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Experimental Investigation of Pressure Drop, Liquid Hold-Up and Mass

Transfer Parameters in a 0.5 m Diameter Absorber Column

Article  in  Energy Procedia · December 2011

DOI: 10.1016/j.egypro.2011.01.095

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Energy
Energy Procedia 4 (2011) 606–613
Procedia
Energy Procedia 00 (2010) 000–000
www.elsevier.com/locate/procedia
www.elsevier.com/locate/XXX

GHGT-10

Experimental Investigation of Pressure Drop, Liquid Hold-Up and

Mass Transfer Parameters in a 0.5 m Diameter Absorber Column

Ali Zakeria, Aslak Einbub*, Per Oscar Wiigb, Lars Erik Øic, Hallvard F. Svendsena

a
NTNU, N-7465 Trondheim, Norway, zakeri@nt.ntnu.no, hallvard.svendsen@nt.ntnu.no
b
SINTEF, N-7465 Trondheim, Norway, per.o.wiig@sintef.no aslak.einbu@sintef.no
c
Telemark University College, N-3901 Porsgrunn, Norway, lars.oi@hit.no

Elsevier use only: Received date here; revised date here; accepted date here

Abstract

Packed towers are common as gas/liquid contacting units for separation processes. Several studies have been performed to
measure and model pressure drop, liquid hold-up and effective mass transfer area. However, most investigations have
concentrated on distillation operation and the correlations obtained may not be directly applicable to reactive absorption. The
present work presents a study of hydrodynamics and mass transfer properties of Sulzer structured packing Mellapak 2X using
both an inorganic and an amine solvent. The pilot plant has an absorber column with packing height of 5 m and diameter 0.5 m.
In this paper results for absorption studies and pressure drop, liquid hold-up and effective mass transfer area are presented.
Dependencies of liquid flow, gas flow and viscosity were in agreement with correlations found in literature. New correlations for
the hydrodynamic characteristics will be implemented in an in-house software as a basis for absorber and desorber design.

⃝
c 2010
© 2011 Elsevier
Published by All
Ltd. Elsevier
rightsLtd.
reserved

Keywords: CO2 capture;liquid hold up;pressure drop;mass effective area..

* Corresponding author. Tel.:+47 9828 3933, E-mail address: aslak.einbu@sintef.no.

1. Introduction

Packed columns have maintained an important role in process industries, especially in separation processes. These
columns are preferred where a high separation performance, low pressure drop and low liquid loads are required (1).
The packings are generally manufactured from different materials such as ceramics, metal and plastics and divided
according to their shape into: gauze packing, grid type packings, metal sheet and random packings (2-7). The most
important parameters in the research connected to the hydrodynamics of packed columns are the pressure drop, the
wetted area, mass transfer effective area and liquid hold-up in addition to the mass transfer coefficient. The aim of
the present work is to perform measurements of pressure drop, liquid hold-up and effective mass transfer area in
reactive absorbent systems.

doi:10.1016/j.egypro.2011.01.095
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2 Author name / Energy Procedia 00 (2010) 000–000

The VOCC (Validation of CO2 Capture) project is a user-driven innovation project with SINTEF and Statoil as
partners. The objective of the project is to create a basis for qualification of improved post-combustion absorption
technologies by experimental studies in a 0.5 m diameter absorber column. In the project, various packing materials
are characterised, varying conditions of gas and liquid flow and chemical system properties are mapped and the
interaction between absorbent and packing properties studied. The experimental data produced will also be used for
validation of in-house software as a basis for absorber and desorber design.
An indoor absorber test rig with a total height of 18 m has been built. The rig has an absorber packing height of 5
m designed for superficial gas velocities up to 6 m/s and a maximum liquid flow of 60 m3/m2hr. The absorption
capacity is up to 300 kg CO2/h and the gas used is air mixed with CO2 added to the gas from an external tank. The
absorber is well instrumented with monitoring of temperature and pressure at every meter of height in the absorber
column. The rig can be run in batch mode with 2 m3 of solvent. The absorber has an adjacent 7 m tall, well
instrumented desorber rig with a 52 kW electric reboiler for the regeneration of the loaded amine solvent. Figure 1
shows an outline of the test rig.

Blower

Cyclone
to ta l h e ig ht: 1 8 m

ABSORBER
G a s c o o le r

CO2-tank

Amine tanks
Figure 1 The VOCC test rig.

2. Pressure drop

Pressure drop in packed columns is an important parameter especially in vacuum and low pressure columns. The
dry pressure drop is measured in packed columns in absence of liquid flow. It is always lower than the wet pressure
drop measured, because the liquid flowing through the column changes the bed structure due to liquid hold-up.
Pressure drops were measured based on pressure measurement at 6 positions along the packing height. Position 1
is below the packing, and positions 2- 6 are 0.5 m, 1.5 m, 2.5m, 3.5m, 4.5 m into the packing respectively. The
liquid flow rates were between 3 and 60 m3/(m2·h), and the gas flow rate was varied between 0 and 17000 m3/(m2·h).
This corresponds to superficial gas velocities ranging from0.6m/s to 5.3m/s. For measuring pressure, six FCX-AII
Fuji pressure transmitters with high accuracy (±0.065%-±0.04%) were used.
Determination of dry pressure drop is often the preliminary tool for characterizing structured packings. First dry
pressure drop was measured. For this purpose all the liquid valves were closed and the fan was started at 0.6 m/s
superficial gas velocity in the absorber column. After establishing steady state conditions, all pressures were
recorded, and the same was done for all velocities tested.
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For measuring the pressure drop with liquid and gas, 4 different liquid systems were used, these system were; 1)
Air-Water 2) Air-water-sugar (5cP) 3)Air-water-sugar (10cP) and 4) Air-MEA (monoethanolamine 30wt%). First of
all the pump was started with a high liquid flow rate,60 m3/(m2h) to properly wet the packing and when steady state
was reached the fan was started at 0.6m/s. Steady state was reached after approximately 8 min, and all pressures
were recorded. This was repeated for other liquid and gas flow rates. The results are presented in Figure 2:
The F-factor is defined as: uG ˜ UG

b c d
a

dry pressure drop dry pressure drop

dry pressure drop dry pressure drop

Figure 2 Experimental results on relationship between pressure drop (mbar/m) and F-Factor (m/s(Kg/m3)0.5)in the
packed column (Sulzer Mellapak 2X) (a)Air/Water -1cP,(b) Air/Water –sugar-5cP,(c) Air/Water-sugar
10cP and (d) Air-MEA(30wt%).

The pressure drop values in the Figure 2 are based on the pressure instruments just below and just above the
packing. However, the internal pressure measurements generally showed a linear relationship between position and
pressure drop. The total pressure drop followed the expected pattern as a function of liquid and gas flows. The
column showed.flooding-like.behaviour.at.superficial.gas.velocities.of.about 3 - 4 m/s depending on the liquid flow.
(The flow factor is about 1.1 times the gas velocity at the given conditions.) The pressure drop was found to increase
slightly with increased viscosity. According to traditional flooding and pressure drop charts (8), the pressure drop
dependency on liquid viscosity can be seen from the capacity factor, which is proportional to the square of the gas
flow and to the liquid viscosity to the power 0.1 (assuming constant liquid density). In the correlations of Rocha et
al. (9), the liquid hold-up is an important parameter in the pressure drop estimation. The liquid hold-up and then
also the pressure drop are expected to increase with increasing liquid viscosity. Also according to traditional
hydraulic diagrams, the flooding velocity should decrease slightly with increased viscosity (to the power of about -
0.05). Our experiments show a small flooding velocity increase with increased viscosity. This slight effect can be
explained by an increased liquid density. In a diagram given by Strigle (8), the liquid density dependence is given by
a power law exponent of -0.5. A liquid density increase of 30 % will give a slightly greater influence on flooding
velocity than a 600 % increase in liquid viscosity and is the reason for our observation.

3. Liquid hold-up

The liquid hold-up in a wetted packed column consists of two parts, the static and the dynamic hold-up. The static
hold-up hL,stat is liquid bound by capillary and adhesion forces and remains in the packing after irrigation is
stopped(10). It describes the liquid prevailing in the pores and gaps of the packing. The static liquid hold-up is a
function of the physical properties of the liquid (density L, dynamic viscosity L, and surface tension ), the
characteristic packing properties (void fraction , and specific packing surface a), the liquid load uL, and the
acceleration of gravity g(10). On the contrary, the dynamic hold-up is the amount of liquid participating actively in
the liquid flow, thus raising the liquid velocity. An increase of the dynamic hold-up normally results in better mass
transfer (10). The liquid hold-up is an important hydrodynamic parameter for gas/liquid flow in packed beds. It
 A. Zakeri et al. / Energy Procedia 4 (2011) 606–613 609
4 Author name / Energy Procedia 00 (2010) 000–000

enables the determination of the pressure drop and the fluid effective velocity within the packing. The latter is
further used for determination of the liquid side mass transfer coefficient, the liquid hold-up is also used to design
support devices for the column since it gives the liquid weight in operation (11).
The liquid hold-up measurements were based on the difference in volume of liquid in the sump with and without
circulation of liquid through the packing. The apparatus was calibrated such that the amount of liquid in pipes and
liquid distributor was known as function of gas and liquid flow rate, the volume of liquid in the packing could be
calculated, thus the liquid hold-up. For measuring liquid level two FCX-AII Fuji level transmitters were used.
The systems investigated including physical properties are given in Table 1. A summary of the experimental results
is given for one packing in Figure 3.

Table 1 Viscosity and densities for different system

system gas Liquid L L
A-W1 air Water 1 cP 999 kg/m3
A-S1 air water-sugar solution 5 cP 1700 kg/m3
A-S2 air water-sugar solution 10 cP 1800 kg/m3
A-MEA air 30% w.t. monoethanolamine 2.6 cP 1010 kg/m3

a b

c d

Figure 3 Experimental results on relationship between Liquid hold up(%) and Superficial velocity (m/s)in the
packed column (Sulzer Mellapak 2X) (a) Air/Water -1cP,(b) Air/Water –sugar-5 cP,(c) Air/Water-sugar
10 cP and (d) Air-MEA(30wt%).
610 A. Zakeri et al. / Energy Procedia 4 (2011) 606–613
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At a given liquid load, the hold-up was close to constant as a function of gas flow, with a sharp increase at very
high (close to flooding) gas velocities. This is in agreement with trends found in the literature (12). Liquid hold-up
was found to increase with increasing liquid viscosity. The influence is higher at high liquid load than at low liquid
load. Alix and Raynal (11) indicate a liquid hold-up dependency on liquid viscosity to the power of 0.13 in
experiments with Mellapak 252Y. We found a higher dependency at high liquid load and a lower at low liquid load.

4. Effective mass transfer area

As far as packed columns are concerned, there exist several definitions of the interfacial area (13), but wetted
surface area is particularly important because the knowledge of it is essential for basic considerations of two-phase
flow in irrigated packing and it also can be taken as a reference surface area when considering experimental mass-
transfer results. In addition, wetted surface area is closely linked to effective interfacial area under particular flow
conditions because only the wetted area can be effective for mass transfer. However, in principle, the difference
between the wetted surface and the effective interfacial area lies in that the wetted surface area incorporates liquid
surface area in dead zones and the effective interfacial area includes surfaces of drops and jets. Despite these
deviations, both the wetted surface area and the effective interfacial area are often applied. The effective interfacial
area can be measured by physical methods, such as electro-resistivity, light transmission, and reflection techniques,
but mostly it is determined by mass transfer measurements in the presence of a fast chemical reaction, controlling
the absorption process.
The effective area of the Sulzer structured packing Mellapak 2X was measured in the VOCC rig test. The pseudo-
first order reactions of air- CO2 with NaOH and with MEA were used.

4.1 CO2-NaOH

The absorption of CO2 into NaOH solution occurs with the following, in practice irreversible, chemical reaction:

CO2  2 NaOH o Na2CO3  H 2O

This reaction is for all practical purposes irreversible so the back reaction can be disregarded. For the calculation
of effective area we assume that the absorption takes place in the pseudo first order reaction regime. This
assumption should be good because of the large excess of NaOH. Gas velocity and temperature have also been
assumed constant in the column. The effective area can then be calculated from:

y C O in
u G ln ( 2
)
y C O o u t
a e
2

Z K G R T
1 1 1

K G k G E ˜ k 0
L

The gas-side resistance was ignored in this analysis. By using the pseudo first order approximation, the enhancement
factor can be set equal to the Hatta number and the last term on the right hand side becomes (16):

k OH  [O H ]D CO2
E ˜ k L0 K G
H CO2

In the equations, y is mole fraction in gas, Z is packing height, kG is gas side mass transfer coefficient, kOH- is reaction rate
constant, DCO2 is the diffusivity and HCO2 is a Henry’s constant. On the basis of studies in a wetted wall column by
 A. Zakeri et al. / Energy Procedia 4 (2011) 606–613 611
6 Author name / Energy Procedia 00 (2010) 000–000

Pohorecki (17), values for kOH- and Henry’s law constants were determined as functions of ionic strength and temperature
and were given as correlations (17).

4.2 CO2-MEA

The reaction between CO2 and MEA in the aqueous solution can be described by:

CO2  R1 NH 2 o R1 N  HCOO 
R1 N  HCOO   B o R1 N COO   BH 
yCO2in  y *CO 2in
uG ln( )
yCO2 out  y *CO 2 out
ae
ZK G RT
k 2 ˜ cMEA
f
˜ Dco2
KG , f
cMEA f0
cMEA (1  2D )
H CO2

In this system all assumptions and calculations are very similar to the CO2-NaOH system.  is the CO2 loading. For
details se Hartono et al.(18). Values for y*CO 2in and y*CO 2 out are based on Aronu et al., calculated from a UNIQUAC
model. Kinetic parameters were calculated according to Versteeg et al. (19).

The experiments were performed at different liquid and gas flow rates, to reach a new steady state condition took
approximately 6-10 min. The gas phase CO2 concentrations (inlet and outlet), the gas temperature (inlet and outlet),
and the gas and liquid flow rates were recorded. Simultaneously an outlet liquid sample was taken. The CO2
concentration in the gas phase was determined continuously by a Fisher-Rosemount CO2 IR analyzer and the liquid
phase CO2 concentration was determined with acid titration using the barium carbonate precipitation method (20).
The amount of amine was determined through a standard monotonic end point titration with 0.1 N sulfuric acid. The
results given as fractional area, defined as ae / anom , are presented in Figure 4:

a b

Figure 4 Experimental results on relationship between Fractional effective area and Liquid flow (m3/m2hr)
in the packed column (Sulzer Mellapak 2X) (a)Air-CO2/Water-NaOH(0.3M),(b) Air-CO2/MEA(30wt%).
612 A. Zakeri et al. / Energy Procedia 4 (2011) 606–613
Author name / Energy Procedia 00 (2010) 000–000 7

During all experiments the gas density was almost constant. This implies that the f-factor, uG ˜ U G , would be
proportional to the gas velocity and actually about 1.1 times the gas velocity. Both the specific liquid load and the f-
factor have a clear influence on the value of the mass transfer area. There is some scatter in the data, but the trends
are clear. Both for NaOH and MEA solutions the active area increases with liquid load up to about 25 m3/m2h.
Above this the trend is more unclear. There is also an increase in active area with increasing gas flow rate. Generally
the active areas found for the MEA solution are higher than for NaOH. A possible explanation is the effect of the
lower surface tension of the amine solution and the better wetting properties. Another explanation for the difference
is the uncertainty in the calculation of the absorption rate, especially for the MEA system. There are important
uncertainties in the reaction rate constant, the diffusivity and the Henry’s constant. Also the effect of gas velocity is
greater for MEA, which again may be related to lower surface tension and easier droplet formation. This could,
however, lead to droplet entrainment and reduced performance at higher gas velocities.

5. Conclusions

Pressure drop, liquid hold-up and effective mass transfer area have been successfully determined in a small pilot
plant absorber (0.5 m ID, 5 m packing height) as function of gas and liquid flow rate. The hydraulic variable
parameter dependencies are in reasonable agreement with correlations found in literature. The values of measured
effective mass transfer area are close to values found in literature. A slight influence of viscosity on pressure drop
and flooding velocity has been found. Increased viscosity has a significant influence on hold-up especially at high
liquid loads.

6. Acknowledgements

Financial support provided from Statoil and the Research Council of Norway through the VOCC project, and
Statoil, Shell Technology Norway AS, Metso Automation, Det Norske Veritas AS, and the Research Council of
Norway through the CCERT project (182607), is greatly appreciated.

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