Standard Is at Ion of SP

VERSION 1 - Standardization of Structured Packing Efficiency Measurements 14 March 2008
A Report on
STANDARDIZATION OF STRUCTURED PACKING

EFFICIENCY MEASUREMENTS
A Work in Progress
Version 1
by
Žarko Olujić
ZO Consulting
Associate Professor
Delft University of Technology

Process & Energy Department
Leeghwaterstraat 44
2628 CA Delft, The Netherlands
Encouraged and Supported

by
BASF SE
Delft, 14 March 2008
z.olujic@tudelft.nl 1
CONTENTS
FOREWORD 5
SUMMARY OF THE PROJECT 6
1. INTRODUCTION 8
2. PURPOSE AND AVAILABILITY OF DISTILLATION PILOT PLANTS 9
2.1 Packing Manufacturers Facilities 10

2.1.1 Sulzer-Chemtech
2.1.2 Koch-Glitsch
2.2 FRI 11
2.3 University Based Facilities 12

2.3.1 SRP
2.3.2 TU Delft
2.3.3 University of Alberta
2.4 User Companies Pilot Plants 14

2.4.1 Bayer Technology Services
2.4.2 Praxair
2.5 Plant Test Columns 14

2.5.1 Koch-Glitsch
2.5.2 Air Products
3. PILOT PLANT DESIGN AND OPERATION CONSIDERATIONS 15
3.1 Column Diameter 15
3.2 Bed Height/Depth 15
3.3 Packing Installation 16
3.4 Liquid Distribution 16

3.4.1 Drip point density
3.4.2 Drip point layout
3.4.3 Distributor positioning
3.5 Vapour Distribution 18
3.6 Test System and Conditions 18

3.6.1 Test system properties estimation
3.7 Liquid Sampling 20

3.7.1 Column profiles
3.8 Measurement of Flow Rates, Pressure, and Temperature 21
3.9 Pressure Drop Measurement 22
3.10 Reproducibility 22
3.11 Mode of Operation 23
3.12 Avoiding Systematic Errors 24
3.13 Process and Mechanical Design Considerations 25
4. TEST DATA EVALUATION, PRESENTATION AND INTERPRETATION 25
4.1 Representative F-factor 28
4.2 Representative Relative Volatility 29
4.3 Representative Efficiency 30
4.4 Representative Pressure Drop 32
4.5 Packing Geometry Effects 33
4.6 Test Documentation 34
5. CONCLUSIONS AND RECOMMENDATIONS 34
NOMENCLATURE 36
REFERENCES 37
APPENDICES
Appendix A Physical Properties of Common Test Systems 42
A1 Orto- / Para-Xylene 42
Table A1 – FRI data
A2 Chlorobenzene/Ethylbenzene (CB/EB) 42
Table A2a – Bayer Technology Services data
Table A2b - Sulzer data
Table A2c – Billet’s data
A3 Cyclohexane/n-Heptane (CH/nH) 44
Table A3a – SRP data
Table A3b - FRI data
Table A3c - TU Delft data
A4 Methanol/Water (M/W) 45
Table A4 – TU Delft data
A5 Methanol/Ethanol (M/E) 46
Table A5 – TU Delft data
A6 Isobutane/n-Butane (IB/nB) 46
Table A6 – FRI data
Appendix B Data Collection and Presentation Sheets 47
B1 Data Collection Sheet 47
B2 Data Presentation Sheet 47
NOTES: 48
FOREWORD
In what follows you will find a document that summarizes the results of a
literature study that was encouraged and supported by BASF SE. The objective was
to collect and evaluate relevant, publicly available information, and to come with a
proposal for standardization of structured packing efficiency measurements, which, in
turn, should lead toward obtaining more reliable basic performance data to be used
with more confidence in (re)design of industrial packed columns.
The present study is made publicly available by BASF SE to serve as a basis

for further improvements in all respects as a sort of open source document. The
home will be the website of Process & Energy Laboratory of TU Delft
(www.pe.tudelft.nl) and the coordination will be in the hands of the author of this
document.
Upon critical evaluation of the present text, the potential contributors are
encouraged to come with comments, discussions, and suggestions for
improvements, which should enable us to arrive at best practices. However, only the
productive proposals will be implemented, and this will occur upon approval of
involved contributors. This will be posted as new version and exposed to critical
evaluations, in form of an open forum. However, coordinator will try to ensure
convergence within a few iterations, i.e. achieving the best solution, to be accepted
and considered to serve as a general standard in the near future.
It is our hope that competent people from user companies, equipment

manufacturing companies as well as academic environment will be willing and
allowed to participate actively in this undertaking that should finally lead to adopting
the best practices as a standard for experimental characterization of structured
packings performance.
This could then serve as basis for establishing basic standards for testing all
types of gas or vapour/liquid contacting devices used in separation processes.
Delft, 12 March 2008 Z. Olujic
SUMARRY OF THE PROJECT
Ambient air/water studies provide in a relatively inexpensive and fast way

limited but highly useful information on hydraulic behaviour of a packing, depending
on gas and liquid loads, in particular on pressure drop and loading and flooding
points as well as related liquid hold-up. In order to establish the mass transfer
capability, the structured packings need to be exposed to more demanding and more
expensive total reflux distillation tests, which are usually carried out using one of
established test systems at operating conditions close to those of intended
application.
If the primary goal is to be able to make realistic comparisons between
performances of different packings then the whole effort can be reduced to choice of
a representative test system, and for structured packings two operating pressures
are essential, about 100 mbar and atmospheric pressure (about 1000 mbar),
respectively. This range covers typical applications of structured packings.
Regarding the test system, it is important to have one of the standard,
recommended binary mixtures, and for the above mentioned range of operating
pressures, chlorobenzene/ethylbenzene (CB/EB) is the best choice, because it is a
well established system adopted long ago at Sulzer and most recently at Bayer
Technical Services. In the USA, FRI and SRP prefer cyclohexane/n-heptane (CH/nH)
in this range and this is the second best choice and a system very well documented
in the literature. The ideal CB/EB system is more convenient because it exhibits a
constant relative volatility over the bed length. This avoids dealing with uncertainties
associated with the effect of the pressure drop on temperature profile, which in case
of mixtures with wider boiling range leads to significant differences in relevant
properties at top and bottom of the bed. A practical deficiency of CB/EB system is
that at atmospheric pressure, which requires a rather high operating temperature, the
highest liquid load encountered is well below values which could be interesting in
case one wish to see how a packing operates at liquid loads above 20 m3/m2h. With
CB/EB system at atmospheric pressure, a liquid load around 25 – 30 m3/m2h could
be reached only in conjunction with structured packings capable of operating at F-
factors around 4 Pa0.5. The CH/nH system is operated at SRP at 4 bar, and allows
reaching liquid loads up to 50 m3/m2h, at an operating temperature not exceeding
150 oC.
For test column diameter we may say: the larger the better, however with
increasing diameter the related costs increase and more time is needed for packing
installation and change, start-up time is longer as well as that required for reaching
the steady-state after changing the column (vapour) load. A reasonable test column
diameter is that corresponding to the double of the packing element height. Montz
and Sulzer sheet metal packings come with element heights about or slightly above
0.2 m, depending on the corrugation angle, and that of wire gauze packings A3 and
BX series is about 0.15 m. Packings manufactured in USA come with element
heights ranging from 0.25 to 0.3 m. With this in mind, 0.45 m represents a fair
average, between 0.3 m on lower and 0.6 m on upper side, respectively.
The test column should be tall enough to accommodate beds allowing for
generation of 5 - 25 (equilibrium or theoretical) stages. Enough height should be
available for installation of packing, 4 m being a good measure. Certainly, a test

section of 7 m, consisting of two flanged sections, would provide a great degree of
flexibility. For instance, it would allow installing two beds of 3 m, separated by a liquid
redistribution section, which also provides an opportunity for performing continuous,
finite reflux operation tests.
The liquid distributor should be a high turndown, high free area (around 50 %)
narrow trough distributor with uniformly distributed drip pipes, providing an initial
irrigation density of 100 to 150 drip points per meter square. If the operating pressure
range of the column is too wide, than two distributors of the same design should be
employed, one for lower and the other one for higher operating pressures, i.e. liquid
loads. Narrow trough distributors are industrial standard and that one or two
designed specially for a pilot plant should be used in all tests. In other words, a
distributor should not be changed, except if one wishes to observe possible
distributor design effect.
Vapour distribution is not critical, however this means not that any solution will
work effectively. Care should be paid and vapour inlet and distribution device should
be designed properly, in accordance with the chosen type of the reboiler. The best
provision in this respect is to have enough space between the gas (vapour) inlet and
packing support to install a chevron type liquid collector/gas redistributor, at a
distance in both directions equivalent to one column diameter, which, in addition can
be used to provide liquid sample representing quite well the composition of the liquid
leaving the bed.
Continuous (non-stop) operation under total reflux conditions is the best
operating mode. The time periods required to get to steady state after column start-
up, change of vapour load, and for taking three samples at each vapour load depend
on the size of pilot plant and need to be established during the start-up and initial
operation period. Then also the decision will be made whether to go from maximum
to minimum vapour load or vice-versa. Middle of the bed conditions are
recommended as reference for presenting tests results and making comparisons
between performances of different packings and operating conditions.
The effort behind this study was motivated by the need to arrive at a standard
for total reflux distillation installation and procedure for the purposes of comparative
testing of structured packing performances, which would enable obtaining results that
could be used with confidence for scale-up purposes. Elaborate analysis provided in
this report and thorough evaluations of all relevant factors provide a good indication
of best choices and practices. The experience gained by building and operating a
pilot-plant along the lines outlined in this report would serve as best foundation for
reaching the final goal, i.e. a standard test.
1. INTRODUCTION
There is no doubt that distillation was and still is by far the most widely applied
separation technique in process industries. Regarding the ever growing needs for
bulk-chemicals and the extent of grow of process industries in Far East it seems that
its importance will even increase in the foreseeable future. A major consequence of
this strong grows is that larger and larger equipment is built to stay competitive,
which implies further challenges regarding the scale-up and design practices. The
amounts of capital and energy involved require as tight as possible column designs
and this posses challenges on scale-up know-how side, which, in turn relies mainly
on efficiency and hydraulics’ data obtained from total reflux experiments carried out
with much smaller equipment using one of standard test systems, often at conditions
different from that of intended application.
Although a lot of experimental work has been done in the past and well
established large companies have also collected addition practical knowledge from
operation of their plants, the design of new as well as redesign of existing columns
still encompasses a wide range of concerns. These are mainly related to
uncertainties with respect to expected hydraulic and mass transfer performance of
novel, performance improving gas/vapour-liquid contacting devices, developed and
brought to the market in the meantime by equipment manufacturers.
All three main families of vapour (gas)-liquid (G-L) contactors for distillation
and related separations, i.e. trays, random packing, and structured packings have
experienced significant improvements in this respect. The main stream of such
developments is concerned with capacity increase (revamps-retrofits) or size
reduction (new designs) of distillation columns, accompanied, if feasible, by energy
saving per unit of product (reduction of external reflux), but most of these
developments aim at reaching the capacity increase goal without affecting the
separation efficiency adversely. The certainty regarding the hydraulic and mass
transfer performance of the G-L contactor considered plays a crucial role for success
of such a total cost reduction effort. In order to get this certainty, i.e. to minimize risks
associated with building very expensive industrial plants, user companies tend to
have dedicated pilot plant scale tests performed, which may be used to
validate/verify the predictive models.
The emphasis of this study is on the performance characteristics of structured
packings, more precisely on clearing the issues associated with usability of total
reflux measurements, carried out with established test systems in pilot to semi-
industrial scale test installations, for (re)design purposes. In this respect the report
follows the line of a presentation given by T. Friese of BASF, at GVC-Fachausschuss
Fluidverfahrenstechniek meeting held in February 2005 in Luebeck, Germany [1].
This presentation moved a group of distillation user companies to consider
establishing standardized testing procedures as a measure to arrive at more
confidence in this respect, and this expectation has been considered and handled
accordingly in this report.
2. PURPOSE AND AVAILABILITY OF PILOT DISTILLATION TESTS
Packing hydraulics’ related experiments are usually carried out using air-water
system at ambient conditions, to observe the suitability of the packing with respect to
the liquid hold-up, pressure drop and capacity. Promising configurations are then
exposed to distillation experiments, most commonly under total reflux conditions, to
get impression on achievable efficiency. In general, the main objective of pilot testing
of a packing under total reflux conditions is to determine:
(i) The mass transfer efficiency of the packing;

(ii) The maximum capacity of the packing; and
(iii) The pressure drop of the packing as a function of vapour load (boil-up
rate).
Usually the packing performance data are generated using large enough total
reflux distillation columns in conjunction with one of established test systems,
described in the booklet “Recommended Test Mixtures for Distillation Columns” [2,3].
Namely, long ago it has been realised that some standardisation is required
regarding the choice of the test system, and the EFCE Working Party on Distillation
came with a proposal in this respect and produced in 1960s under editorship of F.
Zuiderweg the first edition of this booklet [2]. The next, thoroughly revised and
updated edition, written by Onken und Arlt , was published in 1990 [3].
There are several more or less accessible sources of total reflux data. First we
should mention Billets books [4,5]. Until the retirement of Prof. R. Billet the University
of Bochum was the place where many conventional and novel random, and certainly
all first generation structured packings were tested. Unfortunately, the total reflux
column used for these purposes had an insufficient diameter (d = 0.22 m) to be
considered as source of data to be used directly for scale-up purposes. All the details
around this installation, test systems used and many of generated results produced
in cooperation with Dr. J. Mackowiak and later on Dr. M. Schultes are well
documented in Billet’s book Packed Towers [5]. Additional information on packings
tested in Bochum can be found in Mackowiak’s book “Fluiddynamik von Kolonnen mit
modernen Füllkörpern …” [6]. Billet’s book contains also some data on performance
of conventional random packings obtained in a column with an internal diameter of
0.5 m. This one as well as a column with an even larger internal diameter (0.8 m),
available in 1960s at BASF in Ludwigshafen, were extensively used to generate
scale-up know how, needed for design and/or operation of, at that time, extremely
large columns for separation of ethylbenzene/styrene mixture. It should be noted
that in these devoted experiments, the ethylbenzene/styrene system was used at
appropriate operating pressure. A detailed description of the test installations and
obtained results including Sulzer gauze packing BX performance evaluation can be
found in Billets book “Industrial Destillation” [4]. It should however be noted that 0.8
m diameter was chosen for the purposes of testing tray performances appropriately,
and that a 0.5 m diameter total reflux column was considered as large enough
regarding the scale-up needs for packed columns. A recent BASF based study [7],
discussing the needs for even larger, industrial scale testing facilities, suggests that
operating pressure should be considered when choosing the diameter of the test
column, indicating that for most common packed column applications (0.1 bar to
atmospheric pressure operations) the diameters above 0.3 m should be sufficient.
Large scale equipment manufacturers, like presently Koch-Glitsch and Sulzer
Chemtech prefer to relay on their own facilities, and their data are generally not
publicly available. Most prominent source of distillation equipment test data is
Fractionation Research Inc. (FRI), and their data are available to member companies
only. FRI as well as some other institutions (Bayer Technology Services, BTS, and
Separations Research Program, SRP) are willing to perform commercial tests for
customers, which implies that the customer decides whether and to whom to release
the data, and these remain mainly unavailable to public. The chance that some
performance data will be published is largest with data produced using adequate
facilities available at universities, however these are the least consistent regarding
the nature of experimentation and available equipment and technical support. Finally,
the user-companies have often adequate facilities to be used preferably for own
purposes only. However, it must be realized that during the last two decades of last
century due to increased costs and reduced technical support, most of the bulk
chemicals manufacturing companies abandoned this practice. In fact this occurred
everywhere and today there are few facilities left, which can satisfy the growing
needs in this respect. The exceptions in this respect are air distilling companies.
Distilling air at cryogenic conditions to produce high purity oxygen, nitrogen and
argon, respectively, is a very specific activity and a really large scale worldwide
business, and the competition of big players in this field is especially strong.
Therefore they all prefer to use own test facilities, which, due to the nature of the
system and cryogenic test conditions, have been held on smaller size. With the need
to design the columns with larger and larger diameters for very sharp separations
they also got confronted with the need to consider performing experiments at the
scale close to their industrial operations and conditions. From these reasons, few
years ago Air Products decided to design and build a large enough (industrial scale)
test column. On the other hand, Koch-Glitsch invested into transformation of suitable
former industrial column into a test unit. However, soon after performing first series of
dedicated tests, the related expenses appeared that high that this discouraged
offering these facilities for commercial purposes and even discouraged similar efforts
for own purposes. Therefore it looks to be that present day, state of the art facilities
have to be as small as bearable, i.e. technically responsible, to have a chance to be
used frequently.
Regarding this fact, it appears that the overall quality and usability of data
produced using adequate – as small as good enough - size facilities becomes a
concern. In what follows an overview is given of available total reflux test facilities.
2.1 Packing Manufacturers Facilities
2.1.1 SULZER Chemtech

From beginning on Sulzer recognised the importance of the scale of
experimentation and most of their test data on performance of various Mellapak and
MellapakPlus family packings come from a 1.0 m internal diameter column, which is
operated in conjunction with thermodynamically ideal Chlorobenzene/Ethylbenzene
system at two pressures, i.e. at 100 and 950 mbar. It should be noted that in Sulzer
laboratory in Winterthur there are also total reflux columns with smaller diameter
which can be operated at high pressures, as well as a number of hydraulic, air-water
installations which provide for collecting all range of data of interest for understanding
and properly correlating the performance of new packings. The collected data have
been correlated and can be found for all Sulzer packings in the software package
Sulpak, which is available on request from Sulzer Chemtech via their website. It
should be noted that Sulpak simulates the hydraulics of Sulzer structured packings
well, but there are no provisions made for estimation of the packing efficiency with
different systems. The only efficiency related information contained is that on
experimentally determined number of equilibrium stages (theoretical plates)
contained per unit bed height for main types and sizes of Sulzer packings as
determined with CB/EB system using Sulzer test facilities. Occasionally, some of
efficiency data are presented at conferences [8-11], and the results obtained over the
years with Mellapak 250.Y at FRI have been published [12].
2.1.2 Koch-Glitsch (including former Norton)

The Koch-Glitsch Company, which relies on know-how developed by two
companies in the time Glitsch and Koch were on their own. Both however used own
facilities to substantiate development of own packings and perform customer tests,
and this is done presently by Koch-Glitsch. Unfortunately, there is practically no
publicly available information on their experimental work. However, first generation of
Koch structured packings (Flexipack, which was in the time of association with Sulzer
actually Mellapak with larger element height) have been tested at SRP [13].
Nevertheless, Koch-Glitsch is now in possession of the state of the art pilot
scale total reflux distillation installations of former Norton CPP Corporation which was
a very well established manufacturer of random and structured packings and
distillation and absorption columns in general, and until recently a global distillation
equipment player. Some of the comprehensive experimental work carried out with
Norton packings in a column with internal diameter of 0.381 m is documented in open
literature [14], including a thorough description of pilot plant facilities and test
procedures. Norton know-how and design practices as well as experiences with
application of Norton packings in industrial practice are discussed in [15] and in wider
context in the book “Packed Tower Design and Applications–Random and Structured
Packings” [16], written by a pioneer in development of new generation of high
performance packings and designs of large diameter packed columns, Ralph Strigle.
Interestingly, unlike other institutions Norton used the toluene/iso-octane
mixture at atmospheric pressure and 133 mbar (100 mmHg absolute) as standard
system, which does not belong to recommended tests systems [3], but was used
occasionally by Billet [5].
2.2 FRI
This well known independent distillation equipment testing institution makes
dedicated performance tests in one of two 1.2 m internal diameter column, covering a
wide range of operating pressures, from high vacuum (down to 0.1 bar) to high
pressure (up to 27 bar) using appropriate test systems. FRI member companies are
well acquinted with all technical details related to FRI installations and test
procedures. Tables A1, A3b, and A6 in Appendix A summarise average properties of
tests systems used at FRI for performance evaluation and interpretation purposes. A
detailed description of the test facilities and procedures adopted can be found in
recent publications [12,17].
2.3 University Based Facilities

2.3.1 SRP
During the last two decades the Separations Research Program, associated
with the University of Texas at Austin developed into an established pilot-scale
testing institute, where total reflux distillation facilities are extensively used for
commercial testing. Some of these test results are available for the members of the
SRP, and very limited amount of data is available publicly. Limited information on
performance characteristics of first generation of American sheet metal structured
packings can be found in a paper discussing the accuracy of SRP predictive model
for structured packings [13]. Most complete in this respect are recently published
data on performance of some conventional J. Montz structured packings [18] as well
as of some of the first generation Montz high capacity packings [19].
These publications contain a detailed description of the installation used. The
heart of this installation is a 0.43 m internal diameter column, allowing bed heights
between 1 and 4 m, which, however can be nearly doubled by installation of another
bed above the common one. The test system is Cyclohexane/n-Heptane, and the
column is operated at 0.17, 0.33, 1.03, 1.66, and 4.4 bar absolute, depending on the
choice of the customer. Table A3a in Appendix 3 contains typical bottom of the bed
temperature related physical properties and operating data. The liquid distributor
preferred is a wide range, Montz narrow trough type, with 21 drip tubes, which is an
equivalent to 145 drip points per meter square.
In order to be convincing regarding the reliability and usability of
measurements performed in a 0.43 m ID column, SRP carried out an internal study
comparing results obtained with some conventional random and structured packings
with that obtained with the same packings at FRI at same conditions [20]. Although
different types of liquid distributors were used, there were no significant differences
observed in compared efficiencies, except those imposed by a too large difference in
operating stripping factors. Stronger deviations in results were observed only at
lowest F-factors (end effects, due to imperfection of liquid distributor used at FRI),
and hydraulic behaviour was similar enough to exclude any significant difference due
to scale of experimentation. Anyhow, it should be noted that this exercise was
completed using a lot of engineering judgement, because the differences in facilities,
methods and data were too large to provide a basis for an objective evaluation. After
this experience, SRP decided to standardise their equipment and procedures as
much as possible.
It should be noted that SRP facilities, used extensively for proprietary tests,
are handled and operated by an experienced and skilled group of permanent staff
members under supervision of Dr. A. F. Seibert. Since the last complete overhaul of
the available facilities, the tests are run on day and night basis, starting Monday
morning and ending on Thursday evening or Friday morning, depending on the
number of points to be measured. The samples are taken at regular intervals and
during the night this is done by trained external people (mostly UT students) hired for
this purpose.
2.3.2 TU Delft
Thanks to an equipment donation from J. Montz GmbH, the Laboratory for
Process Equipment managed to assemble in the late 1990s a state of the art total
reflux distillation facility, which however appeared to be suitable for a smooth
operation at atmospheric pressure only. This unit was extensively used for screening
test during development of new generation of high capacity Montz packings.
Subsequently it was used for performance evaluation of new generation of Sulzer
catalytic packings from Katapak SP series [21]. A detailed description of this plant
with a column with an internal diameter of 0.45 m and packed heights up to 2.5 m
can be found in a most recent publication on performance evaluation of Sulzer high
performance structured packing MellapakPlus 752.Y [22]. Table A3c in Appendix A
contains the physical properties of the CH/nH system, corresponding to the middle of
the bed temperature.
The tests carried so far at TU Delft have been carried out under direct
supervision of the PhD student and carried out by a number of MSc students who did
their work as part of their graduation programme. These students stayed six to twelve
months with the group and proved to be highly responsible and skilled operators.
There have been some day and night operations carried out and after evaluation it
appeared that there is no visible difference in measurements when compared to
common daily operation practice, provided enough time has been allowed for
reaching the steady state after start-up and each change of conditions. The non-stop
operation enabled completing a test for a packing within one week, while the
discontinuous operation required two to three weeks to complete a test (8 to 10
points). Since the non-stop operation proved to be practically impossible, because a
PhD student or permanent staff member had to be part of the “dead-man shift” from
safety reasons and for students this also appeared to be unacceptable for a longer
period, the TU Delft adopted common daily operation which effectively means that at
least three weeks are needed for a full scale test. Bringing changes, like liquid
distribution quality manipulation, or other research motivated modifications of the
hardware requires additional time and cannot simply be expressed in money.
As reported in [22], the TU Delft column was also operated with non-ideal
Methanol/Water system (M/W), which also was employed in some studies carried out
at the University of Alberta in Edmonton [23]. Properties of M/W system can be found
in Table A4 in Appendix A. Table A5 contains properties of Methanol/Ethanol system
(M/E) which was used earlier at TU Delft [24,25], during imposed maldistribution
studies performed with some of first generation sheet metal, and Montz expanded
metal packings, respectively. Both M/W and M/E belong to recommended tests
systems [3].
2.3.3 University of Alberta

The group of Prof. K.T. Chuang is a frequent contributor of data on
performance of innovative trays and packings. The internal diameter of the total
reflux column is 0.33 m, and the test systems used in conjunction with structured
packings were Methanol/Water, and Methanol/Isopropanol [23].
2.4 User Companies Pilots

2.4.3 Bayer Technology Services
New technical laboratory at Bayer in Leverkusen contains two semi-industrial
scale columns, one with an internal diameter of 0.8 m and the other one with 0.6 m
that are used occasionally for small scale production purposes. The smaller one was
chosen to be used as packing testing column in conjunction with CB/EB system,
operated at 0.1 and 1 bar, respectively. This column was used for testing a number
of prototypes of new generation of high performance Montz packings. The BTS
installation and some results are described in a most recent publication [26].
2.4.4 Praxair
A column with 0.305 m internal diameter operated at total reflux with argon
and nitrogen under cryogenic conditions was used extensively for evaluation of basic
performance of commercially available structured packings suitable for application in
cryogenic distillations. The packed height was typically 2.4 m. This unit was also
used to evaluate performance of new generation of high capacity structured
packings, as introduced by researchers from this organisation [27].
It should be noted that newest generation of air distilling columns with feed
rates well above 100 t/h, require large diameters (large specific area packings are
preferred to reduce column height from energy conserving reasons) and this poses a
challenge regarding the uncertainties related to scale-up based on small column
diameter data. In answer to this Air Products decided to design and operate a small
industrial scale column, described in following section.
2.5 Plant Test Columns

2.5.1 Koch-Glitsch
As described in a paper by Weiland et al. [28], an existing depropanizer
column, with an internal diameter of 1.52 m, available at Koch Hydrocarbon’s
Medford, OK, plant has been transformed into a research column. However, the
reported results concern modern trays only, and there is still no evidence that this
column has been employed for structured packing testing as announced. Since this
column is a part of the production plant and receives the feed from a deethaniser
column, its application is limited to typical depropaniser feed mixture and operating
conditions. Therefore this large scale installation is not suitable for structured packing
tests.
2.5.2 Air Products

The heart of the sophisticated plant scale installation of AIR Product at
Carrington in U.K. is a cryogenic column with internal diameter of 0.9 m and enough
height to install long beds (up to twenty theoretical plates). Argon/Oxygen (Ar/Ox)
separation tests indicated that deeper beds experience deterioration in efficiency due
to developed liquid maldistribution [29]. The essential information came from the
utilised liquid sampling system; with a cross type sampler with four points located
bellow the bed periphery and the fifth sampling point below the middle of the bed.
Interestingly, a comparison with a similar test carried out in their standard 0.2 m ID
column indicated a significant discrepancy in efficiency, i.e. a much lower efficiency
than that obtained with small column. Hydraulics was also affected but not so
pronouncedly as efficiency.
3. PILOT PLANT DESIGN AND OPERATION CONSIDERATIONS
This section addresses factors of importance for test equipment design and
operation as well as operating procedures and measurements.
3.1 Column Diameter

As mentioned before there is a general belief that columns with diameters
above 0.3 m should bi sufficient regarding the usability of efficiency and capacity data
for structured packings. As shown elsewhere [30], early Sulzer studies indicated
absence of diameter effect on efficiency of gauze BX and sheet metal Mellapak
250.Y packings. However, the pressure drop and capacity appeared to be strongly
dependent on diameter and a recent scale-up hydraulics study [31] indicated that
column diameter should be larger than two times the packing element height to
minimize the adverse effect of column wall zone, due to cross section reduction by
wall wipers and increased number of bends in the vapour flow, with respect to that in
the bulk of packing. This indicates that the column diameter should be about 0.40 m
or even larger. For instance, 0.6 m diameter as encountered at BTS is a fine
measure. Namely, Koch-Glitsch and former Norton packings come with element
heights around 0.3 m, and in this case a diameter of 0.6 m meets the two element
heights rule.
However, the larger the equipment the longer the time to reach the steady
state and, importantly, the larger the investment and related operating costs. The
latter suggests that 0.45 m, as encountered in Delft should be the best compromise
between 0.3 m on lower and 0.6 m on larger side.
3.2 Bed Height or Depth

Usually the bed heights involved in performance tests are lower than those
installed in practice. Regarding the tendency of liquid to maldistribute with increasing
bed depth this means that the results obtained with short beds could be on optimistic
side. This is certainly so in case of sharp separations. However a pilot scale
experiment particularly that performed under total reflux conditions can not give full
certainty in this respect. In any case doubling the common bed height would be a
good provision, particularly if additional length is provided to install a redistributor, to
enable a comparison of a short bed and single long bed and a two shorter bed in
series. This kind of experimental exercise is useful and as demonstrated in Ar/Ox
cryogenic distillation case may provide information on the extent of deterioration
expected if the bed height/depth is maximised, which is often the case with retrofitting
the existing tray columns (manhole location imposed).
However doubling the bed depth should not compromise the accuracy of
experiment. This means that a tests system needs to be chosen, which, in
conjunction with maximum bed height, will not result in extreme overheads purity that
could lead to substantial errors in composition and consequently the packing
efficiency. A good measure is to have enough height to ensure 20-25 theoretical
stages in a bed, which will certainly depend on the specific geometric area of the
packing and, in same cases, F-factor. So if a packing with 250 m2/m3 is taken as
reference size and 15 theoretical stages as a basis than 6 m height reserved for
packing installation would be a good choice, in conjunction with a close boiling
system like chlorobenzene/ethylbenzene, which allows having such a high number of
theoretical stages without compromising the above mentioned overheads purity. If
single bed, packing performance comparison studies are main purpose, then a
packed height of 4 m will be sufficient.
Another consideration related to the height of a bed is the mechanical strength
of the packing and the support system. With present very low material thickness
(about 0.1 mm) the weight of packing elements fitting into a test column is that low
that this is not a concern. In any case, the packing should be supported by a highly
open flat grid and installed in layers with each element rotated 90 degrees to
previous one. This is a normal bed configuration, providing for maximum large scale
mixing of both phases. According to our knowledge only Norton deviated from this
practice by rotating the subsequent layers by 60 to 70 degrees, which was most
probably done to keep the pressure drop acceptable. Namely, the surface of Norton
Intalox Structured Packing was very rough, thus causing a pronounced pressure drop
due to skin friction, which had to be compensated somehow, and reducing the angle
of rotation of packing layers was a practical solution to this.
3.3 Packed Bed Installation

Method of packing the test column must be established and used every time
the column is packed. This means that first packing element needs to be placed
properly, because following ones will be placed by rotating them accordingly (90
degrees is standard) with respect to previous one. In TU Delft column the first
element is placed so that parallel channels are oriented perpendicularly to the
orientation of the bayonet liquid sampler. This is done to ensure a representative
sample. Other organizations prefer using cross samplers and take some other
parameter as reference point for placing the first packing element. At SRP in USA, it
is common practice to take South-Nord or East-West orientations as a guide.
Another important thing to do while installing the packing is to ensure that wall
wipers are turned out to fit tight to the column wall (they should scrap the wall while
pushed down the column). The smaller the column diameter the greater is the
certainty that bypassing of vapour and liquid will damage the efficiency of the packing
to some extent.
3.4 Liquid Distribution

The liquid distribution quality is primary concern in this case and a thorough
consideration is needed to arrive at a satisfying distributor design. As proven in
industrial practice the narrow trough distributors appeared to be the best
configuration design in conjunction with structured packings. These are generally
designed with perforations (not bottom, fouling sensible) in trough walls or in the
walls of drip tubes.
The turndown ratio of a test distributor is often maximised to cover a wide
range of liquid loads associated with operations at different pressures. Indeed it is
very practical to use the same distributor for different tests. The high turndown can
be ensured only by having a high enough liquid head in combination with several
levels of orifices. If a turndown above 10 to 1 is required it is common practice to use

two distributors designed to perform well at low and high liquid loads range,
respectively.
3.4.1 Drip points density

The size of packing plays a role in this, because it appeared that the packings
with relatively small specific area, say 250 m2/m3, require less drip points to operate
satisfactorily than the large specific area packings, with 500 or 750 m2/m3. This is so
but not as pronounced as it would be expected. A good choice for testing packings is
a distributor with 100 – 150 drip points per meter square, because this allows both
250 and 500 packings to be tested without sacrifice in accuracy. An advantage of
employing a smaller number of drip points in industrial practice is that orifices
become larger for the same flow rate, which is the best way of avoiding fouling
related problems.
Narrow trough distributor with drip tubes is preferred, because it can ensure a
very large turndown ratio (up to 10) without affecting the pattern of initial liquid
distribution adversely. Such distributors, as designed and delivered by Montz are in
use at SRP, TU Delft and BTS. A practical advantage is that the same distributor can
be used to increase the number of drip points by factor three or even seven, if
necessary, by attaching simply corresponding proprietary type of a drainage sleeve
to the drip tubes.
3.4.2 Drip points layout

Layout, i.e. cross sectional distribution of drip points is more important than the
flow accuracy/variation of individual drip points, which is according to present
standards within 5 % or less deviation from mean flow rate. SRP and TU Delft use
high-turndown Montz type of narrow trough distributors with drip tubes, which
ensures constancy in the initial flow distribution pattern over the whole range of
employed liquid loads. At SRP, two distributors are used to cover the whole range of
operating conditions, ranging from 0.17 to 4.14 bar. The distributor used at TU Delft
contains 10 drip tubes at periphery (wall zone) and six in the centre, which is an
equivalent to 100 drip points/m2. The same type of the distributor used frequently at
SRP contains 21 drip tubes, which is an equivalent to 145 drip points/m2.
3.4.3 Distributor positioning

Depending on column design the liquid distributor can be fixed using support points
on the column wall or placed on the packing. In latter case a support similar to
packing support needs to be used as carrier connected to the distributor with four
vertical bars with screws allowing adjustment, vertically and horizontally. The drip
tubes should be levelled at a distance of 2 to 5 centimetres above the top layer of the
packing.
If the layout of drip points leads to a number of drip points in line, which is
commonly the case with narrow trough distributors, the distributor should be placed
somewhat rotated, 45 degrees being a good angle, with respect to the channels of
the top element of packings. This way it will be prevented that the liquid from one
trough drains onto channels formed between two sheets only, which requires more
packing layers than normal to redistribute properly.
3.5 Vapour distribution

Vapour distribution is not generally a problem in pilot-scale columns if the
packing is placed at least one column diameter above the vapour inlet. Hoverer, in
small diameter columns the distance between gas inlet and packing support is short
and with increasing column load the inlet gas velocity increases and if there is no
effective distributor involved the vapour stream may hit the opposite wall and be
deflected upwardly to enter the packing concentrated in one section leaving some
other areas with much less flow. This strongly maldistributed inlet vapour flow will be
smoothed fast, within few packing elements, however this condition results in
pronounced liquid maldistribution in lowest packing elements, which, in case of short
beds can affect efficiency adversely. Therefore it is recommended to have a working
initial vapour distributor design, and for pilot scale columns with a two-phase feed a
shroud baffle design was found to be effective in this respect. If enough space is
available between vapour inlet and bed and only vapour is entering the column then
a chimney-tray or chevron (vane)-type liquid collector/gas redistributor can be used. It
should have a free area of 40 % or more and be placed at least one diameter below
the bed. This option is recommended.
3.6 Test System and Conditions

This is a crucial point. Certainly the most suitable among recommend test
systems [2, 3] should be chosen. FRI prefers three systems, depending on pressure
range, orto-/para-xylene for high vacuum range (below 0.1 bar), CH/nH for low
vacuum to above atmospheric pressures (0.1 – 1.7 bar-a) and isobutane/n-butane for
high pressure applications (6 – 27 bar). In Europe, the most common tests system is
CB/EB, adopted at Sulzer and BTS, in conjunction with two operating pressures, i.e.
100 (0.1 bar) and 960/1000 mbar, respectively. The characteristic properties of the
systems mentioned are summarised at a chosen test condition in corresponding
tables in Appendix A.
As mentioned under “Bed Height or Depth” there is a correlation between the
test system and bed height, i.e. the number of equilibrium stages contained in a bed.
Practically, this means that separation power of bed should be kept low enough to
avoid extreme purities of the overheads, which can lead to large errors in
composition. In general, bottoms containing less than 10 mole %, and overheads
containing more than 90 % of more volatile component should be avoided. Also, feed
composition should be balanced to avoid depletion of one component. A 50/50 feed
composition is natural choice, but to avoid excessive top purities with installed bed
height, some quantity of more volatile component is removed. So an initial feed
containing around 40 mole % of the light boiling component is a good initial value,
however this is something to be manipulated accordingly to ensure desired distillate
purity.
Since the primary purpose of the experimental effort is to compare the
performances of different packings, relaying on only one proven system is
recommended. Taking all factors mentioned in consideration, the most appropriate
test system for structured packings looks to be the chlorobenzene/ethylbenzene. The
only deficiency may be the limitation with respect to achievable specific liquid load,
which is well below 20 m3/m2h at atmospheric pressure. Nevertheless, higher liquid
loads can be obtained with this system at atmospheric pressure if operated in
conjunction with low specific surface area, high capacity packings that can operate at
F-factors well above 3 Pa0.5. Operation with this system at higher pressure is avoided
because it imposes impractical (very high) operating temperature. CH/nH system is
better in this respect, and 4 bar operation, as adopted at SRP [18,19], allows
reaching specific liquid loads up to 50 m3/m2h at an operating temperature which is
50 degrees lower than that corresponding to the pressure required to reach the same
specific liquid load with CB/EB system (around 200 oC).
In general, 0.1 bar and 1 bar pressures as applied in conjunction with CB/EB
system are standard operating pressures adopted at BTS and Sulzer, which covers
most of industrial applications of structured packings. These two operating pressures
are well established reference values. Going deeper into vacuum, say to 0.05 bar, is
useful because it approaches closer conditions associated with distillation of fine
chemicals, which is usually carried out using high specific geometric area, wire gauze
packings like A3 series from Montz or BX series from Sulzer. An intermediate value,
say 0.3 (roughly factor 3 to both, 0.1 bar on lower and 1 bar on upper side) could be
attempted, but it may prove unnecessary. While going below 0.1 bar is rather easy to
accomplish, provided enough heat transfer area is installed, above-atmospheric
pressure operation with CB/EB system may prove demanding. Major concern is, as
mentioned above, the rather high operating temperature. In addition, relative volatility
is then expected to drop below 1.1, where sensitivity to measurement errors may
become substantial.
3.6.1 Test system properties estimation

For the test system chosen, various properties need to be estimated as a
function of pressure, temperature and composition in the operating range of interest.
First of all, we deal here mainly with binary mixtures and average mixture properties
are used, based on molar or weight fractions of pure components, present in top and
bottoms mixtures, respectively. In other words, the characteristic mixture properties
are determined on additive (weight or molar) basis from pure component properties,
separately for top and bottom conditions. Usually, an average, either geometric or
arithmetic mean is used as representative value, which can be considered as
representing the “middle of the bed” conditions.
For a test system, the pure component properties required for representation
of the results of the experimental work are:
(i) Molecular weights,

(ii) Vapour pressures,
(iii) Densities of vapour and liquid
(iv) Enthalpies of vaporisation
(v) Specific heat capacity of the liquid
For data interpretation and performance modelling studies following properties will be
needed:
(vi) Viscosities of liquid and vapour,

(vii) Diffusivities of the liquid and vapour, and
(viii) Surface tension.
For instance, for an ideal tests system like CB/EB, the relative volatility is
equal to the ratio of vapour pressures of pure components, which can be determined
using Antoine equation with corresponding constants. Gas density can be estimated
with confidence using the ideal gas law based expression. However for liquid density
and for other properties it is best to use polynomials with experimentally determined
coefficients, covering the full range of operating conditions.
The related sensitivities and uncertainties in conjunction with possible sources
of errors will be discussed later on where appropriate.
3.7 Liquid Sampling

Usually liquid samples are preferred, taken above and below the bed. Reflux
return line is a natural choice for taking the representative sample of the overhead
vapour/liquid composition. Certain degree of sub-cooling the reflux is desired to avoid
flashing in reflux return line. The problem is how to obtain a representative sample of
the liquid leaving the bed. Most common practices are using a cross bayonet type of
the sampler (FRI, SRP) or a simple bayonet sampler (TU Delft) placed directly under
the packing support plate. In the latter case, the half-open cut (slotted) tube is placed
perpendicularly to the orientation of the packing sheets in the bottom layer of
packing, to allow collecting the liquid from nearly all channels, which however covers
only limited part of column cross sectional area. This sample is compared with the
sample taken from the line leaving the bottom of the column to get an impression
about the extent of possible mass transfer during the fall of droplets from bed into to
the column sump (negligible in TU Delft case). If a chimney tray or chevron type
liquid collector is placed in between the bottom of the packed bed and the vapour
inlet, then a side draw can be used to collect the liquid sample, which will be a good
representative of the composition of liquid leaving the bed. If partial reboiler is used
and the sample is taken from the line connecting column sump with the recirculation
pump, than a separation effect equivalent to one stage can be expected and this
needs to be accounted for appropriately when determining the number of stages
contained in the packed bed.
The main concern with sampling is to get the representative sample at the
moment of the measurement without taking a lot of liquid out of the column to get a
fresh liquid sample. This can be achieved by using sophisticated commercially
available devices as it is done in Delft, which by virtue of their design enables taking
the fresh sample only. The device itself resembles a ball valve placed in a line, and
does not incorporate any dead volume.
The critical step is transfer of the liquid sample from the sampler’s bottle to
small bottles for gas chromatograph processing. Early days the cheapest way to
analyse liquid samples was using a refractometar, which implies exposure of thin
liquid layer to atmosphere and the possibility for the some loss of the light component
by evaporation. A precaution was to cool the sample to room temperature or lower to
avoid this, but with present gas-chromatograph of other more advanced analysing
techniques the samples do not need to be exposed to atmosphere and by proper
handling the chance for errors is reduced to minimum. A practical advantage of gas
chromatography is that rather small quantities of fluid sample are needed. To reduce
chances for analysis errors the liquid sample should be split into three separate
samples and it is always recommended to run reference samples with compositions
matching the range of change produced during test. This should be done at frequent
basis and duplicate samples should be provided for sample and analysis verification.
3.7.1 Column profiles

As demonstrated in the last paper by Zuiderweg [32], knowing the composition
and temperature profiles of a test column could be very useful. Main reason for this
was tracing and identification of sources of liquid maldistribution, observed during
tests with first generation structured packings at FRI. Indeed, FRI has practised
taking the liquid samples along the bed, utilising bayonet type samplers protruding
through the bed, perpendicularly to the orientation of flow channels in the packing
layer. This worked satisfactorily however it inflicts damage to the packing and creates
possibility for certain extent of lateral transport of liquid, i.e. maldistribution, as well as
for flow disturbances associated with local splitting and acceleration of gas flow. If
concentration profile information is desired, then splitting the bed into corresponding
number of sections, separated by extended packing support structure should be
considered, because it allows practically undisturbed taking of liquid (and if desired
vapour) samples, as well as recording the corresponding temperature, and pressure
if desired.
3.8 Measurements of Flow Rates, Pressure, and Temperature

Certainly, the measurements of all relevant operating parameters must be of
adequate quality and continuously recorded and saved. This includes the flow rate,
temperature, pressure, and composition of reflux and bottom liquid streams. Top
pressure and temperature should be measured continuously as well as the
temperature below the bed. In addition steam pressure at inlet to reboiler and
temperature and flow rate of condensate at the outlet of reboiler need to be recorded
as well as the flow rate and inlet and outlet temperatures of cooling water. The
accuracy of the state of the art devices for measurement of temperature, pressure,
pressure difference, and flow rates is rather high, with deviations usually not larger
than 0.1 % of maximum or measured value. Choice, calibration and use of
thermometers, manometers and flow meters suitable for different purposes should be
done in accordance with established company practices, and will not be considered
here.
With known conditions of external streams overall and component material
balances and overall heat (enthalpy) balance can be calculated. An extremely useful
aid for analysing the performance of a packed bed is the temperature profile obtained
by measuring the temperature at a number of points along the bed. This could be
done by inserting the thermo-wells on top of each second or third packing element.
By placing five equally spaced sensors, one in the middle and four at periphery
forming a cross, reliable average values could be obtained while the differences
between individual readings, if pronounced, could be a good indication of liquid and
vapour distribution across and along the column. This is basically a simple version of
a well known technique implemented by Stichlmair and co-workers to trace and
quantify the extent of liquid maldistribution in packed beds [33,34]. This technique is
much less intruding than that using bayonet type samplers to collect liquid samples
from a bed. However, both techniques are demanding and should be implemented
only if justified by the objective of the tests.
3.9 Pressure Drop Measurement

Accurate differential pressure meters are required. Sources of possible
measurement errors should be eliminated by design, and the most notorious
wrongdoer in this respect is the inevitable condensation of a part of vapour in tubes
connecting pressure taps with sensors which in case of small diameters leads to
pressure line plugging, causing excessive fluctuations in pressure. Namely, vapour
filled lines are preferred because this way pressure is sensed directly, and to avoid
condensation related problems large enough diameters have to be taken say 10 or
12 mm for pressure lines. They must be free draining; otherwise provisions should be
made to enable inert gas blowing the condensate from the line during the start up
and occasionally during operation. Free draining is ensured if pressure sensing
devices are installed above the lower and upper pressure tap. Seal pots are
recommended and should be placed between the pressure tap and pressure tap
tubes. Pressure taps on column walls must be placed on locations that are not
exposed to any lateral flow of vapour as it may be imposed by distributor or vapour
inlet device.
The best practice is to have two pressure drop systems installed in parallel,
one to cover the low pressure drop range, say from 1 to 10 mbar, and the other one
the whole range, say 1 to 100 mbar. In this way more certainty is present regarding
the accuracy of the measured data at low F-factors values.
Since the packed bed height will differ from test to test, and the distributor
needs to be placed immediately above the packing, the best solution is to have top
side pressure tap fixed at highest position. This implies that the pressure drop
measured will include the static pressure related to the height of empty part of the
column, and if shorter beds are installed, also the pressure drop associated with
distributor itself. The first one will be appreciable at high pressure operation (high gas
density) and the second one in case of vacuum operation (high gas velocity).
Providing additional pressure taps along the column to reduce and possibly eliminate
one or both of these sources may prove to be impractical, because it requires a
complex manifold (many valves) to make necessary adjustments. This is complicated
and prone to errors and therefore I would recommend maximum distance option, in
conjunction with appropriate corrections for contributions of static pressure and/or
distributor. The first one is easy to quantify, and a useful correlation for pressure drop
of a narrow trough type liquid distributor can be found elsewhere [35]. If the bottom
side pressure tap is located bellow the liquid collector/gas distributor device, usually
a chimney tray or chevron type device, then there will be an additional pressure drop
involved, which however can be accounted for by using correlations available in the
above mentioned reference.
In case that the top pressure is measured via a separate manometer installed
at the cop of the column, a practical double check is possible if provisions are made
to attach a precalibrated manometer to pressure lines connecting the top and bottom
side pressure taps to the pressure difference cell. If this is done and the difference of
two absolute values does not agree well with that from pressure difference cell I
would trust the latter one.
3.10 Reproducibility
Two to three points at different F-factors should be repeated at the end of the
measurement series, and in some cases the same packing should be tested again,
after a while, to get experience and the confidence regarding the data reproducibility
and interpretation. This implies that the method of installing packing needs to be fixed
and repeated every time a column is (re)packed, as discussed under 3.3.
One of worrying problems associated with this is that running up and down
with respect to vapour load can lead to some hysteresis effect, which is a difficult
situation and needs to be handled with care, to avoid excessive discrepancies in the
same data points. The time required to establish a steady state when going from
higher to lower F-factors is longer than that associated with going up in F-factor.
Liquid hold-up is the most sensitive parameter in this respect, and higher than normal
vales of pressure drop could be expected when going down too fast. Dedicated
experiments should provide proper answer to this question, i.e. to establish the test
procedure and related time intervals.
3.11 Mode of Operation

Performing efficiency tests by doing them at total reflux is practical and
therefore accepted as a common standard. However, the results may differ from
those at finite reflux ratio. A dedicated study carried out at Sulzer in late 1980s has
indicated that there is no significant difference in the results obtained at total reflux
(L/G = 1) and finite refluxes (L/G ≠ 1) [36]. From that moment on Sulzer reports only
the data obtained in total reflux tests. Most recently, a study performed in Japan
included continuous operation and it appeared that the structured packing (Montz-
pak B1-250) performed slightly better under continuous operation than at total reflux
conditions [37]. This indicates that total reflux results may be considered generally to
be on the safe side.
To eliminate uncertainties in this respect, i.e. to gather own experience, it is
advisable to have provisions for simulating experimentally a finite reflux ratio
operation. This could easily be arranged for simulation of a common rectification
section situation, with L/G < 1, by having a provision to divert a part of the reflux
stream to the feed tank, and to simulate (L/G) > 1 a separate pipe could be installed
to enable bringing the liquid from feed tank to the liquid distributor. If continuous
operation is considered as a possibility then enough column height needs to be
arranged, i.e. at least three meter per section and one meter for collector and
redistributor, as well as enough place for placing the top distributor and demister in
the vapour disengagement area.
In general, total reflux operation is the most convenient one and widely
accepted. In order to get ready as fast as possible operators of total reflux distillation
columns prefer to start with highest reboiler load, i.e. at an F-factor around the flood
point, to ensure thorough wetting of the packing before start of measurements, which
is necessary. Being at highest load it is convenient to go down with column load in
predetermined steps. However in this case enough time must be provided upon
change to new F-factor for column to reach the steady state. Other possibility, after
flooding the column is to go down to lowest F-factor, say about FG = 0.5, and
increase the load gradually, increasing the density of the points in the loading region,
where some stronger deviations in performance can be expected. These two options
are normal for a continuous (non-stop) test run. For tests performed on daily basis,
the start-up procedure repeats and every day one or two neighbouring points are
measured. Non-stop runs, starting on Monday morning and ending on Friday, with
sampling performed at predetermined times during both day and night are best
option from the standpoint of operation and the quality of measurements, however,
such operation requires continuous availability of people (shift work) and compliance
with safety regulations, which may differ from company to company. In any case,
once established a test procedure must be adopted as a standard.
3.12 Avoiding Systematic Errors

Conducting packing efficiency tests at total reflux conditions minimizes errors
associated with determining the heat input, feed composition and material balance.
Nevertheless there are other potential sources of errors, which however can be
reduced to minimum or fully eliminated if acting accordingly. Most of these are
mentioned on different places in this text.
A potential threat regarding the test system behaviour is presence of some
undesired components which could for instance affect the thermodynamics of the
system, the most notorious in this respect being water. Since the water always finds
a way to appear in a closed tests system, and is, fortunately not pronouncedly
soluble in common tests mixtures it will tend to settle out if provisions are made to
collect it. The installations at SRP and in Delft have a small boot at the lowest point of
condenser (condensate/reflux return line) to isolate water and to remove it from time
to time. A more radical practice to get rid of water and other potential impurities is to
remove the test system from the column and clean the installation by running the
column filled with one of common hygroscopic solvents, like methanol or even better
acetone. Upon emptying the column the remnants of latter are easily removed by
blowing nitrogen through the installation. However, this is something which should be
done according to standard company practice.
Indeed, the test mixture should be as pure as reasonable, i.e. contain
impurities to a level well below the limiting one. For instance, 250 ppm may be taken
as a safe limit value for water in case of common organic systems, but it may be that
company experience in this respects allows different, may be even significantly
higher values. Samples should not be exposed to atmosphere, to avoid partial
evaporation as well as exposure to oxygen, which in some cases may lead to
undesired reactions.
Certainly, for the chosen tests system and operating conditions an error
propagation analysis needs to be done before the data evaluation and interpretation
is performed to establish the sensitivities of mass transfer efficiency, pressure drop
and, very importantly F-factor to maximum deviations expected in measured
parameters. For instance, F-factor is sensitive to deviations in composition and
pressure and pressure difference measurements, which influence densities of top
and bottoms. In our experience this will result in acceptable deviations, bellow two
percent. However, personal experience in this respect, based on thorough analysis of
new test installation/system is invaluable and therefore highly recommended
exercise.
An additional source of headache is uncertainty around quantification of the
heat loos and its effects on column performance. However, the larger the diameter of
the column the smaller the possible effect, providing a good insulation is ensured. In
any case, placing the test column inside the building, like at BTS in Leverkusen,
would exclude possible climate change related effects, like large temperature
differences, wind effects, etc. A useful base test exercise would be to run an
experiment without insulation. Also, the effect of sub-cooling, which is dealt with in
elaborated way later on, needs to be evaluated appropriately.
Anyhow running a distillation pilot plant will bring necessary amount of
headache to those involved, if striving for absolute accuracy/certainty, which is
difficult if not impossible to achieve in practice.
3.13 Process and Mechanical Design Considerations

Early days it was a common practice to place the column atop of a ketlle
reboiler. To enable high vacuum operation the condenser was usually installed as a
part of the top of the column. Modern pilot plants (FRI, SRP, TU Delft, BTS) prefer
having these three main units as separate devices assembled into a functional unit.
Condenser and reboiler need to be large and flexible enough to cover the operating
range. For structured packings this means operating pressures of 100 mbar on lower
side and atmospheric pressure on upper side. If one wish to be able to operate at
high pressures then additional units, connected in parallel may be considered. Water
is convenient as cooling medium and a small after-cooler unit may be useful to
control properly the extent of sub-cooling of reflux. Falling film evaporators are
convenient as reboilers, and the accompanying tank should allow feed volumes to be
significantly larger than the holdup of the column, condenser and tubing, to avoid
excessive depletion of the more volatile component. Usually a 10 bar steam supply is
enough for heating purposes, but in case a high pressure operation this may be
insufficient, which can be compensated eventually by having extra heat transfer area
available. Certainly, the relevant numbers depend on the system chosen.
From construction point of view, all units should be made of stainless steel,
SS316 being a good choice. A useful provision is to have observation windows. If the
position of the liquid distributor is fixed then one window should be placed to allow
observation of operation of the distributor. This location is important because it
enables observation of the extent of entrainment of liquid in the loading region. An
additional window placed perpendicularly is recommended to enable light to be
provided to increase visibility inside the distributor section of the column. A window
along the bed offers the possibility of observing the piece of periphery of packing in
operation. In preloading region the degree of (active) wetting of packing can be
observed, and under high operating loads, approaching flooding a fluctuating action
(surging) of the bed can be observed which is a useful experience increasing both
the understanding of packing behaviour and confidence regarding the interpretation
of measured data.
Finally, to enable operation at below-atmospheric pressures a vacuum pump is
required with corresponding manifold and control equipment. If all is put together
than we arrive at test installation capable of operating under vacuum and at above
atmospheric pressure, connected to and operated via a computer in the control room,
equipped with appropriate data acquisition and process operation software.
4. TEST DATA EVALUATION, PRESENTATION AND INTERPRETATION
Usually, the HETP and pressure drop of the tested packing are presented in
performance plots as a function of the superficial (based on full cross section area of
the column) vapour load, i.e. F-factor, FG, or/and capacity factor, cG, which are
related through the square of the difference between liquid and vapour densities:
FG = uGs ρ G (1)
and
ρG FGs
cG = uGs = (2)
ρ L − ρG ρ L − ρG
where uGs (m/s) is the superficial vapour (gas) velocity, ρG (kg/m3) is the gas density
and ρL (kg/m3) is the liquid density.
The superficial gas velocity is obtained by dividing the volumetric flow rate, i.e.
the ratio of mass flow rate and the density of vapour, and the cross sectional area of
the column.
MG
uGs = (3)
⎛ π d c2 ⎞
ρ G ⎜⎜ ⎟⎟
⎝ 4 ⎠
where dc (m) is the internal column diameter and MG (kg/s) is mass flow rate of gas.
In case of the total reflux, mass flows of gas and liquid streams along the
column are equal, and the corresponding superficial liquid velocity is:
ρG ρG
u Ls = uGs = FG (4)
ρL ρL
Multiplied by 3600 this equation delivers information on corresponding column liquid

load, expressed in m3/m2h, which is a more practical unit.
Figures 1 and 2 show HETP and pressure drop curves as a function of the F-
factor, for top, middle of the bed and bottom conditions, as measured at total reflux in
a TU Delft experiment with Montz-pak B1-500MN using CH/nH system at
atmospheric pressure, and in a Bayer TS experiment with B1-250MN using CB/EB
system at 0.1 bar, respectively. As it can be seen from Fig. 1, in this particular, wide
boiling test mixture case, even for a rather short bed, the effect is significant. Using
the bottom temperature as representative for data evaluation would lead to lowest
pressure drop and highest capacity, as well as the best efficiency (lower HETP). The
efficiencies differ considerably, because the relative volatility in this case is
significantly higher at top than at the bottom of the bed. For the same bed height and
composition change, lower relative volatility means more equilibrium stages per unit
height, i.e. a lower HETP, and consequently better efficiency at bottom of the bed
conditions. According to Fig. 2, similar situation is with CB/EB system at 0.1 bar, but
in this case the difference in top and bottom efficiencies is much less pronounced,
i.e. practically negligible. The efficiencies hardly differ because the relative volatility in
the top is only slightly larger (third decimal place) than that in the bottom of the bed.
0.4 16
B1-500MN, TUD, CH/nH, 1.013 bar , d = 0.45 m, h = 1.58 m
Pressure drop (mbar/m)

0.3 Ideal mixture, top > bottom 12
HETP (m)
0.2 8
HETP - top
HETP - average
HETP - bottom
0.1 dp/dz - top 4
dp/dz - average
dp/dz - bottom
0.0 0
0 0.5 1 1.5 2 2.5
0.5
F-factor (Pa )
Figure 1 – Effect of operating conditions on packing efficiency and pressure drop for
CH/nH system at top pressure of 1.02 bar
0.5 15
B1-250MN, BTS, CB/EB, total reflux, 0.1 bar, dc = 0.6 m, hpb = 2 m
HETP, top
0.4 HETP, bottom 12
HETP, average
Pressure drop [mbar/m]

dp/dz, top
dp/dz, bottom
0.3 9
dp/dz, average
HETP [m]
F-factor uLs
(Pa0.5) (m3/m2h)
0.54 1.29
0.2 1.04 2.50 6
1.55 3.74
1.92 4.66
2.27 5.54
2.59 6.35
2.94 7.27
0.1 3.22 7.98 3
3.54 8.85
3.67 9.23
3.78 9.56
4.16 10.67
0 0
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5
0.5
F-factor [Pa ]
Figure 2 – Effect of operating conditions on packing efficiency and pressure drop for
CB/EB system at top pressure of 0.1 bar.
It should be noted that the F-factors shown in Fig. 1 and Fig. 2 were calculated
taking into account the effect of bed pressure drop.
The extent of temperature effect is elaborated in more detail for all important
design and operating parameters in what follows. Usually the average values based
on top and bottom of the bed conditions are taken as representative for test results
presentation.
4.1 Representative F-factor

Applying Eq. (3) to Eq. (1) yields a practical expression for gas flow F-factor:
MG
FG = (5)
⎛ π d c2 ⎞
ρ G ⎜⎜ ⎟⎟
⎝ 4 ⎠
indicating that for a given column internal diameter the F-factor is proportional to
internal mass flow rate of the vapour and to the inverse of the square root of vapour
(gas) density. Due to difference in top and bottom pressure and temperature as well
as vapour mixture composition, vapour density will be different at the top and the
bottom of a bed.
The density of the vapour at the top of the bed is defined by the top pressure
and temperature and can be determined for an ideal mixture from:
pT M w,G ,T
ρ G ,T = (6)
R TT
where pT (bar) is pressure of the top of the column, Mw,G,T (kg/kmol) is molecular
weight of the gas mixture, TT (K) is absolute top temperature, and R (kJ/kmol K) is
universal gas constant. In conjunction with pressure expressed in bar: R = 0.08314.
Similarly, for bottom conditions:
( pT + ∆p ) M w,G ,B
ρ G ,B = (7)
R TB
where ∆p (bar) is the measured pressure drop of the packed bed, Mw,G,B (kg/kmol) is
molecular weight of the vapour mixture, and TB (K) is absolute temperature at bottom
of the bed.
A simple arithmetic average of gas density can be taken as representative of
the middle of the bed conditions:
ρ G ,aver =
(ρ G ,T + ρ G ,B )
(8)
2
The situation with the representative internal mass flow rate of vapour
however is not so simple. Namely, as appeared in practice, it is always somewhat
larger than that based on measured reflux flow rate.
Per definition, under total reflux the molar flows of gas and liquid are equal and
constant along the column, however the reflux, obtained by total condensation of the
vapour leaving the top of the bed, returns into the column subcooled. According to
my knowledge, based on evaluation of BTS, FRI, SRP and TU Delft data, the reflux
returns to the top of the column as a liquid at a temperature 10 to 20 degrees K
below its boiling point. Upon entering the column this sub-cooled liquid is heated up
to reach its boiling temperature, and the heat for this is provided by condensation of a
part of the rising vapour. In other words latent heat or enthalpy of condensation of
vapour provides the sensible enthalpy to heat the subcooled liquid to its boiling point.
Fortunately a relatively small amount of total heat is required to get this done.
The liquid created by the condensation of vapour joins the reflux, i.e. liquid
introduced through the distributor, and, therefore, it is reasonable to expect that the
flow rate of this “internal reflux” is greater than the measured flow rate of “external
reflux”. In order to obtain a reasonable estimate of the internal reflux, Seader and
Henley [38] recommend an equation derived from an approximate energy balance
around the top of the bed, which is transformed here into mass units to express the
mass flow rate of the gas at bottom conditions, assuming that under total reflux the
molar/mass flow rates of gas and liquid streams are equal:
⎡ c p ,L ,T TT − c p , L , R TR ⎤
M G ,B = M G ,T ⎢1 + ⎥ (9)
⎢⎣ ∆hv , B ⎥⎦
where cp,L (kJ/kg K) is the specific heat of the liquid at corresponding temperature:
top, TT (K), or reflux, TR (K), and ∆hv,B (kJ/kg) is specific enthalpy of vaporisation or
condensation at bottom temperature.
Then, keeping in mind the fact that the gas flow rate at the top is equal to
(measured) reflux flow rate, a reasonable representative F-factor is that obtained as
an arithmetic average of top and bottom values:
⎡ ⎤
1⎢ M G ,T M G ,B ⎥
FG ,aver = ⎢ + ⎥
2⎢ ⎛ πd c ⎞ ⎛ π dc ⎞ ⎥ (10)
⎢ ρ G ,T ⎜⎝ 4 ⎟⎠ ρ G ,B ⎜ ⎟
⎝ 4 ⎠ ⎥⎦
⎣
Specific vaporisation enthalpies and specific heat capacities of top and bottom
binary mixtures can be determined from pure component properties on additive
basis, using experimentally determined mass fractions of more volatile component.
Suitable simple polynomial equations, with experimentally determined coefficients,
can be used to describe pure component properties.
In case of larger bed heights the pressure drop effect will be more pronounced
and may cause even larger difference between top and bottom related F-factors.
Nevertheless, an average representing the middle of the bed conditions can always
be used with confidence for the purposes of packing performance comparisons.
4.2 Representative Relative Volatility

Only with an ideal close boiling system, such as CB/EB mixture, it is certain
that the assumption of a constant relative volatility will hold for the whole bed length.
With other systems, such as commonly used CH/nH system, there is a significant
difference between relative volatilities of the top and bottom of the bed, resulting, as
demonstrated in Fig. 1, in a rather strong effect on efficiency.
In the case shown in Fig. 1, the bottom temperature was 10 0C higher than the
top temperature, and corresponding relative volatilities were 1.75 at the top and 1.6
at the bottom, respectively. This, nearly ten percent difference in relative volatilities,
results in a nearly twenty percent difference in corresponding HETP values. In other
words, for the same composition change, at bottom conditions more theoretical
plates are contained in given bed height, resulting in a lower HETP value, i.e. better
efficiency.
This is based on assumption of ideal behaviour of CH/nH mixture, which is
generally valid for CH/nH system. However, by considering a certain degree of non-
ideal behaviour in liquid phase, the situation can turn upside down, i.e. a larger
relative volatility obtained at the bottom than at the top conditions. The extent of this
will depend on the method used to estimate the characteristic activity coefficient.
However it should be noted that in this case the average value remained nearly the
same. These kind of thermodynamics related uncertainties is generally avoided if a
close boiling mixture like CB/EB system is used.
If an average is taken then the geometric average of top and bottom values is
preferred:
α = αT ⋅ α B [11]
For binary mixtures, the chosen relative volatility in conjunction with the
representative composition (mole fraction of more volatile component, x) determines
the slope of the equilibrium line, m, via:
dy α
m= =
dx [1 + x(α − 1)] 2
[12]
For total reflux case, (L/G) = 1, the stripping factor, λ = mG/L = m/(L/G), which
represents the ratio of slopes of equilibrium and operating lines, is equal to the slope
of the equilibrium line (λ = m). L and G represent molar flow rates of the liquid and
vapour (gas), respectively.
4.3 Representative Efficiency

It is a common practice to take the most conservative HETP value around the
loading point as representative, providing this value will be larger or equal to that
corresponding to the point of the onset of flooding. Generally the HETP, i.e. the
inverse of the number of theoretical plates (equilibrium stages) per meter bed height
is taken as the measure for mass transfer efficiency of a packing. In other words, the
installed packed bed height, hpb (m), divided by the contained number of theoretical
plates (equilibrium stages), N, determines the efficiency of the packing expressed as
the height equivalent to a theoretical stage (HETP):
h pb
HETP = [13]
N
Another theoretically more appropriate measure is the HTUoG (or HoG), i.e the
height of an overall gas side transfer unit, which however requires the information on
the number of transfer units contained in a bed:
hbed
HTU oG = [14]
NTU oG
The number of transfer units is not readily available and the most common
practice is to use HETP, which is based on the number of theoretical plates, which in
turn can easily be determined using established graphical or analytical methods in
conjunction with accurate equilibrium data.
For ideal systems (CB/EB) and nearly ideal systems (CH/nH), the number of
theoretical plates or stages generated in the installed bed during a total reflux
experiment can be determined with confidence using well known Fenske equation:
⎡⎛ x ⎞ ⎛ 1 − x ⎞ ⎤
ln ⎢ ⎜ ⎟ ⎜ ⎟ ⎥
⎣ ⎝1 − x ⎠D ⎝ x ⎠B ⎦
N = [15]
ln α
where x (-) is the mole fraction of more volatile component in the binary mixture and
α (-) is the relative volatility, i.e. its representative value, most frequently the
geometric mean of top and bottom values (Eq. 11).
The sensitivity of this equation to measurement errors in relative volatility and
compositions on both ends has been thoroughly elaborated in a paper by Deibele
and Brandt [39], indicating that the effect of deviation in relative volatility is stronger
and tends to increase with decreasing relative volatility, and that keeping the mole
fraction of more volatile component in the bottoms in the range between 10 and 40
mole % and in the top between 60 and 90 mole % ensures that relative error will be
kept below 2 %. This exercise clearly indicates that significant errors can be
expected if dealing with relative volatility below 1.1, which is a value the CB/EB
system could assume if operated at pressures above 2 bar. Certainly, it is essential
to use accurate equilibrium data for the test system in question.
From time to time doubts arise about the reliability of Fenske equation. A
recent study of B. Kaibel [40] introduced an alternative, in a way mathematically more
rigorous, integral solution based analytical form of McCabe-Thiele plot, which
indicated that Fenske equation may be wrong to some extent, depending on
difference in top and bottom compositions, which however becomes pronounced at
relative volatilities above 1.5, and should definitely be considered if dealing with non-
sharp separations. From the evaluation of SRP data on Montz structured packings
[17] it appeared that CH/nH system is practically insensitive in this respect and in
case of CB/EB system with relative volatilities in the range 1.1 to 1.2 there is no
effect at all. This means, that Fenske equation in conjunction with proper
thermodynamic model and measured top and bottom compositions can be
considered to be a reliable tool for determination of mass transfer efficiency of
packings tested under total reflux conditions.
Applying the Eq. [15] to Eq. [13] yields the working expression used widely to
determine the efficiency of a packing from measured top and bottom compositions:
h pb ln α
HETP = [16]
⎡⎛ x ⎞ ⎛ 1 − x ⎞ ⎤
ln ⎢⎜ ⎟ ⎜ ⎟ ⎥
⎣⎝ 1 − x ⎠ D ⎝ x ⎠ B ⎦
There are also stage by stage methods available, used in conjunction with
commercial software, but these are useful mainly if it is dealt with multicomponent
mixtures. A common practice for wide boiling binary mixtures is to use McCabe-
Thiele plot cut into concentration regions where the equilibrium line can be
approximated as a straight line and the representative average HETP obtained in
additive way.
HETP and HTUoG are related to each other through stripping factor, λ, i.e. the
ratio of slopes of equilibrium and operating lines in the McCabe-Thiele plot of the
given case. If the equilibrium and operating lines are straight and in parallel: HETP =
HTUoG, and this is the case with CB/EB system. If the lines are straight but not
parallel then following expression holds:
ln λ
HETP = HTU oG [17]
λ −1
A practical demonstration of this equation can be found in a most recent
reference discussing the effect of the test system as experienced during a total reflux
distillation study carried out with a high performance, high specific surface area
packing (Mellapak 752.Y) [21].
Also, it should be noted that the additional internal reflux generated by
condensing the vapour along the column wall is not so pronounced in the columns
with diameters as considered here, to have a substantial influence on efficiency.
Practically, the same is with sub-cooling effect that effectively creates additional
internal reflux, which, however, in total reflux situation appeared to be much less
influential than generally anticipated. However, one should not forget that a
pronounced difference in enthalpies of vaporisation of two components forming the
test mixture could do some harm to efficiency and should be recognised and
accounted for appropriately. This is not a concern with CH/nH and CB/EB systems,
but it is recommended to perform the necessary calculation exercise to determine the
extent of the effect and make appropriate decisions toward standardisation of
calculation methods. The same is recommended for subcooling and heat loss related
effects.
4.4 Representative Pressure Drop

The pressure drop is measured directly and the obtained value divided by bed
height gives the unit pressure drop of the packing in question, expressed usually in
mbar/m. However this is only the case if the pressure taps are placed immediately
above and below the bed, and this may not always be the case. Namely the top and
bottom section pressure taps are usually fixed and if a short bed is measured than
there is a certain length of empty column included. For such a rather short tube the
friction with the column walls may be considered negligible, however, if the operating
pressure is high, i.e. well above atmospheric, the static pressure of the empty column
could play a significant role. In such a case, the packing pressure is that obtained by
detracting the static pressure of the empty part of the column from the measured
pressure drop. If, in conjunction with a short bed, the liquid distributor is placed below
the upper pressure tap, then this needs to be considered, particularly if the free area
of used liquid distributor is on lower side, i.e. well below 50%, and high gas velocities
are involved. As suggested elsewhere [35], for a test column operating at 100 mbar
at a F-factor of 3 Pa0.5, a narrow trough distributor with 40 % free area would cause a
pressure drop of about 0.2 mbar, which is not significant if the measured pressure
drop is above 10 mbar. Also, if a chimney-tray or chevron type liquid collector is used
to distribute gas, and placed above the bottom side pressure tap, then a significant
additional pressure drop can be expected. Reference [35] contains correlations which
enable estimation of related pressure drop of these frequently used devices.
In other words, the pressure drop per meter packed height is:
(∆p / ∆z ) pb = ∆pmeas − ∆pst − ∆pld − ∆plc (18)

h pb
where subscript pb refers to packed bed, and subscripts st, ld, and lc denote
pressure drop associated with static pressure of empty column, liquid distributor and
liquid collector, respectively.
4.5 Packing Geometry Effects

Since the primary purpose of the total reflux distillation tests is to get proper
impression on the performance characteristics of different packings, it is important to
be aware of macro geometry details of each packing tested, because these may
deviate from nominal, which, in some cases could have profound effect particularly
on pressure drop and capacity. This means that packing to be tested needs to be
carefully inspected to observe and notice the design characteristics of corrugations.
The best way to get certainty regarding the relevant dimensions of the corrugations is
to ask the packing manufacturer to deliver separately two-three corrugated sheets
used for manufacture of the test packing. If this is not done then if there are packing
elements in excess or upon completion of tests one packing element could be
dismantled and two-three sheets taken out for closer inspection. Corrugation height
and base width need to be measured precisely, as well as the corrugation inclination
angle. The latter exhibits very strong influence on pressure drop, and can deviate
from the common (nominal) 45 degrees. One should note that novel, high
capacity/performance packings often come with a corrugation inclination angle below
45 degrees! For high performance packings also the height of the bend at the top
and/or bottom part of corrugations needs to be known. A useful aid for evaluation of
possible macro geometry effects is the Delft predictive model for structured packings
[41, 42], and some of the geometry related effects can be found quantified elsewhere
[21, 43].
4.6 Test Documentation

The test should be documented properly, which requires establishing a
standard for preparing a summary report. Excel is the best environment for this
because it allows easy transfer, handling and use of data and can be used in
conjunction with process simulation software. In Appendix B, two Excell sheets are
given, one suitable for data collection (B1), containing values of all measured
parameters, and the other one suitable for data presentation (B2), containing most
important design and operating parameters. The latter ones are supporting the main
result, i.e. a plot showing measured HETP and unit pressure drop as a function of F-
factor. In this plot all measured points, usually three per vapour load need to be
given, including repeated ones, done additionally to check the reproducibility. The
latter ones need to be indicated as such. Useful additional information is a table
inserted in the graph (see Fig. 2), showing the specific liquid loads in m3/m2h,
corresponding to F-factors of measurement points.
5. CONCLUSIONS AND RECOMMENDATIONS
There is no doubt that for a company manufacturing fine and bulk chemicals
the best practice is to have at disposal a test unit of a size sufficient to ensure
obtaining representative packing performance data, to understand and to minimize
technical risk associated with (re)design and operation of an industrial scale
installation if equipped with a new type of packing.
For structured packings, a column diameter of 0.4 m or larger in conjunction
with a maximum bed height of 4 m, allowing 5 to 25 theoretical stages to be
developed, depending on packing size, looks to be a reasonable choice.
Total reflux operation is a natural choice and provisions can be easily made to
ensure performing some tests with a liquid to vapour flow rate ratio below or above
one.
Since structured packings are mainly considered for application under vacuum
(100 mbar is a representative value) and nearly atmospheric pressures, the
reasonable choice is to have an installation capable of covering this range of
operating pressures with one test system and using one, high turndown, high free
area narrow trough liquid distributor with drip tubes to ensure constancy in initial
liquid distribution pattern.
The ideal CB/EB mixture is a good test system, however, being a low
(constant) volatility system it provides higher efficiencies from those obtained with
common wide boiling hydrocarbon mixtures, with like CH/nH system. Also, because
of high operating temperature this system is not suitable for above atmospheric
operation. In other words, it cannot be used for the purposes of evaluating a packing
performance under relatively high liquid load, say above 20 m3/m2h. The exceptions
in this respect are tests carried at atmospheric pressure in conjunction with low
specific surface area, high capacity packings, which operate at F-factors well above 3
Pa0.5. In case of the CH/nH system, operated at SRP at 4.14 bar, at highest F-factor
liquid loads up to 50 m3/m2h are generated, without any temperature imposed
limitation.
Test procedure should be established based on own evaluations and accepted
as a standard to ensure consistence of test results. A continuous, i.e. non-stop
operation is preferred. If safety and/or personal reasons require daily operation then
the equipment size should be minimised, to reduce stabilisation times required to
arrive at steady state conditions after start-up and changes in column loads.
Evaluations of relevant factors, summarised in this report have provided a
good guidance regarding pilot-plant column design and operation, however further
experiences, based on pilot-plant building, start-up and dedicated operation are
needed to arrive at desired final goal, i.e. definition and adoption of a standard total
reflux distillation test, to be considered useful for scale-up purposes.
Nomenclature
cG capacity factor, m/s

cp,L specific heat capacity of the liquid, kJ/kg K
dc internal column diameter, m
F-factor = FG = uGs(ρG)0.5, Pa0.5 or (m/s)(kg/m3)0.5
G molar flow rate of gas or vapour, kmol/s
hbed height of the packed bed, m
hv specific vaporisation enthalpy, kJ/kg
HETP height equivalent to a theoretical plate, m
HTUoG height of an overall gas side transfer unit, m
L molar flow rate of the liquid, kmol/s
MG mass flow rate of gas (vapour), kg/s
Mw molecular weight, kg/kmol
m slope of the equilibrium line, -
N number of equilibrium stages or theoretical plates, -
NTUoG number of gas side transfer units, m
p pressure, bar or mbar
T temperature, oC or K
uGs superficial gas (vapour) velocity, m/s
uLs superficial liquid velocity, m/s
y mole fraction of more volatile component in vapour, -
x mole fraction of more volatile component in liquid, -
Greek letters
α relative volatility, -
∆p pressure drop, bar or mbar
λ stripping factor, -
ρG vapour density, kg/m3
ρL liquid density, kg/m3
Subscripts
aver refers to average value

B bottoms, bottom of the packed bed
D distillate
G gas or vapour
R reflux
T top of the packed bed
lc refers to liquid collector
ld refers to liquid distributor
pb refers to packed bed
st refers to static pressure
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Recommended Test Mixtures for Distillation Columns
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Predicting mass transfer in packed columns containing structured packings
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Experimental Characterization of High Performance Montz Structured Packings
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Development of a new generation of structured packings for distillation
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Large Industrial-Scale Demonstration of Structured Packing Distillation System
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Appearance of Maldistribution in Distillation Columns Equipped with High
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Pressure drop of packed column internals
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Theoretical and Experimental Investigation of the Influence of Maldistribution on the
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APPENDICES
A Physical Properties of Common Test Systems
A1 Orto- / Para- Xylene (OX/PX)
Table A1: Physical properties of O/P-Xylene system and operating conditions as

employed at FRI (average at the middle of the bed temperature)
Pressure (bar) 0.02 0.13

Property
Temperature (0C)
Liquid density, kg/m3 857 817
Liquid viscosity, Pa s 5.83 E-4 3.69 E-4
Liquid diffusivity, m2/s 2.13 E-9 3.83 E-9
Vapour density, kg/m3 0.068 0.488
Vapour viscosity, Pa s 6.43 E-6 7.35 E-6
Vapour diffusivity, m2/s 118.00 E-6 20.02 E-6
Surface tension, N/m 0.028 0.023
Relative volatility, - 1.30 1.24
Slope of equilibrium line, - 0.91 0.93
Reference composition (x), - 0.66 0.70
Liquid load, m3/m2h, at 2.19 6.16
F-factor = 2 m/s(kg/m3)0.5
A2 Chlorobenzene / Ethylbenzene (CB/EB)
Table A2a: Physical properties of CB/EB system at different operating pressures

employed at BTS (average at middle of the bed temperature)

Property
Temperature (0C) 67 134
Liquid viscosity, Pa s 5x10-4 3x10-4
Liquid diffusivity, m2/s 3.4x10-9 6.4x10-9
Vapour viscosity, Pa s 8x10-6 1x10-5
Vapour diffusivity, m2/s 4x10-5 4,2x10-6
Table A2b: Physical properties of CB/EB system and operating conditions as

employed at SULZER Chemtech (average at the middle of the bed temperature)

Property
Temperature (0C) 132
Molecular weight, kg/kmol 110
Liquid density, kg/m3 860
Liquid viscosity, Pa s 2.66 E-4
Liquid diffusivity, m2/s 6.90 E-9
Vapour density, kg/m3 3.22
Vapour viscosity, Pa s 9.41 E-6
Vapour diffusivity, m2/s 5.34 E-6
Surface tension, N/m 0.0186
Relative volatility, - 1.12
Slope of equilibrium line, - 1
Reference composition (x), - 0.50
Liquid load, m3/m2h, at 15.02
Table A2c: Physical properties of CB/EB system at different operating pressures as

extracted from the Table 3.8 in Billets book [4 ]
Pressure (bar) 0.033 0.067 0.133 0.266 0.532 1.000

Property
Temperature (0C) 41 56 72 91 112 134
Liquid density, kg/m3 963 949 926 905 886 866
Liquid viscosity, Pa s 5.78 E-4 4.93 E-4 4.17 E-4 3.71 E-4 3.01 E-4 2.60 E-4
Liquid diffusivity, m2/s 2.33 E-9 2.85 E-9 3.5 E-9 4.33 E-9 5.41 E-9 6.67 E-9
Vapour density, kg/m3 0.14 0.27 0.51 0.97 1.83 3.24
Vapour viscosity, Pa s 6.44 E-6 7.80 E-6 8.11 E-6 8.45 E-6 8.82 E-6 9.51 E-6
Vapour diffusivity, m2/s 64.8 E-6 35.8 E-6 19.9 E-6 11.1 E-6 6.3 E-6 3.7E-6
Surface tension, N/m 0.0285 0.0269 0.0251 0.0232 0.0211 0.0190
Relative volatility, -
Slope of equilibrium line, -
Liquid load, m3/m2h, at
A3 CYCLOHEXANE / n-HEPTANE (CH/nH)
Table A3a: Physical properties of CH/nH system and operating conditions as

encountered at different operating pressures employed at SRP (average at bottom
temperature)
Pressure (bar) 0.17 0.33 1.03 1.65 4.14

Property
Temperature (0C) 49 61 97 114 154
Liquid density, kg/m3 659 657 625 608 561
Liquid viscosity, Pa s 4.67 E-4 4.31 E-4 2.97 E-4 2.32 E-4 1.61 E-4
Liquid diffusivity, m2/s 2.31 E-9 2.72 E-9 4.44 E-9 6.19 E-9 9.17 E-9
Vapour density, kg/m3 0.66 1.19 3.53 5.44 13.14
Vapour viscosity, Pa s 6.67 E-6 6.94 E-6 7.78 E-6 8.33 E-6 9.17 E-6
Vapour diffusivity, m2/s 13.30 E-6 11.40 E-6 4.17 E-6 3.06 E-6 1.39 E-6
Surface tension, N/m 0.018 0.017 0.014 0.012 0.008
Relative volatility, - 1.94 1.86 1.64 1.57 1.42
Slope of equilibrium line, - 1.54 1.50 1.35 1.33 1.32
Liquid load, m3/m2h, at 8.88 11.95 21.64 27.62 46.52
Table A3b: Physical properties of CH/nH system and operating conditions as

encountered at different operating pressures employed at FRI (average at the middle
of the bed temperature)

Property
Temperature (0C) 52 105
Liquid viscosity, Pa s 4.62 E-4 2.48 E-4
Liquid diffusivity, m2/s 2.72 E-9 5.54 E-9
Vapour viscosity, Pa s 7.14 E-6 8.22 E-6
Vapour diffusivity, m2/s 8.39 E-6 2.24 E-6
Table A3c: Physical properties of CH/nH system and operating conditions as

employed at TU Delft (average at the middle of the bed temperature)
Pressure (bar) 1.013

Property
Temperature (0C) 87
Molecular eight, kg/kmol 92
Slope of equilibrium line, - 0.934
A4 METHANOL / WATER (M/W)
Table A4: Physical properties of M/E system at atmospheric pressure as employed

at TU Delft (average at middle of the bed temperature)
Pressure (bar) 1.013

Property
Temperature (0C) 73
Molecular weight, kg/kmol 25
Slope of equilibrium line, - 0.675
A5 METHANOL / ETHANOL (M/E)
Table A5: Physical properties of M/E system at atmospheric pressure as employed

at Billet (average at middle of the bed temperature)
Pressure (bar) 1.00

Property
Temperature (0C)
Liquid diffusivity, m2/s E-9
Vapour diffusivity, m2/s E-6
Relative volatility, -
Slope of equilibrium line, -
Reference composition (x), -
Liquid load, m3/m2h, at
A6 ISOBUTANE / n-BUTANE (IB/nB)
Table A4: Physical properties of IB/nB and operating conditions as encountered at

different operating pressures employed at FRI (average at middle of the bed
temperature)
Pressure (bar) 6.9 11.4 20.7 27.5

Property
Temperature (0C) - - - -
Liquid density, kg/m3 525 491 430 385
Liquid viscosity, Pa s 1.14 E-4 0.89 E-4 0.63 E-4 0.49 E-4
Liquid diffusivity, m2/s 13.0 E-9 17.7 E-9 27.6 E-9 37.9 E-9
Vapour density, kg/m3 16.9 29.0 55.8 84.8
Vapour viscosity, Pa s 8.76 E-6 9.62 E-6 11.3 E-6 12.9 E-6
Vapour diffusivity, m2/s 0.65 E-6 0.40 E-6 0.23 E-6 0.15 E-6
Surface tension, N/m 0.0075 0.0051 0.0022 0.0010
Relative volatility, - 1.30 1.23 1.16 1.10
Slope of equilibrium line, - 1.03 0.99 1.03 1.02
Reference composition (x), - 0.43 0.50 0.39 0.38
Liquid load, m3/m2h, at 56.4 79.0 125.1 172.2
Appendix B Data Collection and Presentation Sheets
APPENDIX B1 - DATA COLLECTION SHEET
Operating conditions: Total reflux, CB/EB system, 0.1 bar, column diameter: 0.45 m, packed height: 2 m
Run number X-A1 X-A2 X-A3 X-B1 X-B2 X-B3 X-C1 X-C2 X-C3 X-D1 …
Packing tested (type) B1-250MN B1-250MN B1-250MN B1-250MN
Reflux flow rate, kg/h

o
Reflux temperature, C
o
Top temperature, C
o
Bottom temperature, C
Reboiler duty, kJ/hr

o
Vapour return temperature, C
o
Liquid to reboiler temp., C
Liquid to reboiler flow rate, kg/h
Steam flow rate, kg/h

Steam pressure, bar
o
Steam temperature, C
o
Condensate temperature, C
Condenser duty, kJ/hr

Cooling water flow rate, kg/h
o
Cooling water temperature, in, C
o
Cooling water temperature, out, C
Column top pressure, bar
Pressure drop, mbar/m

Cell 1
Cell 2
Top composition, weight %

Bottom composition, weight %
APPENDIX B2 - DATA PRESENTATION SHEET

Operating conditions: Total reflux, CB/EB system, 0.1 bar, column diameter: 0.45 m, packed height: 2 m
Run number X-A1 X-A2 X-A3 X-B1 X-B2 X-B3 X-C1 X-C2 X-C3 X-D1 …
Packing tested (type) B1-250MN B1-250MN B1-250MN B1-250MN
Reflux flow rate, kg/h

o
Reflux temperature, C
o
Top temperature, C
o
Bottom temperature, C
o
Average temperature, C
Top pressure, mbar

Pressure drop, mbar/m
Top composition, mole %

Bottom composition, mole %
Average relative volatility, -
Number of theoretical plates, N, -
HETP, m
NTPM = 1/HETP, 1/m
Top flow rate of vapour, kg/s

Bottom flow rate of vapour, kg/s
0.5
Top F-factor, Pa
0.5
Bottom F-factor, Pa
0.5
F-Factor, average, FG, Pa
Capacity factor, cG, m/s
3 2
Liquid load, m /m h
Additional:
3
Top vapour density, kg/m
3
Bottom vapour density, kg/m
Relative volatility, top, -
Relative volatility, bottom, -
N, by alternative method
NOTES:

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VERSION 1 - Standardization of Structured Packing Efficiency Measurements 14 March 2008

STANDARDIZATION OF STRUCTURED PACKING

Delft University of Technology

Encouraged and Supported

Delft, 14 March 2008

SUMMARY OF THE PROJECT 6

2. PURPOSE AND AVAILABILITY OF DISTILLATION PILOT PLANTS 9

2.1 Packing Manufacturers Facilities 10

2.3 University Based Facilities 12

2.4 User Companies Pilot Plants 14

2.5 Plant Test Columns 14

3. PILOT PLANT DESIGN AND OPERATION CONSIDERATIONS 15

3.1 Column Diameter 15

3.2 Bed Height/Depth 15

3.3 Packing Installation 16

3.4 Liquid Distribution 16

3.5 Vapour Distribution 18

3.6 Test System and Conditions 18

3.7 Liquid Sampling 20

3.8 Measurement of Flow Rates, Pressure, and Temperature 21

3.9 Pressure Drop Measurement 22

3.11 Mode of Operation 23

3.12 Avoiding Systematic Errors 24

3.13 Process and Mechanical Design Considerations 25

4. TEST DATA EVALUATION, PRESENTATION AND INTERPRETATION 25

4.1 Representative F-factor 28

4.2 Representative Relative Volatility 29

4.3 Representative Efficiency 30

4.4 Representative Pressure Drop 32

4.5 Packing Geometry Effects 33

4.6 Test Documentation 34

5. CONCLUSIONS AND RECOMMENDATIONS 34

Appendix A Physical Properties of Common Test Systems 42

Appendix B Data Collection and Presentation Sheets 47

B1 Data Collection Sheet 47

B2 Data Presentation Sheet 47

The present study is made publicly available by BASF SE to serve as a basis

It is our hope that competent people from user companies, equipment

Delft, 12 March 2008 Z. Olujic

SUMARRY OF THE PROJECT

Ambient air/water studies provide in a relatively inexpensive and fast way

available for installation of packing, 4 m being a good measure. Certainly, a test

2. PURPOSE AND AVAILABILITY OF PILOT DISTILLATION TESTS

(i) The mass transfer efficiency of the packing;

2.1 Packing Manufacturers Facilities

2.1.1 SULZER Chemtech

2.1.2 Koch-Glitsch (including former Norton)

2.3 University Based Facilities

2.3.3 University of Alberta

2.4 User Companies Pilots

2.5 Plant Test Columns

2.5.2 Air Products

3. PILOT PLANT DESIGN AND OPERATION CONSIDERATIONS

3.1 Column Diameter

3.2 Bed Height or Depth

3.3 Packed Bed Installation

3.4 Liquid Distribution

levels of orifices. If a turndown above 10 to 1 is required it is common practice to use

3.4.1 Drip points density

3.4.2 Drip points layout

3.4.3 Distributor positioning

3.5 Vapour distribution