Article

pubs.acs.org/IECR

Mass-Transfer Performance of CO2 Absorption with Aqueous

Diethylenetriamine-Based Solutions in a Packed Column with Dixon
Rings
Miaopeng Sheng,† Chenguang Liu,† Chunyuan Ge,§ Moses Arowo,†,‡ Yang Xiang,†,‡ Baochang Sun,*,†,‡
Guangwen Chu,†,‡ and Haikui Zou*,†,‡
†
Research Center of the Ministry of Education for High Gravity Engineering and Technology and ‡State Key Laboratory of
Organic−Inorganic Composites,Beijing University of Chemical Technology, Beijing 100029, PR China
§
Troops 92609 of People’s Liberation Army, Beijing 100077, PR China
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ABSTRACT: This study investigated the absorption perform-

ance of CO2 into a diethylenetriamine (DETA)-based solution
containing piperazine (PZ) or 1-(2-aminoethyl)piperazine
(AEPZ) as an activator in a packed column with Dixon
rings. The effects of various operation conditions such as the
activator concentration, gas flow rate, liquid flow rate, CO2
partial pressure, and solution temperature on overall gas-phase
volumetric mass-transfer coefficient (KGav) were explored.
Results indicate that the presence of PZ in DETA solution
yields a better enhancement effect on KGav than AEPZ, and,
thus, a combination of 5%PZ+25%DETA solution is expected
to be a promising absorbent for CO2 absorption. The results
further show that KGav increases with an increase in the liquid
flow rate and a decrease in CO2 partial pressure and first increases and then decreases with an increase in solution temperature.
On the other hand, the gas flow rate has an insignificant effect on KGav. A simplified empirical correlation for KGav as a function
of the operation parameters has been proposed, and most of the calculated values are in agreement with the experimental data
with a deviation within ±15%.

1. INTRODUCTION
CO2 is considered as a major greenhouse gas (GHG) and a
main contributor to global warming which consequently results
into a series of serious environmental problems.1 Its continued
rise in atmospheric concentration largely due to emissions from
combustion of fossil fuels is thus a major concern all over the
world, and hence the need to promptly carry out significant and
sustainable mitigation measures.2
Currently, the end-of-pipe treatment process of chemical
absorption is one of the most feasible and matured technologies
for reducing CO2 emission.3,4 Monoethanolamine (MEA)
solution is a typical chemical absorbent that is the most
commonly used for CO2 absorption owing to its fast reaction
rate with CO2. Nonetheless, its limitations of low capacity, high
regeneration energy, corrosion, and degradation significantly
expand the operation costs.5 As a result, efforts in developing
new amine absorbents such as piperazine (PZ),5 diethylenetri-
amine (DETA),6 1-(2-aminoethyl) piperazine (AEPZ),7 and 4-
diethylamino-2-butanol (DEAB)8 have been made in attempt
to accelerate the absorption rate, improve CO2 capacity, or
lower the regeneration loss.
DETA containing two primary amine groups and one
secondary amine group exhibits high reaction rate and CO2
capacity. A study on reaction kinetics of CO2 with DETA
solution shows that DETA has a much higher third-order rate
constant (k3) than MEA but lower than PZ.6 As a result, PZ has
been adopted as an activator in aqueous or nonaqueous DETA
solutions to enhance CO2 absorption performance.9−11
However, the application of PZ is somewhat limited due to
its low solubility in water.5 AEPZ, which is one of the PZ
derivatives, also acts as a good activator in MDEA solution and
has been proposed for CO2 absorption owing to its high
reaction rate with CO2 and better solubility in water as
compared to PZ.7,12 A comparison of CO2 absorption
performance between DETA and MEA in a packed column
with Dixon rings reveals higher overall gas-phase volumetric
mass-transfer coefficient (KGav) of DETA than that of MEA.13
Although some studies previously performed in a rotating
packed bed or stirred tank reactor indicate that PZ+DETA
solution is a promising absorbent and exhibits good perform-
ance for CO2 absorption,9−11 to the best of our knowledge,
there is limited report on the study of CO2 absorption into PZ
+DETA solution in a packed column with Dixon rings.
Received: June 13, 2016
Revised: September 2, 2016
Accepted: September 19, 2016
Published: September 19, 2016

© 2016 American Chemical Society 10788 DOI: 10.1021/acs.iecr.6b02280

Ind. Eng. Chem. Res. 2016, 55, 10788−10793
Industrial & Engineering Chemistry Research Article

Moreover, there is inadequate information on the application of
AEPZ+DETA solution for CO2 absorption.
To investigate the absorption performance of CO2 into
DETA-based solution in the presence of PZ or AEPZ as an
activator, this work presents a study on the absorption of CO2
into PZ+DETA or AEPZ+DETA solution in a packed column
with Dixon rings. Experiments are performed to investigate the
effects of various operation conditions including activator
concentration, gas flow rate, liquid flow rate, CO2 partial
pressure, and solution temperature on the overall gas-phase
volumetric mass-transfer coefficient (KGav). A simplified
empirical correlation to predict KGav in the CO2 absorption
process with DETA-based solution in a packed column with
Dixon rings is also developed.
absorbents solution, Zeng et al.15 assumed that CO2 is
completely exhausted in the liquid film during the absorption
process, and therefore y*CO2 could be neglected in the calculation
of KGav.
The reaction kinetics of CO2 absorption into individual PZ,
AEPZ, or DETA solutions have been reported,6,7,17 and the
comparison of reaction kinetics constants (second-order rate
constant k2 or third-order rate constant k3) is shown in Figure
1. It can be seen that k2 of PZ and AEPZ are much higher than

2. MASS TRANSFER IN A PACKED COLUMN

Based on the two film theory, at a steady state, the absorption
rate of CO2 (NCO2av) into a liquid solution can be expressed
as14
* )
NCO2a v = K Ga v P(yCO − yCO
2 2 (1)
where KGav is the overall gas-phase volumetric mass transfer
coefficient; P is the total pressure; and yCO2 and y*CO2 are mole
fraction and equilibrium mole fraction of CO2 in gas phase,
respectively.
Owing to the small size of the packed column as well as Figure 1. Comparison of the reaction constant between CO2 and
relatively low gas flow rates adopted in this study, there were no different absorbents in the literature.
sampling points installed along the packing section of the
column in order to avoid interference with the mass-transfer
process. Also, the mass transfer coefficient varies vertically
along the packed column since the total gas flow rate constantly that of DETA, MEA, and NH3. Also, k3 of DETA is much
reduces along the column due to chemical absorption of CO2. higher than that of MEA and NH3. Therefore, the reaction rate
However, during the chemical absorption process, mass-transfer of CO2 with PZ+DETA or AEPZ+DETA solution can be
resistance mainly exists in liquid film, and hence the variation of assumed to be much higher than that with MEA or ammonia
the total gas flow rate has an insignificant effect on mass solution. According to Bishnoi and Rochelle13 and Chang et
transfer when yCO2 of the inlet gas stream is relatively low. al.,23 the equilibrium CO2 partial pressure of low-loaded PZ
Furthermore, owing to very low CO2 loading of solution, the +DETA solution used in this work is much less than 0.8 kPa
amount of DETA-based solution is sufficient during the whole (5%PZ+25%DETA with a loading of 0.84) and 0.042 kPa (0.6
absorption process as long as the liquid flow rate remains mol L−1 PZ with a loading of 0.32), further indicating that y*CO2
unchanged. Consequently, it is reasonable to assume that the
is very small relative to yCO2. In addition, research on y*CO2 of the
variation of the mass transfer coefficient along the column is
small and can be neglected.15,16 two absorption systems is still scarce. Therefore, it is reasonable
Considering an element of packing with a height of dh, the and acceptable that yCO * 2 is assumed to be negligible and equals
mass balance equation can be expressed as zero for convenience of calculations. Therefore, eq 3 can be
⎛ y ⎞ rewritten as
NCO2a v dh = G Id⎜⎜ ⎟
CO2
1 − y ⎟ ⎛ ⎞
⎝ CO2 ⎠ (2) GI 1 ⎜ yCO2 ⎟
dh = d⎜
where GI is the inert gas flow rate and is unchanged along the K Ga v P yCO ⎝ 1 − yCO ⎟⎠
2 2 (4)
column.
Then, dh can be derived from eqs 1 and 2 as By integral calculation, packing height h can be expressed as
⎛ y ⎞ ⎡ y
GI 1 (1 − yCO ,out )
d⎜⎜ ⎟
CO2
GI
dh = × ⎢ln
CO2 ,in
1 − yCO ⎟⎠
2
* h=
K Ga v P yCO − yCO
2 2 ⎝ 2 (3) K Ga v P ⎢⎣ yCO ,out (1 − yCO ,in )
2 2

According to the fast reaction regime between CO2 and ⎛ y yCO ,out ⎞⎤
amine, y*CO2 in eq 3 is very low and is close to zero, which is ⎜
+⎜
CO2 ,in
− 2 ⎟⎥
1 − y 1 − y ⎟⎥
commonly assumed to be neglected.13−15 Although Zhao16 ⎝ CO2 ,in CO2 ,out ⎠⎦ (5)
suggested that y*CO2 should not be neglected because of different
reaction mechanisms between CO2 and absorbents in mixed Thus, KGav can be derived as
10789 DOI: 10.1021/acs.iecr.6b02280
Ind. Eng. Chem. Res. 2016, 55, 10788−10793
Industrial & Engineering Chemistry Research
⎡ y (1 − yCO ,out )
GI
× ⎢ln
CO2 ,in 2
K Ga v =
Ph ⎢⎣ yCO ,out (1 − yCO ,in )
2 2
⎛ y yCO ,out ⎞⎤
+ ⎜⎜
CO2 ,in
− 2 ⎟⎥
1 − y 1 − y ⎟⎥
⎝ CO2 ,in CO2 ,out ⎠⎦
3. EXPERIMENTAL SECTION
3.1. Materials. CO2 (purity ≥99.9%) was supplied by
Beijing Ruyuanruquan Technology Co. Ltd., while air was
obtained through an oil free air compressor (TYW-1, Suzhou
Tongyi Electrical and Mechanical Co. Ltd.). A mixture of the
CO2 and air made up the feed gas. Diethylenetriamine (DETA,
purity ≥98.0%) was purchased from Tianjin Fuchen Chemical
Reagents Factory, while piperazine (PZ, purity ≥99.0%) and 1-
(2-aminoethyl)piperazine (AEPZ, purity ≥99.0%) were sup-
plied by Tianjin Guangfu Chemical Research Institute and
Aladdin Industrial Corporation, respectively. All of the aqueous
solutions were prepared with deionized water. All the chemicals
were used as supplied without further purification.
3.2. Experimental Apparatus and Procedure. Figure 2
shows a schematic diagram of the experimental setup for CO2
Figure 2. Experimental setup for the absorption of CO2 in the packed
column.
absorption. The experiments were conducted in a packed
column containing Φ5 × 5 Dixon rings as packing, and the
column was wrapped by heating band and heat insulating
material to control the temperature. Air and CO2 were first
mixed in a buffer tank and then introduced into the column
from the bottom section. When CO2 concentration in the gas
outlet reached a desired steady value, the DETA-based solution
in the liquid stock tank was introduced into the column from
the top section. The liquid stream contacted countercurrently
with the gas stream inside the column, leading to absorption of
CO2 into the DETA-based solution and its subsequent reaction
with the amines. Finally, the liquid stream and gas stream exited
the column via the liquid outlet and gas outlet, respectively.
Article
During the experiment, the difference in temperature between
the inlet and outlet solution was less than 2 °C, and the average
temperature was used.
During each experimental run, CO2 concentration in the gas
stream at the top of column was monitored by an infrared gas
analyzer (GXH-3010F, Beijing Huayun Analytical Instrument
(6) Institution, detect range from 0 to 30%). DETA-based solution
was used as soon as it was prepared. The initial CO2 loading of
the solution, as determined by chemical analysis,14 revealed a
low initial CO2 loading (α ≤ 0.04 mol CO2 mol−1 amine). All
of the experiments were conducted under atmospheric
pressure, and the corresponding data were obtained only
when the system reached a steady state. Details on the
specifications of the packed column and operation conditions
for the CO2 absorption process are shown in Table 1.
Table 1. Specifications of the Packed Column and Operation
Conditions
packed column
diameter of the column (mm) 39
packing type Φ5 × 5 Dixon ring
packing height (mm) 700
packing surface area (m2 m−3) 1700
absorption solutions PZ+DETA, AEPZ+DETA
concentration of absorption solution 30% (PZ or AEPZ: 0−10%)
temperature of absorption solution (K) 303.15−333.15
inlet CO2 concentration (%) 6.1−14.1
liquid flow rate (m3 m−2 h−1) 6.10−12.36
inlet gas flow rate (kmol m−2 h−1) 27.39−65.48
pressure (atm) 1.03
4. RESULTS AND DISCUSSIONS
4.1. Effect of Activator Concentration. Figure 3 shows
the effect of activator concentration on KGav. It is evident that
Figure 3. Effect of activator concentration on KGav.
KGav increased with an increase in PZ or AEPZ concentration,
and the activation effect of PZ in DETA was higher than that of
AEPZ with the same mass fraction. Since both PZ and AEPZ
possess a higher reaction rate with CO2 than DETA,6,7,9,20 a
small addition of PZ or AEPZ into an individual DETA
solution can enhance the reaction rate between CO2 and
absorbents and thus lead to higher KGav. However, KGav slightly
10790 DOI: 10.1021/acs.iecr.6b02280
Ind. Eng. Chem. Res. 2016, 55, 10788−10793
Industrial & Engineering Chemistry Research
decreased when AEPZ concentration in the aqueous AEPZ
+DETA solution exceeded 5%. This was attributed to that more
AEPZ increased the viscosity of the solution and consequently
weakened the liquid-phase mass transfer process.24,25 Based on
the above discussion and considering the price of PZ and AEPZ
as well as the low solubility of PZ, the activator concentration
was maintained at 5% in the ensuing studies in this work.
4.2. Effect of the Gas Flow Rate. Figure 4 shows the effect
of the gas flow rate on KGav. It is evident that varying the gas
Figure 4. Effect of the gas flow rate on KGav.
flow rate had little effect on KGav. This observation is in
agreement with that of both Fu et al.13 and Aroonwilas et al.,14
who also noted that the gas flow rate has an insignificant effect
on KGav. This means that mass transfer resistance mainly exits
in liquid film. The results confirm that the liquid-phase mass-
transfer process dominates in the CO2 absorption into aqueous
DETA-based solution in a packed column, and thus varying the
gas flow rate has an insignificant effect on KGav.
4.3. Effect of the Liquid Flow Rate. Figure 5 shows the
effect of the liquid flow rate on KGav. It is clear that KGav
increased with an increase in the liquid flow rate. As
aforementioned, the mass-transfer resistance mainly exists in
the liquid film in the CO2 absorption process. Therefore,
increasing the liquid flow rate means increasing the turbulence
Figure 5. Effect of the liquid flow rate on KGav.
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of liquid on the packing surface which consequently reduces
liquid-phase mass-transfer resistance. Increasing the liquid flow
rate also leads to an increase in wetted surface area of packing
and thus provides a more effective gas−liquid interfacial area.
Furthermore, a higher liquid flow rate means bringing in
additional fresh amine solution, leading to a lower CO2 loading
of the solution and consequently an increase in the liquid-phase
mass-transfer driving force. All of these factors favor an increase
in KGav with increasing the liquid flow rate.
4.4. Effect of CO2 Partial Pressure. Figure 6 shows the
effect of CO2 partial pressure on KGav. It is evident that KGav
Figure 6. Effect of CO2 partial pressure on KGav.
decreased with an increase in CO2 partial pressure. Although
increasing CO2 partial pressure can increase the gas-phase mass
transfer drive force and thereby enhance the mass-transfer
process, the mass-transfer resistance mainly exists in liquid film
in the two absorption systems employed in this work, and
therefore an enhancement in gas-phase driving force has a
limited effect on KGav. Also, an increase in CO2 partial pressure
means more CO2 per unit of absorption solution. However, the
restricted diffusivity of CO2 and amine molecules in the liquid
phase means that the solution may only hold a relatively steady
amount of CO2.26 This suggests that the term of P(yCO2 − y*CO2)
increases, while NAav remains constant in eq 1. As a result,
increasing CO2 partial pressure results in a drop in KGav.
4.5. Effect of Solution Temperature. Figure 7 shows the
effect of solution temperature on KGav. It is evident that KGav
first increased and then decreased with an increase in solution
temperature. Higher solution temperature accelerates the
reaction between CO2 and amines and consequently yields a
higher reaction rate constant as is illustrated in Figure 1. Also,
higher temperature leads to lower viscosity of solution, which is
favorable to CO2 and amine molecules traveling in the liquid
phase. Both of the two factors favor a higher value of KGav. On
the other hand, higher solution temperature also results in a
decrease in CO2 solubility and a growing volatilization loss of
absorbent, which is unfavorable to CO2 absorption.5,23 The
latter factor was more predominant when the solution
temperature exceeded 323.15 K in this work and hence the
observed reduction in KGav.
4.6. Empirical Correlation for KGav. The overall gas-phase
volumetric mass-transfer coefficient (KGav) is an important
parameter in designing a packed column for CO2 absorption.
DOI: 10.1021/acs.iecr.6b02280
Ind. Eng. Chem. Res. 2016, 55, 10788−10793
Industrial & Engineering Chemistry Research
Figure 7. Effect of solution temperature on KGav.
Many empirical correlations for KGav with relation to operation
parameters have been developed on the basis of experimental
data.13,15−17,27,28 According to previous studies,13,15,28 KGav is
related to amine concentration (Camine) and CO2 loading (α)
and equilibrium CO2 loading (αeq) of absorbent, i.e. (αeq-α)
Camine. However, to the best of our knowledge, there is no
published data on equilibrium CO2 loading (αeq) of AEPZ
+DETA solution. Thus, a simplified empirical correlation of
KGav for CO2 absorption into an aqueous DETA-based solution
in the packed column with Dixon rings was developed on the
basis of a previous study28 and the experimental data, and it can
be expressed as
K Ga v = m1Lm2Gm3e m4(WA / WB)Wtotale m5PCO2 + m6 / T (7)
where m1−m6 are the coefficients for the respective parameters
in eq 7, and WA, WB, and Wtotal are the mass fraction of
activator (PZ or AEPZ), DETA, and total amine in the
solution, respectively. An average absolute relative deviation
(AARD) was used to assess the deviation between the
experimental data and the calculated values as
N K Ga v,cal − K Ga v,exp
1 absorbent for CO2 absorption. The results further show that
AARD = ∑ × 100%
N K Ga v,exp (8)
i=1
where N is the number of experimental data.
By trial and error, the optimum coefficients of m1−m6 were
obtained, and the specific correlations for PZ+DETA and
AEPZ+DETA solutions are shown respectively as
K Ga v ‐ PZ + DETA
= 12.658L0.557G 0.118e1.576(WPZ / WDETA)Wtotale−0.047PCO2 − 1303/ T
(9)
K Ga v ‐ AEPZ + DETA
= 4.191L0.726G 0.140e 0.0234(WAEPZ / WDETA)Wtotale−0.035PCO2 − 1337/ T
(10)
Comparisons between the experimental data and the
calculated values of KGav by eqs 9 and 10 are shown in Figure
8. It is evident that most of the calculated values of KGav are in
agreement with the experimental data with a deviation within
±15%, and the corresponding AARDs calculated by eqs 9 and
10 are 5.35% and 7.32%, respectively.
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Figure 8. Comparisons between the experimental KGav and the
calculated KGav as determined by eqs 9 and 10.
However, due to the lack of physicochemical property data,
further studies are needed for more precise correlations for the
two absorption systems. Also, more research is needed to
examine whether the established correlation in this work can be
applied to other absorption columns with different packing.
5. CONCLUSIONS
This work separately employed two aqueous solutions of PZ
+DETA and AEPZ+DETA as absorbents for CO2 absorption in
a packed column with Dixon rings. The overall gas-phase
volumetric mass-transfer coefficient KGav under various
operation conditions including activator concentration, gas
flow rate, liquid flow rate, CO2 partial pressure, and solution
temperature was evaluated in each of the absorption systems.
The results indicate that both PZ and AEPZ can enhance CO2
absorption performance of DETA solution, with PZ displaying
a better enhancement effect than AEPZ. This suggests that a
combination of 5%PZ+25%DETA solution can be a promising
KGav increased with an increase in the liquid flow rate and a
decrease in CO2 partial pressure. Also, KGav first increased and
then decreased with an increase in solution temperature,
whereas it was insignificantly affected by the gas flow rate. A
simplified empirical correlation was also developed for
predicting KGav, and the results show that most of the
calculated values are in agreement with the experimental data
with a deviation within ±15%.
■ AUTHOR INFORMATION
Corresponding Authors
*Phone: +86 10 64443134. Fax: +86 10 64434784. E-mail:
sunbc@mail.buct.edu.cn. Corresponding author address: P.O.
Box 35, No. 15 Bei San Huan Dong Road, Beijing, China
100029 (B.C. Sun).
*Phone: +86 10 64449453. E-mail: zouhk@mail.buct.edu.cn.
Corresponding author address: P.O. Box 35, No. 15 Bei San
Huan Dong Road, Beijing, China 100029 (H.K. Zou).
Notes
The authors declare no competing financial interest.
DOI: 10.1021/acs.iecr.6b02280
Ind. Eng. Chem. Res. 2016, 55, 10788−10793
Industrial & Engineering Chemistry Research
■ ACKNOWLEDGMENTS
This work was supported by National Key Technology R&D
Program of China (No. 2008BAE65B02) and the National
Natural Science Foundation of China (No. 21406009).
■
NOMENCLATURE
α = CO2 loading of solution (mol mol−1)
AARD = average absolute relative deviation
G = gas flow rate (kmol m−2 h−1)
GI = inert gas molar flow rate (kmol m−2 h−1)
h = height of the packing (cm)
KGav = overall gas-phase volumetric mass-transfer coefficient
(kmol m−3 h−1 kPa−1)
L = liquid flow rate (m3 m−2 h−1)
NCO2av = absorption rate of CO2 into solution (kmol m−3
h−1)
P = total pressure (kPa)
PCO2 = partial pressure of CO2 (kPa)
T = temperature (K)
W = mass fraction (%)
yCO2 = mole fraction of CO2 in gas phase (%)
y*CO2 = equilibrium mole fraction of CO2 in gas phase (%)
yCO2,in = inlet mole fraction of CO2 in gas phase (%)
yCO2,out = outlet mole fraction of CO2 in gas phase (%)
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DOI: 10.1021/acs.iecr.6b02280
Ind. Eng. Chem. Res. 2016, 55, 10788−10793