Advanced Powder Technology 21 (2010) 279–283

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Advanced Powder Technology

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

Original Research Paper

Conversion of high silicon fly ash to Na-P1 zeolite: Alkaline fusion followed

by hydrothermal crystallization
H. Kazemian a,b,*, Z. Naghdali a, T. Ghaffari Kashani a, F. Farhadi a
a
SPAG Zeolite R&D Group, Technology Incubation Centre, Science and Technology Park of Tehran University, Tehran, Iran
b
Department of Chemical and Biochemical Engineering, Faculty of Engineering, The University of Western Ontario, London, Ontario, Canada N6A 5B9

a r t i c l e i n f o a b s t r a c t

Article history: In this research, we converted high silicon fly ash to a high ion-exchange capacity zeolite using a two
Received 5 August 2009 stages conversion process. Alkaline fusion was applied to collapse the fly ash crystalline phases and
Received in revised form 29 November 2009 release Si content. Then Si/Al ratio of the synthesis sol adjusted with appropriate amount of industrial
Accepted 8 December 2009
grade materials. A synthesis solution with the molar ratio of 2.2 SiO2:Al2O3:5.28 Na2O:106 H2O was
hydrothermally crystallized to Na-P1 zeolite at 120 °C for 4 h. The as-synthesized zeolite characterized
by means of X-ray diffraction, infrared spectroscopy, scanning electron microscopy and thermal analysis.
Keywords:
Cation exchange capacity of the zeolite was determined using ammonium acetate method. The zeolitiza-
Flyash
Zeolite Na-P1
tion remarkably improved the cation exchange capacity of the final product (e.g. 3.23 meq/g in compar-
Synthesis ison to the raw fly ash 0.005–0.02 meq/g).
Ion-exchange capacity Due to the high CEC and sufficient whiteness of the final product, we suggest that the as-synthesized
zeolitic powder is a potential candidate as a detergent builder.
Ó 2009 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder
Technology Japan. All rights reserved.

1. Introduction hydrothermal synthesis from alkali-fused fly ash [6], and hydro-

Most of the world’s produced fly ashes (FA) are solid wastes of
coal combustion in the electricity generation processes. However,
some other industries such as steel and ferrosilice industries also
encounter hazards of this solid waste. Different industries produce
FA with various chemical and mineralogical compositions. Disposal
of fly ash that is a very fine submicron powder, has become an
increasing economical and environmental burden. So far, the only
realized utilization of FA is by low technology applications such as
in construction materials and cements. Nevertheless, more than
500 million tones/year of fly ash is produced globally, of which
only 20% effectively used [1]. This implies that finding techno-eco-
nomically viable methods to treatment FA in a safe manner is an
urgent need of the industries. In the recent decades, many efforts
are being made to explore other potential applications such as
using in cements and concretes, roadbed, gas absorbents and fertil-
izers. One possible new application for FA is the synthesis of value
added zeolitic materials. Many researchers have investigated fly
ash as starting material for hydrothermal synthesis of various zeo-
lites. Fly ash has been used for direct hydrothermal synthesis [2–5],
* Corresponding author. Address: Department of Chemical and Biochemical
Engineering, Faculty of Engineering, The University of Western Ontario, London,
Ontario, Canada N6A 5B9, Tel.: +1 519 694 9453.
E-mail addresses: hossein.kazemian@uwo.ca, hosseinkazemain@gmail.com
(H. Kazemian).
thermal synthesis of zeolite using extracted silica [7]. Possible
zeolitization of FA is a process analogous to the formation of natu-
ral zeolites of the volcanic bedrocks. Both volcanic ash and FA are
fine-grained and contain large amounts of aluminates and silicates
glasses [8]. In natural conditions, this glass fraction might be con-
verted into zeolites by the influence of percolating hot groundwa-
ter, while the zeolites may subsequently be converted into other
minerals.
This similarity of fly ash to some of volcanic minerals stimu-
lated the idea of using fly ash solid wastes for conversion into
the value added synthetic zeolites [9].
Since the results of preliminary studies on this issue were
promising, more researchers have been dedicated their research
life on this issue. As results of these activities, many articles related
to manufacturing of various zeolitic materials from FA were pub-
lished and many patents were registered. Most of the conversion
procedures are based on alkaline hydrothermal crystallization, in
which by applying different temperatures, pressures and crystalli-
zation duration times on various chemical compositions, varieties
of zeolitic materials have produced with different potential appli-
cations [3].
While this conversion process may take tens to thousands of
years in the nature, in a laboratory, the reaction duration can be re-
duced remarkably to some days or even to hours [10]. This implies
that using of fly ash as a cheap and abundant source of Si and Al for
making artificial zeolites can be considered as a promising method

0921-8831/$ - see front matter Ó 2009 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.
doi:10.1016/j.apt.2009.12.005
280 H. Kazemian et al. / Advanced Powder Technology 21 (2010) 279–283

to treatment all type of FA based solid wastes. Usually, this method the crystalline zeolitic product was examined by mean of scanning
is an alkaline hydrothermal crystallization process, in which the fly electron microscopy using a Philips instrument (Model; XL30).
ash is mixed with an alkali hydroxide such as NaOH and fuse at an Further characterization of the product was carried out by investi-
elevated temperature to release the silica and alumina content in gation of its thermal behavior by mean of thermal analyses tech-
the form of water soluble sodium silicate and sodium aluminate. niques using a simultaneous thermal analyzer (STA-Rheometric
Then the chemical composition of resultant solution will be ad- Scientific). In order to evaluate the ion-exchange property of the
justed by adding sufficient amounts of Al and/ or Si, etc. according as-synthesized zeolite, its cation exchange capacity (CEC) was
to the desirable zeolitic phase. Such treatment processes can lead measured by mean of ammonium acetate saturation method
to the formation of various types of zeolite with different Si/Al ra- [15–16]. This method is based on saturation of all ion-exchange
tios such as the zeolites P, A, X types, etc. The type of zeolite formed sites in ion-exchanger with ammonium ion at equilibrium condi-
is a function of the temperature, pressure, chemical composition of tion. The time required for saturation (e.g. achieving to equilib-
synthesis gel/sol (e.g. concentrations of Al, Si and cation and type of rium) depends to the ion-exchange reaction kinetic.
the used salts), aging time, pH, and crystallization duration, etc. In this research, due to relatively fast reaction kinetic of the as-
[11]. synthetic zeolite P, the ammonium solution and the zeolite pow-
Following to the previous research of our group on the synthesis ders were in contact for 24 h in order to make sure that exchange
of various zeolites of NaA and FAU from high silicon fly ash [12– reaction reaches to equilibrium. The zeolite to ammonium solution
14], this paper reports the results of a new research work on the ratio was kept at 1/50. The Kjeldahl ammonia distillation technique
successful hydrothermal conversion of a high silicon fly ash from was used to determine the ammonium concentration in the zeo-
Iran Ferrosilice Company into zeolite P powders. Details of hydro- litic phase. The CEC was calculated accordingly.
thermal treatment of the fused fly ash, characterization results as
well as ion-exchange capability of the converted product in com-
parison to the raw FA and some of other zeolitic materials will 3. Results and discussion
be compared and discussed.
The sodium hydroxide present in the fusion mixture, acts as an
activator during fusion to form soluble silicate salt. Fusion of NaOH
2. Experimental with fly ash produces sodium silicate and amorphous aluminosili-
cate, which can be easily dissolved in aqueous solution. The X-ray
All of the chemicals used in this research were domestically diffraction patterns of the used high silicon FA and the as-synthe-
produced industrial grade materials. High silicon fly ash was pro- sized zeolitic material are shown in Fig. 1. The XRD pattern of zeol-
vided by Iran Ferrosilice Company, Semnan, Iran. itized FA, exhibits several sharp diffraction peaks, which are
For fusion step, sufficient amount of the FA was mixed with different from those present in the untreated FA.
appropriate amounts of NaOH in a FA/NaOH weight ratio of
1/1.2. The resultant mixture then fused in a muffle furnace at
550 °C for 1 h in air atmosphere. The heating rate of 5 °C/min
was applied to elevate the temperature from ambient to 550 °C.
The melted materials was then cooled to room temperature with
cooling rate of 20 °C/min , well milled to fine particles using an
agate mortar. Then 50 ml of 0.2 M solution of NaOH added to the
mixture. The resultant slurry was then agitated vigorously by a
mechanical stirrer for several hours at 70 °C. The resultant silica
solution (Solution A) was cooled to room temperature and slowly
added to the sodium aluminate solution. The aluminate solution
was prepared by adding sufficient amounts of sodium aluminate
to a NaOH solution (Solution B). Solution A was then added to solu-
tion B in several steps and the mixture was stirred to achieve a
homogenous gel. Chemical composition of the resultant synthesis
gel was as following:

2:2ðSiO2 Þ : ðAl2 O3 Þ : 5:28ðNa2 OÞ : 106ðH2 OÞ

To crystallize the zeolite, the prepared synthesis gel was trans-
ferred into a PTFE lined stainless steel reactor, sealed and heated in
an electrical oven equipped with an ‘‘end over end” shaker, at
different temperature of 100 °C and 120 °C under autogenously
produced pressure with and without shaking. After 4 h of crystal-
lization duration, in order to assure that the reaction is stopped,
the reactor was quenched in cold water. The solid product then
separated from supernatant by filtration using a filter paper,
washed with excess amounts of de-ionized water to remove excess
amount of sodium hydroxide and other none reacted materials and
then dried overnight at 60° C in an electrical oven. Chemical com-
positions of the utilized FA and the produced zeolite P was mea-
sured by X-ray fluorescence technique using an Oxford
instrument (XRF; ED2000). The crystallinity of the final zeolitic
product was evaluated by mean of X-ray diffraction technique
using a Philips1130/90 instrument and furrier transform Fig. 1. X-ray diffraction patterns of the raw fly ash and as-synthesized zeolite
infra-red spectroscopy (FT-IR; Vector 22-Bruker). Morphology of Na-P1; Q = quartz, M = mullite, H = iron oxides, P = Na-P1 zeolite.
 H. Kazemian et al. / Advanced Powder Technology 21 (2010) 279–283
The X-ray patterns show that the original crystalline phases of
fly ash are defaced in the final product. With comparing of the
main peaks in the XRD pattern of as-synthesized material with
the reference [17], formation of Na-P1 zeolitic phase ascertains.
Furthermore, several crystalline phases of quartz, mullite and iron
oxides were distinguished in the raw FA sample, whereas the main
crystalline phase in the final product is Na-P1. There are four
phases in the used fly ash (e.g. amorphous aluminosilicates glass,
quartz, mullite and iron oxides), in which three of them (e.g. glass,
quartz, mullite) contribute as sources of silicon and aluminum. It is
obvious that the amorphous aluminosilicates glass is the most
unstable phase in the hydrothermal environment with the highest
rate of dissolution and therefore the main provider of Si and Al pre-
cursors for zeolitization process [2]. Although quartz and mullite
phases are remarkably more stable than glass phase, quarts is less
stable than mullite [3].
According to the previous findings of our team, zeolite LTA is
predominant phase at lower hydrothermal temperature of
100 °C, whereas zeolite Na-P1 forms at higher crystallization tem-
peratures of 120 °C [12,13]. The characterization results reveal that
at the examined synthesis condition, Na-P1 zeolite is more stable
than zeolite A. Higher curing temperatures allowed the more stable
zeolite Na-P1 to be formed. It has been shown the high tempera-
tures and higher Si concentrations favor the formation of mono-
mers of smaller oligomer silicate species such as S4R secondary
building unit (SBU), whereas low temperature and high Si concen-
tration favor larger silicate species such as D6R unit and b-cage
[18]. Zeolite Na-P1 framework is based on S4R unit. Therefore, at
different hydrothermal temperatures and different silicate concen-
trations, wide varieties of silicate species can be formed. This can
be lead to formation of different type of zeolites. The influence of
shaking on the crystallization product was also investigated. It
was found that the stirring speed from 200 RPM to 550 RPM has
not a signification influence on the final zeolite content which in
Table 1
Chemical composition of the used FA and as-synthesized zeolite P by mean of XRF
technique.
Sample SiO2 Al2O3 Fe2O3 CaO MgO Na2O K2O SiO2/Al2O3
FA 97.7 0.9 1.3 0.6 0.6 0.2 1.1 108.5
Na-P1 63.1 26.3 0.9 1.1 1.5 5.5 0.6 2.4
Fig. 2. FT-IR spectra of the synthesized Na-P1 zeolite in the wave number range of 400–4000 cm1.
281
all cases amounted to ca. 40% of zeolite Na-P1 formed .An increase
in speed was resulted, however, shorter induction periods and thus
in the shorter reaction time necessary to reach the maximum crys-
tallization of zeolite material. Presumably, this is due to an in-
crease in the rate of dissolution of silica .In addition the speed of
stirring proves to influence the morphology of the zeolite formed.
At the higher speeds, newly formed crystals appear to be smaller.
This was resulted a hard cemented aggregates on the bottom of
the reaction vessel which contains crystals of zeolite Na-P1 used
in most experiments carried out below 100 °C.
Chemical composition of the raw FA and as-synthesized zeolite
P are summarized in Table 1. This data reveals that the high Si con-
tent of raw FA with SiO2/Al2O3 = 108.56, was reduced to 2.36 by
increasing of the Al2O3 content from 0.9% to 26.30% in the final
product. Increasing of Na2O content of the final product up to
4.50%, in comparison to the raw FA, which was only 0.20%, is a very
clear and promising evidence of CEC improvement in the final
product. These remarkable changes can be considered another evi-
dence of successful conversion.
Furrier transform infra-red spectroscopy (FT-IR) is a powerful
technique for structural characterization of organic and inorganic
materials. Zeolites IR spectra include two groups of vibrations: (i)
internal vibrations of TO4 units (T = Si, Al in zeolite), which are
insensitive to the structural vibrations; and (ii) vibrations of the
external linkage of the TO4 units. The Later is sensitive to structural
vibrations. However, some common features including asymmetric
and symmetric stretch, double ring vibrations, T–O bending modes,
and possibly pore opening modes observe in all zeolitic structure.
The IR spectra of the as-synthesized zeolite P illustrated in
Fig. 2. The two most intense bands for zeolites usually occur at
400–4000 cm1, which are shown more clearly in the figure. The
first band assigns to an asymmetric stretching mode, whereas
the second one assigns to a bending mode of the T–O bond. All
these bands are more or less dependent on the crystal structure.
The mid infra-red region of the spectrum contains the fundamental
framework vibration of Si (Al) O4 groups. The absorbance band in
between the wave numbers of 400–4000 cm–1 represents the pres-
ence of substituted Al atoms in the tetrahedral forms of silica
frameworks. According to Fig. 2, bands at 565, 1061, 650, 1115,
480, 3400, 1375 cm–1 are correspondent to doubling stretching,
asymmetric stretching, symmetric stretching, T–O stretching, T–O
bending, H–O stretching, and H–O bending modes, respectively.
282 H. Kazemian et al. / Advanced Powder Technology 21 (2010) 279–283

Fig. 3. Thermal analysis (TGA, DTA) curves of the as-synthesized Na-P1 zeolite.

aggregate of zeolite Na-P1 with crystallite size ranging up to

Fig. 4. SEM image of the as-synthesized crystalline Na-P1 zeolite obtained at
optimum hydrothermal condition.
One of a typical SEM micrograph of the final product is shown in
Fig. 4. According to the SEM image, formation of polycrystalline
2–3 lm can be clearly observed The observed morphology of the
crystals corresponds to other reports [19–21],
Thermal analysis curves (TGA and DTA) of the as-synthesized
zeolite P is shown in Fig. 3. The curves were obtained by thermal
treatment of 10 mg of the sample from ambient temperature to
800 °C, by a heating rate of 10 °C/min in argon atmosphere. Endo-
thermic peak exists in the DTA and weight losing slope in the TGA
curve demonstrates the maximum rate of H2O loosing is tempera-
ture around 100 °C. According to the TGA curve, the maximum
weight loss, which is corresponded to water content of the sample,
is about 12 wt.%. The DTA curve of the as-synthesized zeolite
shows several thermal effects. The first endothermic effect with
its maximum around 110–140 °C is relevant to water release from
Na-P1 zeolite, accompanied by sharp and sudden loss of mass. It
seems that an exothermic effect at 510–540 °C may be connected
with partial decomposition of the zeolite Na-P1 structure. Usually
a process of crystal decomposition is of exothermic character.
Moreover, in certain cases it has been reported that decomposition
of zeolites is related to the collapse of free duct spaces at this tem-
perature. This may be happened for the largest ducts (0.320 nm) in
Na-P1 zeolite structure[22].
One of the main applications of zeolite P type is known as deter-
gent builder. The main determining factor in this application is cat-
ion exchange capacity of the builder. In order to evaluate the ion
exchange capability of the as-synthesized zeolite sample, CEC of
the zeolite was measured. The cation exchange capacity (CEC) of
the synthesized zeolite was measured by means of the ammonium
acetate method. The results obtained reveal that the applied
zeolitization process was increased the cation exchange capacity
(CEC) of the product to 3.23 meq/g. In Table 2, cation exchange

Table 2
Cation exchange capacity (CEC) of the as-synthesized zeolite P in comparison to raw FA and some related typical zeolites [12,13,21,22].

Sample R-Na P1a Na-P1-FAb Na-P1-FAc P-Clinod A-FAe FAf

CEC (meq/g) 4.4 3.23 1.40 1.65 3.55 0.005–0.02
a
R-Na P1: Reference Na-P1 zeolite (Ref. [12]).
b
Na-P1-FA: Fly Ash based zeolite P. This work.
c
Na-P1 from coal fly ash (Ref. [21]).
d
P-Clino: Clinoptilolite based zeolite P (Ref. [22]).
e
A- FA: Fly Ash based zeolite A (Ref. [13]).
f
FA: Fly Ash (Ref. [10]).
 H. Kazemian et al. / Advanced Powder Technology 21 (2010) 279–283
capacity of the prepared zeolite is compared with the raw FA [3],
and some other relevant zeolites in the literature [11,12,23,24].
The CEC of final zeolite product that we measured in this re-
search (i.e. 3.23 meq/g) is far higher than what recently reported
by a research group, who recently reported the synthesis of a Na-
P1 zeolite from coal fly ash with a CEC of 1.4 meq/g [23]. The
achieved CEC is comparable to other zeolitic materials such as
LTA and NaX that are usually use as detergent builder. This implies
that the product can used as a cation exchange material for various
applications such as water softener, detergent builder, and so forth.
Comparison of CEC of the as-synthesized zeolite with raw fly ashes
(e.g. 0.005–0.02 meq/g); will be highlighted the achieved values
added in this conversion [3].
4. Conclusion
In this work, we successfully converted a high silicon fly ash (a
solid waste (byproduct) of Iran Ferrosilice Company) to Na-P1 zeo-
lite, by mean of a two stages conversion process. It can be con-
cluded that:
(1) Results revealed that a synthesis gel with the molar ratio of
2.2SiO2:Al2O3:5.28Na2O:106H2O can be converted to zeolite
Na-P1 powder at the temperature of 120 °C and the crystal-
lization time of 4 h. The higher crystallization temperature
of 120 °C, was resulted a more stable zeolitic phase.
(2) Formation of P zeolite was ascertained by mean of different
characterization techniques including XRF, XRD, FT-IR, TGA-
DTA. The XRD results also revealed that the mullite phase in
the raw FA sample is stable enough to remain unchanged
during the whole conversion processes.
(3) We measured the cation exchange capacity (CEC) of the as-
synthesized zeolite using ammonium acetate method. The
measured CEC of 3.23 meq/g, was remarkably higher than
the used raw FA that is in the range of 0.005–0.02 meq/g.
(4) This research achievement, along with the previous works of
our group on the zeolitization of high silicon FA to LTA and
FAU zeolites [12–14] ; implies that the FA solid waste is a
suitable source of Si and Al for manufacturing of different
zeolites .
(5) Due to the high CEC and sufficient whiteness of the final
product, we suggest that the as-synthesized zeolite powder
can be used as a potential candidate for detergent builders.
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