Microporous and Mesoporous Materials 284 (2019) 476–485

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Microporous and Mesoporous Materials

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

Process regulation of microwave intensified synthesis of Y-type zeolite T

a,b,c b,c,d a b,c,d b,c,d,∗ c,∗∗
Thiquynhxuan Le , Qi Wang , Bo Pan , A.V. Ravindra , Shaohua Ju , Jinhui Peng
a
Faculty of Environmental Science and Engineering, Kunming University of Science and Technology, Kunming, 650500, Yunnan, China
b
State Key Laboratory of Complex Nonferrous Metal Resources Clean Utilization, Kunming University of Science and Technology, Kunming, 650093, Yunnan, China
c
Key Laboratory of Unconventional Metallurgy, Kunming University of Science and Technology, Kunming, 650093, Yunnan, China
d
Faculty of Metallurgical and Energy Engineering, Kunming University of Science and Technology, Kunming, 650093, Yunnan, China

A R T I C LE I N FO A B S T R A C T

Keywords: A rapid microwave heating method is proposed for the liquid phase synthesis of Y-type zeolite under high-
Microwave synthesis temperature conditions. The effect of microwave heating temperatures, crystallization time and silica to alumina
Y-type zeolite ratio on the synthesis of Y-type zeolite is systematically investigated. The synthesized samples are characterized
High temperature by XRD, SEM, FT-IR, N2 sorption and particle size analysis. Microwave treatment was found to promote the high-
Enhancing mechanism
temperature synthesis of Y-type zeolite with the advantages of shorter crystallization time and product prop-
erties of the produced Y-type zeolite. Specifically, under the optimized conditions, such as input ratio of Si/Al of
4, microwave heating temperature of 150 °C, crystallization time of 0.5 h, pure Y-type zeolite is synthesized with
BET specific surface area of 645 m2/g and the total pore volume is 0.322 cm3/g. The evolution order of zeolites
with crystallization temperature is as follows: amorphous phase, Y-type zeolite, and P2 zeolite. An extended
crystallization time or increased ratio of Si/Al facilitated the formation of P2 zeolite and analcime-C. The
synthesis process promoted by microwave is explained by the high-speed rotation of polar water molecules, the
formation of isolated water molecules and the dispersion of initial aluminosilicate gel in the microwave field.

1. Introduction consumption and the overall process time are considerably reduced.
Correspondingly, microwave heating is superior to conventional
Y-type zeolite is a kind of faujasite-type (FAU) zeolite with excellent heating in terms of heating rate and uniformity, because the heating
thermal stability and catalytic activity. It has been extensively applied rate of microwave heating is not limited by the heat transfer from the
in the petroleum refining industries, mainly as a catalyst in the fluid external heat sources [11–13]. Therefore, microwave heating tech-
catalytic cracking and hydrocracking processes [1–5]. Generally, Y-type nology is befitting and advantageous to synthesize Y-type zeolite at
zeolite is synthesized from the aluminum sources, the silicon source, the moderate times and temperatures.
sodium source and the guiding agent at 100 °C by a conventional hy- Arafat et al. [14] reported that the microwave-assisted crystal-
drothermal process. The crystallization time in the traditional hydro- lization of Y-type zeolite could be completed in a much shorter synth-
thermal synthesis method is very long, sometimes it takes few days esis time and also found that the product was free of undesired phases,
[6,7]. Therefore, reducing the crystallization time is one of the most as compared with conventional heating. Araújo et al. [15] used a
important targets for commercial synthesis of Y-type zeolite. modified commercial microwave oven in order to provide pulsed mi-
Microwave heating has attracted a great attention in the synthesis of crowave pumping on the synthesis of cubic Y-type zeolite. They found
variety of materials owing to its striking features such as; fast reaction that the Y-type zeolite samples prepared displayed a good degree of
rates, more uniform heating, generating less amount of waste [8,9]. crystallinity and were suitable for use in adsorption and catalysis ex-
Microwave heating also increases the product yield and improves the periments. Katsuki et al. [16] reported the synthesis of NaY-type zeolite
quality of the product. The conversion of microwave radiation into heat crystals from colloidal silica, sodium aluminate, sodium hydroxide and
is efficient in microwave heating, unlike conventional heating, because deionized water at 100 °C for different synthesis times by using mi-
the materials are heated based on the interactions of the polar mole- crowave-hydrothermal (M − H) process and found that the M − H
cules and ions with the electromagnetic field [10]. So, the energy treatment led to increase the rate of formation of NaY-type zeolite by

∗
Corresponding author. State Key Laboratory of Complex Nonferrous Metal Resources Clean Utilization, Kunming University of Science and Technology, Kunming,
650093, Yunnan, China.
∗∗
Corresponding author.
E-mail addresses: [email protected] (S. Ju), [email protected] (J. Peng).

https://doi.org/10.1016/j.micromeso.2019.04.029
Received 28 January 2019; Received in revised form 9 April 2019; Accepted 16 April 2019
Available online 17 April 2019
1387-1811/ © 2019 Published by Elsevier Inc.
T. Le, et al. Microporous and Mesoporous Materials 284 (2019) 476–485

3–4 times compared to that of via conventional hydrothermal (C-H) amount of 10% of the expected mass of to be synthesized Y-type zeolite.
treatment. It can be seen that, compared to conventional hydrothermal After vigorous stirring for 1 h at room temperature, the mixture ob-
synthesis, microwave synthesis has the advantages of a very short tained in the above steps was poured into different PTFE reaction tanks
synthesis time, narrow particle size distribution and high purity for the and then placed in a microwave digestion oven to obtain Y-type zeolite.
synthesis of NaY-type zeolite. During the synthesis using microwave heating, a microwave power of
On the other hand, during the synthesis process, Y-type zeolite often 1600 W, a working frequency of 2450 MHz, and a pressure of 2 kg/cm2
transforms into other crystal structure of zeolites with the increase of were set up at each experiment. Samples were rotated by the rotation of
temperature [17–19]. In order to avoid this problem as much as pos- PTFE reaction tanks in the microwave digestion oven. The synthesis
sible, the crystallization temperature is usually selected to be 100 °C. solution was quickly heated to different temperatures (80, 100, 120,
However, working at a low temperature necessitates longer synthesis and 150 °C) and then it was held at the temperature for different
times which may prove too costly or impracticable for industrial ap- crystallization times (0.3, 0.5, 1, 2, and 3 h). After the completion of
plication. Therefore, reducing the crystallization time may be one of the synthesis, the reaction mixture was allowed to cool down naturally to
most important targets for commercial synthesis. With regard to the room temperature and the obtained zeolite product was thoroughly
synthesis of Y-type zeolite under high-temperature conditions, Xiong washed with deionized water and dried at 100 °C overnight. The zeolite
et al. [20] reported the synthesis of Y-type zeolite by conventional thus obtained is found to have the following chemical composition:
hydrothermal synthesis method at temperatures from 100 to 140 °C and 3Na2O:Al2O3:(2x)SiO2:209H2O (x is the Si/Al ratio, x = 3, 4, 5 and 6).
holding times from 4 to 144 h. Shan et al. [6] hydrothermally synthe-
sized sheet-like crystals of zeolite Y at high temperature (140 °C) for 2.2. Characterization
24 h using methyltriethoxysilane as an additivity. They observed that
compared with the zeolite Y synthesized at 100 °C, the zeolite Y syn- Mineral phases of samples were determined by powder X-ray dif-
thesized at high temperature has a high Si/Al ratio, a large crystalline fraction analysis (XRD, Rigaku dX 2000, Cu-Kα radiation, operating at
width/thickness ratio and has good adsorption for organic volatile 40 kV and 25 mA). The microstructure was investigated using scanning
compounds. However, their studies were carried out under conven- electron microscope (SEM, PhilipsXL20 ESEM-TMP). Analysis by FT-IR
tional heating, which required long crystallization times. Through a spectroscopy was conducted in a Perkin–Elmer Spectrum 100 FT-IR
series of experiments, we found that the crystallization temperature is spectrometer using the KBr pellet technique. BET surface area and N2
inversely proportional to the crystallization time in the synthesis of Y- adsorption-desorption isotherm were measured at −196 °C on a
type zeolite. Therefore, in order to further reduce the crystallization MicroActive ASAP 2460 (Version 2.01) volumetric adsorption analyzer.
time, a higher temperature is applied in Y-type zeolite synthesis with The pore size distribution was derived from the desorption branch of
the help of microwave, making the synthesis process faster and po- the isotherms using H-K method. The particle size was performed by a
tentially more cost effective. Laser Particle Size Analyzer (JL-1177). Thermal analysis curves were
In this work, an effective microwave synthesis of Y-type zeolite obtained using NETZSCH STA 449F3. Measurements were performed in
under high temperature is proposed. The effects of microwave heating a nitrogen flow with heating rate of 10 K/min.
temperature, crystallization time, and the ratio of silicon to aluminum
(Si/Al) on the synthesis of Y-type zeolite are studied in detail. Through 3. Results and discussion
adopting various modern analysis techniques such as X-ray diffraction
pattern (XRD), scanning electron microscope (SEM), surface area ana- 3.1. The effect of microwave crystallizing temperature
lysis, the microstructure, phase composition, and BET surface area of
the prepared Y-type zeolite are studied. Based on the obtained results, In order to understand the influence of crystallization temperature,
the phase transformation of zeolite crystal under microwave high- Y-type zeolite were crystallized with an input ratio of Si/Al of 4 for 2 h
temperature conditions is discussed, which can provide a reference for in the microwave field at 80, 100, 120, or 150 °C. The XRD patterns of
the preparation of other zeolites. synthesized products at different temperatures are shown in Fig. 2.
It can be seen that at low crystallization temperature (80 °C), the
2. Experimental work nucleation of Y-type zeolite is not favorable with an amorphous phase
as the main phase of the product. The diffraction peaks of Y-type zeolite
2.1. Synthesis process phase can be determined by XRD pattern (Fig. 2), however, the peak
intensity is weak. The possible reason is that the formation of Y-type
Fig. 1 shows the flow chart of microwave synthesis of Y-type zeolite. zeolite nucleation from the amorphous phase gel is slow at 80 °C. In-
creasing the temperature facilitates the enhancing nucleation rate and
2.1.1. Synthesis of the directing agent growth rate of Y-type zeolite. As a result, the peak intensity of the Y-
An aluminosilicate solution was prepared by dissolving 7.6 g of type zeolite increases significantly after 100 °C, especially when the
sodium hydroxide in 22 mL of deionized water, and subsequently 0.98 g temperature increases to 120 °C. This is mainly because the temperature
of sodium aluminate and 20.1 g of silica sol (d = 1.16 g/mL, containing increase promotes a series of processes, such as the increase of pressure
26.0% SiO2) were added into the caustic solution. After vigorous stir- in the reaction tank, the formation of the amorphous gel layer of alu-
ring for 1 h at room temperature, the obtained mixture was aged at minosilicate, the transformation of the amorphous gel phase into the
room temperature for 20 h to obtain the directing agent. The directing nucleation, and the crystal growth through the fusion of the nucleation.
agent was synthesized according to the following chemical composi- As the temperature rises to 150 °C, the phenomenon that Y-type
tion: 17Na2O.Al2O3.17SiO2.345H2O. zeolite gradually transforms to P2 zeolite is discovered by the XRD
characterization. The main reasons for this phenomenon are: (a) Y-type
2.1.2. Synthesis of Y-type zeolite zeolite phase is regarded as a metastable phase during crystal growth.
The Y-type zeolite was synthesized by microwave heating in a mi- Moreover, the growth of zeolite crystals is an autocatalytic process with
crowave digestions system (METASH, Model MWD-620, Shanghai a high growth rate. Therefore, higher temperatures will make Y-type
Metash Instruments Co., Ltd, China). Initially, an aluminosilicate solu- zeolite phase rapidly transform into P2 zeolite phase that is more stable.
tion was prepared by dissolving the sodium hydroxide in deionized (b) In the solution of the synthesis process, the porous product is sta-
water, and subsequently adding sodium aluminate and silica sol into bilized through the pore filling process, also known as densification
the caustic solution, similar to the synthesis of directing agent. To the process. Therefore, the increase of temperature favors the phase
aluminosilicate solution, the directing agent was then added in an transformation of Y-type zeolite （Na2Al2Si4.5O13.xH2O, Cubic, Fd3m

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Fig. 1. Flow chart of microwave synthesis of Y-type zeolite.

(227), Density (c) = 1.42）into P2 zeolite（Na4Al4Si12O32.14H2O， product crystallized at 150 °C, as shown in Fig. 3d.
Orthorhombic, Pnma(62), Density (c) = 2.15）with a higher density. It can be seen that the synthesis of Y-type zeolite includes many
SEM images in Fig. 3 shows that the morphological evolution of the processes, such as the formation of the amorphous gel layer of alumi-
reaction product with temperature during microwave synthesis. Many nosilicate, the formation of Y-type zeolite nucleation obtained by the
aggregates are found to be formed by the amorphous gels covered the ordered combination of the amorphous gel network, and the crystal
zeolite particles in the product synthesized under microwave at 80 °C, growth process, which formed by the aggregation and densification of
as shown in Fig. 3a. Nevertheless, the grain boundaries between these small Y-type zeolite nucleus with their surrounding amorphous gel
particles or between these aggregates are difficult to be distinguished. phases. In the microwave synthesis process of Y-type zeolite, increasing
When crystallized in the temperature range of 100–120 °C for 2 h, a the temperature effectively increased the nucleation and crystal
single phase of Y-type zeolite crystals is obtained in the synthesized growth, but further increased temperature may result in the formation
product. It is worth noting from Fig. 3b and c that the crystal particular of other types of zeolite crystals. In addition, the evolution order of
sizes of Y-type zeolite products crystallized at 100 °C were only zeolites with crystallization temperature is as follows: amorphous
100–300 nm, which are much smaller than the crystal particle sizes phase, Y-type zeolite, and P2 zeolite.
(about 1 μm) in the case of products obtained at 120 °C. When the
temperature reached 150 °C, a part of Y-type zeolite particles agglom-
erated together, densified and then transformed into the P2 zeolite. As a 3.2. The effect of microwave crystallization time
result, a P2 zeolite with a large particle (6–19 μm) is obtained in the
Different crystallization time (0.3, 0.5, 1, 2 and 3 h) were used on

Fig. 2. XRD patterns of zeolites synthesized under microwave at different temperatures.

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Fig. 3. SEM images of zeolites synthesized under microwave at different temperatures.

Fig. 4. XRD patterns of zeolites synthesized under microwave with different crystallization times.

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Fig. 5. SEM images of zeolites synthesized under microwave at different crystallization times.

the synthesis of Y-type zeolite with an input ratio of Si/Al of 4 at 150 °C product with the crystallization time. From Fig. 5a, it is clear that Y-
under microwave. The XRD patterns of synthesized products with dif- type zeolite crystals are covered by a small amount of amorphous gel
ferent microwave heating times are shown in Fig. 4. layer after 0.3 h crystallization. The particular size increased to 1–2 μm
It can be seen that at 150 °C when the microwave crystallization when the crystallization time extended to 0.5 h (Fig. 5b), and the
time was increased from 0.3 to 0.5 h, the peak intensity of the Y-type boundaries between these crystal particles are clearly visible. After 1 h
zeolite increased significantly. The Y-type zeolite is a single phase in the of microwave crystallizing, a part of Y-type zeolite particles began to
products. Clearly, an appropriate prolonging of crystallization time is aggregate together and densified to form P2 zeolite, as shown in Fig. 5c.
beneficial to the crystal growth, including the aggregation and densi- From Figs. 3d and 5d, it can be seen that as the crystallization time
fication of the small Y-type nucleus or small Y-type nucleus with their increased to 2 or 3 h, the densification process was further promoted.
surrounding amorphous gel phases. As a result, larger particles of Y- The Y-type zeolite crystal disappeared, and P2 zeolite particles
type zeolite are formed in products. (3–12 μm) or the spherical analcime-C particles (10–15 μm) are clearly
However, the phenomenon of crystallizing transformation is easy to observed in the product crystallized after 3 h (Fig. 5d).
occur when the holding time is prolonged under high temperatures. It is It can be seen that with prolonging the crystallization time, the
generally transformed from relatively loose structure to a more compact crystal evolution of zeolite at high temperature follows: Y-type zeolite,
structure. As a result, Y-type zeolite gradually crystallized into P2 P2 zeolite, and analcime-C. Prolonging the crystallization duration ef-
zeolite in the product crystallized for 1 h at 150 °C. After prolonging the fectively intensifies the nucleation and crystal growth processes, but it
crystallization time to 2 h, the peak intensity of P2 zeolite with a denser is easy to produce other structural types of zeolites with exceeded
crystal structure is continuously enhanced, while the peak intensity of crystallization time. Crystallization time and temperature are com-
Y-type zeolite was significantly weakened, as shown in Fig. 4. After plementary factors in the synthesis reaction. We thus concluded that the
further microwave synthesis (3 h), Y-type zeolite phase completely crystallization time should be increased if the temperature is low; on
disappeared in the products, the peaks of analcime-C phase (NaAl- other hand, the crystallization time could be shortened if the tem-
Si2O6.H2O, Cubic, la-3d(230), density (c) = 2.26）are detectable by perature is high enough. The experimental results showed that the
XRD. Therefore, after crystallization at 150 °C for 3 h, P2 zeolite par- preferred conditions for high-temperature synthesis of Y-type zeolite by
ticles can undergo a densification process to form analcime-C phase using microwave are: at 150 °C for 0.5 h.
with a more compact structure.
SEM images in Fig. 5 shows the morphological evolution of the

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Fig. 6. XRD patterns of zeolites synthesized under microwave with different Si/Al ratios.

Fig. 7. SEM images of zeolites synthesized under microwave at different Si/Al ratios.

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It is possible that the reaction activities of aluminum-contain phase and

silicon-contain phases are different in the synthetic solution. In the
microwave synthesis system, most of the aluminum containing phase
can be activated at low temperatures and enters into the zeolite struc-
tures quickly due to its high reactivity in microwave field; while a small
part of the silicon-contain phase is activated due to its low reactivity.
The sodium aluminosilicate gel is formed by the activated silicon-con-
tain phase and the activated aluminum-contain phase, and crystallized
into Y-type zeolite. With the increase of input ratio of Si/Al, more si-
licon containing phases are activated and entered into the zeolite
structures to form P2 zeolite with higher Si/Al ratio.

3.4. Properties of products and mechanism of microwave synthesis

The Y-type zeolite product synthesized under the input ratio of Si/Al
of 4, microwave heating temperature of 150 °C and crystallization time
of 0.5 h is selected for performance analysis.
The FT-IR spectra of the Y-type zeolite is shown in Fig. 8. The
Fig. 8. FT-IR spectra of synthesized Y-type zeolite.
spectra of the synthesized zeolites contain the Y-type zeolite char-
acteristic bands, which are the bending vibrations of T–O (468 cm−1)
3.3. The effect of silica to alumina ratio (where T = Si or Al), double-ring (569 cm−1), symmetric stretching
(689 cm−1 and 766 cm−1) and asymmetry stretching (999 cm−1) [21].
In order to understand the effect of Si/Al ratio on the synthesis of Y- The band at 1640 cm−1 is originated from H2O deformation mode due
type zeolite under microwave, different Si/Al ratios (3, 4, 5 and 6) were to incomplete dehydrate of the sample [22]. Moreover, the band at
used at 150 °C for 0.5 h. The XRD patterns and SEM images of synthe- 3460 cm−1 is originated from the asymmetry stretching of inner tet-
sized products with different Si/Al ratios are shown in Figs. 6 and 7, rahedral and water hydroxyl bond [23].
respectively. The N2 adsorption-desorption isotherm and micropore distribution
From Figs. 6 and 7a, when the Si/Al ratio equal to 3, the size of Y- of the synthesized Y-type zeolite are presented in Figs. 9 and 10, re-
type zeolite crystals is smaller and non-uniform. The particles of the Y- spectively. The obtained isotherm demonstrates that the Y-type zeolite
type zeolite crystallized with a Si/Al ratio of 4 are larger and more has a type I isotherm, which is a characteristic of microporous mate-
homogeneous than the crystal particles in the case of products obtained rials. The adsorption is fast at low pressure and becomes nearly con-
with a Si/Al ratio of 3, as shown in Fig. 5b. When the Si/Al ratio is 5 stant due to a monolayer formation. From Figs. 9 and 10, typical type I
(Fig. 7b), the agglomeration between particles is serious. According to isotherm and pore size around 0.76 nm confirm that the product is
the XRD pattern, it can be seen that a part of Y-type zeolite particles zeolite Y. The BET specific surface area, the micropore area, the ex-
aggregated together, densified and transformed to P2 zeolite. In the ternal surface area and the total pore volume of the Y-type zeolite are
case of the Si/Al ratio of 6 (Fig. 7c), the P2 zeolite is the only phase of found to be 645 m2/g, 605.4 m2/g, 39.7 m2/g and 0.322 cm3/g, re-
the product. spectively. The performance of the zeolite synthesized by our method is
It can be seen that with the increase of input ratio of Si/Al, the similar to that of the commercial Y-type zeolite (BET specific surface
density of synthesized products also increases. However, the Si/Al ratio area is 659 m2/g and total pore volume is 0.382 cm3/g).
in the synthesized product is often lower than that of the input material. The particle size distribution of synthesized Y-type zeolite is shown

Fig. 9. N2 adsorption-desorption on synthesized Y-type zeolite.

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Fig. 10. Micropore distribution of synthesized Y-type zeolite.

in Fig. 11. It can be seen that the particle size of the sample is mainly
distributed in the range of 0.5–1.9 μm with the highest peak at 1.3 μm.
The reason is that at a high crystallization temperatures, a small
amount of crystal nuclei are dissolved and then recrystallized, thus
forming large particles. Liu et al. [24] reported that the particle size of
Y-type zeolite increased gradually, and the particle size distribution was
broadened with the increase of crystallization temperature. They got
the particle size distribution of the Y-type zeolite obtained at 110 °C was
0.1–8 μm under conventional heating. However, the particles with a
particle size in the range of 0.5–1.9 μm account for about 70% of the
total sample obtained at 150 °C under microwave heating in our work.
This result shows that microwave synthesis has more advantages in
controlling the particle size distribution of the Y-type zeolite than
conventional synthesis.
The thermal degradation of the Y-type zeolite prepared was induced
at a heating rate of 10 K/min in an N2 atmosphere, and the result is
shown in Fig. 12. As shown in Fig. 12, the TG curve shows a ∼26%
weight loss between 30 and 300 °C that can be attributed to the loss of
Fig. 11. Partice size distribution of synthesized Y-type zeolite. water. It does not appear the weightlessness peak as the temperature
increased from 300 to 900 °C, indicating that the framework of Y-type
zeolite product has not collapsed. Yang et al. [25] reported that the
framework of Y-type zeolite synthesized by conventional heating
usually collapses, resulting in weight loss when the temperature is
above 800 °C. Therefore, compared with Y-type zeolite synthesized by
conventional heating, the thermal stability of Y-type zeolite synthesized
by microwave heating is higher.
Table 1 shows the synthetic conditions and product properties of Y-
type zeolites reported in the literature. Compared with other methods
for the synthesis of Y-type zeolite from pure materials, the present
method has the advantages of a very short crystallization time (only
0.5 h) and large specific surface area of Y-type zeolite.
The role of the microwave in the synthesis of Y-type zeolite is dis-
cussed through the mechanism of the liquid phase transformation. The
mechanism of zeolite synthesis is considered in the liquid phase tran-
sition theory [28]: (a) In the synthesis process of zeolite, the initial
aluminosilicate gel is firstly formed at a disordered state after the raw
materials are mixed uniformly. However, there may be simple primary
units of zeolite structural that are contained in the disordered state of
Fig. 12. TG curve of synthesized Y-type zeolite. aluminosilicate gel. (b) A dynamic dissolution equilibrium is reached
between the initial aluminosilicate gel and the liquid phase composition

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Table 1
Synthetic conditions and product properties of Y-type zeolites reported in the literature.
Heating method Crystallization temperature Crystallization time (h) BET surface area Total pore volume Reference
(°C) (m2/g) (cm3/g)

Conventional heating 80–120 15–25 247–524 0.125–0.272 [26]

Conventional heating 100 24 775 0.34 [7]
Microwave heating 100 2 474 0.35 [7]
Using pulsed microwave irradiation 100 Microwave emission time of 10–25 min, 192–340 [15]
Crystallization time of 3–6 h.
Ultrasonic/microwave synergistic 100 6 752 0.37 [27]
synthesis hydrothermal
This work 150 0.5 645 0.322

in the synthesis solution. When the initial aluminosilicate gel dissolves, 4. Conclusions
the concentration of aluminosilicate in the liquid phase increases, re-
sulting in the formation of nuclei and the growth of crystals. A detailed study on the synthesis of Y-type zeolite under microwave
Therefore, microwave heating enhances the synthesis process of reveals that:
zeolite for the following reasons:
(1) The microwave irradiation is beneficial to the synthesis of Y-type
(1) In microwave field, due to the dipole moment in the structure of zeolite with the advantages of short crystallization time and similar
water molecule, the polar water molecules will rotate at high speed, product properties to industrial Y-type zeolite.
and change the direction of movement with the change of the di- (2) The evolution order of zeolites with increasing crystallization
rection of the microwave field. Therefore, water can absorb mi- temperature is: amorphous phase, Y-type zeolite, and P2 zeolite.
crowave energy easily and then convert the energy into heat (3) An extended crystallization time or increased input ratio of Si/Al
[29,30]. In the microwave synthesis reaction, the microwave acti- facilitates the formation of P2 zeolite and analcime-C with more
vates the rotational energy level of the water molecules in the compact structures.
synthetic solution, making the rotation of water molecules origin- (4) Under the optimized conditions, such as input ratio of Si/Al of 4,
ally associated with hydrogen bonds. As a result, on one hand, it microwave heating temperature of 150 °C, crystallization time of
provides the heat energy needed for crystallization. On the other 0.5 h, pure Y-type zeolite is synthesized with BET specific surface
hand, it destroys the hydrogen bonds and releases the isolated area of 645 m2/g and the total pore volume is 0.322 cm3/g.
water molecules. The same view of the mode of action of micro- (5) The promoted zeolite formation by microwave is explained by the
wave heating in zeolite synthesis has been discussed by other au- high-speed rotation of polar water molecules, the formation of
thors [31,32]. isolated water molecules and the dispersion of initial aluminosili-
(2) The isolated water molecules have a higher potential energy due to cate gel in the microwave field.
the presence of the lone pair electrons of oxygen atoms and OH
bonds. Therefore, isolated water molecules attack the initial alu- Acknowledgment
minosilicate gel more easily than the water molecule group asso-
ciated with hydrogen bonds [33], which accelerates the dissolution The authors acknowledge the financial support provided by China
of aluminosilicate gels and thus nucleates a large number of initial Postdoctoral Science Foundation, China (2018M633424); the first
aluminosilicate gels. batch of Yunnan Provincial Postdoctoral Research Fund Project, China;
(3) Because of the high-frequency oscillation of the microwave, the Yunnan Province Post-Doctoral Training Fund, China in 2018; Applied
initial aluminosilicate gel in the crystallization system is highly Basic Research Program of Yunnan Province, China in 2019 and
dispersed, forming reaction areas with uniform temperature dis- Kunming University of Science and Technology, China for Post-Doctoral
tribution, which is more conducive to the crystallization process. Fellowship.
This conclusion can be clearly verified from Figs. 3 and 4. It can be
seen that only a small portion of Y-type zeolite is observed at 80 °C References
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