Rev. Fac. Ing. Univ. Antioquia N. º74 pp.

213-225, March, 2015

Effect of the melting and aging process on the

synthesis of zeotypes from fly ash

Effect of the fusion and aging process in the synthesis

of zeotypes from fly ash

Jeimer Alexander Lizcano-Head 1, Luis Fernando Avila-Ascanio 1, Carlos Alberto Ríos-Reyes two*, Luz
Yolanda Vargas-Fiallo 1

1 Research Group in Basic and Applied Geology (GIGBA), School of Chemistry,

Universidad Industrial de Santander. Cra 27 Cl 9. AA. 678. Bucaramanga, Colombia.

two Research Group in Basic and Applied Geology (GIGBA), School of Geology.
Industrial University of Santander. Cra 27 Cl 9. AA. 678. Bucaramanga, Colombia.

(Received on August 28, 2013. Accepted on January 20, 2015)

Summary

In this study, the use of a fly ash sample from TERMOPAIPA (Boyacá, Colombia) as a
starting material for the synthesis of zeotypes on a laboratory scale is evaluated
through its transformation by alkaline fusion, using solid NaOH or dissolved in water. ,
followed by aging for 6, 12 and 24 h under static or ultrasound conditions prior to
hydrothermal treatment for 6, 12 and 24 h of reaction. The experimental data reveal
that the method, the alkaline melting state, the temperature and the reaction time
strongly affect the zeotype to be synthesized. Low silica sodium zeotypes were
synthesized, which include NaP1 zeolite, faujasite, and traces of sodalite. The
synthesis of zeotypes from fly ash represents an interesting alternative for the
mitigation of the environmental problem, associated with the disposal of industrial
waste. Therefore, the fly ash-based zeotypes synthesized under optimal experimental
conditions can be used in various applications for the environmental treatment of
waste.

- - - - - - - - - - Keywords: fly ash, aging method, synthesis, zeotypes, fusion

*
Corresponding author: Carlos Alberto Ríos Reyes, email: carios@uis.edu.co

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Abstract

In this study, we evaluate the use of a sample of fly ash from TERMOPAIPA (Boyacá,
Colombia) as the starting material for the synthesis of zeotypes on laboratory scale
through its transforming via alkaline fusion, using solid or water dissolved NaOH,
followed by aging during 6, 12 and 24 h under static or ultrasound conditions prior to
hydrothermal treatment during 6, 12 and 24 h of reaction time. Experimental data
reveal that the method, state of alkaline fusion, temperature and time of reaction
strongly affect the zeotype to be synthesized. Low-silica sodium zeotypes were
synthesized, which include zeoliteNaP1, faujasite, and traces of sodalite. The synthesis
of zeotypes from fly ash represents an interesting alternative for the mitigation of the
environmental problems associated to the disposal of industrial wastes. Therefore,

- - - - - - - - - - Keywords: fly ash, aging method, synthesis, zeotypes, fusion

Introduction
The synthesis of zeolites from by-products of the national coal industry,
such as fly ash (CEVs), by various methods has been receiving much
attention. There are numerous studies carried out in relation to the
synthesis of zeolites from CEVs. The conversion of CEVs into zeolites can
be carried out in a conventional way by hydrothermal crystallization under
alkaline conditions, which has been reported by different authors [1-17].
Recently, the conventional alkaline conversion of these materials has
been improved by using more sophisticated treatments [2, 16-24]. Zeolites
have been used mainly as ion exchangers, molecular sieves, adsorbents
and catalysts. The resulting zeolitic materials have great potential to be
used as high-efficiency and low-cost adsorbents, this is a good application
for environmental problems [25-29]. In this article, we want to demonstrate
how the results obtained from the variation in the fusion method change,
modifying the aging process and using hydrothermal conditions for the
synthesis of different types of zeolites, and from these results obtain the
most crystalline phases . For this reason, the investigation of the synthesis
of zeotypes from CEVs was carried out at the scale of modifying the aging
process and using hydrothermal conditions for the synthesis of different
types of zeolites, and from these results obtain the most crystalline
phases. For this reason, the investigation of the synthesis of zeotypes
from CEVs was carried out at the scale of modifying the aging process
and using hydrothermal conditions for the synthesis of different types of
zeolites, and from these results obtain the most crystalline phases. For
this reason, the investigation of the synthesis of zeotypes from CEVs was
carried out at the scale of
laboratory and through two fusion methods and two
aging methods. Several parameters were selected:
alkaline activator / CEVs ratio = 1: 2, temperature and
reaction time 800 ° C and 2 h, respectively. During the
process
melt, the melt product ratio H two O / melt = 5 mL / g. The
variables were: state of
the alkaline pre-melt (solid or liquid), aging method
(ultrasound or static), aging time (6, 12 and 24 h) and
hydrothermal treatment time (6, 12 and 24 h). This
study establishes the conditions for the future synthesis
of better and more abundant zeolitic materials using
low-cost materials, such as CEVs.
Experimental procedure
Materials
The CEVs, which are part of the by-products of coal
combustion, used as raw material in the synthesis of
zeotypes, were supplied by the TERMOPAIPA thermal
power plant (Boyacá). The CEVs sample was initially
sieved on a Ro-Tap sieve shaker, using a 200 sieve in
order to obtain a particle size smaller than 63 µm,
selected for the synthesis process.

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 Effect of the melting and aging process on the synthesis of zeotypes from fly ash

To activate this by-product, sodium hydroxide (NaOH) in the
form of granules (97%, Carlo Erba) and distilled water were
used.
Zeotype synthesis
The zeotype synthesis process was carried out by
performing an alkaline fusion, using solid NaOH or
dissolved in water, followed by aging under static or
ultrasound conditions prior to hydrothermal treatment.
The optimal conditions for the synthesis of zeotypes
from CEVs with a maximum value of the cation
exchange capacity have been obtained using a CEVs /
NaOH ratio of 1: 1.2 [17-19]. Therefore, the NaOH
powder was mixed with the CEVs using two methods:
one with dry NaOH and the other with NaOH dissolved
in water, forming a saturated solution of NaOH in water.
The resulting mixture was calcined at 800 ° C for 2 h.
The alkaline reagent added to the starting material is
used as an activating agent.
during the merger. The products obtained during the
melting process were then dissolved in water (HO / melt
ratio = 5 mL / g), under stirred conditions. two n for 30
minutes and a speed of 600 rpm on a Scientifica VELP
magnetic stirrer, until the reaction gels were
homogenized. The mixtures were transferred to 65 ml
polytetrafluoroethylene (PTFE) reactors to carry out
aging for 6, 12 and 24 h under static or ultrasound
conditions, then the hydrothermal treatment was carried
out at 80 ° C for 6, 12 and 24 h on a stove. The pH was
measured before and after the hydrothermal treatment.
Finally, the reactors were removed from the oven at the
programmed times and washed with cold water. After
hydrothermal treatment, the reaction mixtures were
filtered and washed with distilled water and the
synthesized products were dried in an oven at 60 ° C
for 2 h. The experimental conditions are summarized in
Table 1.

Table 1 Experimental conditions for the transformation of CEVs into zeotypes under hydrothermal conditions

Fusion Relationship Treatment

Test Relationship Aging time
Alkaline PF / HO hydrothermal
Do not. CEVs: NaOH two

T (° C) t (h) (g / mL) Static (h) Ultrasound (h) T (° C) t (h)

1 1 / 1.2 800 two 5.0 / 25.0 6 80 6
two 1 / 1.2 800 two 5.0 / 25.0 12 80 6
3 1 / 1.2 800 two 5.0 / 25.0 24 80 6
4 1 / 1.2 800 two 5.0 / 25.0 6 80 12
5 1 / 1.2 800 two 5.0 / 25.0 12 80 12
6 1 / 1.2 800 two 5.0 / 25.0 24 80 12
7 1 / 1.2 800 two 5.0 / 25.0 6 80 24
8 1 / 1.2 800 two 5.0 / 25.0 12 80 24
9 1 / 1.2 800 two 5.0 / 25.0 24 80 24
10 1 / 1.2 800 two 5.0 / 25.0 6 80 6
eleven 1 / 1.2 800 two 5.0 / 25.0 12 80 6
12 1 / 1.2 800 two 5.0 / 25.0 24 80 6
13 1 / 1.2 800 two 5.0 / 25.0 6 80 12
14 1 / 1.2 800 two 5.0 / 25.0 12 80 12
fifteen 1 / 1.2 800 two 5.0 / 25.0 24 80 12
16 1 / 1.2 800 two 5.0 / 25.0 6 80 24
17 1 / 1.2 800 two 5.0 / 25.0 12 80 24
18 1 / 1.2 800 two 5.0 / 25.0 24 80 24

CEVs, fly ash; PF, fused product

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Characterization X-ray diffraction (XRD)

The mineral phases in the raw materials and the Figure 1 illustrates the X-ray diffraction profile of the CEVs
synthesized products were studied by X-ray diffraction used in the present study for the synthesis of zeotypes.
(XRD) of polycrystalline samples, using a Bruker D8 CEVs are characterized by the presence of an amorphous
ADVANCE diffractometer, with Da Vinci geometry, with phase giving rise to a broad band between 18 and 30º 2θ.
CuKα1 radiation at 40 kV and 30 mA. The identification There are, however, peaks of little intensity indicating the
phase was performed using the crystallographic powder presence of crystalline phases, such as quartz.
diffraction file database (PDF-2) of the International
Center for Diffraction Data (ICDD). The morphological
analysis was carried out by scanning electron
microscopy (SEM), using a QUANTA FEG 650
equipment, FEI brand, under the following analytical
conditions: magnification = = 1000-20000x, WD =
7.0-11.0 mm, HV = 10 kV, signal SE and Z = CONT,
detector = BSED and ETD, EDS EDAX APOLO X
detector with resolution of 126.1 eV (in. Mn Kα). 1, and
the application of 30 scans for the sample. A
PLATINUM BRUKERATR cell was used. However, only
the 400-1200 cm- region is discussed. 1, however, in this
the spectra showed the most important changes.

Figure 1 X-ray diffraction pattern of CEVs

Figures 2 and 3 show the X-ray diffractograms of the

Results and Discussion
The results obtained show that the hydroxide
Sodium (NaOH) is an efficient activating agent in the
hydrothermal transformation of CEVs. The main zeotypes
synthesized following the aforementioned methods were
NaP1 zeolite (GIS), faujasite (FAU) and sodalite (SOD);
type of structural code according to Database of Zeolite
Structures [30]. The structures of these aluminosilicates
are composed of tedrahedra
by [SiO 4] - and [AlO -
4 was that f 4]
starting material (CEVs), as well as the products
obtained from it, following the experimental protocol
described above. The most important changes
observed in the X-ray diffraction profiles are the
reduction in the intensity of the characteristic peaks of
the CEVs and the appearance of new peaks
corresponding to the synthesized zeotypes, which
increase in intensity with the monitoring time. Figure 2
reveals that following the solid-solid state alkaline
fusion method, 12 h aging under static conditions and
hydrothermal treatment for 6, 12 and 24 h, the main
crystalline phases obtained were NaP1 zeolite and
faujasite, with traces of sodalite, the latter not shown in
the X-ray diffraction profiles due to its weak intensity.
Figure 3 reveals that following

of such a man or
connected
5 , which are
by linked rman cages
defined size channels.

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 Effect of the melting and aging process on the synthesis of zeotypes from fly ash

The alkaline fusion method in solid-liquid state, 12 h

aging under static conditions and hydrothermal
treatment for 6, 12 and 24 h, again the appearance of
the characteristic peaks corresponding to NaP1 zeolite
and faujasite, accompanied by small traces of sodalite.
Comparing the results obtained, it can be observed that
after 6 h of reaction the main crystalline phases (zeolite
NaP1 and faujasite) began to form, although showing
peaks of greater intensity for zeolite NaP1 (except after
6 h of reaction) from solid-solid melt and for faujasite
from solid-liquid melt. With the reaction time it is
observed how the intensity of the peaks progressively
increased. Another difference that can be noticed by
comparing the X-ray diffraction profiles shown above is Figure 3 X-ray diffraction profiles of zeolitic products,
the appearance of numerous peaks of little intensity in
obtained from solid-liquid melt of CEVs in alkaline
the second case (solid-liquid melt), which is associated
solutions during different reaction times
with the presence of other crystalline phases that were
obtained in the synthesis process. The cancrinite, which
represents a zeotype, reported in previous works [2,
On the other hand, the activation of another by-product
16-17], was not obtained by any of the developed
of spontaneous coal combustion (natural clinker) has
methods, which can be attributed to time
been carried out under the same experimental
conditions (results not shown in the present study),
which reveal that faujasite is the only crystalline phase.
obtained from solid-solid fusion, while only sodalite
crystallized from solid-liquid fusion.

Scanning electron microscopy

(SEM)

The studies carried out by scanning electron

microscopy reveal not only the morphology but also the
composition of the CEVs, as well as the products
(zeotypes) obtained from their alkaline activation under
hydrothermal conditions.

The SEM image of secondary electrons (SE) of Figure

Figure 2 X-ray diffraction profiles of zeolitic products,
obtained from solid-solid melt of CEVs in alkaline
solutions during different reaction times
4 reveals that the particles that constitute the CEVs
have a predominantly spherical morphology and
various sizes (microspheres, cenospheres and
plenospheres), with a relatively smooth surface. In
some cases it is possible to observe the smaller
particles adhering to the surface of the larger ones.
CEVs have a high proportion

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irregular fluffy-looking particles. The semi-quantitative
analysis of CEVs by energy dispersive spectroscopy
reveals in the EDS spectrum of Figure 4 that the spherical
particles of CEVs are composed of oxygen, silicon,
aluminum and iron, with traces of magnesium, titanium,
sodium, potassium and phosphorus. . The mass ratios of
O: Si: Al: Fe are 44.03: 28.12: 16.70: 6.41. Therefore, the
chemical composition of the
CEVs disclose that the contents of SiO two and to two OR 3
Figure 4 Photomicrograph obtained from the scanning electron microscope, showing the morphology of the particles in the CEVs (left).
Elemental spectrum and Wt% and At% from an EDS analysis (right)
The im to Secondary electron SEM (SE) genes in Figure
5 reveal that the alkaline activation of CEVs was
manifested in the transformation of the original
morphology of the spherical particles with the
appearance of different morphologies in the synthesized
products, including the following: lepispheric in sodalite ,
octahedral in faujasite and acicular prismatic in NaP1
zeolite. Obviously, the change in morphology observed
between the CEVs particles and the synthesized
zeotypes can be explained by a process of dissolution of
the amorphous phase of the aluminosilicates present in
the CEVs, followed by a nucleation process
218
and low content of impurities (Ca and S), make this
starting material an alternative source for the synthesis of
zeotypes. These impurities in some cases can show an
inert or inhibitory character during the synthesis process.
However, the chemical composition of the starting
material (CEVs) plays an important role not only in the
hydrothermal synthesis process but also in the
environmental impact that its application may generate.
and crystallization of zeotypes on the external surface
of the spherical particles of the CEVs, in some cases
developing pseudomorphs, considering that the
resulting aggregates maintain the original shape of the
spherical particles of the CEVs. However, the NaP1
zeolite develops radial aggregates of tetragonal
crystals, which could indicate its nucleation and growth
out from the surface of the spherical particles of CEVs.
In the case of sodalite, this zeotype generally develops
randomly oriented blade-shaped crystal aggregates that
have a hollow appearance to the surface.
 Effect of the melting and aging process on the synthesis of zeotypes from fly ash

Figure 5 Microphotographs obtained from the scanning electron microscope, showing the characteristic morphologies of the synthesized

zeotypes: sodalite (SOD), faujasite (FAU) and zeolite NaP1 (GIS)

Infrared spectroscopy with
Fourier transform (FTIR)
Fourier transform infrared spectroscopy analyzes were
used for the characterization of the different bands that
both CEVs and zeotypes have obtained, since they
help to corroborate the results obtained from X-ray
diffraction and scanning electron microscopy. As can be
seen in Figure 6, the main absorption bands presented
by the CEVs are attributed to the vibration of the SiO
group. 4-
4 That
presented as a broadband between 9 00-1250
cm- 1 centered at 1061 cm- 1, associated with the asymmetric
tension of TO [31-32] and the vibration of the AlO - groups
twothat presents bands centered on 57 cm- 1. The
447 cm- 1 and 5 presence of quartz in
CEVs give rise to a series of bands [33] in
1150, 1084, 796–778 cm −1, of which I only know
observed the bands at 1061 and 798 cm −1 as the
closest. On the other hand, the demullite presence is
responsible for a series of bands at 1180–1130 cm −1 and
570–550 cm −1, which in turn are associated with Al SAW present
in its structure [34]. However, only the band was
observed at 572 cm- 1. The characteristic peaks of the
CEVs weakened, giving rise to the appearance of new
vibration bands at different frequencies that reveal the
formation of the zeotypes. After the hydrothermal
reaction under alkaline conditions with respect to time
and type of aging (static and ultrasound) the changes
that are described below occurred. For both solid-solid
melt and solid-liquid melt in the area between 500-800
cm- 1 Changes were observed in the synthesized
products, which correspond to the vibration bands of
the secondary structural units of the zeotypes.

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Figure 6 FTIR spectra of CEVs and the products synthesized from their alkaline activation with fusion (a) solid-solid and (b)
solid-liquid during different reaction times
In general terms, the following aspects stand out in
relation to the structure of the zeotypes: The bands in
the region 300-420 cm- 1
related to the opening of pores [35] are not well defined.
A change in intensity and width of the band was
observed at 447 cm- 1
in the region 420-500 cm- 1, which represents an internal
vibration of TO. Bands in the region 500-650 cm- 1, which
are related to the presence of double rings (D4R and
D6R) are not well defined. There was an increase in the
band at 557 cm- 1 and the appearance of two new bands
at 750 cm- 1 and 619 cm- 1. The band at 750 cm- 1 could be
attributed to TO bonds in interconnected tetrahedra that
form single (S4R) or double (D4R) ring units, while the
band at 619 cm- 1 it could be associated with the presence
of single (S6R) or double (D6R) ring units [32]. The broad
band centered at 1061 cm- 1 moved to 960 cm- 1 with a
higher intensity and with the presence of a shoulder at
1100
220
cm- 1 ( asymmetric TO tension). These data are similar to
those obtained previously in other studies (eg [2, 29]),
highlighting the presence of crystalline phases (NaP1
zeolite, faujasite and sodalite) that promote important
changes in the region of 500-800 cm- 1. Comparing the
FTIR spectra, a difference is observed in relation to the
appearance of numerous bands of low intensity in the
second case, that is, from solid-liquid melt, which
indicates once again the presence of other crystalline
phases that were obtained in the synthesis process.
Reaction history during the synthesis of
zeotypes
The transformation of CEVs has been in zeotypes
investigated with the purpose of the to establish
reaction mechanism or experimental optimize the
conditions of the process of
hydrothermal synthesis. During the last years,
 Effect of the melting and aging process on the synthesis of zeotypes from fly ash

Several research groups have made great efforts to considers that the solid-liquid reaction presented greater
successfully bridge the gap between the general diffusion (movement of the molecules from a region of
mechanisms of crystalline phase formation and the high concentration to another of lower concentration),
crystallization of structures as complex as those of because this favored a greater mobility of the molecules
zeolites [36]. However, there is little information within the liquid phase, better contact surface, greater
regarding these mechanisms and crystallization kinetics reactivity and better homogenization of the reaction
[35]. The reaction mechanism of zeotypes, such as mixture in relation to the solid-solid reaction.
NaP1 zeolite, faujasite and sodalite, can be affected by
different factors, which include the formation of
intermediate metastable phases (for example, NaP1
During the reaction gel formation stage,
zeolite), the simultaneous occurrence of precipitation
el Al (OH) 3 formed during the alkaline melting stage that
and dissolution reactions. of the reaction gel, the
produced sodium aluminate, reacted
nucleation and growth of the zeotypes, the dissolution
with silicates to produce the reaction gel [17]. The
of the early metastable phases, and the nucleation and
structure of the gel is due to a reaction in which large
growth of more stable phases such as sodalite and
molecules are formed from many small molecules
cancrinite (the latter not formed in the present study)
(polymerization). The composition and structure of the
that reached chemical equilibrium. The reaction history
hydrated polymerized gel are controlled by the size and
of the synthesis process developed in this study is
structure of the polymerizing species, which is
summarized below. The reaction mechanisms of the
manifested in the differences observed in the
synthesis of zeolites from coal combustion by-products
synthesized zeotypes. Typical gels are prepared from
(CEVs) via alkaline fusion prior to the hydrothermal
sodium aluminate, sodium silicate, and sodium
reaction are discussed in detail by [17], which can be
hydroxide because they are all soluble.
divided into several stages: (1) fusion alkaline, (2)
formation of the reaction gel and (3) hydrothermal
crystallization.
During the hydrothermal crystallization stage, three
events properly occurred: induction period, nucleation
and crystal growth. The crystallization of the zeotypes
took place after an induction period, in which the
reaction gel and the species in solution undergo
During the alkaline melting stage, a modification of the
constant changes between monomers and clusters, for
classic solid-solid reaction was introduced between the
which a constant appearance and disappearance of
alkaline activator (NaOH) and the spherical particles of the
nuclei occurs through the hydrolysis and condensation
CEV, also using the solid-liquid reaction. In both cases,
reactions, which are responsible for the formation of
the alkaline fusion process played an important role in the
solid phase embryos that, upon reaching their critical
collapse of the crystalline phases of the CEVs from which
size, constitute the nuclei [37]. Longer aging time,
the Si content is released, with the formation of sodium
shorter induction times and faster crystal growth. The
silicate and aluminate salts that constitute the precursors
induction period can be influenced by factors such as
for the synthesis of zeotypes. and they represent more
supersaturation, agitation, the presence of impurities,
reactive compounds that were dissolved in water more
viscosity, among other aspects [38]. However, aging
easily than the crystalline phases present in CEVs (quartz
conditions also affect this process. At that time,
and mullite), which are less reactive and have a low
equilibrium reactions take place between sodium ions
dissolution rate, as demonstrated by their appearance as
and the components
relict phases in the products. synthesized [17]. However,

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Rev. Fac. Ing. Univ. Antioquia No. 74. March 2015

aluminate and sodium silicate, thus leading to their However, these rates are also influenced by different
redistribution and a distribution of the reaction variables, particularly the molar composition of the
components between the solid and liquid phases, reaction gel. Hydrothermal treatment of the reaction gel
reaching an equilibrium between both and tending to at the programmed temperature and reaction time
the ordered structure of a crystal, which is due to the produced crystallization of NaP1 zeolite, faujasite and
depolymerization of the gel due to the hydroxyl ions sodalite.
(OH) present in the reaction mixture. The induction
period was followed by nucleation and crystal growth
The results presented above suggest that CEVs
processes. The sodium silicate solution releases ionic
represent an interesting alternative not only for mitigating
species that were transported to the nucleation sites. As
the environmental impact generated by the disposal of
the condensation of aluminate and silicate ions took
industrial waste associated with the combustion of coal in
place, precipitation of an aluminosilicate gel occurred.
Thermal Power Plants, but also for the production of
Nucleation is the phase transition by which a critical
products with suitable properties for their application in
volume of a semi-ordered gel is transformed into a
different fields. scientific-technological and of great
sufficiently ordered structure to form a growth center,
benefit on an industrial scale. Conventional hydrothermal
from which the crystalline structure can propagate.
treatment (without alkaline melting) indicates that
Polymerization was the process responsible for the
dissolved Si and Al concentrations under equilibrium
formation of the precursors that gave rise to the
conditions are not proportional to the content of oxides
zeotypes, which are made up of Si and Al tetrahedra
present in CEVs, since Al is apparently much more
distributed randomly along polymer chains that are
soluble than Si [32], in Contrary to what was stated by
cross-linked to provide cavities large enough to
[39], who reported the existence of an apparent
accommodate the ions. alkaline load balance. The
synchronization between Si and Al that can be dissolved
formation of different nucleation sites developed
from the surface of the CEVs particles during the
according to the Ostwald rule,
aluminosilicate polymerization process. Therefore, it is
necessary to carry out future studies that allow the
zeotype synthesis process to be carried out under
optimal experimental conditions in order to successfully
prepare highly crystalline pure products, varying the Si /
Al ratio of the starting material, which could increase the
growth rates of the zeotypes. In this way, it is expected
that the crystalline and amorphous phases in the CEVs
will be converted into soluble compounds that promote
the formation of zeotypes, such as NaP1 zeolite, faujasite
and sodalite, avoiding the presence of relict crystalline
and promoting the growth of zeolite crystals
phases of the starting materials in the synthesized
progressively. Crystallization generally involved the
products. On the other hand, preliminary works carried
assimilation of material from solution by a growth
out by the authors reveal that the synthesized zeotypes
process, which began when the nuclei reached a critical
can be efficient materials as selective cation exchangers,
size and the crystals began to grow. Crystal growth
being an alternative of great importance for the
occurred during the hydrothermal reaction. A stable
remediation of wastewater.
phase reached the equilibrium conditions necessary to
promote the growth of the NaP1 zeolite, faujasite and
sodalite crystals. The linear growth rates of zeolites
show a strong dependence on temperature [37].
Without

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 Effect of the melting and aging process on the synthesis of zeotypes from fly ash
Conclusions
The present study in which different parameters are
varied, such as the alkaline fusion procedure between
CEVs and NaOH (solid-solid and solid-liquid), the aging
time under static and ultrasound conditions, and the
hydrothermal treatment time, reveals that the synthesis
of zeotypes from CEVs from Termopaipa (Boyacá) was
successful with alkaline activation in solid-solid state,
obtaining as primary phase NaP1 zeolite with static
aging times of 12 h and hydrothermal treatment of 12 h
as primary phase and with very few phases secondary
crystalline. However, the synthesis also showed good
results for alkaline activation in solid-liquid state,
obtaining faujasite as the primary phase with static
aging times of 12 h and hydrothermal treatment of 24 h.
The aging with ultrasound in both solid-solid and
solid-liquid alkaline activation for the CEVs did not
present good results since low intensities were obtained
in the crystalline phases in the diffractograms for these
zeotypes, which indicates that the ultrasound process
inhibits the formation of precursor crystals during aging.
In some cases, the formation of zeotypes was not
successful, taking into account that the products
obtained contain traces of quartz and mullite, while only
a very small fraction of the zeotypes (eg, NaP1 zeolite
or faujasite) was obtained. The industrial application of
these zeotypes depends on their CEC, their pore size
and their residual charge. A product with a high CEC,
such as NaP1 zeolite, can have great applicability in
wastewater treatment,
Thanks
The authors thank the Vice-rector for Research and
Extension of the University
Industrial de Santander for the financial support granted
through Research Project No. 5454 "Synthesis of
zeolites from solid waste from the National Coal Industry
for the removal of chromium (Cr) from industrial
effluents". This research is part of the undergraduate
thesis of the Industrial University of Santander de LF
Ávila and JALizcano. The authors also thank the
Universidad Industrial de Santander for facilitating the
use of its research facilities (DRX, SEM and FTIR), as
well as the human resources linked to these specialized
laboratories. AOfelia Ciendúa of the Environmental
Management Unit of GENSA SAESP, for facilitating the
entry and collection of samples of CEVs.
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