Gas-Phase Mass Transfer Coefficient of CO in Different Alkanolamine Solutions Within Packed-Bed Absorption Column

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Gas-phase mass transfer coefficient of CO2

in different alkanolamine solutions within


packed-bed absorption column
Cite as: AIP Conference Proceedings 2279, 090001 (2020); https://doi.org/10.1063/5.0023685
Published Online: 26 October 2020

P. Vaewhongs, K. Photein, R. Nimchareon, et al.

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AIP Conference Proceedings 2279, 090001 (2020); https://doi.org/10.1063/5.0023685 2279, 090001

© 2020 Author(s).
Gas-Phase Mass Transfer Coefficient of CO2 in Different
Alkanolamine Solutions within Packed-bed Absorption
Column
P. Vaewhongs1, K. Photein1, R. Nimchareon1, T. Limlertchareonwanit1,
K. Minakanishtha1, K. Maneeintr2 and T. Charinpanitkul1, 3, a)
1
Center of Excellence in Particle Technology, Department of Chemical Engineering,
Faculty of Engineering, Chulalongkorn University, Bangkok, THAILAND
2
Department of Mining and Petroleum Engineering
Faculty of Engineering, Chulalongkorn University, Bangkok, THAILAND
3
Research Network of NANOTEC-KU on Nanocatalyst and Nanomaterials for Sustainable Energy and
Environment, Bangkok, THAILAND.
a)
Corresponding author: ctawat@chula.ac.th

Abstract. For suppressing the global warming phenomenon, CO2 capture and storage has increasingly drawn attention
from many research groups. Among various methods, absorption of CO2 using aqueous solution has been recognized as
one of effective alternatives. As a result, there are many absorbents explored for improving CO2 capture and storage
capability, which is limited by the mass transfer step between gaseous CO2 and liquid absorbent. In this work,
comparison of overall volumetric gas-phase mass transfer coefficient (KGav) of CO2 in solution of alkanolamine
(Monoethanolamine, 2-(methylamino)ethanol and Dimethylaminoethanol) was comprehensively examined within a
packed-bed absorption column containing Raschig ring packing. Effect of alkanolaime types, concentration and solvent
flow rate were experimentally investigated under the atmospheric pressure and temperature. Typically, MEA with a
concentration of 3.0 kmol/m3 could provide the KGav value of 0.36 kmol/(m3·kPa·h). Meanwhile, KGav of CO2 in 2-MAE
could achieve the highest value of 0.73 kmol/(m3·kPa·h) when 2-MAE solution was supplied with a concentration of 5.0
kmol/m3. All of experimental results revealed that 2-MAE exhibited the highest KGav when compared to those of other
two alkanolamine species, suggesting that 2-MAE would be a potential absorbent effective for CO2 capture and storage
application.

INTRODUCTION
Global warming phenomenon resulted from an increase in CO2 content in the atmosphere exerts significant
effect to many environmental problems. According to International Panel on Climate Change (IPCC) 2014, CO2
concentration would increase to 500-1000 ppm by the end of 2100 [1]. Therefore, reduction in CO2 content in the
ambient is an important and urgent issue considered for mitigating the global warming threat. Fossil fuel-burning
power plants are one of the largest sources emitting CO2 up to one fourth of total CO2 emission [2]. So far, there are
many research attempts to improve CO2 capture and storage (CCS) technology employed in such industrial power
plants. Among various CCS technologies, chemical absorption or chemisorption of CO2 using a reactive absorbent
within packed absorption columns has been recognized as a technology applicable for many industrial processes due
to its capability to operate at the atmospheric pressure and temperature and high CO2 capturing efficiency [3-5].
There are specific criteria for selection of CO2 absorbent based on its absorption characteristics, i.e. CO2
solubility, CO2 absorbing kinetics, volumetric mass transfer coefficient, and enthalpy change of absorption and
regeneration as well as corrosion and degradation properties [6-10]. Li et al reported that CO2 solubility in an
absorbent is the first key parameter to be explored in prior to the actual application. In addition, CO2 loading and

The Second Materials Research Society of Thailand International Conference


AIP Conf. Proc. 2279, 090001-1–090001-9; https://doi.org/10.1063/5.0023685
Published by AIP Publishing. 978-0-7354-4009-8/$30.00

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cyclic capacity of the selected absorbent would be necessary for design of an effective CO2 absorption process.
Based on some previous studies on CO2 solubility in many alternative absorbents, alkanolamine solution has been
recognized as an effective alternative because of its chemical absorption characteristics which are superior to
physical absorption using water. However, there is still lack of understand in the equilibrium condition, chemical
reaction of CO2 within alkanolamine solution, which would generally be required for effective design of such
absorption process. Application of such alternative solvent would lead to greater CO2 absorption capacity and higher
possibility for reutilization after its regeneration [10-12].
Over the past few decades, monoethanolamine (MEA) known as primary alkanolamine has been widely used as
a commercial absorbent according to its advantages, such as fast absorption rate, and high mass transfer rate [12].
However, the major drawback of MEA is high enthalpy change ( 3.3 GJ/ton of CO2) required for the complete
regeneration [13]. Accordingly exploration of other alternative alkanolamines, which would provide better CO2
absorption capacity and require less enthalpy change of regeneration, has been of interest by many researchers in the
field of CCS technology. Meanwhile, secondary and tertiary amines have drawn attentions of many researchers
because of their potential as effective candidate for CO2 capture and storage [13-16]. To date, there are some
fundamental investigations on solubility of CO2 in such alternative alkanolamines within small scaled isothermal
absorption vessels [16,17]. To the best of our knowledge there are only some previous works reporting
comprehensive results of effects of secondary and tertiary alkanolamines as well as operating variables on CO2
absorption within a packed bed absorption column. However, obvious and clear evidences on effect of alkanolamine
flow rate on the overall mass transfer coefficient of CO2 in such absorbent are still not available.
In this study, overall gas-phase mass transfer coefficient based on unit volume of absorber (KGav) of 3 types of
alkanolamine solutions was thoroughly examined in a lab-scale packed bed column. Effects of controlling variables,
which were solvent type, solvent concentration, and solvent flow rate were investigated with regard to two-film
model [14-16]. With comprehensive experimental data analyses, it was found that secondary alkanolamine solution
could exhibit the superior KGav when compared to other alkanolamine solutions. These results would suggest an
insight that such alkanolamine solution would be effective absorbent for CO2 capture and storage within a packed
bed absorption column.

EXPERIMENTAL

Chemicals
99.6% purity nitrogen (N2) (industrial grade) and 99.6% purity carbon dioxide (CO2) were purchased from
Praxair (Thailand). 99.9% purity monoethanolamine (MEA), which represents primary alkanolamine, was supplied
by DOW Chemical (Thailand). As secondary and tertiary alkanolamines, 2-(methylamino)ethanol (2-MAE) and
dimethylaminoethanol (DMAE) with the same purity of 99.9% were purchased from Merck (Thailand). All
chemicals were used as receive without any further purification.

Experimental Methodology
Figure 1 depicts a schematic diagram of our experimental setup and relevant instrumentation. The packed-
bed absorption column with an inner diameter of 0.25 m and a height of 1.80 m contains randomly packed Raschig
ring packing with an outer diameter of 5.0 mm and a length of 5.0 mm. Such packing was employed for providing
stable surface area to accommodate the contact between the alkanolamine solution and gas flow containing CO2
[18]. The bulk gas flow was prepared by mixing CO2 and N2 which were separately fed through a set of feeding
equipment consisting of two needle valves and two mass flow meters (CO2 in a range of 0-5 L/min and N2 in a range
of 0-10 L/min, Aalborg). Then two gaseous streams were mixed in a mixing chamber for preparing simulated gas
before being supplied into the packed-bed column. An IR CO2 analyzer (IEQ Chek, Bacharach) was employed to
measure CO2 content at each sampling point along the length of the column. There were totally eleven sampling
points along the column height. The first five sampling points were set ten centimeters apart and other six sampling
points were set twenty centimeters from one another. For liquid side, an alkanolamine (MEA, 2-MAE and DMAE)
solution was fed by a peristaltic pump (60-600 rpm, BT600-2J, Longer) equipped with a PTFE rotameter (0-200
mL, Cole-Palmer) within an adjustable speed of 0.04-0.12 L/min. After the steady liquid flow was achieved CO2
content within the gas stream sampled from each sampling point was measured using the IR CO2 analyzer.

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FIGURE 1. Schematic diagram of experimental setup

Determination of Overall Mass Transfer Coefficient (KGav)

According to two-fluid film theory, overall CO2 flux ( N CO2 ) moving from bulk gas to bulk liquid could be
determined by Eq (1) where the total driving force is the difference between partial pressure of CO2 in bulk gas
( pCO2 , g ) and the equilibrium partial pressure of CO2 with regard to its concentration in bulk liquid. The overall gas-
phase mass transfer coefficient ( KG ) would be a key parameter which could be affected by temperature, pressure as
well as flowrates of gas and liquid [15,19].

 
NCO2  KG pCO2 , g  pCO2
 (1)

where N CO2 is molar flux of CO2 (kmol/m2·h), KG is mass transfer coefficient kmol/(m2·kPa h), pCO2 , g is partial

pressure of CO2 in bulk gas flow (kPa) and pCO2
is equilibrium partial pressure of CO2 (kPa).
Within a packed-bed absorption column, overall volumetric gas-phase mass transfer coefficient ( KG av ) is
generally taken into account because the total volume of a packed-bed absorption column would be essentially
required for its engineering design. Therefore, CO2 flux based on unit volume of absorber could be determined using
Eq (2).

 
NCO2 av  KG av P yCO2 , g  yCO2
 (2)

Where av is volumetric surface area of the packed-bed column (m2/m3).


It should be noted that N CO2 av could only be indirectly determined from the experiment. Therefore, the total
mole balance of CO2 expressed in Eq (3) would be taken into account.

 yCO2 , g   yCO2 , g 
GI    N CO2 av dz  GI   (3)
 1  yCO , g   1  yCO , g 
 2  z z  2 z

where GI is molar flux of gas (kmol/m2·h), yCO2 , g mole fraction of CO2 and z is vertical position along the
column height (m).

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According to previous study reported by Vaida and Kenig, the chemisorption of CO2 within alkanolamine
solution obeys the fast reaction scheme, resulting in the absence of CO2 content at the interface of the liquid phase

( xCO2  0) [15]. Therefore, yCO 2
which is an equilibrium concentration of CO2 in bulk gas subsequently achieves
zero. Integration of all change of CO2 content along the column height from the top to the bottom would yield
overall mass transfer coefficient as described by Eq (4).

GI  y z  H 
K G av  ln  ( yz  H  yz 0 )  (4)
HP  yz  0 

Where KG av unit is kmol/(m3·kPa·h), H is the total height, and P is the atmospheric pressure (101.325 kPa).
To determine the CO2 loading within a sample of the alkanolamine solution, 2 mL of liquid sample was taken
and titrated with 1 M HCl while methyl orange was used as an indicator. Finally CO2 content analyzed at each
sampling point and dissolved CO2 content within each liquid sample would be employed for examining dependence
of KG av on alkanolamine types, concentration, and solvent liquid flow rate.

RESULTS AND DISCUSSION

Analysis of Alkanolamine Molecular Structure


It should be noted that alkanolamine possess both hydroxyl and amine groups. The presence of hydroxyl group
plays an important role in enhancing the solubility of alkanolamine in water because of its polarity [19]. Meanwhile,
amine group could lead to alkalinity which would enhance the dissolution of CO2 in the aqueous solution [20]. As
summarized in Table 1, there are an amine group and a hydroxyl group in MEA while a hydrogen atom in the amine
group is replaced by a methyl group within the 2-MAE. However, in DMAE, both hydrogen atoms in the amine
group are replaced by two methyl groups, resulting in its higher molecular weight but lower density [19]. According
to the different molecular structure, the reaction mechanism between dissolved CO2 and alkanolamines can be
explained by the following set of equations [21].

Carbamate formation : RNH 2  CO2  RNHCOO   H  (5)

Protonation of alkanolamine : RNH 2  H   RNH 3 (6)

For primary and secondary alkanolamines, such alkanolamine could react with CO2 resulting in formation of
carbamate ion ( RNHCOO  ) and proton ( H  ) . Meanwhile, alkanolamine could simultaneously react with proton to
produce alkanolammonium ( RNH 3 ) . Therefore, combining reactions in Eqs (5) and (6) would lead to Zwitterion
Mechanism which could be derived as follows,

2 RNH 2  CO2  RNHCOO   RNH 3 for primary alkanolamine (7)


 
2 R2 NH  CO2  R2 NHCOO  R2 NH for secondary alkanolamine (8)

Regarding to Eq. (7) or (8), 2 mole of primary or secondary alkanolamine could respectively react with one mole
of CO2 because both alkanolamines contain hydrogen atoms attached to their nitrogen atom within their amine
group. Therefore, it could be implied that a mole of MEA or 2-MAE could basically absorbed only a half mole of
CO2.
However, DMAE, which is a tertiary alkanolamine, consists of no more hydrogen atom attached to nitrogen
atom, leading to the hindered protonation of DMAE. Vaidya and Kenig reported that the reaction between CO2 and
DMAE would follow the route of alkaline-catalyzed hydration as described by Eq. (9) [21].

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R3 N  H 2O  CO2  R3 NH   HCO3 (9)

According to Eq (9), it could be implied that a mole of DMAE could react with a mole of CO2, leading to its
higher CO2 loading [22]. However, the presence of bicarbonate ion would affect the dissolution of CO2 into the
aqueous solution of DMAE. As a result, the different molecular structure of each alkanolamie would result in its
performance in absorbing CO2, leading to requirement of further investigation.

TABLE 1. Basic properties of MEA, 2-MAE and DMAE

Molecular Density,
Absorbents Structures Type Weight 20ºC
(g/mol) (g/cm3)

Monoethanolamine
Primary 61.08 1.02
(MEA)

2-(Methylamino)ethanol
Secondary 75.11 0.94
(2-MAE)

(Dimethylamino)ethanol
Tertiary 89.14 0.89
(DMAE)

Effect of Alkanolamine Type on Mass Transfer of CO2


Based on experimental data of CO2 content absorbed in the sample of alkanolamine along the height of the
packed-bed absorption column, volumetric overall gas-phase mass transfer coefficient (KGav) of each corresponding
alkanolamine could be determined using the set of equations described in previous section. All repeated experiments
were conducted with the designated alkanolamine concentration of 3.0 kmol/m3, 15.0 v/v% CO2 concentration in
bulk gas, liquid flow rate of 10.6 m3/(m2·h) and total gas flow rate of 5.0 L/min. Fig. 2 depicts typical results of
depletion of CO2 content remaining in the bulk gas stream along the column height. At the bottom of the column
CO2 concentration was constant regardless of types of alkanolamine solution because the fresh stream of gas just
came to contact with the alkanolamine solution. CO2 concentration gradually decreased until achieving an
infinitesimal small value (zero with regard to the accuracy of the analyzer) when MEA or 2-MAE was employed. It
should be noted that 2-MAE could totally capture all of CO2 when the gas flow achieved the height of 0.9 m from
bottom while all of CO2 was completely absorbed by MEA at the height of 1.5 m. However, for DMAE the CO2
concentration at the top (exit) of the column was approximately 12.5 v/v%. These results would suggest that the
absorption rate of CO2 within 2-MAE was the highest when compared to those of MEA and DMAE.
Generally, the reactions between CO2 and alkanolamines are fast process which could enhance the dissolution of
CO2 within the alkanolamine aqueous solution [16]. Therefore, mass transfer process is generally considered as the
rate limiting step [22]. As mentioned above, volumetric KGav could be determined based on these experimental
results and Eq. (4). As summarized in Fig. 3, KGav of CO2 in MEA was 0.46 kmol/(m3·kPa·h) while KGav of CO2 in
2-MAE and DMAE was 0.56 and 0.01 kmol/(m3·kPa·h), respectively. These results would confirm the highest CO2
absorption rate within 2-MAE. These consistent results would be attributed to the difference in the reaction
mechanisms resulted from different characteristics of MEA, 2-MAE and DMAE. Kortunov et.al. reported that
though MEA and 2-MAE could react with CO2 via the same reaction mechanism 2-MAE could exhibit lower
carbamate stability when compared to MEA [23]. This is ascribed to an additional methyl group in 2-MAE, which

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could result in inferior electrophilicity over MEA. Moreover, based on thermodynamic analyses of Gangarapu et al.,
Gibbs energy change of carbamate ( RNHCOO  ) hydrolysis reaction of MEA and 2-MAE are 4.80 and 5.83
kcal/mol, respectively [24]. Therefore, carbamate formation in 2-MAE-CO2 system could proceed further when
compared to that in MEA-CO2 system, resulting in the enhancement of CO2 mass transfer rate. For DMAE-CO2
system, the gradual depletion of CO2 content within the gas stream would lead to a higher driving force for mass
transfer of CO2 across the interface. However, as described in the previous section, the presence of bicarbonate ion
within DMAE-CO2 system would significantly retard CO2 dissolution [22]. These results would suggest that the
longer bed height of packed bed column would be required for improving CO2 capturing in DMAE.

FIGURE 2. Effect of alkanolamine types on CO2 concentration depletion along the column height

FIGURE 3. Overall gas-phase mass transfer coefficient of CO2 in each alkanolamine

Effect of Liquid Flow Rate on Mass Transfer of CO2


Repeated experiments under designated conditions (alkanolamine concentration of 3.0 kmol/m3 , CO2 content of
15.0 v/v% and total gas flow rate of 4.0 L/min) were carried out for examining effect of liquid flow rate on the mass
transfer of CO2. The liquid flow rate was controlled by a set of flow controllers with 5.3, 10.6 and 15.9 m3/(m2·h).
According to Fig. 4(a)-(c), it could be observed that an increase in the liquid flow rate could attribute to the
enhanced depletion of CO2 content remaining in the gas flow along the column height. For MEA, the liquid flow
rate of 15.9 m3/(m2 h) could result in the complete capturing of CO2 when the gas flow achieved the column height
of 1.3 m. Similar results could also be observed in the case of 2-MAE. Meanwhile, even with the highest liquid flow
rate of 15.9 kmol/m3 the CO2 content at the exit of the absorption column using DMAE, which could provide slower
capturing of CO2, was 12.1 v/v%. Under our observation, an increase in the liquid flow rate could directly lead to

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the increased alkanolamine flow covering the outer surface of Raschig ring. Chen et al. reported that an increase in
liquid flow rate supplied into a packed column could also result in turbulent mixing of liquid within the column [25].
Regarding to all supporting reasons, it could be implied that the higher liquid flow rate would be preferable to the
enhanced CO2 capturing.
Based on all experimental data of CO2 content along the column height and Eq. (4), KGav of CO2 which was
absorbed by each alkanolamine solution with different liquid flow rate was determined and compared in Fig. 5. It
could be clearly observed that with the same liquid flow rate, 2-MAE exhibited the higher KGav when compared to
those of MEA and DMAE. With the liquid flow rate of 5.3 m3/(m2·h) KGav of CO2 in 2-MAE was 0.48
kmol/(m3·kPa·h) and it was elevated to 0.71 kmol/(m3·kPa·h) when the liquid flow rate was increased to 15.9
m3/(m2·h). However, the liquid flow rate exerted insignificant effect on KGav of CO2 in DMAE. These results would
be ascribed by the slow CO2 capturing behavior of DMAE due to the reaction mechanism involving with the
formation of bicarbonate group as described in Eq. 9.

(a) MEA (b) 2-MAE (c) DMAE


FIGURE 4. Effect of liquid flow rate on CO2 concentration depletion along the column height with (a) MEA, (b) 2-MAE and (c)
DMAE

FIGURE 5. Effect of liquid flow rate on overall gas-phase mass transfer coefficient of CO2

Effect of Alkanolamine Concentration on Mass Transfer of CO2


In general, it could be implied that a higher content of absorbent would be beneficial to a higher absorption of
CO2 because of a higher mass transfer driving force [18,22]. In this work, another set of experiments under
designated conditions, which the liquid flow rate was 10.6 m3/(m2·h), CO2 content in gas flow was 15.0 v/v% and
the total gas flow rate fixed was 4.0 L/min, was carried out to examine effect of alkanolamine concentration within a
range of 3.0, 4.0 and 5.0 kmol/m3.
Figure 6 reveals the effect of the increased alkanolamine concentration on KGav of CO2 within each alkanolamine
solution. As a basis, capturing of CO2 using MEA with a concentration of 3.0 kmol/m3 could provide the KGav value
of 0.36 kmol/(m3·kPa·h). It could be elevated to 0.42 kmol/(m3·kPa·h) (16% higher) when the concentration of
MEA was increased to 5.0 kmol/m3. Meanwhile, 2-MAE also exhibited superior KGav when compared to other two
alkanolamine solutions. KGav of CO2 in 2-MAE could achieve the highest value of 0.73 kmol/(m3·kPa·h) when 2-
MAE solution was supplied with a concentration of 5.0 kmol/m3. On the other hand, capturing CO2 by using DMAE

090001-7
with the concentration of 5.0 kmol/m3 could result in the lower KGav of 0.02 kmol/(m3·kPa·h). Sena et al. reported
that the absorption of CO2 into alkanolamine solution is a process dominated by the mass transfer resistance on gas-
phase side but the higher content of absorbent could also enhance capturing CO2 due to its chemisorption
mechanism [20]. As explained by the set of reactions in Eqs. (7), (8) or (9), an increase in the concentration of
alkanolamine could provide a higher content of reacted CO2 to form carbamate or bicarbonate groups, respectively
[18]. Therefore, a detectable effect of the increased alkanolamine concentration could exert on the higher KGav.

FIGURE 6. Effect of solvent concentration on overall gas-phase mass transfer coefficient of CO2

With all experimental and analytical data discussed about, it could be summarized that alkanolamine solution
could be employed for capturing CO2 effectively within a packed-bed column. Though MEA which is recognized as
primary alkanolamine could exert acceptable performance in CO2 absorption, 2-MAE which is secondary
alkanolamine could provide superior results in CO2 capturing. Nevertheless, further investigation on performance of
DMAE would be further explored for its actual application in CCS.

CONCLUSION
A systematic experimental investigation of gas-phase mass transfer of CO2 in 3 types of alkanolamine solution
was conducted. Incorporating mass balance concept with reaction pathways between CO2 and different
alkanolamine species could reveal that CO2 could be captured effectively by alkanolamine solution supplied into a
packed-bed absorption column containing Raschig ring packing. It was found that 2-MAE which is secondary
alkanolamine could provide the superior KGav while DMAE which is tertiary alkanolamine exhibited the lower KGav.
It was confirmed that KGav of CO2 in 2-MAE could achieve the highest value of 0.73 kmol/(m3·kPa·h) when it was
supplied with a concentration of 5.0 kmol/m3. Finally, KGav in all alkanolamines was significantly affected by their
flow rate and concentration.

ACKNOWLEDGEMENT
The authors are grateful to the Ratchadapisek Sompoch Endowment Fund (2015), Chulalongkorn University
(CU-58-064-CC) for financial support. T.C. acknowledges partial support by the National Nanotechnology Center
(NANOTEC), NSTDA. Ministry of Science and Technology, Thailand through the program of Research Network of
NANOTEC (RNN). Also, partial support from the PTT Innovation Institute is acknowledged.

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