Energy Procedia 00 (2010) 000000

Energy
Procedia

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GHGT-10
Equilibrium absorption of carbon dioxide by amino acid salt and
amine amino acid salt solutions
Ugochukwu E. Aronu
a
, Erik T. Hessen
a
, Tore Haug-Warberg
a
, Karl A. Hoff
b
,
Hallvard F. Svendsen
a,*

a
Department of Chemical Engineering, Norwegian University of Science and Technology, N-7491 Trondheim, Norway
b
SINTEF Materials and Chemistry, N-7465 Trondheim, Norway
Elsevier use only: Received date here; revised date here; accepted date here
Abstract
Experimental vapour liquid equilibrium (VLE) measurements were conducted for an amino acid salt(AAS), 3.5M potassium
sarcosinate and an amine amino acid salt (AAAS), the 5.0M sarcosinate salt of 3-(methylamino)propylamine.The study was
performed in two VLE apparatuses from 40 to 120
o
C and for CO
2
partial pressures ranging from 0.08 to 995 kPa.
Thermodynamic models representing the AAS and AAAS solvent systems were developed using the extended UNIQUAC
model. Model results gave a good representation of the partial pressures of CO
2
above the solvent systems for all measured
temperatures, pressures and CO
2
loadings.

2010 Elsevier Ltd. All rights reserved
Keywords: CO
2
capture, Vapour liquid equilibrium (VLE); Amino acid salt (AAS); Amine amino acid salt (AAAS); Extended UNIQUAC.
1. Introduction
Industrial activities such as natural gas purification, fossil-fuel-fired power plants, petrochemical manufacturing,
steel production and cement production etc. are very essential for human existence but their operation may result in
large emissions of greenhouse gases, notably CO
2
. Thus, CO
2
capture and storage from effluent industrial gas
streams is essential for the reduction of anthropogenic greenhouse gas emissions. Amines, in particular
monoethanol-amine (MEA), are the most studied absorbents for CO
2
recovery and much experimental data on CO
2

solubility in MEA, as well as models predicting these solubilities, are available in the literature, [1], [2], [3]. Present
day amines, however, are still deficient in many aspects related to CO
2
absorption [4]. Thus the need to find new
solvents or better amines to improve the efficiency of acid gas scrubbing by absorption, persists.
Accurate correlation and prediction of the equilibrium behaviour of any new chemical solvent for carbon dioxide
removal is of fundamental importance in the design, optimization and operation of absorption based CO
2
capture
processes. Amino acid salts, as well as amine amino acid salts, have been proposed as suitable alternatives to

*
Corresponding author. Tel.: +47-73594100; fax: +47-73594080.
E-mail address: hallvard.svendsen@chemeng.ntnu.no; ugochukwu.aronu@chemeng.ntnu.no.

c 2011 Published by Elsevier Ltd.
Energy Procedia 4 (2011) 109116
www.elsevier.com/locate/procedia
doi:10.1016/j.egypro.2011.01.030
2 U.E. Aronu et al./ Energy Procedia 00 (2010) 000000
amines, [5] [6] [7]. Amino acid based solvents have the advantage that amino acids are green chemicals, implying
that they have no detrimental environmental effect. In addition the solvents are in salt form, thus their ionic state
results in reduced solvent volatility [8]. Aronu et al., [9, 10] showed that amine amino acid salt solvents have the
additional advantage of a potentially reduced energy requirement as compared to MEA or an amino acid salt
solution.
Presently, experimental VLE data and thermodynamic models of amino acid based solvent systems are very
scarce in the literature. This work presents a basis for modelling of the vapour-liquid equilibrium of an amino acid
salt (AAS) formed by neutralization of sarcosine with an inorganic base, potassium hydroxide (KSAR), as well as
for an amine amino acid salt (AAAS) formed by neutralization of sarcosine with an organic base, 3-
(methylamino)propylamine (SARMAPA). The extended UNIQUAC model, see Thomsen and Rasmussen, 1999
[11], Nicolaisen et al., 1993 [12], Sander et al. 1986 [13] was used to calculate the activities required to predict the
equilibrium partial pressure of CO
2
as function of temperature and composition. The parameter estimation for the e-
UNIQUAC model was based on experimental data from both low and high temperature equilibrium measurements.
2. Equilibrium Experiments
The chemicals were obtained as follows: Sarcosine (Fluka, purity98%), 3-(methylamino)propylamine, MAPA
(purity > 99%) and potassium hydroxide (KOH) (Merck KGaA, purity85%). All the solution samples were
prepared with deionized water. The gases used; CO
2
, purity > 99.99mol%, CO2, 4.96 mol % and N
2
, purity >
99.999 mol% were supplied by AGA Gas GmbH. The amine amino acid salt (AAAS), SARMAPA, was prepared by
mixing sarcosine with an equinormal amount of amine(MAPA). Similarly, the potassium salt of sarcosine (KSAR)
was prepared using equimolar amounts of KOH and sarcosine.
2.1. Low temperature( atmospheric) VLE apparatus
Vapour liquid equilibrium for the loaded 3.5M KSAR and 5M SARMAPA systems from 40 to 80
o
C and at
atmospheric pressure were measured using a low temperature/atmospheric vapor/liquid equilibrium apparatus,
figure 1, designed to operate up to 80
o
C. 150cm
3
solutions of loaded sample are placed in three equilibrium cells,
and the gas phase is circulated and analyzed online. Details are given by Mamun et al., 2006 [14]. Liquid phase
compositions were obtained by sampling about 50cm
3
for analysis by the barium chloride method. Equilibrium gas
phase partial pressures of CO
2
in the system were calculated by the equation:

2 2 2 2
[ ( ) ( )]
IR IR IR
CO CO H O H O Am Am
P y P P P P P = (1)

where , %CO
2
IR
CO
y
2
in analyzer; , atmospheric pressure; and are partial pressures of water and
amine at cell 4 temperature while
P
2
IR
2
H O
P
Am
P
H O
P and
IR
Am
P partial pressures of water and amine at the cooler temperature.
The amino acid salts are ionic thus is considered negligible.
Am
P

Figure 1: Low temperature (atmospheric) equilibrium apparatus.
110 U.E. Aronu et al. / Energy Procedia 4 (2011) 109116
U. E. Aronu et al./ Energy Procedia 00 (2010) 000000 3
+
3

+
2.2. High temperature VLE apparatus
Equilibrium data at 100 and 120
o
C for the systems were obtained using a high temperature apparatus as described
by Mamun et al.,2005 [15], consisting of two connected autoclaves (1000 and 200cm
3
) rotating 180
o
C with 2 rpm
and designed to operate up to 10bar and 150
o
C.
3. Chemical and Phase Equilibria
3.1. Chemical Equilibrium
Dissociation of Water
2 3
2
w
K
H O H O OH
+
+
ZZZX
YZZZ
(2)
Dissociation of Carbondioxide
2
2 2 3 3
2
CO
K
H O CO H O HCO
+
+ +
ZZZZX
YZZZZ
(3)
Dissociation of Bicarbonate
3 2
2 3 3 3
HCO
K
H O HCO H O CO

+
+ +
ZZZZX
YZZZZ
(4)
Dissociation of KOH
KOH
K
KOH K OH
+
+
ZZZZX
YZZZZ
(5)
Dissociation of zwitterion/protonated sarcosine
2
2 3
SAR
K
H O SAR H O SAR
+ +
+
ZZZZX
YZZZZ
(6)
Sarcosinate carbamate reversion to bicarbonate
2
2
SARCOO
K
H O SARCOO SAR HCO

+
ZZZZZX
YZZZZZ
(7)
Dissociation of protonated SARMAPA
2 3
SARMAPA
K
H O SARMAPAH H O SARMAPA
+ +
+ +
ZZZZZX
YZZZZZ
(8)
Sarcosinate carbamate reversion to bicarbonate
2 3
SARMAPACOO
K
H O SARMAPACOO SARMAPA HCO

+ +
ZZZZZZZX
YZZZZZZZ
(9)

Eqs. 2 to 7 represent equilibrium reactions for the AAS while eqs. 2, 3, 4, 8 and 9 represent equilibrium reactions
for AAAS. The equilibrium reactions presented for AAAS represent a simplified set of equilibrium reactions
expected in an amine amino acid salt system where the carboxyl group in the amino acid is assumed to be
completely deprotonated by the amine. This may not be the real situation as was pointed out by Aronu et al. 2010
[7], it is expected that since the amine is a weak base, only partial neutralization can occur thus allowing the
existence of some free amine. But for development of the model, the assumption is deemed adequate at this stage.
Future work will present a rigorous model for the amine amino acid salt system. The equilibrium point of the
reactions for each system was found by minimizing the Gibbs energy, G at a fixed T and P in terms of mole
numbers, subject to the material balance constraints (atom or element matrix). This was solved as a constrained
U.E. Aronu et al. / Energy Procedia 4 (2011) 109116 111
4 U.E. Aronu et al./ Energy Procedia 00 (2010) 000000
optimization problem using non-stoichiometric method [16]. Detailed discussion on the solution method is given by
Hessen, 2010 [17].
3.2. Vapour-liquid equilibrium
For a complete model of each system, chemical and vapour-liquid equilibrium must be solved simultaneously.
Each system is formulated as a standard VLE problem through the thermodynamic equilibrium criteria at given
temperature and pressure.

( ) ( )
, , , ,
vap liq
i i
T P n T P n = (10)
Where
vap
i
and
liq
i
are the chemical potentials of the species in the vapor and liquid phase respectively. An
activity coefficient model, e-UNIQUAC, was used for the liquid phase while an equation of state, Soave-Redlich-
Kwong (SRK), was used for the vapor phase. The amino acid salts are ionic and thus considered non-volatile. The
equilibrium distribution of the volatile solute, CO
i
2
, between the vapor and liquid was modeled based on Henrys
law and with infinite dilution in water at system pressure and temperature as reference state. Because of the
unsymmetric reference state of CO
2
, its phase equilibrium is calculated from:
( )
2 2
2 2 2 2 2
exp
S
CO H O
CO CO CO CO CO
v P P
y P x H
RT
|

| |

|
=
|
\ .
(11)
where
2
CO
and
2
CO
| are activity and fugacity coefficients of CO
2
respectively, P the total pressure. is
Henrys law constant at infinite dilution [18] and
2
the infinite dilution partial molar volume of CO
2
CO
H

CO
v

2
[19]. The
reference state for water was pure water at system temperature and pressure, thus the phase equilibrium of water was
calculated from:
( )
2 2
2 2 2 2 2 2
exp
s S
H O H O
s
H O H O H O H O H O H O
v P P
y P x P
RT
| |
| |

|
=
|
\ .
(12)
Here
2
H O
is the activity cofficient for water,
2
H O
| ,
2
s
H O
| are fugacity coefficients for water vapour and
saturated water vapour respectively while
2
s
H O
v is the partial molar volume of water [28]. The fugacity coefficients
for CO
2
and water in gas phase were calculated using the SRK equation of state. Because of the assumption of
complete neutralization of the amine, no amine volatility was calculated. The standard chemical potentials for most
of the species in the CO
2
-amino acid based solvents are not available in the literature. However, the equilibrium
constant for the reaction j is related to the standard chemical potentials,
o
i
as follows:

( ) ( ) ln
O
j ij i
i
RT K T v T =
_
(13)

Equilibrium constant for reactions 2, 3 and 4 were taken from Edwards et al. 1978 [21], 6 and 8 were determined
experimentally, reaction 5 dissociates completely while 7 and 9 were fitted to experimental data. For the CO
2
-AAS-
water system, there are eleven species and six reactions while in the CO
2
-AAAS-water system there are nine species
and four reactions, hence eq. 13 is underspecified for both system. This was resolved by setting five of the standard
state chemical potentials to zero in the CO
2
-AAS-water system, while in the CO
2
-AAAS-water system four were set
to zero and then solved for the remaining ones. This solution approach has been described by Hessen et al., 2010 [2].

112 U.E. Aronu et al. / Energy Procedia 4 (2011) 109116
U. E. Aronu et al./ Energy Procedia 00 (2010) 000000 5
4. Model
The original non-electrolyte UNIQUAC equation from Abrams and Prausnitz, 1975 [22] was extended for
electrolyte systems by addition of an electrostatic term as by Sanders et al., 1986 [13] forming a modified
UNIQUAC equation. The model thus consists of three terms: a combinatorial, a residual (short range terms) and the
electrostatic (long range) term of Debye-Hckel type. The extended UNIQUAC model used for thermodynamic
calculations in this work is as presented by Nicolaisen et al., 1993 [12] and Thomsen, 1997 [23].

E E E E
Combinatorial Residual Debye Huckel
g g g g
RT RT RT RT

( ( (
= + +
( ( (


(14)

The combinatorial, entropic term, eq. 15, is independent of temperature. It accounts essentially for the differences
in size and shape of the species; where 10 z = is the coordination number, the number of the nearest neighbors
around a central solvent molecule,
i
x is the mole fraction,
i
| is the volume fraction,
i
u is the surface fraction of
the component i . The model parameters and are respectively the volume and surface area parameters for the
component . These may be calculated using the method of Bondi, 1968 [24] for non-electrolyte molecules and
Marcus, 1997 [25] for ions, but better results are obtained if these parameters are fitted to experimental data [26].
i
r q
i
i

ln ln
2
E
C i i
i i i
i i
i i
g z
x q x
RT x
| |
u
| | | |
=
| |
\ . \ .
_ _
(15)

;
i i i i
i i
l l l l
l l
x r x q
x r x q
| u = =
_ _
(16)

The residual, enthalpic term is given by eq. 17. The parameter
ki
is given by eq. 18, where and are
temperature dependent binary interaction energy parameters.
ki
u
ii
u

ln
E
R
i i k ki
i k
g
x q
RT
u
| |
=
|
\ .
_ _
(17)

exp
ki ii
ki
u u
T

| |
=
|
\ .
(18)
( 298.15)
O t
ki ki ki
u u u T = + (19)

The Debye-Hckel, electrostatic term is

( )
2
3
4
ln 1
2
E
DH
w w
g A b I
x M b I b I
RT b
(
= + +
(

(20)

U.E. Aronu et al. / Energy Procedia 4 (2011) 109116 113
6 U.E. Aronu et al./ Energy Procedia 00 (2010) 000000
w
x is the mole fraction of water,
w
M kgmol
-1
is the molar mass of water and b = 1.5(kg/mol)
1/2
. The Debye-
Hckel constant A is approximated in the temperature range 273.15 383.15 K T K s s [27], [12] by

( ) ( )
1 1
2
3 5
2 2
1.131 1.335 10 273.15 1.164 10 273.15 A T T kg

(
= + +

mol

(21)
I is the ionic strength in mole/kg H
2
O:

2 2
1 1
2 2
i i i i w w
i i
I m z x z x M = =
_ _
(22)
i
m is the molality of ion i , is the charge of ion i . Activity coefficient expressions of the extended UNIQUAC
i
z
implemented in this work were found by differentiating the total excess Gibbs energy expression, eq. 23.

( )
,
ln
j
E
i
i
T n
ng RT
n

=
(
c
( =
c
(

(23)

The symmetric activity coefficient for water and the unsymmetric activity coefficients for ions were found from
eq. 24 and 25 respectively.

ln ln ln ln
C R DH
w w w w
= + + (24)
( )
, ,
ln ln ln ln ln ln
C R C R DH
i i i i i i

-
= + + + (25)


5. Results and Discussion
Experimentally determined CO
2
partial pressures and loadings were used for regression of the e-UNIQUAC model
volume, and surface area, parameters as well as the temperature dependent interaction energy parameters
and . Figure 3a shows model prediction results from the e-UNIQUAC implementation for 40 to 120
r q
O
ki
u
T
ki
u
o
C for the
AAS, 3.5M KSAR, while figure 4a shows similar results for the AAAS, 5.0M SARMAPA. Figure 3b and 4b show
predicted species distributions at 40
o
C for the AAS and AAAS respectively. Speciation results in AAS, figure 3b
clearly shows the ionic nature of the solvent with deprotonated sarcosine (SAR
-
) decreasing as it reacts with CO
2
,
K
+
remained inert thus maintained a constant concentration. KOH and zwitterion sarcosine do not exist in solution
due to complete neutralization. Speciation results for AAAS, SARMAPA in figure 4b do not give a detailed species
distribution in AAAS as was the case for AAS. This is because SARMAPA was treated as a whole amine due to the
simplifying assumption of complete deprotonation of sarcosine, thus it does not show separate distributions of
MAPA and sarcosine species.
114 U.E. Aronu et al. / Energy Procedia 4 (2011) 109116
U. E. Aronu et al./ Energy Procedia 00 (2010) 000000 7
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
10
-4
10
-3
10
-2
10
-1
10
0
10
1
10
2
10
3
10
4
CO
2
loading (mol CO
2
/ mol SAR)
P
C
O
2

(
k
P
a
)
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
0
0.01
0.02
0.03
0.04
0.05
0.06
0.07
0.08
CO
2
loading (mol CO
2
/mol SAR)
L
i
q
u
i
d

m
o
l
e

f
r
a
c
t
i
o
n
SAR
-
CO
2
SARCOO
2-
+
SAR
-
K
+
HCO
3
-

( )
a ( )
b
Figure 3: a. CO
2
partial pressure as function of loading for 3.5M KSAR. b. Speciation at 40
o
C. Experimental data: , 40
o
C; , 60
o
C; , 80
o
C;
, 100
o
C; V , 120
o
C; , e-UNIQUAC.
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
0
0.02
0.04
0.06
0.08
0.1
0.12
0.14
0.16
0.18
CO
2
loading (mol CO
2
/mol SARMAPA)
L
i
q
u
i
d

m
o
l
e

f
r
a
c
t
i
o
n
0 0.1 0.2 0.3 0.4 0.5 0.6
10
-4
10
-3
10
-2
10
-1
10
0
10
1
10
2
10
3
10
4
CO
2
loading (mol CO
2
/ mol SARMAPA)
P
C
O
2

(
k
P
a
)
SARMAPA
HCO
3
-
SARMAPAH
+
SARMAPACOO
-
CO
2

( )
a ( )
b
Figure 4: a. CO
2
partial pressure as function of loading for 5M SARMAPA. b. Speciation at 40
o
C. Experimental data: , 40
o
C; , 60
o
C; , 80
o
C;
, 100
o
C; V , 120
o
C; , e-UNIQUAC.
6. Conclusions
Equilibrium measurements of partial pressure of CO
2
over an aqueous amino acid salt solution, 3.5M KSAR and an
aqueous amine amino acid salt solution, 5.0M SARMAPA were carried out from 40 to 120
o
C for pressures 0.08 to
995 kPa using both low and high temperature equilibrium apparatuses. A thermodynamic model using the extended
UNIQUAC model to calculate activities was applied to calculate partial pressures of CO
2
over these systems. The e-
UNIQUAC model results gave a very good representation of experimental data.
U.E. Aronu et al. / Energy Procedia 4 (2011) 109116 115
8 U.E. Aronu et al./ Energy Procedia 00 (2010) 000000
Acknowledgement
This publication forms a part of the BIGCO2 project, performed under the strategic Norwegian research program
Climit. The authors acknowledge the partners: Statoil AS, GE Global Research, Statkraft, Aker Clean Carbon, Shell,
TOTAL, ConocoPhillips, ALSTOM, the Research Council of Norway (178004/I30 and 176059/I30) and Gassnova.
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116 U.E. Aronu et al. / Energy Procedia 4 (2011) 109116