Chemical Engineering Research and Design 1 3 8 ( 2 0 1 8 ) 116–124

Contents lists available at ScienceDirect

Chemical Engineering Research and Design

journal homepage: www.elsevier.com/locate/cherd

Describing physical properties of CO2 unloaded

and loaded MDEA + PZ solutions

Stefania Moioli ∗ , Laura A. Pellegrini

GASP — Group on Advanced Separation Processes and GAS Processing, Dipartimento di Chimica, Materiali e
Ingegneria Chimica “G. Natta”, Politecnico di Milano, Piazza Leonardo da Vinci 32, I-20133 Milano, Italy

a r t i c l e i n f o a b s t r a c t

Article history: Acid gas (CO2 and H2 S) removal from industrial gas streams by amine scrubbing is usually
Received 29 November 2017 employed in industry. Among different amines, n-MethylDiEthanolAmine (MDEA) is pre-
Received in revised form 31 July 2018 ferred because of its high equilibrium loading capacity and low heat of reaction with carbon
Accepted 10 August 2018 dioxide, associated to low energy requirement in the regeneration section. Piperazine (PZ)
Available online 22 August 2018 can be used as promoter because of its rapid transformation to carbamates with carbon
dioxide when mixed to MDEA (PZ rate constant value has been found to be one order of mag-
Keywords: nitude higher than the one of MEA). A correct representation of properties of the absorbent
MethylDiEthanolAmine solution, such as density and viscosity, is essential for rate-based calculations.
Piperazine This paper gives an in-depth analysis and calculation of the properties involved in the
Acid gas modeling of mass transfer of absorbed species and on the development of general correla-
Density tions for the description of density and viscosity of the MDEA + PZ solution to be applied for
Viscosity a wide range of concentrations and temperatures. In this work, in addition, the influence of
carbon dioxide loading on the solvent properties has been taken into account too.
© 2018 Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

1. Introduction
MethylDiEthanolAmine (MDEA) can be successfully used for capture
of carbon dioxide, which is emitted from various sources, as power
plants, industries, transportation, agriculture, residential buildings and
energy sector, in order to avoid further substantial greenhouse effects
(Sedransk Campbell et al., 2015) and their potentially adverse envi-
ronmental, social and economic impacts (Borhani et al., 2015; Huang
et al., 2015), for which many studies have been carried out (Duke et al.,
2010; Huang et al., 2010; Mansoori et al., 2011; Mumford et al., 2015;
Ravanchi et al., 2011). The technology is also employed to purify the
process streams, as natural gas, to the desired specification for possible
utilization of the final user, as for LNG (Pellegrini et al., 2014).
After the use of traditional amine-based solvent
(monoethanolamine (MEA), diethanolamine (DEA)) for a long time,
various potential drawbacks, as inadequate lifetime due to amine
oxidation degradation (Chi and Rochelle, 2002; Kennard and Meisen,
1985; Kim, 1988; Reza and Trejo, 2006), losses of amines, low capacity of
the solvent and high energy costs in the regeneration section (Shaikh
et al., 2013) have been identified. MDEA, for its properties, allows a
reduction of the problems above mentioned (Khoo and Tan, 2006)
and, in addition, is characterized by a greater operating capacity for
carbon dioxide. However, this amine has the disadvantage of low rate
of absorption of carbon dioxide and consequent need of high reaction
times. Piperazine (PZ) (Moioli and Pellegrini, 2015; Zheng et al., 2014)
has a different molecular structure (Ma et al., 2012) and leads to higher
rates of absorption in the absorbing column while maintaining a
low heat of regeneration in the stripper section. Indeed, PZ-activated
aqueous MDEA or AMP (2-amino-2-methyl-1-propanol) (Bishnoi and
Rochelle, 2002; Kachko et al., 2015) solvents have been studied and
using PZ-blended MDEA solutions (Moioli and Pellegrini, 2016) was
found to be a possible way to improve the absorption characteristics
of traditional amine solvents (Choi et al., 2014; Xu et al., 1998).
As stated in the literature,
“solution density and viscosity are important in the mass-transfer rate
modeling of absorbers and regenerators because these properties affect
the liquid-film coefficient for mass transfer” (Weiland et al., 1998)

∗
Corresponding author.
E-mail addresses: stefania.moioli@polimi.it (S. Moioli), laura.pellegrini@polimi.it (L.A. Pellegrini).
https://doi.org/10.1016/j.cherd.2018.08.018
0263-8762/© 2018 Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
 Chemical Engineering Research and Design 1 3 8 ( 2 0 1 8 ) 116–124
and
“the accurate determination of the physical properties of solvents over a
wide temperature range is essential for the rational design and optimiza-
tion of gas treating units” (Muhammad et al., 2009).
Moreover, it has been recognized that also design of related opera-
tions such as pumps and heat exchangers would benefit from better
knowledge of the physical properties of process solutions (Weiland
et al., 1998). Therefore, a correct description of properties of the
absorbent solution, such as density and viscosity (Samanta and
Bandyopadhyay, 2006), is essential for properly modeling the equip-
ment involved in the absorption and in the regeneration of the acid
gas removal unit. However, for the system MDEA + PZ, very few sources
considering physical properties of MDEA + PZ have been found in the
literature (Derks et al., 2008; Frailie, 2014; Khan et al., 2017; Muhammad
et al., 2009; Paul and Mandal, 2006), with correlations developed only for
being suitable to specific sets of experimental data, so that deviations
occur when different ranges are considered.
In this work an in-depth analysis of the properties involved in the
calculation of mass transfer of absorbed species, i.e. CO2 , has been per-
formed, taking into account all the data available in the literature. New
correlations for the prediction of density and viscosity of the MDEA + PZ
solution, also in the presence of carbon dioxide, and for a wide range
of operating conditions (not in the previous literature), are proposed.
The obtained expressions can be implemented also in a commercial
®
software (as ASPEN Plus ) and used for simulations.
2. Experimental data
In literature few sources of experimental data for density and
viscosity of mixtures containing water and both MDEA and
PZ are available. Most of them refer to unloaded solutions,
with only one considering complete results with CO2 loaded
solutions (Frailie, 2014).
Table 1 reports all the sources of experimental data avail-
able in the literature to the author’s knowledge, for mixtures of
MDEA and PZ. Only five of them, published from 2006 to this
year (2017), deal with MDEA/PZ solvents (Derks et al., 2008;
Frailie, 2014; Khan et al., 2017; Muhammad et al., 2009; Paul
and Mandal, 2006).
2.1. Available experimental values for density
Paul and Mandal (2006) published values of densities of aque-
ous blends of PZ and MDEA at different temperatures (from
288 K to 333 K), by keeping the total amine fraction in all solu-
tions at 30% wt.
Derks et al. (2008) considered values of density and vis-
cosity at several temperatures (from 293.15 K to 323.15 K) and
concentrations (by keeping the concentration of MDEA con-
stant at 1, 2, 3 or 4 mol/dm3 and varying the concentration of
PZ from 0 to 1 mol/dm3 ).
Muhammad et al. (2009) reported measurements of density
and viscosity for the aqueous blends of MDEA and PZ with
% mass fractions ratios (MDEA/PZ) ranging from 32.28/1.74 to
48.80/10.35 and with temperatures varying from 298.15 K to
338.15 K.
Freeman (2011) focused on the physical properties of
piperazine in mixture with substituted PZs (1-MPS, 1-
methylpiperazine; 1,4-DMPZ, 1,4 dimethylpiperazine; 2-MPZ,
2-methylpiperazine) and Chen (2011) extended the data to
take into account additional concentrations.
Frailie (2014) performed a complete experimental work on
the mixture MDEA/PZ, measuring the density not only for
different temperatures, wMDEA and wPZ, but also in the pres-
117
ence of carbon dioxide. This is the only experimental work
presenting this type of data.
In 2017 new data (Khan et al., 2017) have been published
for mixtures of MDEA and PZ, with or without the addition of
ionic liquids.
All the data referring to MDEA and PZ solutions have been
critically analyzed, compared, and reported and discussed in
this study.
2.2. Available experimental values for viscosity
Experimental data of viscosity of MDEA + PZ solution at dif-
ferent compositions and temperatures are reported by Paul
and Mandal (2006), by Derks et al. (2008), by Muhammad et al.
(2009), by Frailie (2014) and by Khan et al. (2017) and in the
same concentration and temperature conditions of density
measurements. As for density, Chen (2011), Freeman (2011)
and Patzschke et al. (2017) focused on other types of amine
mixtures.
Paul and Mandal (2006) measured the viscosity with a vis-
cometer immersed in a thermostated bath (the uncertainty in
the measurement of temperature was 0.1 K). Similarly to their
density measurements, each reported value was the average
of three measurements.
Derks et al. (2008) took experimental values using a vis-
cometer with a suitable viscosity range, submerged in a
thermostat bath for temperature control within 0.1 K, with an
estimated experimental uncertainty of 1%.
Experimental points were taken also by Muhammad et al.
(2009) with a viscometer immersed in a thermostatic bath,
whose temperature was regulated with an accuracy of 0.02 K.
Frailie (2014) is the only researcher focusing on determining
values of viscosity for carbon dioxide loaded solutions, at two
different MDEA and PZ concentrations.
Later, Khan et al. (2017) published new data of viscosity for
MDEA and for PZ solvent, in the framework of a study on the
influence of ionic liquids on solvent properties.
3. Representation of density and viscosity
of MDEA/PZ solutions
3.1. Published correlations
Few correlations are available for the description of the den-
sity and viscosity of the considered aqueous amine system.
Most of them are focused on the dependence of density and
viscosity on the temperature and on the composition of the
free solvent. The work by Frailie (2014) is interesting, because
this author is the only one proposing an expression for con-
sidering also the influence of the mole fraction of CO2 in the
solvent.
3.1.1. Available correlations for density
Paul and Mandal (2006) correlated the molar volume of liquid
mixtures with parameters assumed to be temperature depen-
dent.
Muhammad et al. (2009) presented a correlation for the
experimental data considered in their work, stating that the
density points Z can be expressed according to Z = A0 + AT1
being A0 and A1 the fitting parameters obtained by the authors.
The expression is based on parameters constant with the mass
fraction of amines, that would be changed by the user if the
wMDEA /wPZ varies. The model well agrees with experimental
118 Chemical Engineering Research and Design 1 3 8 ( 2 0 1 8 ) 116–124

Table 1 – Experimental data available in the literature for the MDEA/PZ mixture.
Source Year Mixture Composition Temperature [◦ C] CO2 loading

Khan et al. (2017) 2017 MDEA/PZ/ionic 30% MDEA/3% PZ/(5–20%) 25–70 0

liquids ionic liquids

Patzschke et al. 2017 PZ/DMAE; (10–40%) DMAE/(0–10%)PZ; 25–80 0–0.75

(2017) PZ/DEAE (10–40%) DEAE/(0–10%)PZ

Frailie (2014) 2014 MDEA/PZ 7 m MDEA/2 m PZ; 5 m 20–60 0–0.4

MDEA/5 m PZ

Chen (2011) 2011 2MPZ; 8 m 2MPZ; 4 m 2MPZ/4 m PZ 20–60 0–0.4

2MPZ/PZ

Freeman (2011) 2011 PZ; 2–20 m PZ; 5 m PZ/2 m 20–60; 10–80 0–0.5
PZ/1MPZ/1,4DMPZ; 1MPZ/1 m 1,4DMPZ; 4 m
PZ/2MPZ PZ/4 m 2MPZ

Muhammad 2009 MDEA/PZ 32.28% MDEA/1.74% PZ; 25–65 0

et al. (2009) 48.80% MDEA/10.35% PZ

Derks et al. (2008) 2008 MDEA/PZ (1–4)M MDEA/0–1 M PZ 25–50 0

Paul and Mandal 2006 MDEA/PZ 27% MDEA/3% PZ; 24% 15–60 0
(2006) MDEA/6% PZ; 21% MDEA/9%
PZ; 18%MDEA/12% PZ

Fig. 1 – Parity plot for comparison of values of density Fig. 2 – Parity plot for comparison of values of density
®
obtained using the correlation proposed by Paul and obtained using the ASPEN Plus default correlation and all
Mandal (2006) and all the available experimental data. the available experimental data.

data of density, but it is able to represent only the experimental
data considered by these authors.
The correlation by Frailie (2014) shows a dependence on the
carbon dioxide loading, temperature and amount of MDEA and
PZ in the considered solvent.
Generally, all the authors developed correlations suitable
for the data they experimentally collected, which can be con-
sidered applicable only in the range of temperature and for
the specific composition of MDEA and PZ considered. There-
fore, the predicted values according to these expressions may
be not very close to experimental data referring to different
conditions.
Fig. 1 is representative of this situation. The process sim-
®
ulator ASPEN Plus uses a quadratic mixing rule for the
expression of the liquid molar volume of a mixture, with an
interaction parameter Kij for the mixing rule. According to
what reported in a template by AspenTechTM on MDEA + PZ
scrubbing, only values for the interaction coefficient between
MDEA and water and between PZ and water are available,
and regressed only on experimental data of binary mixtures
(MDEA + H2 O and PZ + H2 O), without considering the ternary
mixture MDEA + PZ + H2 O. Though presenting results within a
5% error if compared with experimental data, these values are
not able to well reproduce all the experimental values avail-
able (Fig. 2).
3.1.2. Available correlations for viscosity
To correlate their experimental data of viscosity, Paul and
Mandal (2006) proposed a temperature dependent expres-
sion provided with parameters obtained by regression of their
experimental data. As shown in Fig. 3, results obtained with
their model are in very good agreement with data for which
the model has been created (Paul and Mandal, 2006) but show
high deviations in reproducing experimental values of all the
other sources.
Muhammad et al. (2009) expressed a temperature depen-
dence for viscosity similarly to the one for density, though
considering logarithmic terms and with fitted parameters,
 Chemical Engineering Research and Design 1 3 8 ( 2 0 1 8 ) 116–124 119

Table 2 – Values of binary interaction parameters

obtained in this work for density calculation.
i/j PZ MDEA H2 O

PZ 0 0.260844 0.00267
MDEA −0.32459 0 −2.68337
H2 O −0.96157 2.513075 0

Table 3 – Values of parameters obtained in this work for

density of CO2 loaded solutions.
Parameter a1 a2 b1 b2

Value 0.0178 0.1217 −4.1756 214.29

species must be considered for a proper representation of the

property of the mixture.

3.2. Proposed method

3.2.1. Density
Fig. 3 – Parity plot for comparison of values of viscosity The proposed correlation in this work is based on the calcula-
obtained using the correlation proposed by Paul and tion of molar volumes according to:
Mandal (2006) and all the available experimental data.
    0.5
Vm = xi Vi + xi xj Kij Vi · Vj (1)
i i j

for unloaded solutions and of an additional term for consid-

ering the density of CO2 loaded solutions, explained in the
following.
Molar volumes of single compounds are calculated accord-
®
ing to the process simulator ASPEN Plus (tests on default
expression and experimental data show that no further
improvement is required). The interaction parameters Kij of
MDEA in mixture with PZ have been considered because the
mixture is composed of both the amines. The matrix of param-
eters obtained from a regression of all the experimental points
is reported in Table 2.
The same expression, with the same parameters, can be
used to describe mixtures where carbon dioxide is present. In
this case, an additional term is considered to take into account
the influence of this acid gas, so the density is expressed as
proposed below:
Fig. 4 – Parity plot for comparison of values of viscosity
®
 wMDEA

obtained using the ASPEN Plus default correlation and all  CO2 solution =  unloadedsolution + ˛CO2 a1 + a2 T +
wPZ
the available experimental data.  
wMDEA
b1 + b2 (2)
wPZ
which well reproduce experimental data by the authors. The
use of their model is limited by the fact that parameters are with T being the temperature in [K] and the density being
specific for each concentration considered by the authors, expressed in [kg/m3 ].
without a general expression. The values of a1, a2, b1 and b2 can be found in Table 3.
As for density, Frailie (2014) is the only source proposing
an expression which includes also the dependence on the
3.2.2. Viscosity
amount of carbon dioxide present in the solvent. Figures pro-
The procedure employed for the validation of available corre-
vided in the reference show that it well represents the data
lations for the calculation of density has been followed also
experimentally collected by the author.
® for the study of viscosity.
ASPEN Plus uses a generalized correlation with binary
The correlation:
interaction parameters kij and lij considering only MDEA and
water. No parameters for the influence of the piperazine addi-

NC

NC−i
 
tion are taken into account. Moreover, no parameters for the ln (m ) = wi ln (i ) + kij wi wj ln ij
influence of temperature are considered. As shown in Fig. 4, i=1 j>i
the obtained trend is not in very good agreement with experi-
®
⎡ ⎤3
mental values. The default parameters by ASPEN Plus make NC
NC
  13
the software underestimate the experimental values up to + wi ⎣ wj lij ln ij ⎦ (3)
about 50%. It follows that the influence exerted by the PZ i=1 j=
/ i
120 Chemical Engineering Research and Design 1 3 8 ( 2 0 1 8 ) 116–124

with:
Table 4 – Values of binary interaction parameters for the
calculation of viscosity of unloaded solutions obtained
Bij in this work.
kij = Aij + (4)
Tr Parameter i/j PZ MDEA H2 O

Aij PZ 0 −73.0494 −847.22

bij MDEA −73.0494 0 −1.0906
lij = aij + (5)
Tr H2 O −847.222 −1.0906 0

Bij PZ 0 86.7454 1242.76

T
with Tr = 298.15K has been considered and proper parame- MDEA 86.7454 0 1.2472
ters obtained from regression of all the available experimental H2 O 1242.77 1.2472 0

data have been determined. aij PZ 0 98.1595 −3.9189

Viscosities of pure compounds are obtained according to MDEA −98.1595 0 −1.5803
® H2 O 3.9189 1.5803 0
the expression and parameters by ASPEN Plus default (a pre-
vious check by comparison with experimental data had been bij PZ 0 −115.12 −289.79
performed), but on the basis of data with both MDEA and PZ MDEA 115.12 0 0.5036
as solvents. H2 O 289.79 −0.5036 0
The influence of temperature has been considered for the
determination of values of binary interaction parameters.
Regressions have been performed both considering the tem- The influence of carbon dioxide has been determined
perature dependent terms (Bij and bij ) and both setting them according to the newly developed expression:
equal to 0. A deep analysis, not reported here for limiting  wMDEA

space, has shown that by considering the influence of tem- ln(CO2 solution ) = ln(unloadedsolution ) + ˛CO2 a1 + a2 T
perature the lowest deviation from the experimental values wPZ
 wMDEA

can be obtained. Therefore, all four types of binary interac-
+ b1 + b2 (6)
tion parameters must be considered for properly calculating wPZ
viscosity and are reported in Table 4.
A similar approach was used also for density, but no further with T being the temperature in [K] and the viscosity being
improvement had been obtained, so non-temperature depen- expressed in [mPa s].
dent binary interactions have been considered for density. The values of a1, a2, b1 and b2 can be found in Table 5.

Fig. 5 – Results obtained with the proposed method and experimental data from a) Paul and Mandal (2006), b) Derks et al.
(2008), c) Muhammad et al. (2009) and d) Frailie (2014) of density of MDEA + PZ solution vs. temperature at different amine
concentrations.
 Chemical Engineering Research and Design 1 3 8 ( 2 0 1 8 ) 116–124
Fig. 6 – Parity plot for comparison of values of density obtained using the proposed method and all the available
experimental data a) for unloaded solutions and b) for CO2 loaded solutions.
Table 5 – Values of binary interaction parameters for the
calculation of viscosity of CO2 loaded solutions obtained
in this work.
Parameter a1 a2 b1 b2
Value 0.0005 0.0108 0.1123 −3.1195
Fig. 7 – Results obtained with the proposed method and
experimental data from Frailie (2014) of density of
MDEA + PZ solution of CO2 loaded solutions vs. loading.
4. Results and discussion
Table 2 reports the matrix of values of binary interaction
parameters obtained for the description of the density of
MDEA + PZ aqueous solutions, with results of calculations
reported in Figs. 5 and 6. All the points result within the 0.5%
error range, and are very close to the y = x line, considering that
the axis scale of Fig. 6 is the same of that in Fig. 2.
Fig. 7 shows the result obtained considering the influence
of the loading of carbon dioxide, with calculated values match-
ing the experimental points. This is also confirmed by Fig. 6b),
reporting the parity plot. The resulting AAD% is lower than
0.65%.
It can be outsourced that the proposed values are able to
well represent the experimental data of density for a wide
121
range of concentrations and temperatures, also in the pres-
ence of CO2 .
The parameters obtained for the description of viscosity
are reported in Table 4 for unloaded solutions and in Table 5
for CO2 loaded solvents. They allow a good description of the
considered physical property of the MDEA + PZ solvent, with
a % Absolute Average Deviation (AAD%) lower than 5%, much
lower than the ones obtained with the already available meth-
ods. This can be inferred also from Figs. 8 and 9, showing
results of calculations with the regressed parameters.
Fig. 10 shows the result obtained considering the influence
of the loading of carbon dioxide. The calculated values are
in good agreement with the experimental data, and show an
AAD% equal to 4.7%.
Table 6 reports the % Absolute Average Deviations obtained
with the available methods and the proposed parameters.
The comparison of values confirms that a relevant improve-
ment in the calculation of both density and viscosity has been
obtained.
The model by Muhammad et al. (2009) well agrees with
experimental data of density, covering all the range of tem-
peratures for which experimental values of these authors are
available. This model, however, is based on parameters con-
stant with the mass fraction of amines, that should be changed
by the user if the wMDEA /wPZ varies, so it cannot be applied to
the calculation of different experimental points.
The expression for viscosity by Frailie (2014) could not be
tested because information referring to one variable could not
be found in the source.
5. Conclusion
This work focuses on the development of correlations for
calculation of density and viscosity of PZ + MDEA aqueous
solutions, also when CO2 is present. For this system, published
correlations are rather limited. A model for the calculation of
these properties in liquid mixture is present in the commercial
®
software ASPEN Plus , however the employed expressions are
not provided with binary interaction parameters for the mix-
ture, and this affects the accuracy in describing the behavior
of the amine system.
In the present work improved correlations have been
proposed. The considered parameters are able to take into
account the influence exerted by both the amines and their
amount in the aqueous phase, the influence of tempera-
122 Chemical Engineering Research and Design 1 3 8 ( 2 0 1 8 ) 116–124

Fig. 8 – Results obtained with the proposed method and experimental data from a) Paul and Mandal (2006), b) Derks et al.
(2008), c) Muhammad et al. (2009) and d) Frailie (2014) of viscosity of MDEA + PZ solution vs. temperature at different amine
concentrations.

Fig. 9 – Parity plot for comparison of values of viscosity obtained using the proposed method and all the available
experimental data.

Table 6 – % Absolute Average Deviations (AAD%) obtained for density and viscosity calculations performed with the
®
correlations from the literature and from ASPEN Plus default and with the proposed method.
®
Property Paul and Mandal (2006) Frailie (2014) ASPEN Plus default This work

Density 17.61 11.04 1.52 0.32

Viscosity 43.35 NA 25.29 5.04
 Chemical Engineering Research and Design 1 3 8 ( 2 0 1 8 ) 116–124
Fig. 10 – Results obtained with the proposed method and
experimental data from Frailie (2014) of viscosity of
MDEA + PZ solution of CO2 loaded solutions vs. loading.
ture and also the influence of carbon dioxide in the solvent.
Results show that with the proposed expression all the avail-
able experimental data can be properly represented, with low
AAD%.
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