen that all gas and liquid rates but are de-
because poor liquid distribution a t the experimental data fall between pendent upon the nature of the
low liquid rates and rapidly chang- the two as expected, and a t high surface of the paekings; operating
ing holdups a t gas and liquid rates concentrations there is close agree- holdups are independent of the
above loading would add to the ment with the limiting value. packing surface.

Page 252 A.1.Ch.E. Journal June, 1955


The holdups can be used to ex- water or extremely dilute 11. Jesser, B. W., and J. C. Elgin,
plain the differences between gas- absorbents Trans. Am. Znst. Chem. Engrs.,
phase mass transfer rates obtained 39, 277 (1943).
by vaporization and absorption 12. McCune, L. K., and R. H. Wil-
Greek Letters helm, Znd. Eng. Chem., 41, 1124
techniques and t o provide the Iimit- a = constant in Equantion ( 2 ) (1949).
ing mass transfer rates for low = constant in Equation (2) 13. Payne, J. W., and B. F. Dodge,
and high absorbent concentrations Y = constant in Equation (3) Znd. Eng. Chem., 24, 630 (1932).
when absorption is followed by an 6 = constant in Equation (4) 14. Perry, J: H., “Chemical Engineers’
irreversible chemical reaction. E = void fraction, cu.ft./cu.ft. Handbook,” 3rd ed., Section 10,
0 = constant in Equation ( 3 ) McGraw-Hill Book Company, Inc.,
NOITATION New York (1950).
a = effective interfacial area, sq. h = constant in Equation (4)
15. Piret, E. L., C. A. Mann, and T.
ft./ cu.f t. Wall, Znd. Eng. Chem., 32, 861
D , = diameter of sphere possessing LITERATURE CITED (1940).
the same surface area as a 1. Chu, J. C., J. Kalil, and W. A. 16. Sherwood, T. K., and F. A. L.
piece of packing, f t . Wetteroth, Chem. Eng. Progr., 49, Holloway, Trans. Am. Znst. Chem.
G = superficial gas rate, lb.1 (hr.) 141 (1953). Engrs., 36, 21 and 39 (1940).
(sq.ft.) 2. Cooper, C. M., R. J. Christl, and 17. Sherwood, T. K., and R. L. Pig-
ho = operating holdup, cu.ft./cu.ft. L. C. Perry, Trans. Am. Znst. ford, “Absorption and Extrac-
Chem. Engrs., 37, 979 (1941). tion,” 2nd ed., McGraw-Hill Book
h, = static holdup, cu.ft./cu.ft. 3. Elgin, J. C., and F. B. Weiss, Company, Inc., New York (1952).
ht = total holdup, cu.ft./cu.ft. Znd. Eng. Chem., 31, 435 (1939). 18. Shulman, H. L., and J. J. De-
kG = gas-phase mass transfer coef- 4. Ergun, S., Chem. Eng. Progr., 48, Gouff. Znd. Eng. Chem... 44,. 1915
ficient, Ib. moles/ (hr.) (sq. 89 (1952). (1952).
ft.) (atm.) 5. Ergun, S., Chem. Eng. Progr.,
~. 48, 20. Simm’ons, C. W., and R. B-
kL = liquid-phase mass transfer 221 (i952). Osborn, Znd. Eng. Chem., 26, 529
coefficient, lb. moles/ (hr.) (sq. 6. Evans, G. C., and C. F. Gerald, (1934).
ft.) (lb. mole/cu.ft.) Chem. Eng. Progr.,- . 49. 136 21. Surosky, A. E., and B. F. Dodge,
L = superfieial liquid rate, 1b.i (1953). Ind. Eng. Chem., 42, 1112 (1950)-
7. Fellinger, L., Sc.D. thesis, Mass. 22. Tillson, P., S.M. thesis, Mass.
(hr.) (sq.ft.) Inst. Technol. (1941). Inst. Technol. (1939).
N = pieces of packing/cu.ft. of 8. Fenske, M. R., C. 0. Tongberg, 23. Uchida, S., and S. Fujita, J. SOC.
packing and D. Quiggle, Znd. Eng. Chem., Chem. Znd. (Japan), 39, 432
Subscripts 31, 435 (1939). (1936) ; 40, 238 (1937).
9. Furnas, C. C., and F. M. Bellin- 24. Vivian, J. E., and R. P. Whitney,
vap = obtained by vaporization or ger, Trans. Am. Znst. Chem. Chem. Eng. Progr. 43, 691 (1947).
absorption in very concen- Engrs., 34, 251 (1938). 25. Whitney, R. P., and J. E. Vivian,
trated absorbents 10. Gamson, B. W., Chem. Eng. Chem. Eng. Progr., 45, 323
abs = obtained by absorption in Progr., 47, 19 (1951). (1949).

11. Wetted and Effective-interfacial Areas,


Gas - and Liquid-phase Mass
Transfer Rates
H. L. Shulman, C. F. Ullrich, A. Z. Proulx, and J. 0. Zimmerman
Clarkson College of Technology, Potsdam, New York

A study was made of separating the volumetric mass transfer coefficients, kau and kLa, into their components ko, h,and
u so that the effects of variables might be determined separately for each component. Mass transfer rates for four packings, %-
and 1%-in. Raschig rings and Yz-in. and 1-in. Berl saddles, made of naphthalene, were determined by vaporization into air
at gas rates from 100 to 1,OW lb./(hr.) (sq. ft.).
The correlation for ka was used to determine the wetted areas of those packings when irrigated with water and to calculate
the effective interfacial areas, u, from Eellinger’s data for ammonia absorption. These effective areas were then used to evahate
RL from previously published kLu data, and a correlation was obtained for all packings.
The correlations far ka and k~ and the effective-interfacial-area data make possible a more rigorous method for the design
of packed columns than was heretofore available.

To predict the performance of liable data such as those of Fellin- by the following relation t o give
columns employing ring and saddle ger(4) for volumetric gas-phase for a limited number of packings
packings for design purposes re- coefficients, kGa, and of Sherwood the over-all mass transfer coeffi-
~ and Holloway(8) f o r volumetric cients desired for design.
Additional tabular material may be obtained liquid-phase coefficients, &a, a r e
from the American Documentation Institute
Auxiliary Publications Project Photoduplication
used. Such coefficients can be esti- -
1 - 1 1 - 1
(0
Service Library of Congress’ Washington 25 mated f o r aqueous Systems from KGa kGa HkLa HKLa
D.C., a‘s document 4566 by r;mitting $2.50 fo; these sources of data and combined Although these sources of data are
photoprints or $1.75 for microfilm.

Vol- 1. No. 2 A.1.Ch.E. Journal Page 253

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