2096

Ind. Eng. Chem. Res. 1988,27, 2096-2100

Scale-up of Laboratory Data for Distillation Columns Containing

Corrugated Metal-Type Structured Packing
Jeffrey R. Hufton, Jose L. Bravo, and James R. Fair*
Department of Chemical Engineering, The University of Texas, Austin, Texas 78712

Laboratory-scale measurements were made of the mass-transfer efficiency of a gauze-type distillation

column packing. T h e test mixture, chlorobenzene/ethylbenzene,was used, and several operating
pressures in the range 40-750 mmHg were studied. It was found that the HETP data were correlated
well by available models developed for commercial-scale structured packings. T h e final result of
the work is a procedure that enables tests a t 25-mm column diameter size to be used for predicting
performance of a large-scale system utilizing structured packing, gauze, or sheet metal.
For many years, packed columns for distillation, absorption, and stripping contained solid elements that were
dumped into the columns in a random fashion. The elements often were metallic or ceramic pieces with ring or
saddle shapes. In more recent times, the elements were
also fabricated from plastic materials. These randomly
packed columns operated with gas and liquid flowing
countercurrently, and mass transfer between the phases
occurred across interfaces formed on the packing surfaces,
thought to be covered by flowing liquid films.
While the randomly packed column continues in use,
a new type of packed column has emerged in recent years.
This is the column containing ordered elements formed
from corrugated metal gauze and sheet metal that are
placed together in a careful arrangement and which are
dimensioned to fit snugly into the column. In todays
parlance, these devices are known as structured packmgs.
A photograph of a typical structured packing element,
sized to fit in a relatively small diameter column, is shown
in Figure 1.
Structured packing is used most often in vacuum distillation service, where it exhibits a very low pressure drop
in the flowing vapor while maintaining high efficiency for
mass transfer. The flow of liquid and vapor through
prescribed channels results in near elimination of pressure
losses due to form drag. The result is a high conversion
of momentum loss to effective mass transfer, a phenomenon often sought by process engineers charged with the
design of separation equipment to operate within tightly
prescribed pressure limits.

Scale-up of Packed Columns

Pilot-plant technology has evolved to a state such that
very small catalytic chemical reactors can be used to
prepare products of commercial interest. The associated
separation sequences of these reactors have not been
subjected to the same degree of miniaturization, however,
particularly when packed distillation columns are involved.
In many instances, the size and cost of a pilot plant is
determined by the smallest feasible separation device that
can still produce reliable results amenable to scale-up.
The hydraulic characteristicsof packed columns are such
that a minimum relationship between the column and
packing sizes should not be exceeded if the performance
of the small column is to be adequate. A ratio of column
diameter to packing diameter of 8 to 1is frequently used.
Designers have found that extrapolation of laboratory data,
using specialty packings, to a commercial device is extremely unreliable. As a result, the tendency has been to
install commercial-type internals in pilot columns; such
internals result in relatively large and expensive equipment.
0888-5885/88/2627-2096$01.50/0

There is a clear need for a reliable and consistent method to scale from a small laboratory packing to a large
commercial packed device. The use of structured packings
that can vary in size significantly but maintain geometric
similitude provides an opportunity to do this in a fairly
rigorous manner.

Previous Work
Structured packing in its present form was introduced
in the mid-l960s, largely on the basis of developmental
work at Sulzer Brothers, Ltd., in Switzerland (Huber, 1966;
Billet, 1969). The initial product was formed from metal
gauze which had been perforated. Later versions were
fabricated from less-expensive sheet metal (Huber and
Meier, 1975; Meier et al., 1977, 1979), and currently there
are both gauze and sheet metal versions of structured
packing marketed by a number of companies throughout
the world.
In 1985, Bravo et al. presented a mechanistic model
which was shown to correlate quite well the mass-transfer
characteristics of the commercial-size gauze-type packing
(specificallythe Sulzer BX geometry). Basically, a wetted
wall column model was adapted to represent the flow of
vapor and liquid through the channels formed by the elements of corrugated and perforated metal gauze. These
workers concluded that, because of the enhanced liquid
spreading characteristics of the gauze material, essentially
the entire surface was wetted and effective for mass
transfer.
Recently, Sulzer Brothers (1985) has made available a
laboratory-scale version of the gauze packing (Figure 2).
This packing can be placed in distillation columns of 2530-mm inside diameter with the advantage of reduced cost
demonstration of a structured packing application. For
tray-type distillation columns, the advantages of scale-up
from similar size columns, using Oldershaw equipment,
have been described by Fair et al. (1983). The advantages
include not only reduced cost because of the smaller scale
but also the capability of bypassing the expensive and
sometimes ill-defined parameters of phase equilibria,
theoretical stage calculations, and tray efficiency determination.
The present work was initiated with the hope that a
method comparable to the Oldershaw scale-up technique
could be developed for structured packing.
Experimental Work
A laboratory distillation system was assembled as shown
in Figure 3. The glass column was 25-mm i.d., to accommodate gauze-type packing of 22-mm o.d., obtained from
Sulzer Brothers, Ltd., Winterthur, Switzerland. The
distillation setup was conventional and designed for total
0 1988 American Chemical Society

Ind. Eng. Chem. Res., Vol. 27, No. 11, 1988 2097

Figure 1.
Figure 3.
Table 11. Comparison of Dimensions of Industrial-Scale
and LahoratoN-Scale Sulzer Gauze-Type Structured
Packin@
dimension
commercial BX
laboratow
element diam., em
typically 20+
2.2
crimp height, mm
6.4
1.55
channel side, mm
8.9
2.02
crimp angle, deg
89
80
specific area, m2/ms
492
1300
void fraction
0.90
0.96
inclination angle, deg
60
58

~~~

Figure 2.
Table I. Typical Values of Relative Volatility at
Experimental Run Conditions for
Chlorobeuzeue/Ethylbnzene System
pressure. mmHg
av temp, O C
re1 volatility
40
52
1.197
78
67
1.173
300
103
1.141
750
134
1.131

reflux operation. Heated parts were well-insulated t o

minimize heat losses. The entire setup was placed in a
walk-in-type fume hood.
The test liquid mixture was the binary ethylbenzene/
chlorobenzene. This mixture has been recommended for
test work by the European Federation of Chemical Engineering (Zuiderweg, 1969)and has been used extensively
for large-scale tests with structured packing (e.g., Huber
and Meier (1975), Meier et al. (1977, 1979), and Billet
(1986). The mixture has been shown to behave ideally in
the liquid phase (Maher and Smith, 1979); values of the
relative volatility for the test pressures are shown in Table
I. Other properties of the mixture may be found in
Zuiderweg (1969) or derived from compilations of pure

'Dimensions of the laboratory packing are shown as measured

(Hufton, 1987). They may differ somewhat from thme provided
by the manufacturer.

component data (e.g. Yaws (1977)). Each of the mixture

components had a purity of 99.8%.
The packing elements were 22-mm 0.d. by 5%"
long.
Ten elements were fitted together tightly, giving a total
packed height of 58 cm. The reflux stream was directed
to the center of the top element. It should be noted that
the 22-mm-0.d. elements contain metal gauze bands of
about 1-mm thickness; thus, the elements fit snugly in a
25-mm column. Communications from Sulzer Brothers
indicated that a 30-mm column would represent a more
convenient size for installation and removal of elemenk,
however, this would provide additional free volume around
the elements which would become imponderable in analysis of the true mass-transfer efficiency of the packing,
since the free volume would represent about 40% of the
total volume for contacting. Dimensions of the laboratory
packing, together with those for commercial-scale Sulzer
BX packing, are given in Table 11.
Total reflux runs were made at head pressures of 40,78,
300, and 750 mmHg. Overhead and bottoms samples were
analyzed by refractive index, calibrations of which confirmed the results of Hawkins and Brent (1951). Care was
taken to ensure stable operation, and separate runs were
made a t replicate sampling conditions. Further details

7.0

-5
d

s
h

5.0

4.0

6.0

MODEL

3.0

gw

Table 111. Comparison of Model and Experimental Values

of HETP for Chlorobenzene/Ethvlbenzene at Total Reflux
calcd HETP/exptl HETP
pressure,
mmHg
F. = 0.4"
F. = 0.8"
40
1.33
1.11
78
1.44
1.15
300
1.55
1.09
750
1.32
1.00

20
1.0

PRESSURE = 40 mm Hg

7.0
6.0

7.0

8
E

Ex
.Bg

3.0

'-

2.0

1.0

1-

5.0
4.0

1
I

SULZER DATA

flu

PRESSURE = 40 mm Hg

POINTS: THIS WORK

il.U

0.0

0.2

0.4

0.6

0.1

1.0

1.2

Vapor Rate (F, (l/s)@g4n)o')

SULZER DATA

7.0

60

yu

'

50-

$-

4.0

00

2 30-

E
5
E

2.0

0.0
0.0

0.2

0.4

0.6

0.8

1.0

POINTS: THIS WORK

'

0.2

'

0.4

'

"

0.6

'

0.8

'

1.0

1.2

~ ~ p o r(F"
~ ~
(l/s%um)oJ)
t c

".U

00

PRESSURE: 78 mm

1.o
PRESSURE = 300 mm Hg

1.2

Figure 5.

Vapor Rate (F,, (l/s)&g/m)O5)

2 is the height of the packing (58 cm), aZlis the relative

AnnPRESSURE = 750 mm Hg

Y
0.2
0.6
0.8

0.0
0.0

0.4

1.0

1.2

Vapor Rate F,, (l/s)Org/m)o-?

Figure 4.

may be found in the thesis of Hufton (1987).

Results
Overhead and bottoms compositions for each run were
converted to height equivalent to a theoretical plate
(HETP) values by means of the Fenske relationship:

where x is the mole fraction, 2 is the subscript for the more

volatile component (chlorobenzene), 1is the subscript for
the less volatile component (ethylbenzene), D is the subscript for the distillate, B is the subscript for the bottoms,

volatility, and HETP is in centimeters.

The resulting HETP values are plotted in Figure 4.
Also plotted are curves based on the model of Bravo et al.
(1985),utilizing geometric data given in Table 11. It is clear
that for most of the practical range the industrial-scale
model is conservative; i.e., it predicts higher HETP values
than were observed. For the particular range of F, =
0.4-1.0 (l/~)(kg/m)O.~
the deviations are given in Table 111.
Thus, if the laboratory column is operated in the vicinity
of F, = 0.8-1.0 (l/~)(kg/m)O.~,
the industrial-scale model
gives a reasonable and slightly conservative fit. This has
implications for scale-up procedures, to be discussed later.
Experimental curves (not data points) for this test
mixture at 40 and 76 mmHg top pressure have been provided by Sulzer Brothers (1985), and these are shown in
Figure 5. At the lower pressure, the fit is excellent,
whereas at the higher pressure the Sulzer HETP values
are higher by about 1 to ll/zcm. Details of the Sulzer
experimental work are not available, although it is known
that a 30-mm column was used. The reasons for the
performance differences are not known; the important
conclusion is that approximately the same values of HETP
were obtained in the two laboratories.

Scale-up Procedure
The development of a scale-up method may be based
on the Bravo et al. (1985) model. For the system at hand,

Ind. Eng. Chem. Res., Vol. 27, No. 11, 1988 2099
as for most distillation systems, the majority of the
mass-transfer resistance is in the vapor phase. The vapor
mass-transfer coefficient for the structured packing is
expressed through the Sherwood number:

This relationship was developed by Bravo et al. from an

extensive collection of data on the performance of gauzetype structured packings. The data were taken for column
diameters ranging from 75 to 1000 mm and for Sulzer BX
packing. Eight different systems were represented and
were operated at pressures ranging from 10 to 760 mmHg
absolute.
The Bravo et al. model is based on defined packing
geometry which determines dimensions of the flow channels for vapor and liquid. This formalized approach of
relating the performance of a packing to its geometry as
well as to the properties and flow rates of the fluid phases
constitutes the basis for using the model in the following
scale-up procedure.
If large (subscript 1) and small (subscript 2) column
conditions are compared a t the same temperature and
pressure (no change in physical properties), and if the
liquid velocity is considered negligible compared with the
gas velocity, then eq 2 leads to
delUge,l

kgldel

0.8

GG=(GG)

(3)

The height of a vapor-phase transfer unit is defined as

(4)

- -

and if H g Hpg HETP (strictly true if there is no

liquid-phase resistance and the operating and equilibrium
lines have the same slope), then
(5)
Since Uge= U , / ( Esin

e),

where

For many applications, $/

(HETP),

sin O2
sin O1

(7)

1.0. Finally, since 2 = Nt

demonstration that the desired separation can be made,

for a known packed height and reflux ratio, leads directly
to the specification of required packed height for the
commercial separation. This approach is similar to the one
proposed for tray columns using laboratory Oldershaw
tests (Fair et al., 1983). It can be a powerful tool for dealing
with scale-up problems during process development.
While the method described here has been developed
strictly for gauze-type structured packings, where the effective area, a,, may be taken as the specific surface area,
up (complete wetting of the surface), there are indications
that it can be useful when sheet metal packings are to be
used. The recent paper of Fair and Bravo (1987) shows
that the earlier mass-transfer model (Bravo et al., 1985)
can be used for such packings by applying an appropriate
discount factor, p. Thus, for the laboratory scale, a, = up,
then for the commercial scale, ae2= papz. For many industrial situations, /3 is in the range 0.60-1.00.
Since the value of p is inversely proportional to the
HETP obtained for the large packing, an accurate prediction of the effective interfacial area for the conditions
of the large column is important. Predictive methods for
/3 are not available a t this time, but as indicated by Fair
and Bravo (1987),at loadings equivalent to pressure drops
of 8-10 mbar/m of packing or greater, the value of @ approaches 1.0. Current research efforts are focusing on ways
to predict effective interfacial areas of sheet metal structured packings in distillation service.

Liquid Distribution Considerations

The scale-up technique that has been outlined above can
be used effectively to obtain a value of HETP or H for
a commercial packing when data for a laboratory packing
are available, as long as both packings are of the corrugated
metal (gauze or sheet metal) type. The value of HETP
thus obtained becomes the basic HETP of the packing
as defined by Zuiderweg et al. (1987). This basic HETP
is not affected by liquid maldistribution factors and is the
one achievable with near perfect liquid distribution. The
HETP specified for the large-scale column should take into
account the distributor design and the packing distribution
characteristics. In particular, wall fit and bed depth can
influence HETP in the larger size systems. Studies such
as those of Hoek et al. (1986) and Zuiderweg et al. (1987)
should be consulted for further information on liquid
distribution in large packed columns.
The study of Zuiderweg et al. indicates that one does
not need to be particularly careful about initial liquid
distribution in small laboratory columns (50-mm i.d. and
less) such as the one used in the experiments described
above. For this reason, the column liquid feed was a simple
reflux tube centered over the top packing element. Still,
a reasonable effort should be made to provide the laboratory column with adequate initial liquid distribution.

when Ntl = Ntz. If the liquid velocity is not neglected in

the step from eq 2 to eq 3, then eq 8 becomes

Equation 8 is especially useful for cases where there is

poor definition of vapor-liquid equilibria or even of the
composition of the mixture to be separated. A laboratory

Stepwise Scale-up Procedure

On the basis of work reported here, the following stepwise scale-up procedures are recommended:
Case A. Reliable equilibrium and physical property data
are available.
A l . Estimate the required height of packing for the
laboratory column. The estimate may be based on vendor
packing information or on scale-down estimates from the
correlation of Bravo et al. (1985).
A2. Set up the laboratory distillation system, using a
column inside diameter slightly larger than the packing
outside diameter. If the height of packing is greater than
1m, more than one bed of packing should be used, with
collection and redistribution of the liquid between beds.

2100 Ind. Eng. Chem. Res., Vol. 27, No. 11, 1988

A3. Make experimental runs a t the same pressure as

planned for the commercial-scale unit. The first runs
should be to determine the flooding velocity at total reflux.
A4. Run the column at an F factor of 1.0 ( l / ~ ) ( k g / m ) ~
if lower than the flood F factor. If not, use an F factor of
75% of the flood F factor.
A5. At a design reflux ratio, sample above and below
the packing to determine the separation accomplished. For
cases when more than one bed is used and physical
properties changed significantly throughout the column,
it may be desirable to sample between beds.
A6. Compute the number of theoretical stages equivalent to the separation accomplished. On the basis of height
of packing used, determine HETP for the laboratory
packing.
A7. Compute the commercial-scale packing HETP by
using eq 6 and 7, using appropriate vapor and liquid flow
conditions.
Case B. Reliable equilibrium and physical property data
are not available.
B1. Set up the laboratory column, and run the real
system. Determine by test the necessary packed height,
Z1,to perform the separation. The same guidelines for step
A2 above apply here.
B2. Use eq 8 to determine the packed height requirement, Z,, for the commercial column operating a t a vapor
velocity specified a t an appropriate approach to flooding
for the packing specified.

U,, = effective gas velocity through packing, m/s

U,, = superficial gas velocity through packing, m/s
UL,= effective liquid velocity through packing, (3r/
2 ~ ~ ) ( ~ ~ ~ g / m/s
3~~r)~/~,
x = mole fraction in liquid phase
z = height of packing, m or cm
Greek Letters
a = relative volatility

fl = discount factor for packing wetted surface, fractional

r = liquid flow based on packing perimeter, kg/cm
t = void fraction of packing
= angle of inclination of packing channels from horizontal,
deg.
I.L = vlscosity, mPa s
p = density, kg/m3
$ = parameter defined by eq 7
Subscripts

B = bottoms condition
D = distillate condition
g = gas or vapor
L = liquid

Literature Cited

Billet, R. Znst. Chem. Eng. Symp. Ser. 1969,32,4/42.

Billet, R. Packed Column Analysis and Design; Glitsch: Dallas,
1986.
Bravo, J. L.; Rocha, J. A.; Fair, J. R. Hydrocarbon Process. 1985,
64(1),91.
Fair, J. R.; Bravo, J. L. Znst. Chem. Eng. Symp. Ser. 1987,104,A183.
Summary and Conclusions
Fair, J. R.; Null, H. R.; Bolles, W. L. Znd. Eng. Chem. Process Des.
Deu. 1983,22,53.
Laboratory tests with 22-mm-diameter structured
Hawkins, J. E.; Brent, A. B. Znd. Eng. Chem. 1951,43,2611.
packing have shown that efficiency models developed for
Hoek, P.J.; Wesselingh, J. A.; Zuiderweg, F. J. Chem. Eng. Res. Des.
commercial-scale structured packings can be applied on
1986,64,431.
a reasonable basis to laboratory operations. This opens
Huber, M. US Patent 3 285 587, 1966.
Huber, M.; Meier, W. Sulzer Tech. Rev. 1975,57(1) 1.
the way to bench-scale testing on an economic basis that
Hufton, J. R. Performance and Scale-up of Laboratory-Scale Disprovides reliability of prediction for design. The method
tillation Columns Containing Structured Packing. M.S. Thesis,
should be regarded as tentative, pending additional
The University of Texas a t Austin, 1987.
scale-up testing. It has been developed on the basis of
Maher, P. J.; Smith, B. D. J. Chem. Eng. Data 1979,24,363.
structured packings fabricated from metal gauze, but inMeier, W.; Stoecher, W. D.; Weinstein, B. Chem. Eng. Prog. 1977,
dications are that with a suitable area discount factor it
73(11) 71.
Meier, W.; Hunkeler, R.; Stoecker, W. D. Znst. Chem. Eng. Symp.
can be used also for scaling to commercial-sized sheet metal
Ser. 1979,56,3.3/1.
structured packings.
Sulzer Brothers, Ltd. Sulzer Laboratory-Scale Structured Packing.
Leaflet VT2008/e, May 1985. Also, Aeschbach, S.,(Sulzer), priNomenclature
vate communication to J. R. Fair, Sept 25, 1986.
Yaws, C. L. Physical Properties; McGraw-Hill: New York, 1977.
a, = effective interfacial area for mass transfer, m2/m3
Zuiderweg, F. J., Ed. Recommended Test Mixtures for Distillation
up = specific surface area of packing, m2/m3
Columns; Institution of Chemical Engineers: Rugby, England,
de = equivalent diameter of packing, m
1969.
D, = gaseous diffusion coefficient, m2/s
F. J.; Hoek, P. J.; Lahm, L. Znst. Chem. Eng. Symp. Ser.
F, = superficial F factor for gas = U$s!pg)1/2,
(l/~)(kg/m)O,~ Zuiderweg,
1987,104, A217.

H, = height of a gas-phase tranfer unit, m or cm

H = height of an overall gas-phase transfer unit, m or cm
H8TP = height equivalent to a theoretical plate, m or cm
k , = mass-transfer coefficient for gas phase, m/s

Received for review January 14, 1988

Revised manuscript received June 14, 1988
Accepted July 6, 1988