Energy

Procedia
Energy Procedia 4 (2011) 525–532
Energy Procedia 00 (2008) 000–000
www.elsevier.com/locate/procedia
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GHGT-10

Kinetics and mass transfer of carbon dioxide absorption into aqueous

ammonia
Jinzhao Liu, Shujuan Wang*, Guojie Qi, Bo Zhao, Changhe Chen
Key laboratory for thermal science and power engineering of Ministry of Education
Tsinghua University, Beijing 100084, China
Elsevier use only: Received date here; revised date here; accepted date here

Abstract

Aqueous ammonia can be used to capture CO2 from flue gas of coal -fi red power plant with acceptable CO2 removal
efficiency, high loading capacity of CO2 , low corrosion, low cost, and less degradation, and it could remove other acid
gas pollutants at the same time. However, the CO2 absorption rate and mass transfer in aqueous ammonia still need to
study more deeply. The mass transfer characteristics of CO2 in aqueous ammonia were investigated in this paper.
A small wetted wall column (WWC) was used to study the kinetics of CO2 absorbed in aqueous ammonia. The
correlation of gas -side mass transfer coefficient kg was fitted as Sh ! 3.79(Re∀ Sc ∀ d / h ) 0.486 based on the experimental
data of CO2 absorption in 30%wt MEA solution for this WWC reactor. The reaction rates of CO2 in 1 wt%, 2.5 wt%, 5
wt% to 7.5 wt% aqueous ammonia were measured at the temperatures of 10℃, 20℃,30 ℃to 40 ℃, and the second-order
reaction rate constant k2 was calculated. The termolecular mechanism model was used and discussed according to the
experimental results. The kinetics constants of kTNH and kTH O in termolecular mechanism were also fitted in this paper.
3 2

⃝
c© 2010
2011 Elsevier
Published byAll
Ltd. Elsevier Ltd. Open access under CC BY-NC-ND license.
rights reserved

Keywords: Carbon dioxide, Aqueous ammonia, Absorption, Mass transfer, Kinetics, Separations

1. Introduction

Alkanolamines, such as monoethanolamine (MEA), are common absorbents in CO2 capture process. The drawbacks
o f normal alkanolamines include easily degradation, high corrosion rate, and a high energy requirement fo r
regeneration. Different from organic amines, aqueous ammonia has recently been considered to have potential as an
effective and economic solvent for CO2 capture since its high loading capacity o f CO2 , low corrosion, low cost, and less
degradation, and it could remove other acid gas pollutants at the same time, and has also an acceptable CO2 removal
efficiency[1-9].
Detailed kinetic data are required fo r the optimal design and operation of an absorber. Studies have reported kinetic
reaction rate constants fo r different temperatures. A rapid method of measuring the absorption rate was developed and
[10]
applied to CO2 absorption in partially carbonated ammonia solution at 0–40℃ by Andrew , and the reaction was
considered to be first order for both CO2 and ammonia. The reaction rate was determined by Pinsent et al[11]. in a bubble
[10] [12]
reactor for the same temperature range as Andrew . Gibson et al . presented the relations hip between mass transfer
and the solution flow rate/concentration in a packed column. Hsu[13] studied the rate o f r eaction between CO2 and
ammonia in a semi -batch reactor from 25℃ to 65℃. The rate of reaction in a spray tower was given by Diao et al [2]. for

* Corresponding author. Tel.: +86-10-62788668; fax: +86-01-62770209.

E-mail address: [email protected]

doi:10.1016/j.egypro.2011.01.084
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526 J. Liu et al. / Energy Procedia 4 (2011) 525–532

temperatures from 28℃ to 43℃.The important parameters for the gas -liquid reaction such as the gas -liquid contact time
and area cannot be accurately measured in these studies.
Wetted-wall column studies on the kinetics of C O2 absorption in unloaded and partially carbonated ammonia solution
[14] [15]
were conducted by Qin et al . and Zheng et al . at temperatures from 20℃ and 50℃, and the reaction was
considered to be first order fo r both CO2 and ammonia. The zwitterion mechanism was applied to C O2 absorption in
[16]
ammonia solution in a well-stirred cell reactor from 5 ℃ to 25℃ by Derks and Versteeg . In addition, Puxty et al[17].
presented their latest kinetics results for a reaction in a wetted-wall column reactor at temperatures from 5℃ to 20℃.
Though these studies use the reactors with fixed gas-liquid contact area such as wetted-wall column to measure the
kinetic parameters o f CO2 absorption into ammonia, the data do not agree well, as shown later in this paper, and the
experimental ranges of the concentration and temperature of ammonia solution were not wide enough.
In this work, more data will be contributed to the study of the kinetics o f CO2 absorption in aqueous ammonia. The
gas-side mass transfer coefficient kg was fitted based on the experimental dat a of CO2 absorption in 30 wt% MEA
solution. The termolecular mechanisms were applied to characterize the kinetics and mechanisms of the reaction. The
2
kinetic experiments, using a wetted-wall column with a contact area of about 41.45 cm , cover the concentration o f
aqueous ammonia from 1wt% to 7.5wt% and temperature from 10℃ to 40℃, which expanded the range of temperature
and concentration of aqueous ammonia, and also laid an experimental basis for a more comprehensive and systematic
description of the absorption process of CO2 into aqueous ammonia.

2. Chemical reaction

2.1 Reaction description

The total reaction of C O2 absorption into aqueous ammonia can be described as the eq. (1):
CO2 # NH 3 # H 2O NH 4 HCO3 (1)
The actual process o f the reaction is more complicated, which can be described as step-by-step reactions.
First of all, the eq. (2) occurs, that is, CO2 and NH3 react to generate NH2 COONH4 , and then NH2 COONH4
hydrolyzes in solution instantaneously.
CO 2 # 2 NH 3 # H 2O N H 2 COO ∃ # N H 4 # (2)
Secondly, NH4 and NH2 COO- have an irreversible reaction (3) in solution:
+

NH 2 C O O ∃ # NH 4 # # 2 H 2 O % N H 4 H C O3 # N H 3 H 2 O (3)
2.2 Reaction mechanism
The zwitterion mechanism was proposed to describe the reaction between CO2 amines firstly by Caplow[17] and
further discussed by Danckwerts[18]. Based on the mechanism, amine and CO2 fo rm zwitterions firstly, and then
zwitterion is further deprotonated by a base (B). Eq. (4 ) and eq. (5) show the reaction between ammonia and CO2 when
the zwitterion mechanism is applied to this non-amine system.
N H 3# C O O ∃
k2
C O2 # N H 3 k∃ 1
(4)

N H 3# C O O
∃ kB ∃ #
# B k∃B
N H 2C O O # BH (5)
[19]
The termolecular mechanism was proposed by Crooks and Donnellan , which concluded that the reaction between
amine and CO2 is single-step and termolecular. The initial product is not zwitterion, but a loosely bound encounter
complex. Most of the complexes break up to give reagent molecules again. The reagent molecules do not react with a
second molecule of amine or a water molecule to give ionic products. Bond fo rmation and charge separation occur only
in the second step.
This mechanism was reviewed by da Silva and Svendsen[20] in their ab initio study of carbamate formation from CO2
and alkanolamines, and the termolecular mechanism was further developed. A single-step third-order reaction
mechanism is most likely for the formation of carbamate from CO2 and alkanolamines in solution. The observed
broken-order and higher-order kinetics can be explained by this mechanism.
The mechanism applied to the ammonia system is written as
N H 2 C OO ∃ # BH #
kB
C O 2 # NH 3 # B k∃ B
(6)
If ammonia and water are the dominating bases, the reaction rate fo r the termolecular mechanism can be given as
follows:
rC O ∃ N H T ! ( k NH
2 3
T
[N H 3 ] # k TH O [ H 2 O ])[ CO 2 ][ NH 3 ]
3 2
(7)
The termolecular mechanism was used to describe the reaction of aqueous ammonia and CO2 in this work, and the
correlation of k2 , kTNH3 and kTH2 O with temperature were fitted by the experimental data in this paper.
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J. Liu et al. / Energy Procedia 4 (2011) 525–532 527

2.3 Correction of the reaction rate for hydroxyl ions

Aqueous ammonia is a weak alkali solution. CO2 reacts with both of ammonia and hydroxyl when carbon dioxide
dissolves into aqueous ammonia solution. The reaction rate is determined by both reactions as shown in eq. (9). Pinsent
[11]
et al . suggested that the effect of reaction (8) should be taken into account.
k ∃
C O 2 # OH ∃ & & OH
&% H C O 3∃ (8)
robs ! rC O 2 ∃ NH 3 # k O H ∃ [ O H ∃ ][ C O 2 ] (9)
rC O 2 ∃ N H 3
k obs ! # k OH ∃ [ O H ∃ ] (10)
[ CO 2 ]
kOH ∃ could be calculated by the following eq. (11).
lg( k O H ∃ ) ! 13.635 ∃ 2 8 9 5 / T (11)
- [21-24]
[OH ] could be calculated by eq.(12), and the correlation of K NH is shown as eq. (13) .
3
∃ #
[O H ][ NH ] (12)
K NH3 ! 4
[ NH 3 ][ H 2O ]
ln K N H 3 ! A # B / T # C ln T # DT (13)
And the value of the parameters A, B, C and D in eq.(13) could be -1.256563, -3335.7, 1.4971 and -3.7056, according
to Aspen Plus. So the apparent kinetic rate constant for the formation of carbamate in the NH3 -C O2 -H2 O system can be
written as:
k app ! k obs ∃ k O H ∃ [ O H ∃ ] ! k 2 [ N H 3 ] (14)
k 2 ! k NT H 3 [ N H 3 ] # k HT 2 O [ H 2 O ] (15)

3. Experimental apparatus and methods

3.1 The wetted-wall column

A wetted wall column with a contact area of about 41.45 cm2 has been built[25]. The gas-liquid contactor was
constructed from a stainless steel tube, meas uring 11.0 cm in height and 1.2 cm in diameter. The gas-liquid contact
region is enclosed by a 31.0 cm thick-walled glass tube, separat ed from a water-bath.The chemical solution is pumped
through the inside of the tube, overflows on the top, and is evenly distributed across the outer surface of the tube. After
collection at the base of the column, the liquid is pumped to a liquid reservoir. Gas enters near the base of the column,
counter-currently contacting with the liquid as it flows up into the gas outlet.

Fig.1. Overall experimental flowsheet of WWC.

The water/oil-bath, with circulation o f the water/oil inside, is used to control the temperature of the inlet gas, liquid
and the reactor. Two reservoirs are used in this system, one of which is used fo r the amine solution storage, and the
other is used to holdup the waste solution out o f the reactor. A micro-pump pushes the solution from the reservoir
through a coil submerged in the water/oil -bath, fl owing through a rotameter for flowrate determination. The liquid flow
rate was 2 -3 cm3 /s. After heat ed, the solution fl ows into the wetted-wall column, contact with the gas stream, and then
returns to the reservoir.
3.2 Aqueous Ammonia and CO2 Reactions
The mass flux with chemical absorption can be described as follows based on two-film model, where the total
resistance to mass transfer was divided as the sum of resistances from gas side and liquid side as eq.(16).
1 1 1 (16)
# !
kg kG ' K G
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The overall gas transfer coeffi cient K G can be calculated by the Flux and PCO , in and PCO , out . At the same temperature
2 2

and concentration of ammonia, the value of K G is fixed and can be calculated by the Flux- CO2 partial pressure curve.
Flux
KG ! (17)
PCO2 , b ∃ PCO
*
2

Where, PCO2 ,b is the operational partial pressure of CO2 in the wetted wall column, which was the log mean average,
as eq. (18):
PCO2 , in ∃ PCO2 , out (18)
PCO2 , b !
Ln( PCO2 ,in / PCO2 ,out )
The gas–liquid mass transfer process is enhanced by chemical absorption when the acid gas is treated with
amines/ammonia. The mass flux with chemical absorption is as eq.(19):
1 (19)
Flux ! (C *A ∃ CA, b )
1 RT
#
E Ak L Hkg

Where E A ! 1 # Ha 2 and Ha ! k obs D A .

kL
The reaction is considered to be a pseudo-fi rst-order irreversible reaction. If the Hatta number Ha>>3, the expression
for the enhancement factor (EA) based on the two-film model, penetration model and surface renewal model can be
simplified as eq. (20) [26-27].
k obs DA (20)
EA ! Ha !
kL 0
Physiochemical properties o f the aqueous ammonia solution required in determination of mass transfer, such as
density, viscosity, solubility and diffusivity, were measured or taken from the literature before the experiment.
The viscosities of ammonia solutions of different concentrations and water were calculated using eq. (21) and (22) [28].
17900 (21)
∋ N H 3 ! (0.67 # 0.78 x N H 3 ) e x p ( )
RT
16400
∋ H 2 O ! 1.18 ∀ 10 ∃ 6 exp( ) (22)
RT
The methods used to estimate the diffusion coefficient of C O2 in aqueous ammonia are described below. The
diffusion coefficient of CO2 is estimated from the solution’s viscosity using a modified Stokes-Einstein equation[29].
NH 3 ∃ H2 O
∋ H 2O 0.8 (23)
DCO ! DCO
H 2O
( )
2 2
∋ NH 3 ∃ H2 O
∃ 2119
D CHO2 O2 ! 2.35 ∀ 10 ∃ 6 exp(
) (24)
T
In this paper, the concentration of ammonia is very low, so we can use Henry's law constant of C O2 in water to
estimate the Henry's law constant HCO 2 in aqueous ammonia. Pacheco[30] re-calibrate the Henry's Law constant using
the following correlation.
∃1886.1
H CO2 ( atm ∀ cm3 / mol ) ! 1.7107 ∀107 ∀ exp( ) (25)
T (K )
If we can calculate the gas -side mass transfer coefficient kg , therefore, the value of kG’ can be got by eq. (16), and we
can get the value of the observed reaction rate constant kobs by eq. (26).
kl0 E A kobs DCO2
kG ' ! ! (26)
HC O2 HCO2
The correlation of gas film mass transfer coefficient kg for this WWC is very important and need to be fitted by the
experiment.
3.3 The correlation of gas film mass transfer coefficient kg
The characterization of gas-side mass transfer coefficient kg was given by eq. (27).
Sh ! ) (Re∀ Sc ∀ d h / h ) ( (27)
Where Sh ! RTk g d h / DC O , Re ! ∗ gV g d h / + g , Sc ! , / D , dh is the hydraulic diameter of the annulus and h is the
2

length of the column. The parameters of ) and ( were fitted based on the experimental data of CO2 absorption into
MEA solution. The reaction rate between CO2 and MEA solution is supposed to be high enough that the resistance from
film side can be dominated[30].
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J. Liu et al. / Energy Procedia 4 (2011) 525–532 529

This work determined the gas –phase mass transfer coefficient of the apparatus by absorption of carbon dioxide into
30 wt% MEA solution. The experimental temperature was from 20℃ to 60℃, and the gas flow rate range chosen as 3 -
40 cm3 /s.

Fig.2. Correlation of gas-side mass transfer coefficient k g fitted by CO2 absorption into 30 wt% MEA solution from 20℃ to 60 ℃.

The kg is fitted by fig.2 and the correlation is given by the eq. (28) for this WWC.
S h ! 3.79(Re∀ Sc ∀ d / h ) 0.486 (28)

4. Results and discussions

4.1 Experimental data of CO2 absorption rate in aqueous ammonia

According to the results of this work, the reaction is considered to be a pseudo-fi rst-order irreversible reaction. With
Hatta number Ha>>3, the expression for the enhancement factor (EA) based on the two-film model, penetration model
and surface renewal model can be simplified as eq. (17), and therefore, kobs can be calculated using the eq. (29)
kobs D CO2
kG ' ! (29)
H CO2
The apparent kinetic rate constant kapp and the second-order reaction rate constant k2 discussed in section 2 can be
calculated by eq. (14).
4.2 Determination of the kinetics constants and comparison
The second-order reaction rate constant of CO2 with aqueous ammonia k2 was calculated at different temperatures
and ammonia concentrations, shown in fig.3. And 5 wt% aqueous ammonia k2 (m3 /kmol·s) was found to be as
k 2 ! 3.97 ∀ 10 8 exp( ∃ 3861/ T ) (30)

Fig.3. k 2 -Temperture curves at ammonia concentration of 1wt%, 2.5wt% and 5wt%, temperature range from 10℃ to 40℃.

The second-order reaction rate constant k2 o f 5wt% aqueous ammonia in this work was also compared with the prior
researchers’ results at the same temperature. Fig.4 shows that k2 in this paper was in good agreement with Hsu, Pinsent
and Qin, and significantly lower than Versteeg and Ptux[11,13,14,16,31]. Moreover, this work expanded the range o f
6 Author name / Energy Procedia 00 (2010) 000–000
530 J. Liu et al. / Energy Procedia 4 (2011) 525–532

temperature and concentration of aqueous ammonia, which has laid an experimental basis fo r a more comprehensive
and systematic description of the absorption process of CO2 into aqueous ammonia.

Fig.4. Experiment results comparison of k 2 at different temperature.

The termolecular mechanism, discussed deeply in section 2, was used to describe the reaction of aqueous ammonia
and CO2 in this work, and the correlation of k2 , k TNH3 and k TH 2O with temperature were fitted by the experimental data
in this paper.
k2 ! kTN H 3 [ NH 3 ] # k HT 2O [ H 2 O ] (15)
T T
The kinetics constants k NH 3 and k H 2O in termolecular mechanism were fitted and expressed as a function o f
temperature according to the k2 and the concentrations of aqueous ammonia.

Fig.5 k 2 -[NH3 ] lines used for k TNH3 and k TH 2O fitted at 10℃, 20 ℃, 30 ℃ and 40℃.

Fig.6 The correlation of k TNH3 and k TH 2O with temperature fitted curves.

T
kNH and kHT 2O were important constants to describe the reaction process of CO2 absorption into aqueous ammonia.
3

T
The correlation of kNH and kHT 2O with temperature were given as eq. (30) and eq. (31) according to fig.6.
3

kNT H 3 ! 4.69 ∀10 7 exp( ∃3793/ T ) (30)

k T
H 2O
! 4.36 ∀ 10 exp( ∃ 3 8 4 7 / T )
6
(31)
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J. Liu et al. / Energy Procedia 4 (2011) 525–532 531

These correlations provide an effective method fo r the calculations of k2 and gas -liquid reaction liquid phase mass
transfer coefficient kl at different ammonia concentration and temperature.
T T
The kinetics constants kNH and kH were also compared with some amines solution. The reaction rate of aqueous
3 2O

ammonia was much lower than MEA and some other amines according to the results shown in table 3.
Table 3 Comparison of kinetics constants between aqueous ammonia and amines at 25℃

10 ∃3 kabsorbent
T
kHT 2 O
Absorbent Source
(m6 kmol-2 s-1) (m6 kmol-2 s-1 )
NH3 0.139 10.79 This work
[32]
NH3 0.13 17.10 Qin, 2010
[33]
MEA 1.7 73.7 Aboudheir, 2003
[34]
AEEA 2.35 161 Ma’mun, 2007
[35]
EDAa 2.79 17.72 Li, 2007
[36]
DETA 17.5 179.7 Hartono, 2009
[37]
PZ 70.1 550 Cullinane, 2007

5. Conclusions

The reaction rates of CO2 in 1 to 7.5 wt% aqueous ammonia were determined at the temperatures of 10 to 40 . The
second-order reaction rate constant k2 of CO2 with aqueous ammonia was calculated and also compared with the prior
researchers’ results. The second-order reaction rate constant k2 of aqueous ammonia was much lower than MEA and
some other active amines.
T T
The kinetics constants kNH3 and kH 2O in termolecular mechanism were fitted and expressed as a function o f
T
temperature. The correlations o f kNH and kHT 2O with temperature provide an effective method for the calculations o f
3

second-order reaction rate constant k2 and liquid phase mass transfer coefficient kl. Moreover, this work expanded the
range of temperature and concentration of aqueous ammonia and laid an experimental basis for future research.

Notation

B base species
D diffusivity, m2 s–1
E enhancement factor
H Henry constant, kPa m3 kmol–1
Ha Hatta number
-1 -2 -1
KG overall mass transfer coefficient, mol·pa ·cm ·s
kG’ mass transfer coefficient based on gas phase, mol·pa -1 ·cm-2 ·s-1
k2 forward reaction constant, m3 kmol–1 s–1
kapp apparent reaction rate constant, s–1
kg gas-side mass transfer coefficient, mol·pa-1 ·cm-2 ·s-1
kTH2O termolecular reaction rate constant contributed by water, m6 kmol–2 s–1
kl liquid-side mass transfer coefficient, m s–1
kTNH3 termol ecular reaction rate constant contributed by ammonia, m6 kmol–2 s–1
kobs observed reaction rate constant, s–1
–1
kOH- reaction rate constant for CO2 hydration, s
N absorption flux, kmol m–2 s–1
r reaction rate, kmol m–3 s–1
R universal gas constant, 8.314 J mol–1 K–1
Re Reynolds number
Sc Schmidt number
Sh Sherwood number
T Temperature, K
v velocity, m s–1
η viscosity, Pa s
ρ density, kg m–3
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