Journal of the Association of Arab Universities for Basic and Applied Sciences (2013) xxx, xxx–xxx

University of Bahrain
Journal of the Association of Arab Universities for
Basic and Applied Sciences
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ORIGINAL ARTICLE

Synthesis and characterization of zeolite A by

hydrothermal transformation of natural Jordanian kaolin
a,* b
Mousa Gougazeh , J.-Ch. Buhl

a
Natural Resources and Chemical Engineering Department, Faculty of Engineering, Tafila Technical University, P.O. Box 179
Tafila 66110, Jordan
b
Institute of Mineralogy, Leibniz University Hannover, Callinstr. 3, D-30167 Hannover, Germany

Received 6 March 2012; revised 4 March 2013; accepted 31 March 2013

KEYWORDS Abstract The synthesis of zeolite materials by hydrothermal transformation of natural Jordanian
Zeolite A; kaolin in NaOH solutions of various concentrations was investigated at 100 C for 20 h. A mixture
Kaolin; of zeolite A, quartz and hydroxysodalite (HS) was obtained. Zeolite A was the main product with
Metakaolin; the NaOH concentrations of 1.50–3.50 M, which was confirmed by XRD, IR and SEM. Zeolite A
Hydrothermal synthesis; can be obtained from natural kaolin under the conditions applied showing that metakaolinization
Hydroxysodalite can be observed at 650 C which is much lower than the temperatures given in the previous works,
700–950 C. The products obtained from the experiments were characterized by X-ray diffraction
(XRD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM).
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1. Introduction usually mono- and bi-valent metal ions and/or their combina-
tions (Engelhardt and Michel, 1987; Takaishi et al., 1995; Earl
Zeolites are crystalline, microporous, hydrated aluminosili- and Deem, 2006). In accordance with the Loewenstein’s rule
cates of alkaline or alkaline earth metals. The frameworks (Loewenstein, 1954), Al–O–Al bonds do not exist in alumino-
are composed of [SiO4]4 and [AlO4]5 tetrahedra, which cor- silicate frameworks of zeolite. Instead of the tetrahedrally
ner-share to form different open structures. Negative charge of bonded atoms Si and Al, so-called ‘‘T-atoms’’, others such
lattice is compensated by the positive charge of cations located as P, Ga, Ge, B, Be, etc. can exist in the framework as well
at specific positions of zeolite framework (Bekkum et al., 1991; (McCusker and Baerlocher, 2001; Takaishi et al., 1995).
Breck, 1974). In most of zeolites the compensating cations are The synthesis of zeolites in forms suitable for industrial
applications is of great importance. The first synthesis of zeo-
lite was attempted by St. Claire-Deville in 1862. Barrer’s pio-
* Corresponding author. Tel.: +962 776731158. neering work in 1948 demonstrated that a wide range of
E-mail addresses: [email protected] (M. Gougazeh), zeolites could be synthesized from aluminosilicate gels.
[email protected] (J.-Ch. Buhl). At present, synthetic zeolites are used commercially more
Peer review under responsibility of University of Bahrain. often than natural zeolites due to the purity of crystalline prod-
ucts and the uniformity of particle sizes (Breck, 1974; Szoztak,
1998). However, the preparation of synthetic zeolites from
Production and hosting by Elsevier chemical sources of silica and alumina is expensive. Such costs

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Please cite this article in press as: Gougazeh, M., Buhl, J.-C. Synthesis and characterization of zeolite A by hydrothermal trans-
formation of natural Jordanian kaolin. Journal of the Association of Arab Universities for Basic and Applied Sciences (2013),
http://dx.doi.org/10.1016/j.jaubas.2013.03.007
2 M. Gougazeh, J.-Ch. Buhl

may be reduced by the use of clay minerals, volcanic glasses

Table 1 Properties of natural Jordanian kaolin.
(perlite and pumice), rice husks, diatoms, fly ash or paper
sludge ash as starting materials (Adamczyk and Bialecka, Chemical constituents in wt.% [X-ray fluorescence analysis (XRF)]
2005; Querol et al., 1997; Saija et al., 1983; Tanaka et al., SiO2 53.86
TiO2 0.74
2004; Walek et al., 2008; Wang et al., 2008). Zeolite has also
Al2O3 32.45
been developed by the transformation of one zeolite type into
Fe2O3 0.65
other zeotypes (Rios et al., 2007; Sandoval et al., 2009). MnO 0.01
Previous work has shown that kaolin is not stable under MgO 0.08
highly alkaline conditions and different zeolitic materials can CaO 0.13
form, and that kaolin is usually used after calcinations to ob- Na2O 0.06
tain a more reactive phase (metakaolin). After dehydration K2O 0.54
(endothermic dehydroxylation), kaolin is transformed into P2O5 0.12
amorphous metakaolin (Fialips, 1999; Gougazeh and Buhl, Loss on ignition (LOI) 11.21
2010; Smykatz-Kloss, 1975). Raw kaolin and metakaolin have Total 99.85
SiO2/Al2O3 ratio 1.65
been used as the Al and Si sources for synthesis of zeolite Lin-
Particle size distribution in wt.% [Atterberg method]
de Type A, X, Y, P, 4A, NaA, KI, cancrinite, sodalite,
Microns 63–45 lm 1.2
hydroxysodalite, faujasite, phillipsite, chabazite and several Microns 45+6 lm 5.2
other types of zeolites (e.g., Akolekar et al., 1997; Alberti Microns 6+2 lm 20.6
et al., 1994; Barnes et al., 1999a, 1999b, 1999c; Bauer and Ber- Microns 2 lm 73.0
ger, 1998; Bauer et al., 1998; Buhl, 1991; Buhl et al., 2000a,b; Quantitative analysis in wt.% [using XRD (Rietveld method with
Buhl and Loens, 1996; Covarrubias et al., 2006; Dudzik and DIFFRACplus TOPAS software) + XRF]
Kowalak, 1974; Gualtieri et al., 1997; Lin et al., 2004; Loiola Kaolin 72.0
et al., 2012; Marcelo et al., 2007; Mon et al., 2005; Rees and Quartz 27.0
Chandrasekhar, 1993; Sanhueza et al., 1999; Vilma et al., Others 1 .0
Brightness (% ISO) 82.73
1999; Zhao et al., 2004.
NaA Zeolite is of great industrial importance due to its
molecular sieving, ion exchange and water adsorption proper- mixtures were prepared separately with gentle stirring and then
ties. With the molar ratio Si/Al nearly equal to one, kaolin is distributed among the required number of autoclaves. The
an ideal raw material for preparing NaA zeolite. Kaolin was autoclaves were kept in a conventional air oven at 100 C for
one of the most versatile industrial minerals and was used 20 h at autogenous pressure. The synthesized products were
extensively for many applications (Murray, 1991). The synthe- washed with distilled water three times and then dried at
sis of NaA zeolite from kaolin source was started from the 80 C for 24 h.
1970s (Breck, 1974; Barrer, 1978) by the hydrothermal reaction
of dehydroxylated kaolin with sodium hydroxide solution. 2.3. Characterization techniques
No attempt has been made previously to produce zeolite
type A from natural Jordanian kaolin. In this work, Zeolite
The original kaolin sample was dispersed in deionized water
A was hydrothermally synthesized from Jordanian kaolin,
and shaken mechanically and then sieved through a 63 lm
and the effect of NaOH concentration (1.0, 1.5, 2.0, 2.5, 3.5
sieve. The portion of the <63 lm fraction (98 wt.% of the
and 4 M NaOH) was investigated. The synthesized products
original kaolin sample) was allowed to settle in an Atterberg
were characterized by X-ray diffraction (XRD) scanning elec-
cylinder according to Stock’s law (Jachson, 1975) to separate
tron microscopy (SEM) and Fourier transform infrared (FT-
the size fractions of 63–45 lm, 45–6 lm, 6–2 lm and <2 lm
IR) spectroscopy.
(Gougazeh and Buhl, 2010).
The chemical composition of kaolin was determined using a
2. Experimental Bruker S4 wavelength X-ray dispersive fluorescence spectrom-
eter (WDXRFS), with a Rh X-ray tube. Phase characterization
2.1. Raw materials and chemical reagent was carried out by X-ray diffraction (XRD) using a Bruker
AXS D4 ENDEAVOR diffractometer using Ni filtered Cu
The natural well crystallized kaolin (a combined source for sil- Ka radiation at 40 kV and 40 mA. The measurements were
ica and alumina), from the kaolin deposits in south Jordan carried out with a step width of 0.03 2h and scan rate of 1 s
(Gougazeh and Buhl, 2010) was used for the present study. per step. The diffraction data were analyzed by the Rietveld
The sodium hydroxide used was of analytical grade. Properties method using DIFFRACplus TOPAS software. Fourier trans-
of Jordanian kaolin are shown in Table 1. Metakaolin was ob- form infrared spectra (FTIR) were obtained by using a Bruker
tained by calcining kaolin in a muffle furnace at 650 C for 2 h. IFS66v FTIR spectrometer in 4000–400 cm 1 regions by the
KBr wafer technique. The morphology was characterized by
2.2. Hydrothermal synthesis a scanning electron microscope (SEM) at 20 kV, using a JEOL
JSM-6390A model.
Metakaolins were separately mixed with NaOH solutions of
various concentrations, 1.0, 1.5, 2.0, 2.5, 3.0, 3.5 and 4.0 M. 3. Results and discussion
The samples were initially gently stirred for 10 min at room
temperature for homogenization. The solid/liquid ratio of The kaolin used was fully characterized (mineralogical and
metakaolin to alkaline solution was 1.0 g/25 ml. The reaction chemical composition, thermal behavior, particle size distribu-

Please cite this article in press as: Gougazeh, M., Buhl, J.-C. Synthesis and characterization of zeolite A by hydrothermal trans-
formation of natural Jordanian kaolin. Journal of the Association of Arab Universities for Basic and Applied Sciences (2013),
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Synthesis and characterization of zeolite A by hydrothermal transformation of natural Jordanian kaolin 3

K K Qz

Qz
Intensity

K
K
K Qz
Qz KK
M Fs Qz K
K KK K
K a
K

5 10 15 20 25 30 35 40 45 50 55 60
o2θ (CuKα)

Figure 1 XRD patterns of Jordanian kaolin (a) and metakaolin at 650 C (b).

tion, and so on) in previous study (Gougazeh and Buhl, 2010). kaolin produces structural changes of this mineral, promoting
The grain size analysis of bulk kaolin sample was separated by its reactivity to synthesize zeolitic materials.
Atterberg methods. The quantitative analysis of the mineral The phase composition of the synthesized zeolite material
content of the natural Jordanian kaolin has been worked out which was obtained from the activated kaolin samples reacted
by a combination of XRD (Rietveld method using DIF- with 1.0, 1.5, 2.0, 2.5, 3.0, 3.5 and 4.0 NaOH solutions was
FRACplus TOPAS software) and XRF investigations (Gou- analyzed by X-ray diffractometry (XRD). Quantitative analy-
gazeh and Buhl, 2010). sis of the obtained zeolite products was performed using the
The physical, chemical and mineralogical properties of the Rietveld method with DIFFRACplus TOPAS software and
kaolin under study are presented in Table 1. the exact percentage of each phase was calculated (Table 2).
The SiO2/Al2O3 ratio is found to be 1.65. The properties of The results suggest that the synthesized zeolite products con-
the reaction intermediates and products were determined by tain zeolite A as the major constituent phase, whereas
various techniques to give the following results. hydroxysodalite (HS) and quartz were found as minor phases
(Table 2).
3.1. X-ray diffraction analysis
Fig. 2 illustrates the X-ray powder diagrams of metakaolin
and the reaction products which were obtained from the acti-
The XRD patterns of the natural (unheated) kaolin and vated kaolin samples reacted with 1.0, 1.5, 2.0, 2.5, 3.0, 3.5 and
metakaolin are shown in Fig. 1. In accordance with XRD data, 4.0 M NaOH solutions at 100 C for 20 h and the commercial
the starting material contains 72 wt.% of kaolin, 27 wt.% of zeolite A sample (Fluka No. 69836) given for comparison. The
quartz and minor amount (about 1 wt.%) of other compo- formation of synthesized zeolite A in the products was
nents (see Table 1). Kaolinite is identified by its characteristic
X-ray diffraction peaks at 12.34 and 24.64 2h as has been re-
ported in previous studies (Gougazeh and Buhl, 2010; Zhao Table 2 Phase composition of the obtained zeolite products
et al., 2004). The XRD pattern of metakaolin obtained by (wt.%) was performed using the Rietveld method with DIF-
heating the kaolin for 3 h at 650 C resembled others, except FRACplus TOPAS software.
for the peaks due to admixed impurities. After thermal treat- NaOH(M) Quartz Hydroxysodalite Zeolite Metakaolin Total
ment, the XRD patterns exhibit a significant change in com- (HS) A (amorphous)
parison to the pattern of untreated kaolin, which was 1.0 30.2 0.0 39.7 30.1 100.0
characterized by disappearance of the diffraction peaks of kao- 1.5 25.6 4.2 70.2 0.0 100.0
lin, accompanied by the appearance of amorphous aluminosil- 2.0 24.3 3.8 71.9 0.0 100.0
icate. Metakaolin is of amorphous structure and the highest 2.5 18.0 7.8 74.2 0.0 100.0
diffraction peaks correspond to the presence of quartz 3.0 16.9 8.5 74.6 0.0 100.0
(SiO2), which is very common (Fig. 1b). The only crystalline 3.5 16.3 15.4 68.2 0.0 100.0
4.0 15.4 33.8 50.8 0.0 100.0
phase in metakaolin is quartz. Therefore, the activation of

Please cite this article in press as: Gougazeh, M., Buhl, J.-C. Synthesis and characterization of zeolite A by hydrothermal trans-
formation of natural Jordanian kaolin. Journal of the Association of Arab Universities for Basic and Applied Sciences (2013),
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4 M. Gougazeh, J.-Ch. Buhl

A
A A A A A
A A A A i

A
S S
A A
A A A
A Qz A S AS
A A Qz h

f
Intensity

5 10 15 20 25 30 35 40 45 50 55 60
o
2θ (Cu Kα)

Figure 2 XRD patterns of zeolite A and associated phases obtained by hydrothermal synthesis (a) unreacted metakaolin, (b) 1.0 M
NaOH, (c) 1.5 M NaOH, (d) 2.0 M NaOH, (e) 2.5 M NaOH, (f) 3.0 M NaOH, (g) 3.5 M NaOH, and (h) 4.0 M NaOH, (i) commercial
zeolite A. A: zeolite A, S: hydroxysodalite, Qz: quartz.

detected, by comparing the d-values of the products obtained 13.96, 19.98, 24.42, and 35.00. Our results showed that
with JCPDS (Joint Committee on Powder Diffraction quartz was also observed in the synthesized zeolitic material
Standards) data of card No.: 39-222 and d-values of commer- in a minor amount (Table 2).
cial zeolite A sample. The most important change observed in
the XRD patterns is the appearance of the characteristic peaks 3.2. FTIR analysis
of zeolite A. The synthesized products matched the character-
istic peaks of zeolite A at 2h values of 7.2, 10.3, 12.6, 16.2, Fig. 3 illustrates the IR spectra of the unreacted and reacted
21.8, 24, 26.2, 27.2, 30, 30.9, 31.1, 32.6, 33.4 and 34.3 metakaolin in various alkalinities and the commercial zeolite
that were reported by Treacy and Higgins (2001). Fig. 2b A sample (Fluka No. 69836) given for comparison. The broad
shows the XRD pattern of the reaction product which was ob- band of metakaolin in the spectral range from about 925 cm 1
tained from the thermally activated kaolin sample with 1.0 M to about 690 cm 1 (spectrum a in Fig. 3), assigned to Al–O
NaOH solution, zeolite A and quartz were determined as the bonds in Al2O3 does not appear in the zeolite products (spectra
dominant mineral phases with a significant amount of metaka- b–g in Fig. 3). The 1080 cm 1 band of metakaolin was shifted
olin (amorphous) and no hydroxysodalite was observed (Ta- to 1000 cm 1 (1035, 1004, 1003, 1001, 1000 and 996 cm 1)
ble 2). The results indicated that the synthesized zeolite (Fig. 3b–h), which could be assigned to antisymmetric stretch-
products obtained from 1.5–3.5 M NaOH concentrations con- ing of T–O bonds (T = Si or Al) in aluminosilicates with zeo-
tain zeolite A as the major constituent phase, whereas lite structure. SiO2 and Al2O3 are transformed to
hydroxysodalite (HS) and quartz were found as minor phases aluminosilicates during the reaction between metakaolin and
(Fig. 2c–h). According to the experimental results and the NaOH. Their vibration bands in the IR spectrum are replaced
XRD data, intensities of the HS peaks in the pattern increase by a single band around 1000 cm 1, characteristic of Si–O–Al
with increasing NaOH concentration (Table 2 and Fig. 2). bonds in TO4 tetrahedra (Nesse, 2000). A broad band of week
Fig. 2 and Table 2 show that the greatest quantities of formed intensity, is observed around 553 cm 1, this peak indicates the
zeolite A are essentially the same for the samples reacted with presence of zeolite A band assigning the cubic prism. The band
NaOH concentration between 1.5 and 3.5 M (zeolite A per- at 553 cm 1 could represent the beginning of the crystallization
sisted as the dominant phase) (Fig. 2c–g), with a sudden de- of a zeolite with double rings (Alkan et al., 2005). The bands at
crease at higher base concentrations (>3.5 M) (Fig. 2h), 462 and 662 cm 1 are close to the bands at 462 and 668 cm 1,
during this reaction some zeolite A was converted into which correspond to the internal linkage vibrations of the TO4
hydroxysodalite. Similar observations were made by Singer (T = Si or Al) tetrahedra and to the asymmetric stretching,
and Berkgaut, 1995, Lin and His, 2004, Querol et al., 1997 respectively, of zeolite A.
who found that zeolite A was formed at low base concentra- There are four well-defined peaks at 662, 693, 718 and
tions (<3.5 M) and HS at higher base concentrations. 724 cm 1 in the spectral zone of 650–745 cm 1 (Fig. 3b–h) as-
Hydroxysodalite shows several common peaks located at signed to symmetric T–O–T vibrations of the sodalite frame-

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formation of natural Jordanian kaolin. Journal of the Association of Arab Universities for Basic and Applied Sciences (2013),
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Synthesis and characterization of zeolite A by hydrothermal transformation of natural Jordanian kaolin 5

1003
553

996

3450
462

1650
1000
i

1001
718
Absorbance units

795
h
g
724

1003

1003 e
1004 d
1035
c
1080
396

486

b
795
396

693

300 800 1300 1800 2300 2800 3300 3800 4300

Wavenumber (cm-1)

Figure 3 FTIR spectra of zeolite A and associated phases obtained by hydrothermal synthesis: (a) unreacted metakaolin, (b) 1.0 M
NaOH, (c) 1.5 M NaOH, (d) 2.0 M NaOH, (e) 2.5 M NaOH, (f) 3.0 M NaOH, (g) 3.5 M NaOH, (h) 4.0 M NaOH, and (i) commercial
zeolite A (Fluka No. 69836).

work in good agreement with the peaks of 660, 701 and common to zeolite A and appears as a weak shoulder due to
729 cm 1 for hydroxysodalite zeolite reported by Flaningen the large amount of quartz present in minor amounts.
et al., 1971. The bands in the region of 420–500 cm 1 are re- The IR spectra at 3.0 and 3.5 M NaOH concentrations cor-
lated to internal tetrahedron vibrations of Si–O and Al–O of respond to those presented by Flaningen et al. (1971) for zeolite
sodalite (T–O–T) bending modes of the sodalite framework. A and the commercial zeolite A (Fig. 3i) except for the contri-
There is an important assignment in the range of 1003– bution of impurities such as quartz (Fig. 3f and g). The IR spec-
970 cm 1 with the literature for the characteristic bands be- tra at 4.0 M NaOH (Fig. 3h) showed that the common shoulder
tween 1250 and 950 cm 1 asymmetric stretching vibration for of zeolite A was shifted to 996 cm 1 and with differences in 462,
all the zeolitic materials (Flaningen et al., 1971). The broad 553, 662 cm 1 shoulders compared to other obtained zeolite
band at about 3450 cm 1 and a band at 1650 cm 1 are attrib- products (Fig. 3). Evidentially the obtained product with
uted to zeolitic water (Fig. 3). The IR spectral analysis results 4.0 M NaOH contained a significantly lower portion of zeolite
thus support the XRD inferences. The reference IR wave num- A than any other products obtained by reaction with NaOH
bers were given as 1003, 662, 553 and 462 cm 1 (Markovic concentrations from 1.5 to 3.5 M (Fig. 3) On the other hand,
et al., 2003). The original IR spectrum of zeolite A sample a higher proportion of hydroxysodalite was detected (Table 2),
(Fluka No. 69836) is shown in Fig. 3i. which could account for the decrease in the amount of zeolite A.
The obtained products contain quartz impurities which ob-
scure some of the features of the spectra. The band at about
462 cm 1, which is assigned to tetrahedral T–O (T = Si or 3.3. Scanning electron microscopy (SEM) results
Al) bending vibrations, is common to the starting metakaolin
(Fig. 3a) and to the different obtained products (Fig. 3b–h). Its SEM micrographs (Fig. 4) show the occurrences of the zeolitic
intensity does not change substantially in the course of zeoliti- products obtained after hydrothermal treatment of metakaolin
zation. A band at 553 cm 1, assigned to external linkages, is in various NaOH concentrations, revealing a marked change
characteristic of zeolite A (Flaningen et al., 1971). Weak bands in the morphology of the original surface of the starting mate-
at about 533 and 1035 cm 1 is characteristic of zeolite A, rials. Kaolinite can be recognized by its platy morphology and
which was obtained at 1.0 M NaOH (Fig. 3b). It appears that hexagonal outlines (Fig. 4a). In accordance with the results of
in addition to some zeolite A, this product contains greater un- other analytical methods quartz can be detected even by SEM
changed metakaolin than the other obtained products in each sample (see Table 2).
(Fig. 3c–h), in agreement with the XRD patterns, in which un- Fig. 4(b–h) represents the effect of different NaOH concen-
changed metakaolin was detected together with zeolite A. The trations (1.0, 1.5, 2.0, 2.5, 3.0, 3.5 and 4.0 M NaOH) on zeolite
IR spectra at 1.5 M NaOH (Fig. 3c) were similar to those ob- A formation obtained after activation of metakaolin at 100 C
tained at 2.0 and 2.5 M NaOH concentrations (Fig. 3d and e). for 20 h. According to the experimental results of this work,
In these products, the absorption at about 1003 cm 1 is the observed morphologies are similar to those reported in

Please cite this article in press as: Gougazeh, M., Buhl, J.-C. Synthesis and characterization of zeolite A by hydrothermal trans-
formation of natural Jordanian kaolin. Journal of the Association of Arab Universities for Basic and Applied Sciences (2013),
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6 M. Gougazeh, J.-Ch. Buhl

Figure 4 SEM micrographs showing the occurrence of zeolite A and associated phases obtained by hydrothermal synthesis: (a)
hexagonal platy crystals of untreated kaolin, (b) very well developed cubes of zeolite A and relicts of metakaolin, (c) zeolite A probably
formed before hydroxysodalite (HS), as shown by the occurrence of HS crystals growing at the surface of zeolite A. (d–f) Spheroidal
aggregates of HS that grew out onto the surface of cubic crystals of zeolite A, showing penetration twining, and (g–h) lephispheric
morphology of HS associated to cubic crystals of zeolite.

previous studies (Heller-Kallai and Lapides, 2007; Lapides and hydroxysodalite (HS), as shown by the occurrence of HS crys-
Heller-kallai, 2007) and the data obtained by SEM correlate tals growing at the surface of zeolite A.
and agree with the mineralogical composition of the zeolite Lephispheric morphologies corresponding to HS grew out
products, which was determined through XRD results onto the surface of cubic crystals of zeolite A, which sometimes
(Fig. 2 and Table 2). display interpenetrating twining (Fig. 4d–f), which were ob-
At 1.0 M NaOH concentration, very well developed cubes tained at 2.0–3.0 M NaOH concentrations. Generally, it is pos-
of zeolite A as well as a large amount of metakaolin debris sible to observe the following relationships between these
were observed in the scanned sample (Fig. 4b). At 1.5 M phases: crystal of HS growing at the surface of a cubic crystal
NaOH solution, zeolite A can be identified by its characteristic of zeolite A, aggregates of spheroidal ‘‘cotton-ball’’ structure
cubic morphology (Fig. 4c); it probably formed before of HS along with cubic crystals of zeolite A.

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formation of natural Jordanian kaolin. Journal of the Association of Arab Universities for Basic and Applied Sciences (2013),
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Synthesis and characterization of zeolite A by hydrothermal transformation of natural Jordanian kaolin 7

By increasing the NaOH concentrations from 3.5 to 4.0 M, synthetic spent bayer liquor. Microporous Mesoporous Mater.
SEM micrographs of treated metakaolin show that a predom- 31, 287–302.
inantly lephispheric morphology is typically observed in the Barnes, M.C., Addai-Mensah, J., Gerson, A.R., 1999b. A methodol-
obtained zeolitic products with spheroidal ‘‘cotton-ball’’ mor- ogy for quantifying sodalite and cancrinite phase mixtures and the
kinetics of the sodalite to cancrinite phase transformation. Micro-
phologies for HS (Fig. 4g and h).
porous Mesoporous Mater. 31, 303–319.
Barnes, M.C., Addai-Mensah, J., Gerson, A.R., 1999c. The solubility
4. Conclusions of sodalite and cancrinite in synthetic spent bayer liquor. Colloids
Surf. A Physicochemical and Engineering Aspects 157, 106–116.
Based on the results of XRD, IR and SEM of zeolite A pro- Barrer, R.M., 1978. Zeolites and Clay Minerals as Sorbents and
Molecular Sieves. Academic Press, London.
duced by treating the activated metakaolin from natural Jorda-
Bauer, A., Berger, G., 1998. Kaolin and smectite dissolution rate in
nian kaolin with various concentrations of NaOH at 100 C for
high molar KOH solutions at 35 and 80 C. Appl. Geochem. 13,
20 h, some observations could be summarized as follows: 905–916.
Bauer, A., Velde, B., Berger, G., 1998. Kaolin transformation in high
 The results indicated that the obtained zeolite products con- molar KOH solutions. Appl. Geochem. 13, 619–629.
tain zeolite A as the major constituent phase, whereas Bekkum, V.H., Flanigen, E.M., Jacobs, P.A., Jansen, J.C., 1991.
hydroxysodalite (HS) and quartz were found as minor Introduction to Zeolite Science and Practice, 2nd revised Ed.
phases. With one exception untransformed metakaolin Elsevier, Amsterdam.
occurred only in considerable amounts at 1.0 M NaOH Breck, D.W., 1974. Zeolite Molecular Sieves: Structure, Chemistry and
(Table 2). Although the amount of untransformed metaka- Uses. John Wiley, New York.
Buhl, J.C., 1991. Synthesis and characterization of the basic and non-
olin probably decreases with increasing NaOH concentra-
basic members of the cancrinite-natrodavyne family. Thermochim.
tion. On the other hand, amount of HS increases with the
Acta 178, 19–31.
increasing NaOH concentration, which could account for Buhl, J.C., Loens, J., 1996. Synthesis and crystal structure of nitrate
the decrease in the amount of zeolite A. enclathrated sodalite Na8[AlSiO4]6(NO3)2. J. Alloys Compd. 235,
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phases as impurities coming from the natural kaolin sam- Buhl, J.C., Stief, F., Fechtelkord, M., Gesing, T.M., Taphorn, U.,
ples (see XRD pattern in Fig. 1a). Taake, C., 2000a. Synthesis, X-ray diffraction and MAS NMR
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(TTU) and the German Sciences Foundation ‘‘Deutsche Fors- conditions deformation de la kaolin. These Doct univ Poitiers France.
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Please cite this article in press as: Gougazeh, M., Buhl, J.-C. Synthesis and characterization of zeolite A by hydrothermal trans-
formation of natural Jordanian kaolin. Journal of the Association of Arab Universities for Basic and Applied Sciences (2013),
http://dx.doi.org/10.1016/j.jaubas.2013.03.007
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Please cite this article in press as: Gougazeh, M., Buhl, J.-C. Synthesis and characterization of zeolite A by hydrothermal trans-
formation of natural Jordanian kaolin. Journal of the Association of Arab Universities for Basic and Applied Sciences (2013),
http://dx.doi.org/10.1016/j.jaubas.2013.03.007