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CERAMICS
INTERNATIONAL

Ceramics International 40 (2014) 58895896

www.elsevier.com/locate/ceramint

Hydrothermal synthesis of hydroxy sodalite zeolite membrane: Separation

of H2/CH4
Mohammad Sadegh Nabavi, Toraj Mohammadin, Mansoor Kazemimoghadam
Research Centre for Membrane Separation Processes, Faculty of Chemical Engineering, Iran University of Science and Technology (IUST), Narmak, Tehran, Iran
Received 28 August 2013; received in revised form 16 October 2013; accepted 7 November 2013
Available online 16 November 2013

Abstract
In this study, hydroxy sodalite (HS) zeolite was synthesized via hydrothermal method. As reported in the literature, the recommended molar
composition of H2O/Al2O3 for HS zeolite synthesis is about 1000. However in our work, HS zeolite was synthesized using new molar
compositions of H2O/Al2O3 for different synthesis times and their effects on morphology and crystallinity of the synthesized zeolites were
investigated. Also, HS zeolite membranes were synthesized on seeded supports using synthesized powders and the effect of seed size was also
investigated. The products were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Gas permeation through the
membranes was also measured. First of all, it was found that synthesis time has a signicant effect on crystallinity and crystal size of the
synthesized zeolite. Also, water molar ratio can control crystal size of the synthesized zeolite.
It was found out that with increasing the seed size, H2 and CH4 permeations decrease, from 3224 to 279 (Barrer) and from 611 to 45 (Barrer),
respectively, while the H2/CH4 selectivity increases from 5.28 to 6.20. Finally, to obtain HS zeolite with desirable particle size, crystallinity and
morphology, optimum synthesis conditions were proposed.
& 2013 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
Keywords: HS zeolite membrane; Crystallinity; Nanostructure; Hydrothermal synthesis; H2/CH4 separation

1. Introduction
Zeolites have crystal structures with uniform and molecular
size channels [1]. They have some applications such as
catalysts, adsorbents and ion exchangers that are useful in
renery industries. Due to their uniform pore sizes, they have
large internal surface area and active sites with high thermal
resistance and high mechanical strength [29].
Although, important parts of zeolites applications are closely
related to their framework and shape, properties of zeolites
crystals also play a crucial role in the mode and efciency of
their applications. More recently, many efforts have been
focused on some factors to control the crystallization pathway
and particulate properties of the nal products. The results
showed that chemical composition and reaction are the most
important factors for controlling the zeolite particulate properties [10,11].

Corresponding author. Tel.: 98 21 7789 6621; fax: 98 21 7789 6620.

E-mail address: torajmohammadi@iust.ac.ir (T. Mohammadi).

Hydroxy sodalite (HS) zeolite is one of the microporous

crystalline aluminosilicate hydrophilic zeolites with a small
pore size of about 2.8 . The small pore size of HS zeolite
makes separation of small molecules via difference in size
possible. Thus, it is expected that small molecules, such as
hydrogen (2.9 ), can be separated via HS zeolite membrane
from short-chain alkanes such as methane (4 ) via molecular
sieving [1216]. This kind of separation may have many
applications in separation of renery gases [17,18]. As mentioned, controlling some synthesis parameters has signicant
impacts on the zeolite performance.
Nowadays, hydrogen is considered as an alternative for
fossil fuels [19]. It can play an important role to change global
society energy resources, specially in transport applications
[20]. However, according to the literature, fossil fuels
are the main source (about 96%) of hydrogen production.
However, 48% of hydrogen resources are natural gas and 30%
from renery gases, and there are some byproducts with this
hydrogen [19]. For example, H2 is produced in reformation
of hydrocarbons and some by products such as CO2, CO,
CH4 and H2O are also produced during the reaction. Zeolite

0272-8842/$ - see front matter & 2013 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
http://dx.doi.org/10.1016/j.ceramint.2013.11.033

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membranes have high chance to selectively separate and purify

H2 from these gas streams. This is due to the fact that zeolite
membranes exhibit both high ux and high selectivity for H2
separation in the presence of those other gas species [21].
Khajavi et al. [22] reported that HS crystals can be
successfully synthesized at different synthesis temperatures
(90140 1C) for different synthesis times (3.524 h) via direct
hydrothermal synthesis. However, synthesis for short time and
at low temperature leads to the co-formation of zeolites A, X,
and -P in addition to HS and synthesis for long time and at
high temperature leads to the transformation of sodalite to
cancrinite, and increasing either temperature or time of
synthesis only increases the size of aggregates. Also, they
showed that changing the Si/Al ratio of the starting gel (114)
does not have any effect on the framework composition.
Although much studies have been performed in synthesizing
and characterizing HS zeolite powder, there are only few
studies reporting formation of highly efcient HS zeolite
membranes. Khajavi et al. [13] were also reported synthesis
and characterization of supported HS zeolite membranes. They
synthesized HS zeolite membranes at different synthesis
temperatures (90140 1C) for different synthesis times (3.5
20 h) via in situ hydrothermal synthesis under rotation. The
best selective membrane was synthesized for only 3.5 h at
413 K with negligible ux. The other membranes exhibit poor
selectivity of about 2 for helium and nitrogen separation.
In this research, HS zeolite crystals were synthesized via
hydrothermal synthesis method. The effects of crystallization
time on the nal crystalline products were studied. Furthermore, the inuence of gel molar ratio of H2O/Al2O3 on the
particulate properties (crystal size and shape) was investigated.
Finally, the effect of synthesized zeolite powder as seeds on
zeolite membrane synthesis was investigated, and the HS
zeolite membranes were characterized using H2 and CH4
permeation measurements.
2. Experimental
2.1. Material
The used silica source was silica foam (Evonika co. with
particle size of 12 nm) and the used alumina source was
sodium aluminate (5056% Al2O3, Riedelde Han) and the
used sodium source was sodium hydroxide (Solid white plate)
that was purchased from Merck Company.
2.2. HS zeolite crystals synthesis
In order to prepare the HS powder, the synthesis solution
was obtained by mixing aluminate and silicate solutions in a
polypropylene bottle. In the rst step, the aluminate solution
was prepared by dissolving sodium aluminate in deionized
water. Then, the silicate solution was prepared by mixing silica
foam, sodium hydroxide and deionized water. After a few
minutes, the clear solutions were obtained.
In the next step, the silica source was added to the alumina
source quickly. The resulting mixture was stirred for 30 min in

Table 1
Synthesized powders.
No.

Molar composition

1
2
3
4
5
6

5SiO2:
5SiO2:
5SiO2:
5SiO2:
5SiO2:
5SiO2:

Al2O3:
Al2O3:
Al2O3:
Al2O3:
Al2O3:
Al2O3:

50NaO2:
50NaO2:
50NaO2:
50NaO2:
50NaO2:
50NaO2:

1000H2O
700H2O
850H2O
1000H2O
1150H2O
1300H2O

Temperature (1C)

Time (h)

100
100
100
100
100
100

18
22
22
22
22
22

order to obtain a homogenous clear solution. The molar ratio

of the resulting synthesis solution was 5SiO2:Al2O3:50Na2O:
xH2O. The solution was then decanted in an autoclave and
placed in an oven. The synthesis was nally carried out at
temperature of 100 1C for 1822 h. Water molar ratio was
varied from 700 to 1300.
Water molar ratio and synthesis time for all the synthesized
seeds are presented in Table 1. After the hydrothermal
crystallization, the powders were recovered, thoroughly
washed with deionized water until a pH value of about 7
was obtained, and then dried at room temperature for 24 h.
2.3. HS zeolite membrane synthesis
2.3.1. Seeding support
To synthesize the membranes, homemade -alumina supports
with 2 cm in diameter, 2 mm in thickness and 100200 nm in
pore diameter were employed. One side of the supports was
polished with 800 and 1500 grit-sand papers to be prepared for
seeding. The supports were put in a cleaned KUDOS SK3310HP
ultrasonic cleaner with deionized water for about 5 min to remove
the loose particles created during polishing.
The zeolite powder was dispersed in distilled water. The
mixture (2 wt%) was then ultrasonicated for a period of time to
have a homogeneous mixture. The supports were dipped in the
homogeneous solution for a short time (10 sec) to cover the
supports with the zeolite particles. It must be mentioned that
one side of the supports was covered with Teon tape to avoid
seeding the both sides of the supports. After that the supports
were treated in an oven at 80 1C for a period time to be dried.
Five synthesized powders as presented in Table 1 (26) were
used in the seeding process.
2.3.2. Membrane synthesis
The gel solution for synthesizing the HS zeolite membranes
was prepared. It should be mentioned that the preparation
procedure of the prepared gel solution for the zeolite powders
and the zeolite membranes were completely the same and there
was no difference between these two gels. The same molar
ratio (5SiO2: Al2O3:50Na2O:1000H2O) was used for all of the
experiments.
The seeded supports were put in PTFE holders and placed
vertically in an autoclave. The synthesis solution was again
poured into the autoclave and the autoclave was put in an
oven. The membrane synthesis was carried out at temperature

M.S. Nabavi et al. / Ceramics International 40 (2014) 58895896

5891

of 100 1C for 15 h and the autoclave was put at room

temperature for 2 h to avoid any defect formation. Finally,
the solution was decanted off and the membranes were washed
with deionized water until a pH value of about 7 was obtained,
and then dried in an oven at 120 1C for 3 h.
2.4. Characterization
XRD experiments were performed to identify the HS
zeolites. The X-ray data were collected using an INEL model
EQuinox 3000 with Cu-k radiation in the range of 9050
with 40 kV and 30 mA.
The exact framework of the HS zeolites structures was
observed using SEM. The SEM images were obtained using
VEGA ll device, TESCAN Company. The membranes were
coated with gold layers before observation.
3. Results and discussion
3.1. Effect of synthesis time

Intensity a.u.

The samples 1 and 2 (in Table 1) were synthesized using the

same molar composition and at the same temperature but for
different synthesis times. The samples XRD patterns are
presented in Fig. 1. The obtained results show that the both
samples are HS zeolite. However, in compare with the
standard XRD pattern, the peaks intensity of sample 2 is more

Intensity a.u.

Intensity a.u.

Fig. 2. (a) The SEM of sample 1 (in Table 1). (b) The SEM of sample 2
(in Table 1).

Fig. 1. (a) The XRD of the 1st sample in Table 1. (b) The XRD of the 2nd
sample in Table 1.

Fig. 3. The XRD of 3rd to 6th samples (in Table 1).

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desirable in compare with those of sample 1. Also, the SEM

micrographs of the two samples are presented in Fig. 2
indicating that synthesis time is effective on morphology of
the synthesized zeolite and the zeolite crystal size. When
synthesis time increases, the particulate size also increases, and

this is because the longer synthesis time the more crystal

growth as reported in the literature [2,22].
Crystal size and crystallinity of the HS zeolite seeds are two
important factors in various applications, especially in synthesis of zeolite membranes [2]. So, the optimum conditions

Fig. 4. (a) The SEM of sample 3 (in Table 1) with (5SiO2: Al2O3: 50NaO2: 700H2O) molar ratios. (b) The SEM of sample 4 (in Table 1) with (5SiO2: Al2O3:
50NaO2: 850H2O) molar ratios. (c) The SEM of sample 2 (in Table 1) with (5SiO2: Al2O3: 50NaO2: 1000H2O) molar ratios. (d) The SEM of sample 5 (in Table 1)
with (5SiO2: Al2O3: 50NaO2: 1150H2O) molar ratios. (e) The SEM of sample 6 (in Table 1) with (5SiO2: Al2O3: 50NaO2: 1300H2O) molar ratios.

M.S. Nabavi et al. / Ceramics International 40 (2014) 58895896

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should be selected to synthesize HS zeolite seeds. In order to

synthesis uniform defect free HS zeolite membranes on the
supports, the nucleation zeolite seeds should be uniformly
small. Also the zeolite seeds should have high crystallinity and
this plays an important role to avoid non-zeolitic pores. As a
result, the maximum synthesis time of 22 h was selected for
further investigations.
3.2. Effect of water molar content
The XRD patterns of the remaining samples (in Table 1)
for the same synthesis time and temperature at different water
molar ratios are shown in Fig. 3.
HS zeolite with 5SiO2: Al2O3:50Na2O:1000H2O gel formula was purely synthesized in our previous work [9]. To
study the effect of water molar content on quality of the
synthesized powder, it was varied for the rst time. By
comparing XRD patterns of the samples with the standard
XRD pattern, it can be observed that most the synthesized
samples are HS zeolite. The most important thing to say is the
feasibility of HS zeolite synthesis in a wide range of water
molar content, and this has not been reviewed in the literature
yet. Also, crystallinity of the samples which means that the
extent of the crystalline solid phase (which is not amorphous),
was checked and it was found out that variation of water molar
content does not have any signicant effect on crystallinity
in the studied range (7001300). In the other words, there is
no difference between them with respect to the presence of
the amorphous phase and the amount of non-zeolites and
amorphous phases are minor and similar in all of the 2nd to 6th
samples.
The SEM images of these ve samples are presented in
Fig. 4. As can be observed, by increasing water molar content,
the crystal size reduces. Low concentration of materials (with
increasing water molar content) creates more space for the
primary nucleus and more distance between them and it causes
that the nucleus grows less in compare with the concentrated
gel. So, it is possible to synthesis zeolite powder with high
crystallinity and small crystal size, together.
To conde the powders particle size, microstructure measurement software was obtained from Nahamin Pardazan Asia
Co. The zeolite powders SEM images were investigated with
this software. The results are shown in Fig. 5. As seen, when
the gel water molar content increases, mean size of the zeolite
particles signicantly decreases.
It should be mentioned that the main goal of zeolite powder
synthesis is using it to synthesize zeolite membrane. From the
literature [3], it can be said that the zeolites begin to transform
into other types of zeolites before a special kind of a
continuous zeolite layer is formed on an unseeded support
under this synthesis condition. So seeding can help and
improve the zeolite membrane synthesis. It should be also
mentioned that there are some peaks in the HS zolite XRD
pattern which can be observed similarly in XRD patterns of
some other zeolites, likes 4A. In other words, the presence of
neighbor zeolites cannot be conrmed without further investigations. Synthesizing the zeolite membranes on seeded

Fig. 5. The particle size distribution of 2nd to 6th samples (in Table 1).

supports is the best way to identify whether the correct zeolite

is synthesized or not. As mentioned, the effects of crystal size
and also crystallinity of the synthesized zeolite seeds on the
support surface were further investigated. The rst synthesized
particles after ultrasonication were used for seeding. It should
be mentioned that it was tried to ultrasonicate as short as
possible to have a homogenous solution without making the
particles signicantly smaller. The particle size of the zeolite
was almost unchanged after ultrasonication.
3.3. Zeolite membrane characterization
3.3.1. SEM and XRD
The synthesis conditions of all the membranes were the
same at 100 1C synthesis temperature and for 15 h synthesis
time. The best XRD patterns and the SEM images of the
zeolite membrane surfaces are shown in Figs. 6 and 7,
respectively. The XRD results show that HS zeolite membranes can be purely synthesized except for the membrane
seeded with the 6th powder with molar content of 1300. It was
found out that this membrane is partially 4A zeolite membrane.
As reported in the literature, zeolites 4A and HS are in the
same zeolite family [22]. The water molar content of 1300 is
too high. This causes zeolite 4A is partially synthesized along
with the main zeolite (HS), and because of some similar peaks
in the XRD patterns, it is not found in the XRD analysis of the
powder. In the membrane synthesis, due to the presence of
zeolite 4A seeds along with HS zeolite seeds (as a minor
phase), zeolite 4A membrane is formed.
The SEM images show that continuous HS zeolite layers
can be obtained after using the seeds (25 in Table 1) and a
continuous 4A zeolite layer using the seed (6 in Table 1). From
the SEM images, it can be concluded that with decreasing the
seed size, a more continuous zeolite layer can be formed. Also,
from the SEM images (Fig. 6), it is clear that the zeolite layer
is more continuous with smaller grains.
However, the XRD and the SEM analysis can only indicate
the presence of zeolite layers. They cannot guaranty formation
of a continuous (defect free) zeolite layers. Thus, selectivity

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Fig. 6. The XRD of membrane of sample 3 in Table 2.

and permeability are two important properties to characterize

the synthesized zeolite membranes.

3.3.2. H2 and CH4 permeation

Considering the pore size and the hydrophilic nature of the
HS zeolite membrane, this can be nominated for H2/CH4
separation. The ideal selectivity can be calculated using the
permeabilities. Because the kinetic diameter of CH4 (0.35 nm)
is larger than the pore size of the HS zeolite channels
(0.28 nm), only H2 molecules can permeate through a defectfree HS zeolite membrane. Permeability through the membrane
(P1) can be calculated as follows:
p1

Q1 ; l
p; A

where Q1, p, l and A are volumetric ow rate of gas 1 at

standard temperature and pressure, pressure drop, effective
thickness of the membrane and surface area of the membrane,
respectively. Permeabilities are reported in Barrer, where 1
Barrer equals to 10  10 (cm3 STP. cm cm  2 cmHg  1 s  1).
Also, selectivity (12) of the membranes can be calculated
with dividing permeability of the rst permeant (p1) by the
second one (p2):
12

p1
p2

Permeability and selectivity of the membranes are presented

in Table 2. As observed in Table 2, the membrane seeded
using the 5th powder with water molar content of 1150
exhibits the higher selectivity of H2/CH4 and lower CH4 and
H2 permeabilities, while the membrane seeded using the 6th
powder with water molar content of exhibits minimum
selectivity and maximum CH4 and H2 permeabilities. It is

conrmed that the synthesized membrane is 4A zeolite and has

larger pores than HS zeolite (about 0.41 nm) [3].
As observed in Fig. 8, permeabilies of the both gases
decrease with increasing water molar content. H2 permeabilty
changes more signicantly than CH4. With paving the
membrane surface, due to increasing water molar content in
the seed synthesis, H2 permeability comes down more signicantly than CH4. It is because of molecular size of
hydrogen and due to the fact that it cannot permeate through
every zone on the membrane surface. But this is not signicant
for the bigger molecule of CH4.
So, the surface crystals of the zeolite membrane are formed
smaller and more continuous, gas permeability strongly
decreases and membrane selectivity slightly increases. This is
the reason for variation in selectivity and permeability of the
membranes as shown in Fig. 8. As observed in Fig. 8, the
maximum deviation of the results is less than 5%. Finally, it
can be said that seed size reduction, an optimum seed size
should be selected to have an optimum selectivity and
permeability.

4. Conclusion
HS zeolite crystals and HS zeolite membranes were synthesized successfully via hydrothermal synthesis method. The
effects of different parameters such as water molar content,
synthesis time and seeding on membrane synthesis were
investigated.
It was shown that by increasing synthesis time, crystallinity
and average particle size of the synthesized HS zeolite particles
increase dramatically. Therefore, to obtain HS zeolite seeds
with suitable particle size and desirable crystallinity, the
maximum synthesis time (22 h) is proposed.

M.S. Nabavi et al. / Ceramics International 40 (2014) 58895896

5895

Fig. 7. (a) The SEM of the 1st membrane seeded with (5SiO2: Al2O3: 50NaO2: 700H2O) molar ratios powder. (b) The SEM of the 2nd membrane seeded with
(5SiO2: Al2O3: 50NaO2: 850H2O) molar ratios. (c) The SEM of the 3rd membrane seeded with (5SiO2: Al2O3: 50NaO2: 1000H2O) molar ratios. (d) The SEM of
the 4th membrane seeded with (5SiO2: Al2O3: 50NaO2: 1150H2O) molar ratios. (e) The SEM of the 5th membrane seeded with (5SiO2: Al2O3: 50NaO2: 1300H2O)
molar ratios.

Also, HS zeolite crystals were synthesized using new water

molar contents based on the original molar composition for
synthesis of HS zeolite with emphasis on the SiO2/Al2O3 ratio

of 5. The obtained results showed that water molar content in

synthesis of HS zeolite controls the morphology and the phase
behavior. However, both XRD patterns and SEM images results

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References

Table 2
Synthesized membranes.
CH4
H2/CH4
No. Molar compositions Sample H2
permeability permeability ideal
of synthesized seed code
(barrer)
(barrer)
selectivity
1
2
3
4
5

5SiO2: Al2O3:
50NaO2: 700H2O
5SiO2: Al2O3:
50NaO2: 850H2O
5SiO2: Al2O3:
50NaO2: 1000H2O
5SiO2: Al2O3:
50NaO2: 1150H2O
5SiO2: Al2O3:
50NaO2: 1300H2O

700

3224

611

5.28

850

2378

415

5.72

1000

1189

202

5.89

1150

279

45

6.2

1300

77,156

45,008

1.71

Fig. 8. (a) The gas permeability of the membranes. (b) H2/CH4 selectivity of
the membranes.

showed that the purest HS zeolite could be synthesized correctly

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membranes perform better selectivity. However, permeabilities of
H2 and CH4 signicantly decrease and an optimum point should
be selected. But it should be mentioned that the obtained selectivities are higher than the selectivities reported in the literature.

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