J Porous Mater (2009) 16:331–335
DOI 10.1007/s10934-008-9204-0
Synthesis of nano crystalline zeolite Y from bentonite
H. Faghihian Æ N. Godazandeha
Published online: 17 May 2008
Ó Springer Science+Business Media, LLC 2008
Abstract Zeolite Y was synthesized from bentonite via
the hydrothermal method. The effects of various parame-
ters on the synthesis were investigated. The samples were
characterized by XRD, XRF, IR, DTG and wet chemical
analysis. The results show that crystallization temperature,
aging time and concentration of sodium hydroxide play
important roles in the formation of the zeolite. P zeolite
was the competitive phase and present in most of the
products. However, under optimized conditions, such as
crystallization temperature (97 °C), aging time (20 h),
concentration of NaOH (3N), pure zeolite Y with high
crystallinity was synthesized. The results showed that
optimization of the process results in a commercial route to
synthesis zeolite Y from bentonite.
Keywords Bentonite
Zeolite Y
Hydrothermal
synthesis
1 Introduction
Bentonite is a rock formed of highly colloidal and plastic
clays composed mainly of montmorillonite, a clay mineral
of the smectite group, and is produced by in situ devitri-
fication of volcanic ash. Bentonite possesses high cation
exchange capacity and absorbs large quantities of water to
from thixotrophic gels with water. The properties of ben-
tonite are derived from the crystal structure of the smectite
H. Faghihian (&)
N. Godazandeha
Department of Chemistry, University of Isfahan,
Isfahan 81746-73441, Iran
e-mail: h.faghih@sci.ui.ac.ir
N. Godazandeha
e-mail: ngodazandeha@yahoo.com
group, which is an octahedral alumina sheet between two
tetrahedral silica sheets. Variation in interstitial water and
exchangeable cations in the interlayer space affect the
properties of bentonite and thus the commercial uses of the
different types of bentonite. Some groups [1–6] have
already studied the preparation of various zeolites from
kaolin or other fly ashes and have made great progress in
synthesis of 4A, mordenite, X, Y zeolite. Zeolite Y is a
parent catalyst in catalytic cracking of hydrocarbons and
petrochemical processes. Synthesis of zeolite Y from
bentonite might be the best way to chemically utilize
bentonite resources in the future [7]. Because the chemical
composition of bentonite from different locations is not
identical, the synthesis conditions must be adjusted
according to the composition of the bentonite. The method
of preparation of zeolite Y suggested by Song [7] was not
effective for the bentonite used herein. We had to alter and
optimize different parameters such as crystallization tem-
perature and aging time in order to obtain pure zeolite
phase. Since aluminium content of the bentonite was not
sufficient for synthesis, we also had to add a suitable source
of alumina in the course of synthesis. XRD pattern of
bentonite is shown in Fig. 1. Of interest is that this ben-
tonite possesses the Si–O or Al–O octahedral and
tetrahedral sheets, which creates a charge imbalance in the
2:1 layer and might be a potential raw material to syn-
thesize zeolites [8].
The Si–O and Al–O structures in bentonite are inactive.
This means that it is difficult to directly synthesize zeolites
and the bentonite must be pre-activated to change this inert
structure [9]. The most effective way to activate such nat-
ural clay is to thermally transform the inert phase into new
phase at elevated temperatures in the presence of alkali
hydroxide, which might also be useful in subsequent
hydrothermal synthesis because the commercial zeolite Y
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Fig. 1 XRD patterns of reference bentonite [9] (a) and Ardestan
bentonite (b)
are synthesized at the basic environment. In this research,
the bentonite is treated with sodium hydroxide at 300–
320 °C. It is believed that the inert skeletal structure of
bentonite was converted into activated silica and aluminate,
which might be soluble in acidic or basic aqueous solutions.
2 Experimental
2.1 Synthesis
Bentonite as starting material was provided from Ardestan
mine in central region of Iran contains SiO2 56.41%, Al2O3
14.28%, Na2O 4.07%, LOI1 17.03% and Fe2O3, BaO, MgO,
CaO, K2O, SrO, ZnO, MnO, TiO2, 7.97%. This bentonite
was reacted with concentrated HCl (30% v/v, 4 mL acid/1 g
of bentonite) for 8 h at 95 °C. The residue was washed with
deionized water on a vacuum filter and added to sodium
hydroxide solution with ratio of 1:1.2 and the dosage of
NaAlO2 was added with AlSiO 2
2 O3
¼ 36 and the material was
activated at 300–320 °C for 1 h. The activated samples
were dispersed in deionized water with stirring for 3 h.
Then the mixture was aged at room temperature for a
desired period of time (aging time) to form gel slurry. The
gel slurry was transferred to the suitable vessel to crystal-
lize, under desired temperature (crystallization temperature)
for 24 h. Subsequently, the precipitate was filtered and
washed with deionized water and dried at 70 °C.
2.2 Characterization
The synthesized samples were characterized with X-ray
diffraction (XRD), infrared spectroscopy (IR), thermal
1
Loss of ignition
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J Porous Mater (2009) 16:331–335
analysis (DTG) and chemical analysis methods. XRD
pattern of the samples were prepared by use of a D8
advanced X-ray diffractometer using CuKa with wave-
length of 1.5406 Å. A S4 Pioneer X-ray Fluorescence was
used for elemental analysis of the samples. Infrared spectra
were recorded with an IR spectrum 435 of Shimadzu
Company. Thermal analysis curves were obtained using
Mettler TG50 model. Measurements were performed in a
nitrogen flow with heating rate of 10 Kmin-1. Scanning
electron microscopy technique (XL30, Philips) was used
for measurement of particle size of the samples at voltage
of 25 kV at 15,0009 magnification. BET surface area, N2
adsorption–desorption isotherm were obtained using a
Micromeritics ASAP 2020 V1 device at 77 K.
3 Results and discussion
3.1 Synthesis of zeolite Y from bentonite
Zeolite Y is synthesized by hydrothermal method when
bentonite after addition of sodium hydroxide is thermally
activated. The problem is that the Si/Al ratio of bentonite is
too high to directly synthesis zeolite Y. Some alumina
source must be made up to be suitable for direct crystal-
lization. Sodium aluminate was introduced as a reinforcing
alumina source prior to hydrothermal synthesis. Upon
hydrothermal synthesis, the active Si and Al species dis-
solve in the alkali solution and from a supersaturated
solution. They react with each other and reconstruct to
form some ring-like structures that are the basic units of
zeolite construction [10]. To optimize the synthesis con-
ditions many operating conditions were optimized that are
summarized in Table 1.
3.2 Effect of crystallization temperature
Crystallization temperature is an important parameter in
the hydrothermal synthesis of zeolites. It might influence
the growth crystal, interface reactions of active crystal
particles. Two crystallization temperatures of 85 and 97 °C
were studied. In the XRD of zeolite Y synthesized at 85 °C
no crystalline phase was observed. Instead a sodium alu-
minum silicate hydrate phase was obtained (Fig. 2). A
mixture of zeolite Y and zeolite P were obtained when the
synthesis performed at 97 °C (Fig. 3).
3.3 Effect of aging time
The aging time was studied between 30, 20 and 24 h. The
diffraction lines of the XRD patterns of samples 2, 3 and 4
(Figs. 3, 4 and 5), illustrate that the zeolite P is competitive
phase present in the resulting products. As shown in the
J Porous Mater (2009) 16:331–335 333

Table 1 Effect of different

Number of Crystallization Aging Concentration of Vessel Type of study
parameters on the synthesis
samples temperature (°C) time (h) NaOH (N) reaction
of zeolite
1 85 30 2 Autoclave Effect of temperature
2 97 30 2 Autoclave Effect of temperature
3 97 24 2 Autoclave Effect of aging time
4 97 20 2 Autoclave Effect of aging time
5 97 20 3 Autoclave Effect of concentration

Fig. 2 The XRD patterns of reference zeolite Y [10] (a) and Fig. 4 The XRD patterns of reference zeolite Y [10] (a) and
synthesized sample 1 (85 °C) (b) synthesized sample 3 (Zeolite P 50.8%, Zeolite Y 49.2%)

Fig. 5 The XRD patterns of reference zeolite Y [10] (a) and

synthesized sample 4 (Zeolite Y 65.6%, Sodalite 13.6%, SiO2 20.8%)
Fig. 3 The XRD patterns of reference zeolite Y [10] (a) and
synthesized sample 2 (97 °C) (zeolite P 57.6%, zeolite Y 42.4%) 3.4 Effect of concentration of sodium hydroxide

figures, low aging time is beneficial to the formation of Y The concentration of sodium hydroxide of the aqueous
crystalline seeds, and at higher times, percentage of P solution significantly influences the crystalline pattern of
zeolites was increased. the synthesized zeolites. The XRD analysis shows that an

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Fig. 6 The XRD patterns of reference zeolite Y [10] (a) and
synthesized sample 5 (b)
increase in the concentration of NaOH from 2 to 3N can
result in an enormous change in the crystalline pattern
(Fig. 6).
The sharp diffraction peak of the zeolite Y when the
concentration of NaOH is 3N is obvious and pure zeolite Y
is synthesized. By taking the conditions used in the syn-
thesis of sample 5, pure zeolite Y is obtained (Table 1).
3.5 Characterization of synthesized zeolite
As shown in Fig. 6, the XRD pattern of the synthesized
zeolite is similar to that of zeolite Y typical crystal struc-
ture of a zeolite Y. Chemical composition of the
synthesized zeolite obtain from the results of XRF was as:
SiO2 47.70%, Al2O3 17.34%, Na2O 9.56%, LOI 18.56%
and Fe2O3, BaO, MgO, CaO, K2O, SrO, ZnO, MnO, TiO2,
6.84%. The ratio of AlSiO 2
2 O3
is 4.8, and within the reported
value for zeolite Y [11]. As shown in Fig. 7 the DTG curve
of synthesized sample is similar to that of the reference of
Fig. 7 DTG curve of synthesized zeolite (a) and reference of Y
zeolite (b)
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J Porous Mater (2009) 16:331–335
Fig. 8 IR spectra of synthesized zeolite (a) and reference of Y zeolite (b)
zeolite Y [11]. The weight loss (18.56%) occurred between
57 and 97 °C is within the reported value for zeolite Y [11].
Because the water molecules are bounded to different
cations, the dehydration was occurred at two distinct tem-
peratures placed in the same dehydration range (Fig. 7a).
Figure 8 represents the IR spectra of skeletal vibration.
It shows that the zeolites Y synthesized with bentonite have
similar skeletal vibration spectra as those zeolites prepared
conventionally. The spectra of the synthesized zeolites
contain some bands at 420–500, 500–650, 650–720 cm-1,
950–1,250 cm-1, 1,050–1,150 cm-1 and 3,000 cm-1 that
are originated, respectively, from the bending vibrations of
T–O, double ring, symmetry stretching, asymmetry
stretching, cross-out bonds, asymmetry stretching of inner
tetrahedral and water hydroxyl bond [11].
3.6 Measurement of particle size of synthesized zeolite
The particle size of synthesized zeolite Y was measured by
scanning electron microscopy technique. Figure 9 shows
Fig. 9 Scanning electron microscopy of synthesized zeolite
J Porous Mater (2009) 16:331–335 335

prepared by activation treatment using hydroxide

sodium and crystallization hydrothermal synthesis
under the proper synthesis conditions.
2. The crystallization temperature, aging time and con-
centration of NaOH play important roles in the
formation of the zeolite prepared from bentonite.
3. There are apparent competitions between zeolite P and
Y during the synthesis from bentonite. Thus, it is
important to control the reaction parameters to obtain
the desired zeolite. So under optimized conditions,
such as crystallization temperature of 97 °C, aging
time of 20 h, concentration of NaOH 3N, pure zeolite
Y was synthesized.
4. Pure zeolite Y with a high crystallinity can be prepared
from bentonite. The sample has small particle size and
Fig. 10 Nitrogen adsorption and desorption isotherm of synthesized good hydrothermal stability.
zeolite

the SEM image of this zeolite. The average of particles size

was 59 nm. References

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