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Simulating the capture of CO2 from natural gas: New data and
improved models for methane + carbon dioxide + methanol
Thomas J. Hughes, Mohamed E. Kandil, Brendan F. Graham, Eric F. May
Centre for Energy, School of Mechanical and Chemical Engineering, University of Western Australia, Crawley, WA 6009, Australia
a r t i c l e
i n f o
Article history:
Received 11 April 2014
Received in revised form 25 August 2014
Accepted 22 September 2014
Available online 29 October 2014
Keywords:
Carbon capture
Rectisol process, Equations of state
Vapor liquid equilibrium
Binary interaction parameters
Methanol
a b s t r a c t
The simulation of carbon capture unit operations often involves predicting the vapor liquid equilibrium
(VLE) for mixtures containing polar, non-polar and quadrupolar compounds. In this work, we investigate how well a simple cubic equation of state (EOS) can predict the results of new low temperature,
high-pressure VLE measurements of the ternary methane + carbon dioxide + methanol system, which
is important to the Rectisol process used for capturing CO2 from natural gas. The ternary p, T, x measurements presented here are the rst such data for this system reported in the open literature. First,
predictions made with the Peng Robinson (PR) EOS as implemented in a commercial process simulator
were compared to binary p, T, x data measured in this work and also taken from the literature. Signicant deviations were found between the measured liquid mole fractions and those predicted with the
EOS using the default binary interaction parameters (BIP): the relative standard errors were 39%, 77%
and 17% for the methane + methanol, methane + carbon dioxide and methanol + carbon dioxide binaries,
respectively. Regression of the PR EOS to the binary VLE data by adjusting the BIPs improved the liquid phase mole fraction predictions for the ternary mixture data by a factor of about 2.5 for methane
and methanol. However, improvement by a factor of 4.4 in the carbon dioxide liquid mole fraction was
achieved by describing the carbon dioxide + methanol binary with an asymmetric composition and temperature dependent mixing rule and tuning the BIPs therein to VLE data for this binary over a wide
temperature range. This reduced the standard error in the liquid phase CO2 mole fractions predicted for
the ternary mixture using the optimized model by 79% relative to the default model.
2014 Elsevier Ltd. All rights reserved.
1. Introduction
Predicting the vapor liquid equilibrium (VLE) of systems containing non-polar, polar and quadrupolar components is important,
especially for processes intended to capture CO2 . One such process is the Rectisol process, jointly developed by Lurgi (Weiss and
Schrie, 2010) and Linde (2014), where methanol is used as a physical solvent at temperatures as low as 200 K for the removal of acid
gases from natural gas or syngas (Kohl and Nielsen, 1997). In this
process the CO2 content of the natural gas can be scrubbed down
to a few parts-per-million (ppm) and it is possible to separate H2 S
from the CO2 in addition to impurities generated during coal or
heavy oil gasication (Kohl and Nielsen, 1997). A further advantage of the process is that the gas is dehydrated and dosed with
methanol which is a hydrate inhibitor. An example of the use of the
Rectisol process to capture CO2 is the Great Plains Synfuel Plant in
Corresponding author. Tel.: +61 8 6488 2954; fax: +61 8 6488 1024.
E-mail address: Eric.May@uwa.edu.au (E.F. May).
http://dx.doi.org/10.1016/j.ijggc.2014.09.020
1750-5836/ 2014 Elsevier Ltd. All rights reserved.
122
T.J. Hughes et al. / International Journal of Greenhouse Gas Control 31 (2014) 121127
Supplier
Methane
Carbon dioxide
Methanol
2-Propanol
Air Liquide
BOC
Sigma-Aldrich
Sigma-Aldrich
0.99995
0.99995
0.999
0.999
with the binary mixture the cell was rst evacuated and ushed
with pure methane several times and was then lled close to the
desired pressure with methane. A high pressure liquid chromatography (HPLC) pump was then used to inject about 15 mL of degassed
methanol into the cell. To ll the cell with the ternary mixture, the
cell was rst evacuated and ushed with carbon dioxide several
times and was then charged with carbon dioxide to a higher pressure. Next the cell was charged with methane to close to the desired
pressure. The approximate relative mole fractions of carbon dioxide and methane were controlled by the lling pressures of each
of these gases. Methanol was then pumped into the cell using the
HPLC pump. After charging the cell, for both mixtures, the contents
were maintained isothermally and were mixed for a period of at
least 12 h. Up to ve samples of both the vapor and liquid phases
were then removed and analyzed by gas chromatography (GC). The
next measurement at a different pressure was made either by venting vapor or adding methane gas to the cell. Between each new p
and/or T the cell contents were mixed and the system was allowed
at least 12 h to equilibrate.
2.1. Gas chromatograph (GC) calibration
As described in our previous works (Kandil et al., 2010, 2011), to
rigorously quantify the uncertainty in composition measurements
by GC it is essential to perform a calibration of the GCs detectors.
The GC was equipped with both thermal conductivity detectors
(TCDs) and ame ionization detectors (FIDs). In this work only liquid mole fraction measurements are reported. Samples from the
equilibrium cell passed through a TCD before being sent to a FID.
Gas sample loops with volumes of 5, 25, 100 and 250 L were
used to obtain absolute response factors for methane on both the
FID and TCD, and for carbon dioxide on the TCD. A xed volume
(nominally 0.5 L) liquid sampling valve was used to obtain the
response factors for methanol. To nd the volume of the valve
more precisely the valve was rstly lled with methane and this
sample was sent to the GC. The area measured using the FID was
compared to the areas measured with the gas sample loops and
the volume of the liquid sampling valve was determined to be
0.43 0.01 L. The methanol FID response factor was then obtained
by passing pure methanol and two gravimetrically prepared solutions of methanol in 2-propanol (x2 = 0.1 and 0.5) from the sample
valve to the GC. Finally, relative response coefcients were determined for methanol relative to methane (FID) and carbon dioxide
relative to methane (TCD) (Kandil et al., 2010, 2011).
3. Optimization of equation of state binary interaction
parameters
The PR EOS (Peng and Robinson, 1976) relates the uids pressure, p, temperature, T. and molar volume, v:
p=
RT
vb
(1)
v (v + b) + b (v b)
N
N
i
xi xj
ai aj 1 kij ,
(2)
T.J. Hughes et al. / International Journal of Greenhouse Gas Control 31 (2014) 121127
and
bmix =
xi bi
SE =
2
xh xcalc,h
(3)
amix =
123
xi xj
ai aj 1 xi kij xi kji
(4)
and
kji = Aji + Bji T
RSE =
2
xh xcalc,h
xh
h
(8)
Nm
and
(7)
Nm
(6)
p/MPab
x1
u(x1 )c
200.10
193.15
193.15
193.15
193.15
193.15
3.069
2.878
2.024
1.471
1.034
0.554
0.0607
0.0641
0.0464
0.0346
0.0252
0.0147
0.0003
0.0002
0.0002
0.0002
0.0002
0.0007
u(T) = 0.10 K.
u(p) = 0.005 p.
c
The u(x1 ) values include the effect of the propagated temperature and pressure
uncertainties on the measured compositions combined with the uncertainties of the
composition measurements.
b
124
T.J. Hughes et al. / International Journal of Greenhouse Gas Control 31 (2014) 121127
Table 3
Summary of the results of tuning the binary interaction parameters (BIP), kij , to binary mixture VLE data, in terms of the models standard error (SE) and relative standard
error (RSE) as dened in Eq. (7) and (8).
Methane (1) + methanol (2) (14 points)
Tmin /K
193.15
Tmax /K
213.15
pmin /MPa
0.554
pmax /MPa
6.910
x1,min
0.0147
x1,max
0.1118
Casea
k12
u(k12 )
k21
u(k21 )
SE
RSE
Default
Symmetric
Asymmetric
0.035
0.073
0.11
0.001
0.02
0.015
0.003
0.0275
0.0045
0.0040
0.387
0.050
0.050
Tmin /K
183.15
Tmax /K
210.15
pmin /MPa
3.407
pmax /MPa
5.788
x1,min
0.3175
x1,max
0.9993
Casea
k13
u(k13 )
k13
u(k13 )
SE
RSE
Default
Symmetric
Asymmetric
0.100
0.0917
0.0932
0.0009
0.0009
0.072
0.004
0.0173
0.0114
0.0095
0.77
0.74
0.75
Tmin /K
213.15
Tmax /K
247.12
pmin /kPa
98.1
pmax /kPa
1372.9
x3,min
0.0246
x3,max
0.47
Casea
k23
k32
SE
RSE
Default
Symmetric
Asymmetric
Symmetric temperature dependent
0.040
0.0547 0.0009
0.019 0.002
(0.13 0.02) +
(7.9 0.8) 104 T
(0.046 0.01) +
(3.0 0.5) 104 T
0.064 0.001
0.0778
0.0432
0.0154
0.170
0.162
0.055
(0.094 0.008) +
(6.5 0.3) 104 T
0.0324
0.134
0.0038
0.015
a
The Default case refers to the use of AspenTech HYSYS default BIP. The Symmetric and Asymmetric cases refer to the optimized BIPs using Eqs. (2) and (4)
respectively.
T.J. Hughes et al. / International Journal of Greenhouse Gas Control 31 (2014) 121127
8000
6000
5500
5000
p/kPa
p/kPa
6000
4000
4500
4000
2000
T= 186 K
T= 183 K
3500
0
0.00
0.02
0.04
0.06
x1
(a)
0.08
0.10
3000
0.12
0.3
0.4
0.5
0.6
0.3
0.4
0.5
0.6
0.06
0.06
x1
(a)
0.7
0.8
0.9
1.0
0.7
0.8
0.9
1.0
0.04
x1 - x1,calc
0.04
x1 - x1,calc
125
0.02
0.00
0.02
0.00
-0.02
-0.02
-0.04
-0.04
-0.06
-0.06
0.00
0.02
0.04
0.06
x1
(b)
0.08
0.10
0.12
Fig. 1. (a) Methane (1) + methanol (2) p, x diagram showing measured methane liquid mole fractions and those calculated with the AspenTech HYSYS PR EOS. , This
work T = 193 K; , this work T = 200 K; , Hong et al. (1987) T = 200 K; Vetere (1986)
T = 213 K. The black curves represent AspenTech Hysys liquid mole fractions calculated with default BIP of k12 = 0.035 and the blue curves represent AspenTech Hysys
liquid mole fractions calculated with the optimized (symmetric) BIP of k12 = 0.073
(, T = 193 K; - - -, T = 200 K, , T = 213 K). (b) Deviations between the measured
liquid mole fractions and those calculated (indicated by subscript calc) with the
AspenTech HYSYS PR EOS using the optimized symmetric BIP of 0.073 0.001
for methane (1) + methanol (2). The measured data are represented by the same
symbols as in part a. The curves represent the deviation between the liquid mole
fractions calculated with the default AspenTech Hysys BIP and with the optimized
(symmetric) BIP: , T = 193 K; - - -, T = 200 K, , T = 213 K. (For interpretation of the
references to color in this gure legend, the reader is referred to the web version of
this article).
included as dashed curves. The solid curves represent the calculated p, x data using an optimized asymmetric temperature
dependent
BIP
[A23 = 0.046 0.012,
A32 = 0.094 0.008,
B23 = (3.0 0.5) 104 , B32 = (6.5 0.3) 104 ]. It is apparent,
even from this p, x diagram, that the PR EOS does a signicantly
better job of representing the VLE data with the optimized BIP
rather than the default BIP, particularly at x3 greater than about
0.25. In Fig. 3b the results of Fig. 3a are shown as a deviation plot. It is
apparent that the PR EOS calculated carbon dioxide mole fractions
with the optimized temperature dependent asymmetric BIP lie
within a band of less than about 0.01 of the measured carbon
dioxide mole fractions and that there are no signicant trends
either with temperature or mole fraction (x3 ). Similarly to Figs. 1b
and 2b, the curves plotted in Fig. 3b represent the carbon dioxide
liquid mole fraction calculated with the default AspenTech Hysys
BIP minus the carbon dioxide liquid mole fraction calculated with
the optimized asymmetric temperature dependent BIP for each
isotherm of the data. Unlike for the other binary mixtures, these
lines for each isotherm do not overlap indicating the need to use
a temperature dependent BIP. It is also noted that the deviations
of the PR EOS using the default Aspen Hysys BIP become very
large at x3 greater than about 0.25 with deviations growing to a
mole fraction of 0.2 or more for two of the isotherms (see inset of
Fig. 3b). Before optimization the SE and RSE of the deviations from
predictions made using the Hysys default BIP were 0.0778 and 17%,
respectively. The optimized symmetric temperature dependent
x1
(b)
Fig. 2. (a) Methane (1) + carbon dioxide (3) p, x diagram showing measured methane
liquid mole fractions and those calculated with the AspenTech HYSYS PR EOS. ,
Mraw et al. (1978) T = 183 K; , Mraw et al. (1978) T = 186 K; , Mraw et al. (1978)
T = 193 K; , Mraw et al. (1978) T = 203 K; , Mraw et al. (1978) T = 210 K; - - -, curves
calculated with the default BIP of 0.010; , curves calculated with the optimized
symmetric BIP of 0.0917 0.0009. (b) Deviations between the measured liquid mole
fractions and those calculated (indicated by subscript calc) with the AspenTech
HYSYS PR EOS using the optimized symmetric BIP of 0.0917 0.0009 for methane
(1) + carbon dioxide (3). The measured data are represented by the same symbols as
in part a. The curves, which are largely superimposed on each other, represent the
deviation between the liquid mole fractions calculated with the default AspenTech
, T = 186 K, ,
Hysys BIP and with the optimized (symmetric) BIP: , T = 183 K;
T = 193 K; - - -, T = 203 K; , T = 210 K.
T.J. Hughes et al. / International Journal of Greenhouse Gas Control 31 (2014) 121127
1400
1200
1000
800
600
400
200
0
Table 5
Comparison of model predictions with the measured data for the methane
(1) + methanol (2) + carbon dioxide (3) ternary mixture using the AspenTech Hysys
default BIPs and the optimized BIP values, in terms of the models standard error
(SE) and relative standard error (RSE) as dened in Eqs. (7) and (8).
Casea
Default Hysys
Optimized
0.0
0.04
x3 - x3,calc
x1
0.1
0.3
0.2
0.1
0.0
-0.1
0.02
0.00
0.2
x3
(a)
0.3
0.4
0.5
-0.02
-0.04
0.0
0.1
0.2
x3
(b)
0.3
0.4
0.5
Fig. 3. (a) Methanol (2) + carbon dioxide (3) p, x diagram showing measured carbon dioxide liquid mole fractions and those calculated with the AspenTech HYSYS
PR EOS. , Shenderei et al. (1959) T = 213 K; , Shenderei et al. (1959) T = 228 K; ,
Shenderei et al. (1959) T = 237 K; , Shenderei et al. (1959) T = 247 K; - - -, curves
calculated with the default BIP of 0.040; , curves calculated with the optimized
temperature dependent asymmetric BIP [Eqs (5) and (6) with A23 = 0.046 0.012,
A32 = 0.094 0.008, B23 = (3.0 0.5) 104 , B32 = (6.5 0.3) 104 . (b) Deviations
between the measured liquid mole fractions and those calculated (indicated by
subscript calc) with the AspenTech HYSYS PR EOS using the optimized temperature dependent symmetric BIP. The measured data are represented by the same
symbols as in part a. The curves represent the deviation between the liquid mole
fractions calculated with the default AspenTech Hysys BIP and with the optimized
temperature dependent symmetric BIP: , T = 213 K, - - -, T = 228 K; , T = 237 K;
, T = 247 K. The inset shows the full scale of the extent of the deviations between
the tuned and default models.
x2
x3
SE
RSE
SE
RSE
SE
RSE
0.0429
0.0186
0.496
0.194
0.0461
0.0186
0.054
0.022
0.0038
0.0008
0.111
0.025
a
The Default Hysys case used the AspenTech HYSYS PR EOS default BIPs. The
Optimized case includes binary optimized symmetric BIP values for methane
(1) + methanol (2) and methane (1) + carbon dioxide (3) and the binary optimized
asymmetric temperature dependent BIP values for methanol (2) + carbon dioxide
(3) (see Table 3 for the values of the BIPs).
The mole fraction deviations (xi xi,calc ) calculated for each component are plotted in Fig. 4. For the default case the xi,calc values
were predicted using the PR EOS with the default BIPs, and the
resulting deviations are plotted as red symbols. For the optimized
case, the x1,calc values were predicted using the PR EOS with the
optimized BIPs, and the deviations are plotted as black symbols. It
is clear that the optimization of the BIPs has improved the prediction of the liquid mole fractions of all the components. Of course, not
all the mole fractions shown in Fig. 4 are independent and clearly
a deviation trend in one component can result in a complementary
trend for another component. In Fig. 4, the results for x1 and x2
show this complementarity.
0.08
x1 - x1,calc
p/kPa
126
0.04
0.00
-0.04
-0.08
0.00
0.04
x1
0.08
0.12
for
the
methane
(1) + methanol
p/MPab
x1
u(x1 )
x2
u(x2 )
x3
u(x3 )
183.15
183.15
183.17
183.17
183.17
183.23
188.15
188.15
193.15
193.15
193.15
193.15
193.15
203.15
203.15
203.15
203.15
213.15
213.15
323.15
3.008
3.260
2.586
2.671
3.270
2.096
2.182
3.225
2.914
2.331
1.841
3.447
4.070
3.245
2.094
2.528
2.533
2.79
4.311
11.380
0.099
0.113
0.091
0.085
0.120
0.075
0.070
0.094
0.079
0.0614
0.0497
0.087
0.100
0.069
0.0461
0.0542
0.0543
0.0510
0.073
0.015
0.004
0.018
0.003
0.008
0.011
0.002
0.004
0.004
0.003
0.0002
0.0006
0.003
0.002
0.001
0.0004
0.0004
0.0004
0.0002
0.001
0.003
0.848
0.83
0.873
0.87
0.83
0.889
0.874
0.857
0.889
0.9072
0.9195
0.867
0.851
0.9027
0.9345
0.9235
0.9231
0.9087
0.893
0.984
0.004
0.02
0.005
0.01
0.01
0.002
0.006
0.005
0.004
0.0003
0.0009
0.004
0.002
0.0008
0.0005
0.0004
0.0006
0.0006
0.002
0.003
0.053
0.055
0.036
0.043
0.055
0.0355
0.057
0.049
0.0321
0.0314
0.0308
0.046
0.0489
0.0281
0.0194
0.0223
0.0226
0.0403
0.0339
0.0015
0.001
0.002
0.003
0.002
0.003
0.0003
0.002
0.001
0.0007
0.0001
0.0003
0.001
0.0004
0.0004
0.0002
0.0001
0.0003
0.0004
0.0006
0.0002
a
b
u(T) = 0.10 K.
u(p) = 0.005p.
0.04
0.00
-0.04
T/Ka
-0.08
0.80
0.85
0.90
x2
0.95
1.00
0.01
x3 - x3,calc
Table 4
Vaporliquid equilibrium measurements
(2) + carbon dioxide (3) system.
x2 - x2,calc
0.08
0.00
-0.01
0.00
0.02
x3
0.04
0.06
Fig. 4. Deviations (xi xi,calc ) for each component in the methane (1) + methanol
(2) + carbon dioxide (3) system (black symbols) plotted against the measured liquid
mole fraction of that component for the ternary mixture using the optimized BIPs
with the PR EOS (see Table 5). , T = 183 K; , T = 188 K; , T = 193 K; , T = 203 K;
T = 203 K. The red symbols are points where the default Hysys BIP with the PR EOS
has been used to calculated the xi ,calc value. (For interpretation of the references to
color in this gure legend, the reader is referred to the web version of this article).
T.J. Hughes et al. / International Journal of Greenhouse Gas Control 31 (2014) 121127
The RSEs of x1 , x2 and x3 for the default case were 49.6%, 5.4%
and 11.1%, respectively compared to optimized case with values of
19.4%, 2.2% and 2.5%. The optimized RSEs represent a 61%, 59% and
77% improvement in the calculation of x1 , x2 and x3 , respectively.
The SEs and RSEs of both case studies are summarized in Table 5.
These signicant improvements, particularly in the x3 , should allow
Rectisol plants to be simulated more accurately.
5. Conclusions
Predictions of the liquid phase mole fractions made for the
ternary mixture with the PR EOS using the default HYSYS BIPs were
found to be poor. A factor of about 2.5 improvement in the RSE
was achieved for x1 and x2 by instead using the symmetric BIPs
obtained from the optimization of the binary systems. The RSE in
x3 for the ternary was improved by a factor of about 4.4 by using
a temperature dependent asymmetric mixing rule with BIPs tuned
to binary VLE data. Tuning the binary systems to the simple temperature dependent asymmetric composition-dependent mixing
rule resulted in a signicant reduction in the RSE of the t for the
methanol (2) + carbon dioxide (3) from 17% to 1.5% (an improvement of 91%). However, no signicant improvement was observed
by applying the asymmetric mixing rule for the other two binaries.
This might be expected given that this mixing rule was initially
developed to improve EOS calculations of carbon dioxide + polar
component VLE. This result illustrates that a simple temperature
and asymmetric compositional dependent mixing rule can greatly
improve the predictions of a simple EOS for the carbon dioxide liquid mole fractions in a polar solvent and the use of the optimized
BIPs should improve the simulation of Rectisol plants.
Acknowledgment
The authors would like to thank Craig Grimm for constructing
and maintaining the apparatus.
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