Article

pubs.acs.org/IECR

The Effect of Column Diameter and Packing Height on the Pressure

Drop and on the HETP of Structured Packings
L. Valenz, J. Haidl, and V. Linek*
Department of Chemical Engineering, Institute of Chemical Technology Prague, CZ-166 28 Prague 6 Czech Republic

ABSTRACT: The standardization of the measuring method for the determination of packing separation efficiency should start
with a full understanding of all the conditions that affect its measurements in order to maintain them at the identical level during
the measurement of different packings with the aim of comparing or evaluating the effects of the geometric modification of newly
See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles.

developed/designed packings. The effect of the column diameter, the bottom concentration of the distillation mixture, and the
Downloaded via UNIVERSIDADE DO PORTO 01100 on August 17, 2021 at 16:58:35 (UTC).

packing height on the HETP and the pressure drop are evaluated on the basis of the data measured in columns with diameters of
0.15, 0.43, and 1.22 m packed with RSP 250, Mellapak 250Y, or Montz BSH 250 structured packing, and utilizing the
cyclohexane/n-heptane distillation system. It was found that below the loading point, the pressure drop was only slightly affected
by the column diameter. The difference between the pressure drops of the 0.15 and 1.22 m diameter columns was within the
experimental data scatter. The effect of the concentration range of distillation mixture on the separation efficiency is more
pronounced than is the effect of the column diameter. HETP increases with increasing bottom concentration and packing height,
and the increase found in this paper reached 50%. The effect of the column diameter onto the packing separation efficiency is not
significant. The HETP, measured in columns with widely different diameters using a distillation mixture of approximately the
same concentration range, did not demonstrate any significant effect of the diameter. The presented data do not support the
recommendation of Ottenbacher et al. (Chem. Eng. Res. Des., 2011, 8, 1427) to consider as relevant only the packing efficiencies
measured on columns with a diameter of at least 0.4 m because the data from the smaller diameter columns are dominated by the
wall effects.

1. INTRODUCTION bulk and this results in a lower local pressure drop. In small
In the article “Structured Packing EfficiencyVital Information columns, there is a comparatively higher proportion of gas or
for The Chemical Industry”, Ottenbacher et al.1 define the vapor channels along the walls which results in a lower pressure
practices that should serve as an open standard for both the drop in comparison to columns with a wider diameter.
measurement and the interpretation of the separation efficiency The effect of the column diameter on pressure drops of
of structured packing. The standardization of the measuring structured packings was studied by Olujic.3 His results,
method is the basis for the comparison of the packings and for presented here in Figure 1, show an opposite behavior: in
the evaluation of the effect of geometric modifications of newly columns with a smaller diameter the Montz B1−250 structured
designed packings. The current state of the art is such that the packing has shown substantially higher pressure drops in
scatter of HETP measured by different teams on the same comparison with the drops measured in columns of a larger
packing can hide the separation efficiency improvements of diameter. For example, the pressure drops in a column with a
newly developed packings.
Ottenbacher et al.1 have recommended many improvements.
We consider as the most relevant the use of the CB/EB
(chlorbenzene/ethylbenzene) system instead of the C6/C7
(cyclohexane/n-heptane) system, since the HETP measured
using the C6/C7 system depends to a greater extent on the
concentration range in comparison with that measured using
the CB/EB system, due to the larger variation of the relative
volatility over the concentration range. The authors published a
comprehensive list of physical and thermodynamic properties
of the CB/EB system. For obtaining reliable efficiency values
the authors also recommend the use of columns with a
diameter of at least 0.4 m because the results from columns
with smaller diameters are dominated by their wall effects. Figure 1. Effect of column diameter on pressure drops in the air−
water system. Data of Montz B1 250 are redrawn from Olujic.3
There are only a few studies in the literature that deal with
the effects of the column diameter on pressure drop and the
HETP. Random packings in columns with a smaller diameter Received: September 5, 2012
achieve lesser pressure drops (Billet and Mackowiak2). The Revised: March 21, 2013
packing density close to the column wall (the number of Accepted: April 4, 2013
packing pieces per unit volume) is lower in comparison to the Published: April 4, 2013

© 2013 American Chemical Society 5967 dx.doi.org/10.1021/ie302397q | Ind. Eng. Chem. Res. 2013, 52, 5967−5974
Industrial & Engineering Chemistry Research
diameter of 0.2 m are 3-times greater in comparison to those
measured in a column with a diameter of 0.8 m. Olujic3
concluded that “A practical consequence of this observation is
that predictions based on academic scale data can lead to grave
overestimates in the pressure drop and consequently column
diameter, when applied to industrial scale columns.” The
recommendation to use columns with a diameter of at least 0.4
m for obtaining reliable data would make the equipment and its
operation more expensive and might discriminate against
academic research which is usually conducted in columns
with smaller diameters. Nevertheless, the following survey of
the literature shows that there is not another work which
confirms such a profound effect of the column diameter onto
the pressure drop or HETP.
The pressure drops of the Montz B1 250 packing presented
by Olujic3 are compared with those of the very similar Mellapak
250Y packing in Figure 1. These packings are of the same size
and wettability of their surfaces by water and have the same
corrugation angle. The diameter effect on the pressure drop of
the Mellapak is described in the Sulcol software package
provided by the supplier Sulzer for its own packings. It was
deduced from experiments performed in columns of different
diameters. Olujic’s data show three-times greater pressure drops
in the column with a diameter of 0.2 m at Fv = 1 Pa0.5 than
those measured in a 0.8 m diameter column, while the increase
evaluated from the Sulcol is only 50% of that for the similar
Mellapak 250Y packing.
At low liquid flow rates (B < 10 m/h), well below the loading
point, when the upwardly flowing gas does not hinder the
downward flow of the liquid, the dry and wet pressure drops of
the packing differ only slightly. For example, based on the data
measured by Olujic,3 it makes only a maximum 15% difference
in a column with d = 0.2 m and is negligible in a column with d
= 0.8 m. Olujic’s data in regard to dry and wet packing are
presented in Figure 1. The data for dry Mellapak 250Y
measured by Stichlmair et al.4 in a column with a diameter of
0.3 m are compatible with those of the Sulcol software for d =
0.4 m. We present this data to illustrate the accuracy and
reliability of this software.
The models described in the literature also provide
unambiguous results of the effect of the column diameter on
the pressure drop of the structured packings. The models that
are based2 on the difference between the packing density close
the column wall and in comparison with the bulk also take into
account the wall factor K, defined as follows5
2
Δp a F 2 1 de
= λ 3 v K; K=1+ ; 2. EXPERIMENTAL SECTION
H ε 2 31−ε d
1−ε
de = 6
ap (1)
On the basis of the large quantity of data in regard to various
types of packings, Mackowiak5 recommends the value of K = 1
for structured packings, meaning that no effect of the column
diameter is expected. The model created by Brunazzi and
Paglianti,6 based on the losses resulting from changes in the gas
flow direction that occur at the transitions between the packing
elements, predicts some increase in the pressure drop in
columns with smaller diameters operating at the same specific
gas and liquid flow rates. This increase is proportional to the
number of bends per unit of the packing height. If the column
diameter is greater than the limiting diameter d = Hp/tg θ, the
number of bends depends only on the element height and the
5968
Article
dependence of the pressure drop on the column diameter
disappears. This limiting diameter is equal to 0.21 m for
Mellapak 250Y. In accordance with this model,6 the pressure
drop of dry packing in a column with a diameter 0.15 m is 15%
greater than that in a column with a limiting diameter of 0.21
m.
The independence of pressure drops and of the HETP of the
column diameter is well documented by the data measured by
Billet7 and Meier et al.8 using the CB/EB distillation system
and Mellapak 250Y. The data measured7 in the small column
with a diameter of 0.22 m coincided with those measured in the
large column with a diameter of 1.0 m in regard to the range of
the vapor capacity factor of 0.4−2.8 Pa0.5. These data are
presented in Figure 8.17 of Billet’s book.7 A similar degree of
consistency between the HETP measured in columns with
diameters of 0.16, 0.25, and 1 m was found by Meier et al.8
The data in the literature led us to the conclusion that the
recommendation to use the smallest 0.4 m diameter columns in
order to obtain reliable data in regard to efficiency is not
generally valid and should be analyzed in greater detail. First,
the situations should be differentiated for when data are being
measured for the design of large scale columns and when they
are being measured for comparing the separation efficiency of
the packings or for evaluating the effect of the geometric
modifications on newly developed packings. The measurement
of data using the large-scale columns is financially more
demanding, and the data are more prone to error because of
misdistribution and the nonuniformity of the flow profile
through the packing. Either of these phenomena may cause a
severe reduction in the separation efficiency and should be
prevented during the packing test experiments. On the other
hand the data from small scale columns may be dominated by
the wall effects. The hydraulic wall effects are demonstrated by
pressure drops. Olujic paper 3 is the only systematic
experimental study dealing with the effect of the column
diameter on pressure drops in structured packings. However
the marked diameter effect revealed3 was not observed by other
authors4,7 nor predicted by the available correlations5,6 (see also
Sulcol). A similar systematic study dealing with the effect of the
column diameter and concentration of the distillation mixture
we did not find in literature at all.
The aim of this study is to evaluate the effect of column
diameter on pressure drops and on separation efficiency and
the dependence of the effect on the concentration range of the
distillation mixture used during the measuring.
2.1. Columns and the Data Utilized. Apart from our own
measured data in Column 4, the data used are taken from the
following reports: The pressure drop and the HETP measured
on the Raschig Super-Pak 250 (RSP250), the Mellapak 250Y,
and the Montz BSH 250 packings, employing the C6/C7
distillation system in columns of different sizes are presented.
Within these reports the columns and the experimental and
evaluation procedures are described in detail. We provide here
the following basic information concerning the columns and
the data utilized for this work.
Column 1 FRI: Report “Test of RSP250” by Cai T.J.,
King D.W., June 15th, 2009. Report made available for
the purposes of this study by Raschig. The data utilized:
Fv, the pressure drop, xbottom, HETP. Conditions: p =
1.62 b; d = 1.22 m; H = 3.5 m.
dx.doi.org/10.1021/ie302397q | Ind. Eng. Chem. Res. 2013, 52, 5967−5974
Industrial & Engineering Chemistry Research
Column 2 FRI: Topical Report 108, 1990. Report made
available for the purposes of this study by Montz. The
data utilized: Fv, the pressure drop, xbottom, HETP, liquid
concentration profile measured at positions z = 0, 0.81,
1.42, 2.03, 2.64, 3.25, 4.01 m. Conditions: p = 1.62 b; d =
1.22 m.
Column 3 SRP: Report “Distillation Characteristics of
the Raschig-Jaeger RSP 250 Structured Packing” by
Seibert F., Perry M., Briggs S., Fair J., December 14,
2009. Report made available for the purposes of this
study by Raschig. The data utilized: Fv, the pressure drop,
xbottom, HETP. Conditions: p = 1.65 b; d = 0.43 m; H =
3.0 m.
Column 4 our laboratory. p = 1.0 b; d = 0.15 m; H = 2.1
m. Sketch of the column and one of the internals are
presented in Rejl et al.9 A description of this column
follows.
Column 4 was packed with 9 (RSP 250) or 10 (Mellapak
250Y) pcs of structured packing to a height of 2.1 m. Each of
the packing units was equipped with two wall wipers that
redirected the wall flow back into the packing. The small
diameter of the column and the large number of wipers justify
our assumption that the higher liquid flow close to the column
wall is noticeably suppressed. An electrically heated reboiler
equipped with an electric power regulator maintained constant
reboiler duty for the batches of different composition. The
volumetric reflux flow rate was measured to an accuracy of
0.001 L/min. A shower distributor with 25 openings (1472
holes/m2) was utilized. The column and the reboiler were
thermally insulated. The heat-loss, evaluated from the temper-
ature decrease of the hot water (90 °C) flowing through the
column represented only 3% of the lowest reboiler duty utilized
(8 kW).
The column was provided with seven openings for placing
thermistor and sampling devices at regular distances along the
column for the withdrawal of liquid and vapor samples. The
holes for this sampling were drilled through the structured
packing using a water jet. We believe that the sampling points
do not significantly affect the flow of phases in the packing
since the volume of the holes affects only 3.3% of the packing
volume and the pressure drop also differs undetectably between
the drilled and undrilled packings (compare the empty and the
full symbols, shown in Figure 2), for the undrilled and the
drilled packings, respectively.
2.2. Pressure Drop Measuring Methods. Great attention
has been given to the avoidance of all the possible causes of
incorrect pressure drop measurements that have been
thoroughly discussed by Cai and Resetarits.10 In the distillation
column, the pressure tap consists of small holes with an inner
diameter of 6 mm that are drilled into the column wall below
and above the packing and are connected to a pressure
transducer via independent tubes. To ensure that no vapor
condensation occurs inside the lines, nitrogen was blown
through both the lines connected to the pressure drop
measurement device at extremely low flow rates eliminating
any pressure drop in the lines.
2.3. HETP Measuring Methods. The HETP were
measured under total reflux and evaluated on the basis of a
number of theoretical stages Ntheor between the mole fractions
of the light component in the liquid phase at the top and the
bottom of the packed bed section H. Rigorous (stage-to-stage)
calculation was used for this purpose. The equilibrium data of
5969
Article
Figure 2. Pressure drop and HETP of Raschig RSP 250 packing
measured in C6/C7 distillation system. Filled and empty symbols are
pressure drops of the packings with and without holes drilled for
sampling of phases.
the C6/C7 distillation system were taken from Onken and
Arlt11 and the HETP was calculated from the relation
H
HETP =
Ntheor (2)
3. RESULTS
3.1. Effect of the Column Diameter on Pressure Drop
and HETP in C6/C7 Distillation System. 3.1.1. Raschig
Super-Pak RSP 250. The pressure drop and the HETP
measured using the C6/C7 distillation system in the columns
of the diameters 0.15, 0.43, and 1.22 m and at the pressures of
0.33, 1.0, and 1.65 bar are plotted in Figure 2 as a function of
the gas capacity factor Fv. The pressure drops measured below
the loading points in columns of different diameters and at
different pressures vary only within the scatter of the
experimental points. As can be expected, the highest value of
the loading point, recognized as the point at which the slope of
the pressure dependence on the Fv starts to increase, was found
at the lowest pressure (0.33 b) and is equal to approximately
3.2 Pa0.5. The 2.5 Pa0.5 loading point found in the columns with
larger diameters (0.43 and 1.22 m) at an elevated pressure of
1.65 b is consistent with the value at which the dependence
curve of pressure drops starts to bend when measured in the
small Column 4 of 0.15 m diameter at atmospheric pressure.
The measuring of higher Fv-factors in Column 4 was restricted
by the maximum output of the reflux pump. Therefore it is not
possible to estimate a reliable value of the loading point in this
column.
The HETP measured in the different columns differ
significantly, see Figure 2. The data measured in the same
column with the same packing also differs. This is caused by a
HETP dependence on the concentration range in which the
measurement was made due to the significant variation of the
relative volatility over the concentration range. In Figure 2, the
concentration range is characterized in accordance with the
bottom molar fraction of C6 and thereby the data measured at
the same xbottom may still differ in accordance with whether they
are determined in a short or a long column. The HETP
dx.doi.org/10.1021/ie302397q | Ind. Eng. Chem. Res. 2013, 52, 5967−5974
Industrial & Engineering Chemistry Research
measured in lean cyclohexane mixtures are much lower than
those measured in rich mixtures. In the short (H = 1.8 m) and
the small diameter (d = 0.15 m) Column 4, the HETP increases
sharply from 0.28 to 0.38 m with the bottom C6-concentration
from 0.03 to 0.10. The HETP dependence on x bottom
diminishes/ceases at concentrations higher than 0.32 in
which the HETP values fluctuate at ca. 0.41 m in the whole
range of the Fv-factor utilized (from 0.7 to 2.5 Pa0.5).
The data measured in FRI Column 1 with H = 3.5 m and d =
1.22 m at low bottom concentrations of 0.10 to 0.12 lie in the
0.32−0.39 m interval and are somewhat higher (by 0.03 m
approximately) than those measured in SRP Column 3 with a d
= 0.43 m diameter. This small difference of the HETP may be
the result of the lower packing height H = 3 m used in Column
3 in comparison with the 3.5 m used in FRI Column 1.
3.1.2. Mellapak 250Y and Montz BSH 250. Both these
packings are of the same size and wettability of their surface.
The pressure drop and the HETP measured in columns with
diameters of 0.15 and 1.22 m at the pressures of 0.35, 1.0, and
1.65 bar are compared in Figure 3. Similarly as with RSP
Figure 3. Pressure drop and HETP of geometrically similar packings
measured using the C6/C7 distillation system.
packing, the measured pressure drops below the loading points
in the columns of the different diameters and at different
pressures differ only in the scatter of the experimental points.
Also the 2.4 Pa0.5 loading point identified in the column of
greater diameter (1.22 m) is consistent with the value at which
the pressure drop in the small column of 0.15 m diameter also
starts to increase. The pressure drops measured below the
loading points in these packings do not confirm the significant
effect of the column diameter reported by Olujic.3
The HETP values measured on short packing depth (1.80 or
1.83 m) in columns of different diameters packed with
Mellapak 250Y (d = 0.15 m) or Montz BSH 250 (d = 1.22
m) increase with bottom concentration in a similar manner as
was revealed for the RSP in the short Column 4 (H = 1.8 m
and d = 0.15 m). The HETP of the Mellapak increases from 0.3
to 0.43 m with an increase of the bottom C6-concentration
from 0.03 to 0.68. Similarly, the HETP of the Montz evaluated
for the short packing sections, in which ΔH = 1.83 m in
Column 2, increases from 0.33 to 0.47 m with an increase of
5970
Article
the bottom concentration from 0.20 to 0.75. The HETP
dependence on xbottom ceases with concentrations higher than
0.5 as is shown by the data of the Montz packing. The HETP
measured in these rich C6 mixtures fluctuates at around 0.46 m
in the whole range of the Fv-factor utilized (from 0.5 to 2.1
Pa0.5).
The effect of the packing height on the HETP can be
assessed from the data provided by the Montz BSH 250
packing, measured at the same bottom concentration of 0.20−
0.26 using different packing heights, specifically 4 and 1.8 m.
The HETP measured at the low packing height is ca. 0.34 m
and is much lower than the HETP = 0.42 m measured at the
higher packing height. Fitz et al.12 measured a somewhat lower
HETP = 0.39 m for the Mellapak 250Y at the lower packing
height of 3.5 m.
3.1.3. Concluding Remarks Concerning the Column
Diameter Effect on Pressure Drops. The pressure drops
presented here in regard to the RSP 250, Mellapak 250Y, and
Montz BSH 250 packing and the C6/C7 distillation system
measured at flow rates below the loading point in columns of
different diameters (0.15−1.22 m) at total pressures (0.31−
1.65 b) show only small differences, far less than 15%, which
indicate zero or an insignificant column diameter effect.
3.1.4. Concluding Remarks Concerning the Column
Diameter Effect on the HETP. The effect of the column
diameter on the HETP is difficult to evaluate from experiments
carried out in columns with different packing heights and
distillation mixtures with different concentrations, because the
impact of both these conditions is more pronounced than is the
potential effect of the column diameter. Nevertheless, the
HETP measured in columns of widely different diameters,
using distillation mixtures of approximately the same bottom
concentration, did not show any significant column diameter
effect that would support the recommendation1 to discount the
data measured in the columns with diameters smaller than 0.4
m. For example, the HETP of the same Mellapak 250Y and
Montz BSH 250 corrugated packings measured in Columns 4
and 2 of very different 1.22 and 0.15 m diameters differ only
slightly (0.36 and 0.34 m, respectively) provided that the same
low packing height 1.80 m and the bottom C6-concentration of
0.2 are used, as is shown in the data in Figure 3. A similar
concordance exists between the data measured in Columns
with xbottom higher than 0.5, in which the HETP dependence on
xbottom has ceased (see Figure 4).
Thanks to lower dependence of the HETP on the
concentration range, as measured by the CB/EB distillation
system, in comparison with the C6/C7 system (due to the
Figure 4. HETP evaluated from short column sections heights of 1.9
± 0.1 m plotted against C6-concentration at the bottom of the
sections.
dx.doi.org/10.1021/ie302397q | Ind. Eng. Chem. Res. 2013, 52, 5967−5974
Industrial & Engineering Chemistry Research
lower variation of the relative volatility over the concentration
range), the results produced by the CB/EB system are more
definitive and therefore more convincing. For example, the
independence of the HETP of Mellapak 250Y from the column
diameter, using this system, was identified by Billet7 and Meier
et al.8 The HETP measured by Billet7 in the 0.22 and 1 m
diameter columns did not differ and was equal to 0.32 ± 0.01 m
in the 0.4 to 2.8 Pa0.5 range of the vapor capacity factor. Meier
et al.8 found a similar concordance between the HETP
measured in columns with diameters of 0.16, 0.25, and 1 m
at various pressures between 50 and 100 mbar and between 400
mbar and the value of the atmospheric pressure. This data did
not depend on the packing heights that were used, that is, 1.4,
4.4, and 6.6 m.
In contrast to the insignificant and rather incomprehensible
effect of the column diameter, the effect of the concentration
range in which the measurement was conducted is considerable.
The HETP increases considerably with the increasing bottom
concentration and the packing height, and this increase reaches
up to 50% of the HETP value measured. For this reason, the
effect of the concentration range is analyzed in more detail in
the next section.
3.2. Analysis of the HETP Dependence on the
Concentration Range Used. 3.2.1. The HETP Dependence
on Bottom Concentration. The HETP evaluated for the short
packing sections ΔH (Column 2, ΔH = 1.83−1.98 m; Column
4, ΔH = 1.80 m) is plotted in Figure 4 against the C6-
concentration at the bottom of the sections. In the small
Column 4 (d = 0.15 m), the variation of xbottom was achieved
utilizing different concentrations of the distillation mixture in
the reboiler. In the large Column 2 (d = 1.22 m), the
concentration profile was measured along the column and the
HETP was evaluated between sample points remote from each
other by 1.98, 1.83, and 1.83 m. The HETP increases linearly
from 0.28 to 0.48 m with the increase of the xbottom from 0.02 to
0.75. The wide scatter of the data is caused by the inclusion of
all the HETPs measured at various values of the Fv capacity
factor.
3.2.2. The HETP Dependence on the Packing Height. The
HETPs calculated from the concentration profiles measured in
Column 2 are plotted in Figure 5 as a function of the packing
Figure 5. HETP calculated for the sections ΔH of the packing taken
from the bottom of the packing.
height. The heights were measured from the bottom of the
packing to sampling points located at the heights of H = 0.76,
1.36, 1.98, 2.59, 3.20, and 4.01 m. The bottom concentrations
were measured at a sampling point just below the packing, the
head concentrations are those measured at the reflux and the
remaining samples were withdrawn from the packing. The
5971
Article
values of the xmean and the Ntheor,mean presented in the figure
represent the arithmetic mean of the C6-concentrations and of
the number of theoretical stages, or are measured at these
points in all the experiments undertaken at the various Fv
factors. The data show a steady increase in the HETP from 0.24
to 0.42 m with an increase in the packing depth from 0.76 to
4.01 m, and they have a tendency to increase further.
If the HETPs were evaluated using the concentrations
measured at the first sampling point located 0.76 m above the
packing bottom (i.e., not from the sampling point situated
below the packing), the resulting dependence of the HETP on
the packing depth would have changed considerably as is
shown in the upper part of Figure 6. Instead of a steady
Figure 6. HETP calculated from concentration profiles plotted as a
function of packing height taken from the first sampling points from
the bottom (z = 3.25 m) and the top (z = 0.81 m) of the packing.
Symbols are the same as in Figure 5.
increase, the HETPs are independent of the packing height.
Similar behavior is shown by the HETP calculated at the first
sampling point situated 0.81 m below the top of the packing;
see the data plotted in the lower part of Figure 6. Only the
HETPs calculated from the concentrations measured just below
the packing are significantly lower. It seems that these
concentrations are significantly undervalued. If these data are
excluded from the evaluation, the HETP values fluctuate
around a constant value. Similar behavior is shown by the
HETP data presented in Figure 3 for Mellapak 250 Y as
measured at a similarly high bottom concentration of 0.6.
Apparently, the concentrations in the liquid that falls out of the
packing may differ from those in the liquid at the bottom of the
packing and their difference may create a significant part of an
equilibrium stage. The evidence that these data are mistaken or
are influenced by the end-effects is also supported by our
further finding that the profiled method was not convergent,
when these concentrations were taken into account for the
evaluation of the concentration profiles.
The end-effects may cause an erroneous appearance of an
improvement in the performance of the packing. Therefore it is
necessary to discount both the top and the bottom samples
from the packing to obtain the correct HETP values reflecting
only the improvements in the performance of the packing.
3.2.3. The Suitable Packing Height for the Measurement
of the Packing Efficiency. Ottenbacher et al.1 recommend
performing the measurement of the packing efficiency in a
“large column comprising 15 to 20 theoretical stages (which
industrial applications usually do contain); this is equivalent to
a bed height of 4−6 m”. A packing height of 4 m represents
approximately 10 theoretical stages of the C6/C7 distillation
dx.doi.org/10.1021/ie302397q | Ind. Eng. Chem. Res. 2013, 52, 5967−5974
Industrial & Engineering Chemistry Research
system, and the further increase in the packing height
dramatically augments the demands on the accuracy of the
analytical method. For example, starting with a bottom C6-
concentration of 0.2 (the same concentration that was used in
the testing of the Montz BSH 250 in Column 2), the
concentration at the top of the 4 m packing, representing 10
stages, equals 0.985. In the next two stages, the C6-
concentrations would be 0.991 and 0.995. At such high
concentrations, the experimental error of the C6-molar fraction
0.003 corresponds to one theoretical stage. In this case, the
application of a packing height of more than 10 stages might
lead to an unacceptable error of the HETP (>10%). A suitable
packing height should be chosen in accordance with the
distillation system utilized and with the accuracy of the
analytical method used.
3.2.4. Comparison of the Shortcut and the Rigorous
Evaluation Methods. The shortcut methods currently used for
the evaluation of the HETP are based on the Fenske equation
deduced for total reflux, a constant relative volatility α, and a
constant molar overflow as shown in the formula
Ntheor =
(
ln
xhead 1 − x bottom
1 − xhead x bottom ); αave = αheadαbottom
ln αave
(3)
The number of theoretical stages Ntheor evaluated using the
shortcut method and the rigorous stage-to-stage method for the
C6/C7 and CB/EB distillation systems are compared in Figure
7, in which their relative differences, calculated for several
Figure 7. Relative difference between number of theoretical stages
calculated between xbottom and xtop by the Fenske eq 3 and by the
rigorous stage-to-stage method.
values of xbottom, are plotted against xhead. The equilibrium data
were taken from Onken and Arlt.11 The differences in terms of
the CB/EB system are negligible (less than 0.03%) and, in
terms of the C6/C7 system, are less than 2%. The linear
interpolation used between zero and one equilibrium stage for
an unlikely separation corresponding to less than one stage is
really obscure and is probable the cause of the sinusoidal
highlighted difference between the Fenske equation and the
stage-to-stage calculation. The comparison shows that the
shortcut method does not lead to any noticeable differences in
the theoretical stages of either distillation system.
3.3. The Suitability of the HETP for the Objective
Evaluation of Packing Efficiency. The two properties that
preclude the HETP from providing a comprehensive
comparison between different packings are (i) dependence on
the concentration range within which the measurement was
carried out and (ii) inability to identify and to distinguish mass
transfer improvements achieved in the liquid and vapor phases.
While the first issue can be minimized by using the distillation
5972
Article
system with the lowest concentration dependence of slope of
equilibrium line m, for example, using the CB/EB distillation
system rather than the C6/C7 system as recommended by
Ottenbacher et al.,1 the second issue is hardly controllable. As
shown in the relation 4 deduced from the basic principles of the
interfacial mass transfer
⎛ 1 m ⎞ ln(m(uL /uV ))
HETP = uL⎜ + ⎟
⎝ kLa k Va ⎠ m(uL /uV ) − 1 (4)
the HETP depends on the relative resistances concentrated in
the individual phases. The local slope of equilibrium line m may
affect considerably the role of resistances of individual phases.
As a result, the HETPs measured by various distillation systems
are variously sensitive/receptive to identifying an improvement
of the mass transfer rate developed in one of the phases. For
example, the improvement of the mass transfer coefficient
achieved solely in the liquid phase is not detectable as an HETP
value when measured using the distillation system with a
controlling mass transfer resistance in the vapor phase. In
addition, this situation is complicated by the fact that the
relative resistance of the phases varies along the column height.
This problem might be solved/avoided by comparison not only
of the HETP values but also of the local volumetric mass
transfer coefficients measured directly in the distillation
columns at the same concentration and flow rates of the
phases. For the determination of the coefficients, the profile
method13−15 was recently developed. The method evaluates the
coefficients from the concentration profiles measured along the
distillation column. Presently, the physical consistency/
relevance of the evaluated coefficients is verified by comparing
absorption and distillation mass transfer coefficients measured
in a wetted-wall column.
3.4. Effect of the Concentration Range on the HETP
Deduced from the Concentration Profiles. The concen-
tration range in which the measurement was carried out is
determined by the two following process parameters: the xbottom
bottom concentration of the distillation mixture and the height
H of the packing used. Their effects on the HETP measured in
columns with different bottom concentrations and packing
heights are quantified below for the data for Mellapak 250Y
measured in Column 4 with the C6/C7 distillation system at
reboiler duty of 16 kW which provides Fv = 2.05 Pa0.5 at a
bottom concentration of 0.0428. The concentration profile
shown in Figure 8 was obtained by the profile method applied
Figure 8. Concentration profile obtained by the profile method at Fv =
2.05 Pa0.5 for various bottom concentrations of the distillation mixture.
dx.doi.org/10.1021/ie302397q | Ind. Eng. Chem. Res. 2013, 52, 5967−5974
Industrial & Engineering Chemistry Research
onto the experimental data measured at four different bottom
concentrations ranging from 0.0428 to 0.7088 at the same
reboiler duty 16 kW. The method starts with the choice of the
mass transfer correlation describing the dependence of the
volumetric mass transfer coefficients on physical properties and
phases velocities. Then, the front factors of the correlations are
varied in a systematic way such that the predictions from the
rate based simulation model are matched to experimental
concentration profiles as closely as possible. The plug flow of
both phases in the column is considered and the film model of
the interfacial mass transfer is used in which the convective flow
is taken into account. The profile method is described in detail
by Linek et al.,13 Rejl et al.,9,14 and Valenz et al.15 For the sake
of completeness, we have used two different mass transfer
correlations, namely the RBF model published by Rocha et
al.16,17 and the Delft model published by Olujic et al.,18 to show
the effect of the choice of the mass transfer correlations on the
results. The profiles obtained using the RBF and Delft model
practically coincide, and their difference is not detectable in
Figure 8 in which the calculated profiles are plotted together
with the experimental data. The mean relative deviation
between the calculated and the experimental concentrations is
3.9% for x-profiles and 2.4% for y-profiles.
Using this profile, the dependence of the HETP on the
bottom concentration and the packing height can be evaluated
from eq 2 for H = z2 − z1 and the corresponding theoretical
stages Ntheor are defined between the mole fractions xC6(z1) and
xC6(z2) using rigorous stage-to-stage calculation. The depend-
ence of the HETP on xbottom calculated for three packing
heights H = 1.8, 3, and 4 m are presented in Figure 9. The
Figure 9. Dependences of HETP onto the bottom concentration
evaluated for three packing heights.
dependences are terminated when the value of xhead reaches
0.985 that is, the value above which an experimental error of
the C6-molar fraction might lead to an unacceptable error in
the HETP as discussed in section 3.2.3. The line calculated for
the height of H = 1.8 m corresponds well with the experimental
data presented in Figure 3 for Fv = 2 ± 0.1 Pa0.5.
The results presented in Figure 9 illustrate the following
findings: (i) At the same bottom concentration of the
distillation mixture, the HETPs measured in the lower columns
are higher than those measured in the higher columns. For
example, the HETP values measured at xbottom = 0.1 in the
columns with packing heights of 1.8, 3, and 4 m increase to
0.32, 0.35, and 0.37 m. (ii) The sensitivity of the HETP values
to changes of the bottom concentration is greater at lower
concentrations and at lower packing heights. This sensitivity is
defined by the local slope of the curves shown in Figure 9. The
slopes equal to 33, 31, and 25 cm for the packing heights of 1.8,
3, and 4 m with xbottom = 0.1 and are approximately half of these
5973
Article
values, that is, 15, 13, and 10 cm, with xbottom = 0.3. (iii) The
conditions in which the effect of the concentration range and of
an experimental concentration error on the measured value of
the HETP is minimal are as follows: a packing height of 3 m
and a bottom concentration of 0.2 C6-mol fraction.
4. CONCLUSIONS
The pressure drops of the RSP 250, Mellapak 250Y, and Montz
BSH 250 packings, measured in columns of different diameters
(0.15, 0.43, and 1.22 m), using the cyclohexane/n-heptane
distillation system below the loading points do not show any
differences that would indicate any significant column diameter
effect. In contrast to the insignificant effect of the column
diameter, the effect of the concentration range in which the
measurement of the HETP was carried out is considerable. The
HETP increases with an increase of the bottom concentration
and the packing height, and this increase can reach up to 50%.
The HETP of the different packings can be compared only if
the concentration range along the packings to be compared is
the same. This requirement is hard to fulfill but the HETP
measured in approximately the same concentration range did
not show any significant column diameter effect.
The results presented do not support the recommendation of
Ottenbacher et al.1 to use columns with a diameter of at least
0.4 m for obtaining significant efficiency values, since the use of
smaller column diameters will result in measurements that are
strongly influenced by wall effects.
■
AUTHOR INFORMATION
Corresponding Author
*E-mail: linekv@vscht.cz.
Notes
The authors declare no competing financial interest.
■ ACKNOWLEDGMENTS
The supports from RASCHIG GmbH and Grant Agency of
Czech Republic through the project no. 13-01251S are
gratefully acknowledged.
■ NOMENCLATURE
a = effective mass transfer area, 1/m
ap = packing geometrical area, 1/m
B = superficial liquid velocity, m/h
c = molar concentration of more volatile component in the
bulk, kmol/m3
de = equivalent diameter, m
d = column diameter, m
FV = uV √ρV gas capacity factor, Pa1/2
H = packing height, m
Hp = height of packing element, m
ΔH = height of packing section, m
HETP = height equivalent to a theoretical plate calculated
from eq 2, m
K = wall factor given by eq 1, -
kLa = liquid-side volumetric mass transfer coefficient, 1/s
kVa = vapor-side volumetric mass transfer coefficient, 1/s
m = slope of the equilibrium line, -
Ntheor = number of theoretical stages
p = pressure, Pa
Δp/H = pressure drop, Pa
u = superficial velocity, m/s
x = liquid phase molar fraction of more volatile component
dx.doi.org/10.1021/ie302397q | Ind. Eng. Chem. Res. 2013, 52, 5967−5974
Industrial & Engineering Chemistry Research Article

z = column height coordinate taken from the top of the (18) (5) Olujič, Ž .; Kamerbeek, A. B.; de Graauw, J. A. Corrugation
packing (z = 0), m geometry based model for efficiency of structured distillation packing.
Chem. Eng. Process. 1999, 38, 683.
Greek Symbols
α = relative volatility, -
ε = packing porosity, -
λ = resistance coefficient, -
θ = corrugation angle, deg
Indexes
bottom = bottom of packing
C6 = cyclohexane
head = top of packing
L = liquid phase
V = vapor phase

■ REFERENCES
(1) Ottenbacher, M.; Olujic, Z.; Adrian, T.; Jödecke, M.; Großmann,
C. Structured packing efficiencyVital information for the chemical
industry. Chem. Eng. Res. Des. 2011, 8, 1427.
(2) Billet, R.; Mackowiak, J. How to use the absorption data for
design and scale-up of packed columns. Fette Seifen Anstrichmittel
1984, 86 (9), 349.
(3) Olujic, Z. Effect of column diameter on pressure drop of
corrugated sheet structured packing. Chem. Eng. Res. Des. 1999, 77,
505.
(4) Stichlmair, J.; Bravo, J. L.; Fair, J. R. General model for prediction
of pressure drop and capacity of countercurrent gas/liquid packed
columns. Gas. Sep. Purif. 1989, 3, 19.
(5) Mackowiak, J. Pressure drop in irrigated packed columns. Chem.
Eng. Process 1991, 29, 93.
(6) Brunazzi, E.; Paglianti, A. Mechanistic pressure drop model for
columns containing structured packings. AIChE J. 1997, 43, 317.
(7) Billet, R. Packed Towers; VCH Verlagsgesellschaft mbH, D-
69451: Weinheim,New York, Basel, Cambridge, Tokyo, 1995.
(8) Meier, W.; Hunkeler, R.; Stocker, W. D. Sulzer Mellapak, Eine
Neue, Geordnete Packung fur Stoffaustausch-Apparate. Chem. Ing.
Technol. 1979, 51, 119.
(9) Rejl, F. J.; Valenz, L.; Linek, V. “Profile Method” for the
measurement of kLa and kVa in distillation columns. Validation of rate-
based distillation models using concentration profiles measured along
the column. Ind. Eng. Chem. Res. 2010, 49, 4383.
(10) Cai, T. J.; Resetarits, M. R. Pressure drop measurements on
distillation columns. Chin. J. Chem. Eng. 2011, 19 (5), 779.
(11) Onken, U.; Arlt, W. Recommended Test Mixtures for Distillation
Columns; The Institution of Chemical Engineers: Rugby, England,
1990.
(12) Fitz, C. W.; Kunesh, J. G.; Shariat, A. Performance of structured
packing in a commercial-scale column at pressures of 0.02−27.6 bar.
Ind. Eng. Chem. Res. 1999, 38, 512.
(13) Linek, V.; Moucha, T.; Rejl, F. J.; Prokopová, E. Simultaneous
determination of vapor- and liquid-side volumetric mass transfer
coefficients in distillation column. Chem. Eng. Res. Des. 2005, 83, 979.
(14) Rejl, F. J.; Linek, V.; Moucha, T.; Prokopová, E.; Valenz, L.;
Hovorka, F. Vapor- and liquid-side volumetric mass transfer
coefficients measured in distillation column. Chem. Eng. Sci. 2006,
61, 6096.
(15) Valenz, L.; Rejl, F. J.; Linek, V. Effect of gas and liquid axial
mixing on the rate of mass transfer in a distillation column packed with
Mellapak 250Y. Ind. Eng. Chem. Res. 2011, 50, 2262.
(16) Rocha, J. A.; Bravo, J. L.; Fair, J. R. Distillation columns
containing structured packings: A comprehensive model for their
performance. 1. Hydraulic models. Ind. Eng. Chem. Res. 1993, 32, 641.
(17) Rocha, J. A.; Bravo, J. L.; Fair, J. R. Distillation columns
containing structured packings: A comprehensive model for their
performance. 2. Mass-transfer model. Ind. Eng. Chem. Res. 1996, 35,
1660.

5974 dx.doi.org/10.1021/ie302397q | Ind. Eng. Chem. Res. 2013, 52, 5967−5974