RESEARCH ARTICLE | MARCH 09 2017

Post combustion CO2 capture using zeolite membrane 

I. G. B. N. Makertihartha; P. T. Dharmawijaya; M. Zunita; I. G. Wenten
AIP Conf. Proc. 1818, 020074 (2017)
https://doi.org/10.1063/1.4979941

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 Post Combustion CO2 Capture using Zeolite Membrane
I.G.B.N. Makertihartha, P.T. Dharmawijaya, M.Zunita, and I G. Wentena)

Chemical Engineering Department, Institut Teknologi Bandung,

Jl. Ganesha 10, Bandung 40132, West Java, Indonesia
a)
Corresponding author: [email protected]

Abstract. Carbon dioxide emission is the major cause of global warming. It is believed that reducing carbon dioxide
emission from fossil fuel combustion is the most effective way to prevent global warming. Membrane separation using
zeolites offers energy efficient way to capture CO2 compared to conventional separation techniques such as amine
absorption. In general, flue gas has high temperature and mainly consisting nitrogen, water, CO 2 and traces of other
compounds. These compounds have similar kinetic diameter thus simple Knudsen diffusion cannot separate CO 2 from
flue gas mixture. Zeolite is beneficial to post-combustion CO2 capture not only because it can withstand high
temperature but also because of its unique sorption-diffusion separation mechanism. However, zeolite membrane faced
a challenge to make it easier to fabricate. Relatively high zeolite price is also a significant hurdle to broaden its
application. In order to relieve this problem, a lot of modifications have been performed. Zeolite modification by
polymer has gained increased attention for post-combustion CO2 capture application. To present a clear background,
this work will present modifications of zeolite membrane using polymer. Special attention will be given to composite
and mixed matrix membrane configuration. Several drawbacks and problems encountered will also be discussed.

INTRODUCTION

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Emission of CO2 from fossil fuel combustion has gained increased attention in recent years. This emission is
depicted to be the main source, contributing around 60%, of global warming as greenhouse gasses.1 To reduce
CO2 emission to the atmosphere, there are three approaches, which are: reducing energy intensity, reducing
carbon intensity, and enhancing CO2 sequestration (Carbon Capture and Storage).2 The first option needs more
efficient energy use, the second option needs fossil fuel substitution such as hydrogen and renewable energy,
and the third option involves the development of technologies to sequester more CO2.3 Concern over global
climate change, sea level rise, and an increase in ocean acidity due to CO 2 emission has led much interest to
cope said problem, especially via CO2 capture.4
There are three approaches that pursued CO2 capture and sequestration during power generation, namely
post-combustion capture, pre-combustion capture, and oxy-combustion. Three approaches of power generation
from fossil fuel that use carbon capture and sequestration (CCS) is shown in FIGURE 1. Post-combustion
capture separates CO2 from other flue gas component both produced from combustion and originated from the
air. Pre-combustion capture removes carbon from fuel mixture before combustion. On the other hand, oxy-
combustion burn fuel using oxygen enriched gas containing little or no nitrogen.5 Among those technologies,
post-combustion CO2 capture has the greatest potential since it can be directly integrated with existing system
that generated two-thirds CO2 emission in the power sector.2
Post-combustion capture has to deal with low CO2 concentration and low pressure. As a consequence of low
pressure and dilute CO2/N2 feed, overall CO2 recovery cost (including capture, transportation, and sequestration
costs) are mostly contributed from the capture process that accounts for 60-80% of the overall cost.6 Present
methods for post-combustion capture available are absorption in liquids like amine, adsorption using materials
like activated carbon, and membrane separation. The Carbon Capture Project, a large study that evaluated CO 2
capture technologies, screened more than 100 different technologies and pointed out amine absorption as the
best currently available technology.7 It also has been widely used in industrial scale especially for natural gas
acid removal unit.6
Unfortunately, absorption using liquid amine suffers several drawbacks and the need for solvent regeneration
being the most significant drawbacks. When using amine absorption, a second process namely stripping is
required to isolate CO2 and regenerate the solvent. This regeneration step consumes about 4-6 GJ/ton of CO2
recovered.8 Experts agree that energy consumption reduction at about 2-4-fold is required to make post-
combustion CO2 capture to make it economically feasible.9

Engineering International Conference (EIC) 2016

AIP Conf. Proc. 1818, 020074-1–020074-9; doi: 10.1063/1.4979941
Published by AIP Publishing. 978-0-7354-1486-0/$30.00

020074-1
 Membrane technology has been used in almost every industrial sector and has started to replace conventional
processes due to advantages of the membrane technology.10-19 The advantages of membrane technology include
relatively low energy consumption, high packing density, smaller foot print, and easy to scale-up.20-22 High-
performance membranes or selective barriers based on novel materials have the potential to meet the stringent
economic criteria of post-combustion CO2 capture. Membrane gas separation technologies also have reduced
space and weight requirements, resulting in 40% savings compared with an amine plant that requires over two
times area and over three times the weight of an equivalent membrane plant.23 Moreover, membrane system is
much safer and easier to operate.2
Because of high regeneration cost of amine system, membrane processes have gained much attention due to
its inherent low energy requirement. Selective permeation of gasses using membrane will make CO 2 capture
only uses one step. Gas permeation process uses permeation rate difference through a polymeric or inorganic
membrane. Gas permeation processes possess several advantages.24
(i) High separation energy efficiency compared with equilibrium-based processes25, 26
(ii) Established processes for air separation, hydrogen recovery and carbon dioxide removal from
natural gas24
(iii) Relatively small installations due to high packing density. Size intensification is particularly
important for carbon dioxide capture due to high flow rates involved27
Microporous inorganic membranes have shown its potential in industrial gas streams separation due to
inherent energy-efficient and cost-effective. Zeolites, in particular, are favored among membrane materials due
to their thermal and chemical stability, tight controlled, well-defined microstructure and porosity, also their
competitive price.28

Post-Combustion CO2 capture

CO2 Separation N2, O2

Combustion
Unit

CO2

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Post-

Environment
Combustion
Fossil

Reformer + CO2 CO2 capture

Fuel

Combustion
separation

CO2

Air Separation
N2
Air

Unit

Oxy-Fuel

and dehydration
Compression
CO2

Combustion CO2

FIGURE 1. Approaches of power generation from fossil fuel that use carbon capture and sequestration (CCS)
adapted from Merkel29

There are many reviews discussing CO2 capture features.3, 6 Some reviews even focused on various materials
membrane for post-combustion CO2 capture.29, 30 However, to the best of our knowledge, there is no review that
specifically discusses composite polymer/zeolite membrane although it has a lot of advantages towards
commercialization for post-combustion CO2 capture. This paper will discuss general research trend related to
post-combustion CO2 capture using zeolite-based membrane including its modification to maintain high
separation factor with potential lower cost approaches. Special attention will be given to composite and mixed
matrix membrane configuration and their interaction towards CO2/N2 separation performance.

POST-COMBUSTION CO2 CAPTURE USING MEMBRANE PROCESS

Gas separation using membrane has been used in industry for the last 40 years, and the gas permeation study
through membrane has had a long history. Both porous and dense membrane can be used as a selective gas
separation layer. Membrane based separation process has been recognized as more promising compared with
conventional CO2 separation methods such as solvent absorption, solid adsorption, and cryogenic distillation.

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Membrane relies on its system compactness, energy efficiency, operational simplicity and kinetic ability to
overcome thermodynamic solubility limitation.31-33
Membrane application in post-combustion CO2 capture comes in various options. Membrane can be used as
a liquid/gas contactor of amine solution and CO2 flow. CO2 will pass through the membrane and absorbed in the
amine via liquid/gas interface while other impurities will remain in the gas phase. Amine will be more stable
due to the lower stable salt formation from impurities. This method also results in higher loading differential
between rich and lean amine, reducing the recycled amine needs. However, this method still needs further
selectivity and permeability increment along with decreased cost.34
CO2 gas separation membranes usually used polymeric or inorganic membrane. Gas transport through most
polymeric membrane follows solution-diffusion mechanism which is based on the solubility and diffusivity of
the gas in a material. Recent work on CO2 separation using polymeric membrane focused on copolymers which
generally have a hard (glassy) polymer segments such as polyamide (PA) or polyester and a soft (rubbery)
polymer segment such as polyethylene oxide (PEO).35 The hard segment supports the materials by giving
sufficient mechanical strength while soft segment act as the main CO 2 selective layer. Solution-diffusion
polymer membranes are limited by permeability and selectivity trade-off as represented by the Robenson upper
bound for membrane performance.36 For example, Polaris™ membrane from membrane Technology and
Research, Inc. (USA) can achieve high CO2 permeances (1000-2000 GPU).37 However, its selectivity is below
30, limited by Robeson upper bound at 57 °C (flue gas temperature).38
Membrane separation performance for CO2/N2 separation from flue gas is mainly described using two
௉಴ೀ
parameters, namely CO2 permeance and CO2/N2 selectivity.39 The CO2 permeance ቀ మ ቁ is defined by equation
௟
(1).
௉಴ೀమ ௃಴ೀమ
௟
ൌ (1)
ቀ௉೑಴ೀ ି௉಴ೀమ ቁ
మ

The permeance is commonly expressed in gas permeation unit (GPU), 1 GPU=10 -6 cm3(STP) / (scm2cmHg).
P is referred as the permeability with Barrer as its common unit, 1 Barrer = 10 -10 cm3(STP)cm/(scm2 cmHg). The
CO2/N2 selectivity is expressed as the ratio of CO2permeabilities over N2 permeabilities as shown by equation

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(2). The main goal of membrane based CO2 separation is to achieve high CO2 recovery (>90%) with high CO2
purity (>95%) from flue gas. In order to do so, high CO2 permeance and selectivity are required.40

௉಴ೀమ
ߙ஼ைమ Τேమ ൌ ௉ಿమ
(2)

Gas separation through zeolite membrane was carried away via adsorption-diffusion mechanism while
polymeric membrane employs solution-diffusion mechanism. In adsorption-diffusion mechanism, a molecule is
first adsorbed on zeolite surface via physical adsorption then diffuses through along zeolite surface due to
chemical potential gradient.41 Zeolite that has a higher tendency to adsorb CO2 is preferable for post-combustion
CO2 capture compared with N2. During operation, zeolite will be saturated by the adsorbed species that further
block the pores of zeolite thus making it harder to permeate via simple diffusion and enhance separation
performance towards adsorbed species. In this respect, there are several parameters that influence the diffusion:
pore diameter, molecule kinetic diameter, temperature, degree of coverage, and the presence of other
components in the case for multicomponent diffusion.42
On the other hand, solution-diffusion mechanism relies on the solubility of species combined with chemical
potential gradient to pass through the membrane. Solubility is a thermodynamic parameter and provides a
measure of the amount of the penetrant is absorbed by the membrane at equilibrium conditions. The solubility of
gas in the elastomeric polymer is very small and can be described by Henry's law. However, steam or organic
liquids, which cannot be reviewed as ideal, Henry's law does not apply. Instead, the diffusivity is the kinetic
parameters that indicate how fast penetrant move through the membrane. Diffusivity depending on the geometry
of the penetrant, so that when the size of the molecule increases the diffusion coefficient decreases. However,
the diffusion coefficient depends on the concentration and interacting and even large organic molecules that
have the ability to swell the polymer can have a large diffusion coefficient.43
Generally, permeation via adsorption-diffusion zeolite is more effective compared with solution-diffusion
polymers that are limited by Robeson plot.44 However, both mechanisms are prevailing in polymer/zeolite
composite membrane. Polymer is usually used to close zeolite defect in composite polymer/zeolite membrane.
Nevertheless, solution-diffusion is the main mechanism in polymer/zeolite membrane because polymer fills
intercrystalline pore plus it directly contacts with feed stream. In addition, many literatures report that zeolite
layer only contributes to additional mass transfer resistance to overall separation process.38, 45 Correct

020074-3
combination mechanism and configuration should be explored further in order to address this issue so that the
resulting composite membrane will gain benefits from materials that composed it.

ZEOLITE MEMBRANE FOR POST-COMBUSTION CO2 CAPTURE

Different types of zeolites and activated carbons are commonly studied physical solid adsorbents for CO2
while commonly studied chemisorbents are alkali earth metal oxides, supported amines, and hydrotalcite.46-49
Physical adsorbents employ van der Waals forces between gas molecule and its surface while chemisorbents
employ specific chemical reaction such as an acid-base type reaction for CO2 and metal oxides or amines.
Physical adsorbents have lower adsorption capacities but are easier to regenerate compared to chemisorbents.
They also have good adsorption and desorption kinetics.50 Among all physical adsorbents, zeolite shows an
attractive trade-off between properties under the condition of post-combustion flue gas CO2 capture i.e.
relatively low CO2 partial pressure (0.1-0.2 atm) and temperature (57°C).46, 47
Zeolites are crystalline aluminosilicates with well-defined microporosity that has enabled their applications
in a wide variety of fields like catalysis, detergency, chemical sensing, and separations.51 Si/Al ratio and the
number of neutralizing cations inside the pores are factors that affect zeolite adsorptive properties.51, 52 The fixed
pores of zeolites can also distinguish one from another. Zeolites have traditionally been used in adsorption
process. For the past few years, zeolite membrane has been used for a continuous separation process. Inorganic
membranes for CO2/N2 separation mainly employ molecular sieving and surface diffusion as its transport
mechanism. However, CO2 and N2 molecules have a similar kinetic diameter (0.33 and 3.64 nm for CO2 and N2,
respectively) thus make it difficult for simple molecular sieving to separate them. Surface diffusion in
combination with said molecular sieving then becomes the main factor for separation. However, the quadrupole
moment and polarizability of the CO2 molecule are about three times and twice those of N2 molecule,
respectively.52, 53 In addition, CO2 is more condensable than N2 (critical temperatures are 304.1 K and 126.2 for
CO2 and N2, respectively).54 Zeolite surface can interact more strongly with CO2 compared with N2 results in
high CO2/N2 selectivity.50

08 January 2025 19:34:35

In order to perform well i.e. have good selectivity, zeolite crystals need to be interconnected with each other
to form a continuous polycrystalline structure. For this purpose, secondary growth method is widely used to
prepare dense zeolite membranes.55-57 This method involves the deposition of a zeolite seed (small pre-
synthesized zeolite particle) layer on a solid support followed by densification via hydrothermal synthesis of the
zeolite membrane or polymer cast on top of zeolite layer.58 A popular framework for CO2 capture is FAU, either
zeolite X or Y due to their excellent CO2 selective adsorption properties.
Faujasite (FAU) type zeolites with relatively low Si/Al ratio show the highest adsorption selectivities
towards CO2 as shown by several experimental and simulation studies.46, 47, 52 FAU type crystal structure has a
pore size of 0.74 nm. FAU-type zeolite is divided by its Si/Al ratio into zeolite X (Si/Al < 1.5) and zeolite Y
(Si/Al 1.5-3.8).51 Calculation of CO2/N2 separation that previously done by Krishna et. al. 52 showed that FAU
membrane can achieve 500 in selectivity and 10000 barrer permeability. The presence of aluminum creates
negative charges in the silicon-aluminum frameworks which are neutralized by metal cations in the pore space.
Most common configurations contain Na+ as the counterion hence are called NaX and NaY. CO2 (compared to
N2) can interact more strongly with micropore electric field whose strength depends on both the number and
type of cations. NaX with lesser Si/Al ratio than NaY has more cations and demonstrates a higher CO2/N2
adsorption selectivity although have a smaller pore volume compared with NaY.59
Even tough interaction between CO2 and zeolite surface decreases as Si/Al ratio, usage of low Si/Al ratio
zeolite may cause the molecules to slow down due to strong interaction when it comes to membrane separation.
This effect may lead to zeolite Y showing a higher CO2 permeance compared with zeolite X and a better trade-
off between selectivity and permeance. Molecular dynamics simulations have shown that pure zeolite Y crystal
can achieve a permeability of > 105 Barrers with a CO2/N2 selectivity of 100-200 at typical flue gas operating
conditions.52 These values are above the Robeson upper bound for polymeric membrane.44, 52 The combination
of large FAU pores and optimum Si/Al ratio are the main factors behind the excellent performance.50
White et al.60 fabricate zeolite Y membrane on alumina support using secondary growth method. The
resulted membrane has a CO2 permeance of 300 GPU with a CO2/N2 selectivity of more than 500. Kuzniatsova
et al.61 indicated that the quality of the deposited zeolite seed layer had significant effects on the quality of
grown zeolite membrane. Other researchers reported that the cracks or defects in the zeolite seed layer could be
dreadful to the membrane separation performance in terms of CO2/N2 selectivity.58, 62 spin coating,63, 64
rubbing,65, 66 and dip-coating67, 68 are common seed deposition methods reported in the literatures. Spin coating
method was only suitable for support that has similar hydrophilicity with the zeolite type.63 Rubbing approach
can be used for various hydrophilicity but this method is hardly reproducible for large-scale purposes.65 Dip-
coating is a more reproducible method and widely used method for zeolite seed deposition in the literatures.45

020074-4
 MODIFICATION OF ZEOLITE MEMBRANE FOR CO2 CAPTURE
The major hurdles in preparing zeolite membrane lie on the difficulties in reproducibly fabricate defect-free
zeolite layer so that it can completely separate components via selective adsorption-diffusion. In addition,
inorganic substrates are thick, brittle, expensive and not amenable to continuous fabrication, the scale-up of
inorganic membranes is complicated and costly. On the other hand, polymeric membrane is easier to be
fabricated continuously in large scale. Polymeric membrane is easier to be scaled up in the form of spiral-wound
and hollow-fiber modules. However, gas separation performance of polymeric membrane is still limited by
Robeson’s upper bound contrary to zeolite membrane which has higher separation performance.45 Integration of
zeolite particle and polymeric membrane usually carried away using either composite membrane or mixed
matrix membrane. Membrane scheme of composite membrane is depicted in FIGURE 2. The reported CO2/N2
separation using zeolite-based membrane is tabulated in TABLE 1.

TABLE 1. CO2/N2 separation performance Using Zeolite-Based Membrane

CO2
Feed CO2/N2
Zeolite Polymer Configuration Support Permeance Refs.
(CO2:N2) Selectivity
(GPU)
NaY PVAm Composite PES 20:80, 57 oC 1100 >200 40

o 38
NaY PDMS/Pebax Composite PES 20:80, 57 C 940 30
NaY PEG-200 Composite PES 20:80, 57 oC 745 25.4 45

CHA PDMS Composite PES 20:80, 50 oC 1269 17.34 72

o 73
NaY - Composite PES 25 C 789 72.3
69
13X PEBAX MMM - N/A 3.43 47

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o 71
NaY PES MMM - 20:80, 25 C 1838 38
CHA PTMSP MMM - 1:7, 60 oC 315 6.2 74

SAPO-34 PSf MMM - 25 oC 314.02 26.1 75

76
LTA PEBAX MMM - N/A 97 54
77
NaX PEBAX/PES MMM - 25-45°C 3.026 42.03
60
NaY - - Al2O3 130°C 11.65 >550
60
NaY - - Al2O3 130°C 328.5 41
78
SAPO-34 - - Al2O3 50:50, 22°C 3583.70 32

020074-5
 FIGURE 2. Integration of zeolite and polymeric membrane using (a) Composite membrane (b) Mixed Matrix
Membrane

Chen et al.38 prepared Pebax®/Zeolite Y composite membrane with three layers for CO2/N2 separation. The
prepared membrane shows 940 GPU of CO2 permeance and CO2/N2 selectivity of 30. The usage of zeolite Y not
only enhances the separation but also improve the adhesion between Pebax® and PES substrate by reducing its
contact angle from 30° to 3° that is useful in preparing thinner membrane.
Besides fabricating composite membrane, mixed-matrix membrane of polymer and zeolite have also been
studied for post-combustion CO2 capture. Mixed matrix membranes (MMMS) are membranes that are
composed of polymers embedded with inorganic particles.69 By combining those two materials, combination in
terms of high inorganic selectivity plus lower cost and better handling of polymer materials can be achieved.70

08 January 2025 19:34:35

Nevertheless, material selection and polymer-inorganic poor interaction are the main hurdles in developing
MMMs. Bryan, et al.69 incorporated zeolite 13X in PEBAX to make MMM for post-combustion CO2 capture.
Nevertheless, exposure of prepared membrane to high temperature accelerated the polymer aging and the free
volume was collapsed. Wang et. al.71 recently fabricated an intergrowth zeolite inside polymer pores. The
resulted membrane is bendable around a radius of 1.5 cm curvature so that it is possible to fabricate spiral
wound module from it.
As displayed on TABLE 1, current zeolite based membrane performance is around 1000 GPU and 50
CO2/N2 selectivity. Even the highest GPU and selectivity is still far below the calculated zeolite membrane
performance using FAU.52 it means that there still are a lot of room for zeolite based membrane development.
At a glance, polymer/zeolite membranes that use composite configuration have better separation than MMM and
have similar separation to those that use inorganic support. It can be said that defect formation from pure zeolite
membrane has the same effect to performance compared with poor zeolite-polymer interaction. Moreover with
the benefits of cost reduction from polymer incorporation, polymer/zeolite composite membrane could be the
sought material for post combustion CO2 capture.

FUTURE OUTLOOK
Typical flue gas stream has atmospheric pressure and 57oC temperature with a typical molar composition of
16% H2O, 14% CO2, and 70% N2.28 The target of CO2 capture from post-combustion to ease the transport and
equestration is 90% recovery with 95% purity.28 The US Departement of Energy (DOE) has set the target cost
for any capture process, as <35% increase in the cost of electricity.79 This can be turned into membrane target
performance of >10-6 mol (m2sPa) or about 3000 GPU and a selectivity of ~200. Highly selective membrane for
CO2 separation using zeolite membrane can be achieved if significant sorption of CO2 in pore windows occurs.
Said selective sorption will reduce the window diameter so that other gasses can be easily blocked by size
exclusion (of pore diameter plus adsorbed molecule). However, most polymer/zeolite composite membrane only
employ seed layer of zeolite that have no intergrown zeolite. This condition makes zeolite layer not completely
dense and has not given its best performance. One modification that can be explored for CO2 separation using
zeolite membrane is employing perfectly dense NaY zeolite. However, polymer support cannot be used as
hydrothermal synthesis is done at elevated temperature. Synthesizing zeolite in lower temperature requires
prolonged time, inefficient for industrial scale application. Recently, Severance et al.80 studied zeolite growth on
a polymer support. They manipulated the supersaturation during synthesis of zeolite FAU via dehydration. The

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result showed that this method could increase crystal rate growth up to 4-fold. This method could be one
possible route towards zeolite membrane commercial application.
A facile fabrication of high performance zeolite based membrane is still needed to achieve efficient carbon
capture and sequestration to save the planet as soon as possible. Aside from membrane performance, membrane
stability should also be further studied due to various impurities in flue gas stream. Most researches use CO2/N2
mixture to test their as synthesized membrane. However, flue gas components such as water vapor, CO, SOx,
and NOx could be a problem during membrane operation. Disturbance from said impurities could reduce the
lifetime of quite expensive zeolite based membrane.

CONCLUSION
Post-combustion CO2 capture can be performed effectively using membrane separation process compared
with other separation processes. However, there is still much room for improvement especially in terms of
membrane performance (permeance, selectivity). Polymeric material suffers from permeance-selectivity trade-
offs as given by Robeson plot that limits its performance. On the other hand, Zeolite is the most effective
membrane materials for CO2 capture due to its excellent performance. However, zeolite price and defect
formation during synthesis are the main hurdles of zeolite membrane commercialization. To court said
problems, many researches has been done towards polymer/zeolite membrane in composite or mixed matrix
membrane configuration. Nevertheless, incorporation of polymer on zeolite membrane reduces its performance
to a certain extent. Polymer-zeolite poor interaction is also another problem to be solved by future materials.
Ultimately, the competitiveness of a membrane post-combustion CO2 capture will hinge on the optimization of
membrane price, reproducibility, and separation performance.

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