Advanced Powder Technology xxx (2015) xxx–xxx

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Advanced Powder Technology

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

Original Research Paper

Hydrothermal synthesis of zeolite A from K-feldspar and its

crystallization mechanism
Shuangqing Su a,b, Hongwen Ma b,⇑, Xiuyun Chuan a
a
Key Laboratory of Orogenic Belt and Crust Evolution, School of Earth and Space Sciences, Peking University, Beijing 100871, China
b
School of Materials Science and Technology, China University of Geosciences, Beijing 100083, China

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

Article history: Zeolite A was indirectly synthesized from K-feldspar using hydrothermal conversion method. In order to
Received 29 July 2015 gain active SiO2 and Al2O3, the K-feldspar powders were pretreated with KOH solution followed by H2SO4
Received in revised form 28 October 2015 solution to form X-ray amorphous materials (AS). The effects of reaction time on the conversion of the
Accepted 28 November 2015
obtained AS to zeolite A were investigated. X-ray diffraction (XRD), wet chemistry analysis, scanning
Available online xxxx
electron microscope (SEM), Fourier Transform Infrared spectroscopy (FTIR), and 29Si and 27Al magic-
angle-spinning nuclear magnetic resonance (29Si MAS-NMR and 27Al MAS-NMR) were used to character-
Keywords:
ize the nucleation and crystal growth processes. The results indicated that the AS was dissolved com-
K-feldspar
Zeolite A
pletely and abundant nuclei were formed during the first hour of the crystallization stage. With the
Hydrothermal crystallization time increasing, the nuclei were rapidly grown into zeolite A crystals and relative crys-
Crystallization mechanism tallinity of pure zeolite A reached its maximum when crystallization time reached to 3 h. An excess time
resulted in further dissolution of zeolite A and replacement by hydroxyl sodalite. The mechanism of syn-
thesis of zeolite A from pretreated K-feldspar can be described by three main stages: (1) the dissolution of
amorphous aluminosilicate releasing [SiO2(OH)2]2
and Al(OH)4
; (2) the formation sodium aluminosil-
icate gel as zeolite precursor; (3) the crystallization of zeolite A.
Ó 2015 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder
Technology Japan. All rights reserved.

1. Introduction K-feldspar (KAlSi3O8) is widespread and common in a wide

Zeolite A (Na12Al12Si12O4827H2O) is a porous aluminosilicate
compound with numerous excellent properties, such as non-
toxicity, high porosity, good thermal stability, high ion exchange
capability, functional molecular sieve, and environmental friendli-
ness [1–3]. It has been extensively used as detergent builders and
water softeners for substitution of sodium tripolyphosphate. More-
over, zeolite NaA has found widespread applications in both labo-
ratories and industries [4,5]. Zeolite A was normally synthesized by
pure chemical grade reagents, such as sodium silicate, silica gels
and aluminate [6]. Recently, concerns about energy consumption,
carbon economy and production costs have called the attention
of researchers to seek cheaper raw materials for zeolite synthesis
[7,8]. Hence, many studies have been published on the synthesis
of zeolite A from nature minerals such as kaolin [9–12], diatomite
[13], and halloysite [14]; as well as industrial and agricultural
wastes such as fly ash [15–17], coal gangue [18], and rice husk [19].
⇑ Corresponding author.
variety of igneous and metamorphic rocks and in some sedimen-
tary rocks [20,21]. The mineral has wide applications in the glass,
ceramic and cement industry [22]. However, synthesis of zeolite
A from K-feldspar is seldom reported. Moreover, in the process of
synthesis of zeolite A, the insoluble potassium can be extracted
from K-feldspar and it is very important for China, because source
of soluble potassium are rare in China.
When used as the stating materials for synthesizing zeolites, K-
feldspar must be pretreated to get active SiO2 and Al2O3. Our pre-
vious work had shown that kalsilite obtained on heating K-feldspar
in KOH or mixed KOH–NaOH solution was soluble in acid solution,
and it was easier to get active SiO2 and Al2O3 from kalsilite [23,24].
The aim of this study was to carry out an inspection of the crystal-
lization behavior of zeolite A from pretreated K-feldspar. The prod-
ucts and intermediates were characterized by means of X-ray
diffraction (XRD), wet chemistry analysis, Fourier Transform Infra-
red spectroscopy (FTIR), 29Si and 27Al magic-angle-spinning
nuclear magnetic resonance (29Si MAS-NMR and 27Al MAS-NMR)
and scanning electron microscope (SEM). The crystallization mech-
anism was discussed.

http://dx.doi.org/10.1016/j.apt.2015.11.011
0921-8831/Ó 2015 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.

Please cite this article in press as: S. Su et al., Hydrothermal synthesis of zeolite A from K-feldspar and its crystallization mechanism, Advanced Powder
Technology (2015), http://dx.doi.org/10.1016/j.apt.2015.11.011
2 S. Su et al. / Advanced Powder Technology xxx (2015) xxx–xxx

2. Materials and methods Table 1

Chemical compositions of the obtained AS (mass fraction, wt.%).

2.1. Materials Sample SiO2 Al2O3 Fe2O3 MgO CaO Na2O K2O LOI
AS 39.87 31.42 0.95 0.17 0.46 0.00 0.63 24.56
The K-feldspar ore used in this work was collected from Moun-
tain Changling, Shaanxi Province, China. Its main chemical compo-
sition was as follows: SiO2 65.00 wt.%, Al2O3 17.26 wt.%, Fe2O3 areas of the peaks appearing at 2h = 7.2°, 10.3°, 12.6°, 16.2°, 21.8°,
1.20 wt.%, MgO 0.84 wt.%, CaO 0.61 wt.%, Na2O 1.09 wt.%, and 24°, 26.2°, 27.2°, 29.9°, 31.1°, 33.4° and 34.2° of the test sample to
K2O 13.92 wt.%, and its main crystal phase was microcline (Fig. 1 the summation of integrated peak areas of the same peaks in
(a)). All chemical reagents (NaOH, KOH, H2SO4) used were analyt- the commercial zeolite A [25], the crystallinity was calculated by
ically pure and purchased from Beijing Chemical Reagent Ltd. Eq. (1):
Commercial-grade zeolite A was purchased from Beijing Chemical  P 
Reagent Ltd. integrated peak areas of sample
%Crystallinity ¼ P
integrated peak areas of commercial zeolite
2.2. Experimental  100
ð1Þ
2.2.1. Pretreated of K-feldspar
The K-feldspar ore was crushed and grinded until most of par- FTIR spectra of the samples were recorded with a NICOLET 750
ticles smaller than 75 lm in size. To destroy the crystal structure (NICOLET) spectrometer in KBr pellet. The 29Si MAS-NMR spec-
of microcline, the K-feldspar powders were first decomposed with troscopy measurements were carried out in a Bruker AvanceIII
KOH solution at 280 °C, and then the solid products were dissolved 400 M spectrometer with a pulse length of 4.0 ls, recycle delay
by H2SO4 solution. After KOH decomposition and acid dissolution, time of 3 s and resonance frequency of 79.3 MHz. The chemical
aluminosilicate (AS) with a higher chemical activity was acquired. shifts are reported from tetramethylsilane. The 27Al magic angle
Table 1 shows the chemical compositions of the AS. Since the Si/Al spinning nuclear magnetic resonance (MAS NMR) measurements
molar ratio in the AS is around 1, additional Si- or Al-sources are were measured at 104.0 MHz with a pulse length of 3.0 ls and a
not required. According to the results of XRD analysis of the K- recycle delay time of 1 s, using 1.0 mol/L Al(NO3)3 aqueous solution
feldspar before and after pretreated (Fig. 1), the obtained AS sam- as the reference solution. The morphologies of the samples were
ple shows the X-ray amorphous feature without any sharp crys- observed by means of SEM (LEO-1450). The chemical compositions
talline diffraction peak, suggesting the poor binding capability of sample were characterized by wet chemistry analysis. The con-
between Si- and Al-. tent of SiO2 in the sample was determined by polyethylene oxide
dehydration method, the content of Al2O3 was determined by
2.2.2. Synthesis of zeolite A EDTA complexometric, the content of Fe2O3 was determined by
The obtained AS was added into 3.0 M NaOH solution with the sulfosalicylic acid spectrophotometric method, the content of
solid to liquid ratio (g/mL) of 1:10 under stirring. After stirring for CaO and MgO was determined by EDTA complexometric, and the
15 min, the reaction mixture was transferred into a Teflon-lined content of K2O and Na2O was determined by flame photometric
stainless steel autoclave for crystallized at 373 K for various times. method.
After hydrothermal treatment, the autoclave was quenched in cold
water. The solid product was filtered out, washed with deionized 3. Results and discussion
water, and dried at 90 °C for 12 h.
3.1. Synthesis of zeolite A
2.3. Characterization
The synthesis of zeolite A depends on the rate of gel dissolution,
The XRD patterns of the samples were collected using a D/Max the number and distribution of nuclei in prepared initial gel, and
2500 X-ray diffractometer operated at 40 kV and 10 mA with the crystal growth rate during hydrothermal treatment [5]. The
nickel filtered Cu Ka radiation, in the 2h range of 5–50°, steps of effect of the crystallization times on the formation of zeolite A
0.02° and scanning speed of 8°/min. The degree of crystallinity
was estimated by taking the ratio of summation of integrated peak

Fig. 1. XRD patterns of the K-feldspar ore (a) and the obtained AS sample (b). Fig. 2. XRD patterns of the products prepared at 373 K for various reaction times.

Please cite this article in press as: S. Su et al., Hydrothermal synthesis of zeolite A from K-feldspar and its crystallization mechanism, Advanced Powder
Technology (2015), http://dx.doi.org/10.1016/j.apt.2015.11.011
 S. Su et al. / Advanced Powder Technology xxx (2015) xxx–xxx
was investigated at 373 K, and the XRD patterns were shown in
Fig. 2. The products prepared from the obtained AS were in the
form of amorphous sodium aluminum silicate and change to a
crystalline structure when they were subjected to hydrothermal
treatment. The crystallinity of zeolite A increased with increasing
time, and then the diffraction intensities of zeolite A increased to
the optimum value in about 3 h of the reaction time. The hydroxyl
sodalite started to appear at 4 h and its diffraction intensity
increased with increasing reaction time. The zeolite A particles
were mostly transformed into hydroxyl sodalite after 8 h of crys-
tallization. The thermodynamic stability of zeolite A was less than
that of hydroxyl sodalite, as a result, the zeolite A formed in the
first step of the crystallization process spontaneously transformed
into thermodynamically more stable hydroxyl sodalite. This result
accords with Oswald’s rule of successive transformations reported
in other literatures [26]. It is clear that controlling crystallization
time is very important to maintain purity of the synthetic zeolite
A samples from pretreated K-feldspar.
The effect of the crystallization times on the percentage crys-
tallinity of zeolite A was shown in Fig. 3. When the reaction time
was less than 1 h, the percentage crystallinity of zeolite A was
increased very slowly with the elongation of reaction time. After
1 h of hydrothermal treatment, the rate of formation of zeolite A
was increased rapidly. The percentage crystallinity of zeolite A
reached the optimal yield of around 87% at 3 h of reaction time.
After 4 h of hydrothermal treatment, the percentage crystallinity
of zeolite A reached to 89%, while hydroxyl sodalite started to
appear in the crystalline phase (Fig. 2). After 6 h of reaction time,
zeolite A was transformed into more stable phase hydroxyl soda-
lite and the percentage crystallinity of zeolite A dropped to 63%.
The chemical compositions of the products prepared at 373 K
for various reaction times were list in Table 2. The reaction mixture
after stirring for 15 min but before crystallization process was
marked for NA-0. Compared to the AS, the mass fractions of SiO2
and Al2O3 in NA-0 decreased, indicating that the AS dissolved in
NaOH solution; the mass fraction of Na2O increased to 8.79 wt.%,
indicating the formation of sodium aluminum silicate gel. In the
hydrothermal treatment process, the mass fractions of Fe2O3 in
the solid products were continuous decreased, demonstrating that
the Fe2O3 was transferred from solid to liquid. Wang et al. [27]
found that the Fe was constantly transferred from solid phase to
liquid phase in process of synthesized zeolite A from metakaolinite,
when they used Fe element in the calcined kaolin as tracer.
Basaldella [28] found the content of Fe2O3 in the products were
lower than that in the raw materials, when prepared zeolite A from
Fig. 3. The crystallinity of zeolite A prepared at 373 K for various reaction times.
Please cite this article in press as: S. Su et al., Hydrothermal synthesis of zeolite A from K-feldspar and its crystallization mechanism, Advanced Powder
Technology (2015), http://dx.doi.org/10.1016/j.apt.2015.11.011
3
Table 2
Chemical compositions of the products prepared at 373 K for various reaction times.
Samples Crystallization SiO2/wt. Al2O3/ Fe2O3/ Na2O/
time/h % wt.% wt.% wt.%
NA-0 – 39.29 28.01 0.99 8.79
NA-1 1 37.54 28.05 0.85 19.51
NA-2 2 36.14 27.25 0.73 18.08
NA-3 3 34.95 26.84 0.60 19.32
NA-4 4 34.82 26.44 0.63 18.25
kaoline with different Fe2O3 contents. These results are agreement
with the result found in this study.
Fig. 4 displays the SEM images of the AS and the products crys-
tallized for 1 h, 2 h, 3 h, 4 h and 6 h, respectively. The AS obtained
from K-feldspar was blocks with no fixed shapes (Fig. 4(a)). The
sample crystallized for 1 h shows only the spherical particles with
the diameter of around 200 nm, indicating that the zeolite A has
not begun to crystallization and 0–1 h was the nucleation stage.
The cubic shape of zeolite A coupled with some incomplete
unformed crystals were observed after crystallization for 2 h, sug-
gesting that spherical particles were aggregated into cubic mor-
phological zeolite A. Moreover, the spherical particles were
gradually decreased as the crystallization time increased. After
3 h, the spherical particles were almost disappeared and the
amount of cubes was significantly increased. The chamfered-
edged cubes with a size around 3 lm were displayed at 4 h, and
some small cubes began to grow in the face of large crystals. This
is due to the zeolite crystal surface adhesion with many nanopar-
ticles and the emergence of secondary nucleation; so that in the
crystal surface which original stop growth opens up new growth
points, and these growing points rapid grow with increasing reac-
tion time [29]. After 6 h, spherical particles of hydroxyl sodalite
grew out onto the surface of well-developed cubes of zeolite LTA
displaying fluorite-type interpenetration-twinning, which indi-
cated that zeolite A is a thermodynamically metastable phase that
was successively replaced by more stable phases like hydroxyl
sodalite. The observed morphologies in this work are similar to
those reported in previous studies [30,31].
The FTIR spectra of the AS and the products crystallized at
100 °C for 1 h, 2 h, 3 h and 4 h were taken and given in Fig. 5,
respectively. All the samples exhibit absorption bands around
3500 cm
1 and 1650 cm
1 assigning to O–H vibrations of the
absorbed water. The vibrational bands at 1050 cm
1 and
600 cm
1, which belonged to the AS, gradually disappeared along
with hydrothermal process. The bands around 1000 cm
1,
700 cm
1 and 447 cm
1, which belonged to sodium aluminosili-
cate gels, appeared when the mixture crystallized for 1 h. These
bands were due to the asymmetric stretching vibration of internal
tetrahedra, the symmetric stretching vibration and the bending
vibration modes of T–O bonds in TO4 tetrahedra (where T = Si or
Al), respectively [15]. The absorption band at 1050 cm
1 of Si–O–
Si bond in the AS was shifted to 991 cm
1 after hydrothermal treat-
ment for 1 h, which indicated that the octahedral Al in the AS
transformed into tetrahedral Al in the sodium aluminosilicate gels,
and part of tetrahedral Al combined with Si–O–Si bond forming Si–
O–Al bond [32]. The band at 554 cm
1 assigned to D4R vibration
which was the major secondary building unit of zeolite A, appeared
when the crystallization time reached to 2 h. Furthermore, the
554 cm
1 band was increased with increasing crystallization time.
This result indicated that zeolite A started to crystallize after 2 h
hydrothermal treatment, and this was agreement with the XRD
result.
Generally, a fully condensed Si atom connected via oxygen
bridge to m Al atoms is labeled as Q4 (mAl), when m varies between
1 and 4, likewise a fully condensed Si atom connected to four Si
4 S. Su et al. / Advanced Powder Technology xxx (2015) xxx–xxx

Fig. 4. SEM images of the AS (a) and the products crystallized at 373 K for 1 h (b), 2 h (c), 3 h (d), 4 h (e) and 6 h (f).

Fig. 6. 29Si MAS NMR spectra of the AS (a) and the products crystallized at 373 K for
Fig. 5. FTIR spectra of the AS (a) and the products crystallized at 373 K for 1 h (b), 1 h (b), 2 h (c), 3 h (d) and 4 h (e).
2 h (c), 3 h (d) and 4 h (e).

obtained from K-feldspar consists of a broad resonance centered at

atom is denoted as Q4 (0Al). The 29Si MAS NMR spectra of the AS
100 ppm, which was characteristic of Si linked to four other Si
and the products crystallized at 100 °C for 1 h, 2 h, 3 h and 4 h were atoms (Q4 (0Al)) in silica polymorphs and indicated the presence
shown in Fig. 6, respectively. The 29Si MAS NMR spectrum of the AS of amorphous silica [33]. Simultaneously, a small shoulder at about

Please cite this article in press as: S. Su et al., Hydrothermal synthesis of zeolite A from K-feldspar and its crystallization mechanism, Advanced Powder
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 S. Su et al. / Advanced Powder Technology xxx (2015) xxx–xxx

76.51 ppm appears, attributable to Q3 (3Al) linkage generated by
the substitution of Al for Si in the tetrahedral position [34]. The 29Si
MAS NMR spectrum of the sample crystallized for 1 h has two
incomplete split resonances one at
87.93 ppm, the other at

84.37 ppm. The former is attributed to Si atom in Q4 (4Al) envi-
ronment, and the latter is ascribed to four-member ring and b cage
suggesting that the sodium aluminosilicate gel contains a large
number of four-member ring and b cage [35]. The typical 29Si
MAS NMR peak for zeolite A, centered at
88 ppm, was already
quite clear when the crystallization time reached to 2 h and
becomes sharper with increasing crystallization time, indicating
the increasing degree of lattice order of zeolite A [36].
The 27Al MAS NMR spectra of the AS and the products crystal-
lized at 100 °C for 1 h, 2 h, 3 h and 4 h were given in Fig. 7,
respectively. The 27Al MAS NMR spectrum of the AS obtained from
K-feldspar consists of two broad resonances at 4.34 ppm, assigned
to 6-coordinated Al and another at 55.88 ppm attributed to 4-
coordinated Al. The broad and asymmetrical peak shapes of the
AS show its disordered structure [36,37]. The result from 27Al
MAS NMR analysis is consistent with that from 29Si MAS NMR.
Both show that the obtained AS is far more likely a hybrid gel com-
posed of a single-phase gel and a diphasic gel. After hydrothermal
treatment, the chemical shift at 4.34 ppm was disappeared,
implying that the 6-coordinated Al completely transformed to
4-coordinated Al. The sample crystalized for 1 h exhibits only
one resonance at 58.58 ppm, implying that the Al was tetrahedral
connected to the framework (Al(OSi)4). With increasing crystalliza-
tion time, the full width at half maximum (FWHM) of resonance
around 58 ppm gradually decreased, indicating that the crys-
tallinity of the products increased. Urbanova et al. [38] also found
the FWHM value of 27Al MAS NMR spectrum decreased when
amorphous geopolymers transformed to crystalline phase.
3.2. The crystallization mechanism of zeolite A
The framework structure of K-feldspar was collapsed when it
suffered from KOH decomposition followed by H2SO4 dissolution,
resulting in the formation of amorphous aluminosilicate (AS) and
thus endowing the AS with outstanding zeolitization reactivity.
When the obtained AS treated with NaOH solution, it is dissolved
forming [SiO2(OH)2]2
and Al(OH)4
, and the process can be
described as:
SiðOHÞ4 þ 2NaOH ! ½SiO2 ðOHÞ2 
2

þ 2Naþ þ 2HO2
AlðOHÞ3 þ NaOH ! AlðOHÞ
4 þ Na þ
Fig. 7. 27Al MAS NMR spectra of the AS (a) and the products crystallized at 373 K for
1 h (b), 2 h (c), 3 h (d) and 4 h (e).
Please cite this article in press as: S. Su et al., Hydrothermal synthesis of zeolite A from K-feldspar and its crystallization mechanism, Advanced Powder
Technology (2015), http://dx.doi.org/10.1016/j.apt.2015.11.011
5
Through the polymerization of [SiO2(OH)2]2
and Al(OH)4
, var-
ious polymeric structures of aluminosilicates (polyatomic rings)
were formed, and the polyatomic rings around Na+ were further
aggregated to form b cage followed by forming the nuclei. After
1 h hydrothermal treatment, the AS has completely dissolved,
and abundant nuclei were formed in the sodium aluminosilicate
gel. The process can be described as:
2


2½SiO2 ðOHÞ2  þ 2½AlðOHÞ4  ! S4R þ 4H2 O
2


3½SiO2 ðOHÞ2  þ 3½AlðOHÞ4  ! S6R þ 6H2 O
6S4R þ 8S6R ! b cage
B cage þ D4R ! a cage
With increasing crystallization time, the synthetic crystals are
gradually formed. The relative crystallinity reaches its maximum
when crystallization time reached to 3 h. The mechanism of syn-
thesis of zeolite A from AS can be described by three main stages:
(1) the dissolution of amorphous aluminosilicate releasing [SiO2(-
OH)2]2
and Al(OH)4
; (2) the formation sodium aluminosilicate
gel as zeolite precursor; (3) the crystallization of zeolite A. The syn-
thesis of zeolite A from pretreated K-feldspar was liquid phase
transformation mechanism.
4. Conclusions
The K-feldspar transformed into amorphous aluminosilicate
(AS) when it suffered from KOH decomposition followed by
H2SO4 dissolution. The effects of reaction times on the conversion
of the obtained AS to zeolite A were investigated. During the first
hour of the crystallization stage, the AS dissolved thoroughly in
NaOH solution, and sodium aluminosilicate gel with abundant
crystal nucleus was formed. With increasing crystallization time,
the synthetic crystals were gradually formed. The relative crys-
tallinity of pure zeolite A reaches its maximum when crystalliza-
tion time reached to 3 h. An excess time resulted in further
dissolution of zeolite A and replacement by more stable phases –
hydroxyl sodalite. The mechanism of synthesis of zeolite A from
AS can be described by three main stages: (1) the dissolution of
amorphous aluminosilicate releasing [SiO2(OH)2]2
and Al(OH)4
;
(2) the formation sodium aluminosilicate gel as zeolite precursor;
(3) the crystallization of zeolite A.
Acknowledgements
This work was supported by the National Key Technologies
Research and Development Program for 11th Five-year Plan
(2006BAD10B04) and the National Natural Science Foundation of
China (Grant No. 51274015). The authors also thank Blue-sky Tech-
nology Corporation for the financial supports.
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