HALDIA INSTITUTE OF TECHNOLOGY

DEPARTMENT OF CHEMICAL ENGINEERING

Project Report

A study on
Kinetics of CO2 absorption in aqueous amine solution

Submitted by

Kunal Roy 14/CH/21 10300614021

Neha Mandhare 14/CH/26 10300614026

Paromita Maity 14/CH/69 10300614069

During the year 2017-2018

----------------------------- ------------------------------------
Project Guide Head of Department
ABSTRACT

The emission of the Green House Gases is a big concern as the accumulation of gases leads
to the temperature increment of more than 20 C will lead us to severe consequences. The
consequences of too high global warming will be melting of glaciers, leading to reduced water and
food resources. The sea level will rise, and there will be more extreme weather, more draughts,
and more floods. CO2 is the most important greenhouse gas, and most efficient way should be
adopted to minimize the emission og CO2.

Aqueous amine solvents have been extensively studied for the purpose of CO2 absorption
to reduce emissions from sources such as industrial power stations. In order to reduce CO2
emissions from a power plant, CO2 can be captured either from the syngas that is to be burned or
from the flue gases exiting the energy conversion process. However, to improve the economic
viability of carbon capture technologies, solvents with higher CO2 absorption capacity and faster
kinetics are required. The choice of the promising molecules depends on many physical and
chemical characteristics (like absorption capacity, kinetics reaction between amine, reaction
enthalpy and solvent stability and toxicity). This work focuses on the absorption capacity of CO2
and the reaction rates of single amines.

In this study, amines such as MEA (Monoethanolamine) and PZ (Piperazine) are used for
determining the absorption kinetics behaviours at different concentrations using a wetted wall
column. The absorption of CO2 gas in amine in an absorber is studied were a gas and liquid
absortion is taking place. The two amines are compared and study with respect to their capability
to capture CO2 from a flue gas stream. The reaction is done by mass transfer followed by chemical
reaction and the experiment data is obtained by assuming and fitting data for determining the order
of the reaction. The results allowed us to develop a kinetics model for CO2 reaction with MEA
solutions which shows the absorption of CO2 for a wide temperature range.
 CERTIFICATE

This is to certify that the project report entitled Kinetics of CO2 absorption in aqueous
amine solution submitted by Neha Mandhare, Kunal Roy and Paromita Maity is absolutely based
upon their work under the guidance of Dr. Asit K. Saha and that neither this report nor any part of
it has been submitted for any degree/diploma or any other academic award anywhere before.

----------------------------------- ------------------------------------
Prof. (Dr.) T.K. Mana Dr. Asit K. Saha
Head of Department Principal
Dept. of Chemical Engineering Dept. of Chemical Engineering
Haldia Institute of Technology Haldia Institute of Technology
 ACKNOWLEDGMENT

Apart from the efforts of myself, the success of any project depends largely on the
encouragement and guidelines of many others. I take this opportunity to express my gratitude to
the people who have been instrumental in the successful completion of this report.

I would like to show my greatest appreciation to my respected teacher Dr. Asit K. Saha of
Chemical Engineering Department, Haldia Institute of Technology for giving me a very interesting
project in Kinetics of CO2 absorption in aqueous amine solution and also for his tremendous
support and help. Without his encouragement and guidance, this report would not have been
materized.

I would also like to express my heartfelt gratitude to our respected H.O.D Mr. Tapas Kumar
Mandal for giving me this opportunity to present this report in front of you.

The constant guidance anf support received from all my family members throughout the
completion of this report is also worth mentioning. And last but not the least I would also like to
thank my group members without whose opinions and ideas the completion of this report would
not have been possible.

Neha Mandhare:

Kunal Roy:

Parimoita Maity:
1.0. INTRODUCTION -
According to the Intergovernmental Panel on Climate Change (IPCC), emission of
greenhouse gas (GHG) must be reduced by 50% to 80% by 2050 to circumvent intense
consequences of global warming. Green-house gas emissions (GHG) will rise the average global
temperature by 1.1 to 6.40 C by the end of the 21st century, as stated by the IPCC. A global
warming with average temperature increment of more than 2o C will lead us to severe
consequences, and IPCC has therefore specified that GHG emissions should be reduced by 50 to
80% by 2050 [1]. The consequences of too high global warming will be melting of glaciers, leading
to reduced water and food resources. The sea level will rise, and there will be more extreme
weather, more draughts, and more floods. CO2 is the most important greenhouse gas, and
anthropogenic CO2 emissions are mainly a consequence of fossil fuels being the most important
global energy sources [1].

Carbon dioxide (CO2) capture is a process consisting of the separation of CO2 from
industrial and energy-related sources for long-term isolation from the atmosphere and to restore in
a preferred location [2]. CO2 capture and appropriation from fossil fuel power plants is gaining
widespread concern as a prospective method to control greenhouse gas emissions [3]. The
widespread application of CO2 Capture and its Storage system would depend on technical
maturity, costs, overall potential, diffusion and transfer of the technology to developing countries
and their capacity to apply the technology, regulatory aspects and environmental issues. However,
CO2 capture technology has the potential to reduce overall mitigation costs and increase exibility
in achieving greenhouse gas emission reductions [2].

The still rising demand for energy and the increase in CO2 emissions typically involved
has become one of the most important environmental topics [4]. Carbon dioxide (CO2) is the most
principal greenhouse gases emitted in comparison with the other greenhouse gases. In the future,
the concentration in the atmosphere will increase and CO2 will continue to pose significant danger
to the climatic system [5].

Many solutions are realized or investigated to trap carbon dioxide. There are different types of
CO2 capture systems (Figure 1). The concentration of CO2 in the gas stream, the pressure of the
gas stream and the fuel type (solid or gas) are important factors in selecting the capture system [2].
a. Post-Combustion: Post-combustion capture of CO2 in power plants is economically
feasible under specific conditions. It is used to capture CO2 from part of the ue gases
from a number of existing power plants.
b. Pre-Combustion: The technology required for pre-combustion capture is widely applied in
fertilizer manufacturing and in hydrogen production. Although the initial fuel conversion
steps of pre-combustion are more elaborate and costly, the higher concentrations of CO2
in the gas stream and the higher pressure make the separation easier.
c. Oxy-fuel Combustion: Oxy-fuel combustion is in the demonstration phase and uses high
purity oxygen. This results in higher concentrations of CO2 in the gas stream and,
henceforth, it will be easier in separation of CO2 and in increased energy requirements in
the separation of oxygen from air.
 Post-combustion CO2 capture technology is the most mature solution [5]. In order to reduce
the environmental impact of power generation from fossil fuels, CO2 can be captured either from
the syngas stream that is to be burned or from the flue gases exiting the energy conversion process.
Post-combustion capture has the advantage that it can be applied for retrofitting existing power
plants [4]. The removal of acid gas contaminations, like CO2 and H2S, from natural, synthesis gas
streams and refinery is a substantial operation in gas processing industry. Most frequently such
sweetening of sour gas streams is done by the regenerative chemical absorption of the acid gas
components into solution of alkanolamines [6]. The most mature technology of CO2 absorption in
gas purification processes uses amines such as Mono-ethanolamine (MEA) as absorbent [7].
Actually, absorption with amine-based solvents has been extensively studied and regarded as the
most effective technology for CO2 capture. Amine-CO2 reaction can be reversed by increasing
the temperature. CO2 capture is based on using various alkanolamines solutions like mono-
ethanolamine (MEA), N-methyl-di-ethanolamine (MDEA), Di-ethanolamine (DEA) or 2-amino-
2-methyl-1-propanol (AMP). As primary amine, MEA, and secondary amine, DEA, have a high
kinetics reaction with CO2 and high regeneration energy. Now MDEA which is a tertiary amine,
has a high CO2 loading capacity, a low regeneration cost and low reaction kinetics with CO2.
There is another kind of amine which is called sterically hindered amine, like AMP, which has the
same characteristics than tertiary amine (high CO2 loading capacity). The benchmark amine,
30wt% MEA solution, has a good characteristics reaction with CO2. Indeed, this amine reacts
rapidly with CO2 and has a high CO2 absorption capacity. However, its commercial deployment
is still limited by a number of techno-economic factors as discussed elsewhere [4 & 8-11].

Here our main objective is to determine the kinetics of the CO2 absorption process in
institutional laboratory using aqueous amine solution and to observe the rate of reactions and its
reaction kinetics considering absorption capacity of the reactor through the most possible, feasible
and economical way.

Fig 1. Schematic Representation of various CO2 Capture Processes [2]

2.0. OBJECTIVE
Carbon dioxide (CO2) is an important trace gas in Earths atmosphere and plays a vital role
in regulating earths surface temperature through the greenhouse effect. Carbon capture and
Storage (CCS) is a promising technique gaining increasing interest among researches and
policymakers. In specific, CCS is a process where CO2 is separated from industrial production or
energy conversion, is transported to the storage site under high pressure, aiming to realize zero
emissions of CO2. CCS refers to the capture of CO2 emissions either before the combustion of the
fuel or directly from the flue gas.

Post combustion methods are more applicable as they have no retrofitting requirements for
the existing equipment. The most applied and efficient post combustion method is chemical
absorption. In comparison with other post-combustion CO2 absorption processes, chemical
absorbents ensure higher absorption efficiency, selectivity and lower energy. [12]

Chemical absorption of CO2 by aqueous solvents, mainly amines, has been studied for
decades by numerous researchers with satisfying results. The developed models include both
kinetic and thermodynamic aspects and are aiming to optimize the absorption. It is only recently
though, that these attempts include dynamic characteristics and more realistic representations of
the process. The current work objective is to

Outline briefly the common modeling approaches in the field of post-combustion CO2 absorption
New ways of absorption of CO2 in amine solution.
Determining the order and kinetics of the absorption of CO2 in amine solutions.
Finally, the aims to conclude on the prediction efficiency of several models, comparing, to the point
it is possible, results of different researchers which are based on the same experimental data. [12]

3.0. LITERATURE -
Chemical absorption (or reactive absorption) is the
process where a gas is absorbed by a liquid phase with
combination of reaction and absorptive mass transport. Amine
based systems, carbonate based systems, aqueous ammonia
and ionic liquids based systems are typical systems for
chemical absorption. In specific for CO2 capture, chemical absorption involves the reaction of
CO2 with a chemical solvent forming a weakly bonded intermediate compound, a process that can
be reversed applying heat and resulting to the original solvent and a CO2 stream [3]. The
regeneration process is the most demanding by means of energy, as it may cost upto 14% of the
power plant efficiency [4]. During chemical absorption the flue gas enters usually an absorption
tower where it contacts counter current the solvent under low temperature (40 60 1C). The rich
in CO2 solvent is compressed, heated in an exchanger and inserted in the desorption column
(stripper) where it is regenerated under low pressure (close to ambient) and high temperatures
(100140 1C). There generated (lean) solvent exits the column and re- enters the absorber after
dissipating its heat in the rich solvent through the above-mentioned exchanger. The chemical
absorption process was initially performed using amine aqueous solvents. The most mature and
commercially applied amine is Monoethanolamine (MEA) due to its high absorptive capacity.
 MEA is considered an attractive solvent at low partial pressures of CO2 in the flue gas due to its
fast reaction rates compared to that of secondary and tertiary amines [5]. Other common amines
are Diethanolamine (DEA), Methyldiethanola- mine (MDEA), Diglycolamine (DGA), and
Diisopropanolamine (DIPA) and Piperazine (PZ) or mixtures of amines that are characterized by
satisfactory reaction rates and lower regeneration energy than MEA. Piperazine is usually added
as a promoter as it has been found to have faster reaction rates than MEA. Due to its high volatility
though, its application in CO2 absorption is more expensive and is still under development. A
special category of amines are sterically hindered amines (SHA) that e.g. 2-Amino-2- methyl-1-
propanol (AMP). SHA form more unstable carbamates in comparison with other amines. Thus,
they are more efficient during regeneration, as the unstable carbamates are easier to be reversed,
leading therefore to quicker desorption and less energy requirements. Alternative solvents for
chemical absorption are aqueous ammonia, ionic liquids and potassium carbonate. In specific,
aqueous ammonia is a strongly promising solvent characterized by many assets, as high absorption
efficiency, high absorption capacity, low energy requirement for absorbent regeneration and wide
distribution of resources [12].

3.1. PROPERTIES OF MONOETHANOLAMINE

Table 3.1: MSDS for Monoethanolamine

SECTION I PRODUCT IDENTIFICATION

Synonym: MEA, Ethanolamine

Chemical family: Alkanolamine

SECTION II HAZARDOUS INGREDIENTS

CHEMICAL NAME GAS %WT TLV PEL

Number
Monoethanol amine 141-43-5 100 3 ppm 6 ppm

SECTION III HAZARDOUS IDENTIFICATION

Potential Acute Health Effects: Corrosive, Causes eye and skin burns
Potential Chronic Health Effects: Swallowing of this material may result in severe ulceration,
inflammation, and possible perforation of the upper alimentary tract.

SECTION IV PHISICAL & CHEMICAL PROPERTIES

Boiling Point Range: 3390F Vapor Density: 2.1

pH: 11.5 Vapour Pressure (mmHg): 0.2
Solubility in water: Soluble VOC %: 98
Appearance/odour: Clear liquid with ammonia like odour Specific Gravity (H2O=1): 1.02
Melting Point/Freezing point: 51 0F
 SECTION V FIR FIGHTING MEASURES

Flash Point: 20.4 0F

Auto Ignition: Not Determined
Extinguishing Media: Use water spray, dry chemical, foam or CO2 to extinguish flames.
Flammable Limits: Lower- 5.0, Upper 17
Fore Fighting Procedure: Cool fine-exposed containers with water spray to prevent
container weakening and possible rupture. Do not enter Fine Zone without self-contained
breathing apparatus (SCBA) with full-face shield operated in positive pressure demand
mode and structural fire fighters protecting clothing.
Unusual Fire and Explosion Hazards: Not considered a fire or an explosion hazard

SECTION VI STABILITY AND REACTIVITY

Stability: Stable under Normal storage conditions.

Conditions to avoid: Materials react violently with acid
Incompatibility: No documented data
Hazardous Decomposition Products: Oxides of cabon and nitrogen plus imitating levels of
aldehydes and ketone.
Hazardous Polymerization: Will not odour

4.0. THEORY -

NOMENCLATURE

Awwc Area (m2)

C Concentration (mol/m3)
d Diameter (m)
D Diffusivity (m2/s)
ds Hydraulic diameter (m)
E Enhancement factor
g Gravitational acceleration (m/s2)
H Henrys constant (Pam3/mol)
h Hight of column (m)
Ha Hatta number
KG Overall mass transfer coefficient (mol/m2/sec/Pa)
k2 Second order rate constant (Pa/m3/mol)
kg Liquid side mass transfer coefficient (mol/m2/sec/Pa)
kg Gas side mass transfer coefficient (mol/m2/sec/Pa)
kl Liquid side mass transfer coefficient (m/s)
kl0 Physical liquid mass transfer coefficient (m/s)
kOH Rate constant for bicarbonate formation (Pa/m3/mol)
LMPD Logarithmic mean pressure difference (Pa)
m Molal (mole/kg solvent)
N Flux (mol/m2/sec)
P Pressure (Pa)
Q Flow rate (m3/sec)
Re Reynolds number
Sc Schmidt number
Sh Sherwood number
T Temperature (K) or (C)
usurf Surface rate (m/s)
v Mean gas velocity (m/s)
W Perimeter (m)
Fitting parameter
Fitting parameter
Film thickness (m)
Dimensionless parameter
Dimensionless parameter
Viscosity (Pas)
am Ratio amine to CO2 from mechanism
Density (kg/m3)

REACTION MECHANISM

The system of AMP in NMP have shown promising potential for lower temperature
regeneration compared to conventional amine solutions. Desorption of CO2 can be achieved at
temperatures ranging from 70-90 C, which opens up the possibility of using low-grade heat for
the regeneration step, thus making the absorption process more cost effective [6]. The reaction
mechanism for amine based absorption in non-aqueous solutions can be described by the reactions
below. First the carbon dioxide is dissolved in the liquid medium (1) where a reaction following
the zwitterion mechanism takes place (2) and a carbamate is formed (3). In the AMP in NMP
system precipitation of a crystalline solid occurs as the loading of the solution is increased,
according to reaction (4) [13].

2 () 2 () (1)
2 () + 2 () 2+ () (2)
2+ () + 2 () 3+ () + () (3)
3+ ( ) + ( ) 3+ () (4)

FILM THEORY

The overall absorption of carbon dioxide can be divided into two steps, physical and
chemical absorption. The physical absorption is described by the diffusion of CO2 from the
gaseous phase through an interface in to the liquid phase. The chemical absorption is then
described by the reaction CO2 undergoes while in the liquid phase [3,9]. The physical mass
transfer, can be described by the two-film theory [10] where the mass transfer of CO2 is explained
by different diffusion steps. These steps include the transport of CO2 from the bulk gas phase to
the interface and then the transport of CO2 from the interface to the bulk of the solvent. Figure 1
shows the mass transfer of CO2 from the gas to the bulk liquid, including fast reaction. The
transport through the gas phase is described by Ficks first law and the driving force is the gradient
of the chemical potential, which can be translated to the concentration gradient and thus be
estimated by the partial pressure of carbon dioxide. For the liquid side the driving force can be
estimated by the concentration difference in the film. If a reaction takes place in the liquid the two-
film theory is not valid. To account for the reaction an enhancement factor can be introduced.
Since the reaction occurs on the liquid side of the system, the enhancement factor is introduced in
the description of the flux through the liquid film. The expressions for the flux through the gas and
liquid film are given in equations (6) and (7). [13]

2, = (2, 2, ) (6)

2, = . (2, 2, ) = . (2, 2, ) (7)

Here 2, and 2, are the fluxes while and are the mass transfer coefficients for
the gas and liquid film, respectively. 2, and 2, are the partial pressures of CO2 in the
gas bulk and at the gas side of the interface. 2, and 2, are the concentrations of CO2 at
the liquid interface and in the liquid bulk. P* CO2, bulk is the liquid bulk concentration of CO2
expressed as a partial pressure, kg is the liquid side mass transfer coefficient and E is the
enhancement factor.

Fig 4.1: Illustration of mass transfer from gas to liquid bulk with fast chemical reaction, inspired
by Dugas

When the system is at equilibrium the concentration at the liquid interface can be calculated
from the equilibrium gas pressure at the interface using Henrys constant. According to the two-
film theory and the assumption of fast reaction where the reaction only takes place in the liquid
film, an overall mass transfer coefficient, KG, can be introduced which includes both the gas side
and the liquid side mass transfer coefficient, as described in equation
1 1 2 1 1
= + = + (8)
.0

The overall flux of CO2 from the gas phase to the liquid in the system can be described by KG and
the driving force:

2 = . (2, 2, ) (9)

where PCO2,bulk is described by the logarithmic mean pressure difference (LMPD) which is defined
as follows:
2, 2,
= 2, = 2, (10)
ln( )
2,

PSEUDO FIRST ORDER REACTIONS

Absorption of CO2 into aqueous amine solutions normally follows a second order reaction
which makes the determination of the enhancement factor quite complex [12]. If instead the
experiments are conducted in the pseudofirst order regime it allows for a simplified model as the
enhancement factor can be set equal to the Hatta number under these conditions [13]. The pseudo-
first order regime is defined by a fast reaction and requires the concentration of amine to be high
enough not to change in the gas-liquid interface during the absorption so that it can be considered
constant [14].

To verify that the reaction follows the pseudo-first order regime, the Hatta number must be
larger than 3 and lower than the infinite enhancement factor, [13].

3 < (11)

The Hatta number is defined by Equation (12). It includes the rate constants for both the
carbamate and bicarbonate formation (bicarbonate is formed in aqueous solutions) together with
the concentrations of the involved species, CMEA and COH. DCO2 is the diffusivity of CO2, kOH is
the rate constant for the bicarbonate formation and kl0 the physical liquid mass transfer.

(2 . + . ).2
= (12)
0

The infinite enhancement factor is the enhancement factor obtained for instantaneous
reactions where the absorbent is depleted at the interface. It can be calculated according to equation
(13), using the diffusivities of amine and CO2 in the liquid phase and the concentration of amine
and CO2 in the bulk and at the interface, respectively. is the ratio amine to CO2 in the reaction
obtained from the reaction mechanism.

, .
= 1 + (13)
.2, .2

In the case where the condition described in equation (11) is valid, and the reaction is of
pseudo-first order, one can make the assumption that the enhancement factor is equal to the Hatta
number based on the following correlation:

= tanh (14)

For values of x higher than or equal to 3, tanh(x) is approximately equal to 1. Thus the enhancement
factor can be set equal to the Hatta number [13].

5.0. EXPERIMENTAL SETUP -

MATERIALS:

The chemicals used were CO2, N2, He, MEA, NMP and AMP. CO2 was obtained from
AGA and He from Air Products with purities of >99,99 % and >99.98 %, respectively. NMP was
obtained from Sigma Aldrich with a purity of 99.5%. MEA and AMP were obtained from Merck
with purities of >99 % and 93-98 %, respectively. All chemicals were used without further
purification. The aqueous solutions of MEA were prepared by mixing with distilled deionized
water. The solutions were prepared using a scale with an accuracy of 0.01 g for weights up to 1200
g.
Gas mixtures with varying partial pressures of CO2 in N2 were used in the experiments,
where the pressure of CO2 ranged between 4.4 and 19.5 kPa. He was used in low concentrations
as internal standard. Table 1 gives an overview of the experiments conducted and the conditions
for the flux measurements.

PROCEDURE:

In order to measure the absorption flux in a gas-liquid system a wetted wall column (WWC)
can be used. This is a counter-current approach where the gas enters at the bottom of the column
and exits at the top. An absorbing liquid medium is pumped and distributed on to a known surface
area from the top, exiting at the bottom of the column. An illustration of the wetted wall column
used in this study is presented in Figure 3.1. It is based on the existing apparatus used by Darde
[12], which in turn has been based on the column used by Dugas [11] with minor updates.
Fig 3.1: Schematic overview of the wetted wall column (left) and experimental set up (right)

The gas is introduced to the reactor by three evenly distributed inlets at the bottom of the
reactor. The absorbing medium is pumped through a stainless steel cylindrical tube and distributed
as a thin film on the outer surface of the tube, before it exits at the bottom. The contact area can
thus be obtained from calculations using the tube dimensions and by adding the dimensions of the
liquid film and dome (at the top of the tube) resulting from the liquid distribution. The experimental
temperature is kept constant through an external cooling system where water with a set temperature
is circulated in a cooling jacket around the reactor.

Figure 3.1 also shows the experimental set-up. The pump circulating the absorbing medium
is placed directly after the column to avoid build-up of liquid in the column. Temperature is
measured both at the inlet and outlet of the reactor to monitor any temperature difference due to
the exothermic absorption reaction. The gas is saturated with solvent before it enters the reactor.
The saturator is placed in the water bath to make sure the gas holds approximately the same
temperature as the absorbing medium. On/off-valves enables the user to choose whether to run the
gas through the reactor, or in by-pass mode for calibration. The gas is analyzed with a mass
spectrometer (MS) (Hiden Analytical) which analyses part of the gas stream, the rest is led out in
the fume hood, making the system work at atmospheric pressure. The MS has an accuracy of 1.00
%. Calibration of the MS was carried out with an inert standard (He) and individual calibration
factors were calculated for each data point.

Gas flows were measured using Bronkhorst mass flow controllers, with an accuracy of
0.6 %, that were controlled through LabVIEW. The temperatures were measured using
thermocouples with an accuracy of 1.5 C.

The theoretical loading was calculated by the flux obtained from the experiments and the
time the gas stream was lead through the reactor. The molar content of the amine was calculated
from the concentration and volume or mass used in the experiment. The loading is defined as mole
CO2 per mole amine, according to equation (15).
 (2 )
= (15)
( )

For some experiments regeneration during the experiment was necessary. This was done
by introducing pure nitrogen to the system between each data point. As pure nitrogen is introduced
the concentration difference will cause the previously absorbed CO2 to desorb from the system
leading to a decrease of the system loading. Nitrogen was introduced for 15 min 1.5 hours,
depending on the amount of CO2 absorbed, to obtain sufficient regeneration.

6.0. REFERENCES
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