Synthesis and characterization of hydrate aluminosilicate

using variable ashes and multi-step methods. A review

By

MUHAMMAD UMAIR

2013-GCUF-01784

Undergraduate Review Paper/Report Submitted in Partial fulfillment of the

Requirement for the Degree of

BACHELOR OF SCIENCE
IN
APPLIED CHEMISTRY

DEPARTMENT OF APPLIED CHEMISTRY

GOVERNMENT COLLEGE UNIVERSITY, FAISALABAD

August 2017
 DECLARATION
The work reported in this review was carried out by me under the supervision of Dr.
Shahzad Ali Shahid Chatha, Assistant Professor, Department of Applied Chemistry,
Government College University,Faisalabad, Pakistan.

I hereby declare that the title of review article Synthesis and

characterization of hydrate aluminosilicate, using variable ashes and multi-
step methods and the contents of the review are the product of my own study and no
part has been as such copied from any published source. I further declare that this work
has not been submitted for award of any other degree/diploma. The University may take
action if the information provided is found inaccurate at any stage.

Muhammad Umair

2013-GCUF-01784
 CERTIFICATE BY THE RESEARCH SUPERVISOR

I certify that the review submitted by Muhammad Umair, Registration No. 2013-GCUF-
02402 has been found satisfactory and in accordance with the prescribed format. I
recommend it to be processed for the evaluation by the panel of experts for the award of
degree.

Supervisor
Dr. Shahzad Ali Shahid Chatha
Assistant Professor
Department of Applied Chemistry
GovernmentCollegeUniversity, Faisalabad

Chairperson
Dr. TahsinGulzar
Associate Professor
Department of Applied Chemistry
GovernmentCollegeUniversity, Faisalabad
Review/Research Report/Industrial Project Scrutiny Committee

Convener .
Dr. Tahir Farooq
Assistant Professor
Department of Applied Chemistry
Government College University, Faisalabad

Member-1.
Dr. ShaziaTabassum
Assistant Professor
Department of Applied Chemistry
Government College University, Faisalabad

Member-2.
Dr. Shazia Abrar
Assistant Professor
Department of Applied Chemistry
Government College University, Faisalabad
Review/Research Report/Industrial Project Evaluation Committee

Chairperson .
Dr. TahsinGulzar
Associate Professor
Department of Applied Chemistry
Government College University, Faisalabad

Member-1.
Dr. Muhammad JawwadSaif
Assistant Professor
Department of Applied Chemistry
Government College University, Faisalabad

Member-2.
Dr. Shahzad Ali Shahid Chatha
Assistant Professor
Department of Applied Chemistry
Government College University, Faisalabad

Supervisor.
Dr. Shahzad Ali Shahid Chatha
Assistant Professor
Department of Applied Chemistry
Government College University, Faisalabad
 Dedication
This work is dedicated to my family
Who taught me that the best kind of knowledge to
have is that which is learned for its own sake
&
It also dedicated to my Supervisor, who taught me
that even the largest task can be accomplished if it is
done one step at a time
Synthesis and characterization of hydrate aluminosilicate using
variable ashes and multi-step methods. A review

Content: page

Acknowledgements

Table

Abstract;
1. Introduction 4

1.1. What is zeolite and Chemistry of zeolite 4

1.2. Application of zeolite 4

1.3. Why we need to synthesis zeolite 5

1.3.1. Organic compound issues

1.3.2. Inorganic compound issues

i. Lithium slag issues

ii. Heavy metal issues

iii. Fly ash issues 6

2. Synthesis of zeolite 7

2.1. Raw materials using in zeolite synthesis

i. Coal fly ash

( a ). Characteristics of coal fly ash

ii. Rice husk ash and its characteristics

iii. Sugarcane bagasse ash

iv. Solid waste of palm oil mill

v. cotton linter ash

 vi. Red mud

2.2. Methods involve in zeolite synthesis

i. Pre-fusion method

ii. Fusion method

( a ). Alkaline fusion process

( b ). Alkaline hydrothermal process

iii. Hydrothermal conventional method

iv. Fusion and hydrothermal method

v. Molten salt method

vi. Membrane preparation

vii. Microwave treatment

viii. Ultrasonic treatment

ix. Replacing fusion with sonochemical treatment

3. Types of zeolite

4. Characterization and morphology

4.1. X-ray fluorescence (XRF)

4.2. X-ray diffraction (XRD)

i. Difference between XRD and XRF

4.3. Scanning electron microscope (SEM)

4.4. Fourier transforms infra- red spectroscopy (FT-IR)

4.5. Inductively coupled plasma-mass spectrometry (ICP-MS)

5. Conclusions

References
ACKNOWLEDGEMENTS

All the praises belong to ALLAH ALMIGHTY, The most merciful beneficent and
compassionate who is entire source of knowledge and wisdom to main kind. Who know
whatever is there in the universe. Countless salutation be upon the HOLLY PROPHET
(S.A.W), the city of knowledge greatest social reformer and revolutioner, who is the most
perfect and a torch of guidance and knowledge for humanity as a whole forever.
Alhamdulillah, all praises to Allah & Holly Prophet (S.A.W) for the strengths and His
blessing in completing this review

I have no words to express my deep gratitude to my supervisor Dr. Shahzad Ali

Shahid Chatha, Assistant Professor Applied Chemistry, Govt. College University
Faisalabad for his affectionate supervision, inspiring guidance, kind cooperation, and
consistent encouragement during these studies. I am extremely thankful to the
honorable Chairperson, Department of Applied Chemistry, Dr. Tahsin Gulzar, for his
valuable suggestions and keen interest in extending research facilities.

I would also like to thank my family, whose inspiration has been a tower of light
for me with his day and night prayers, encouragement, moral and financial support. I am
extremely thankful to Mr. Tabssum Hussain & MR. Muhammad Rafique for their
encouragement technical advice, and tremendous help. At the end, I present my special
thanks to all of them who helped me in completion of my review. May ALLAH bless these
people with delighted and satisfying lives (Ameen)!

Muhammad Umair
Abstract;

Fly ash is an industrial by-product which is obtained as a result of combustion in thermal power
plants and etc. The ever-increasing in consumption of fly ash that is required serious research
attention, because fly ash is most complex anthropogenic material and its improper disposal has
become a major environmental problem. Heavy metals are also another most important
environmental issue. A variety of water treatment technologies exist that propose effective heavy
metals removal. This review describes the brief detail on zeolite synthesis. As the world zeolite
is a Greek word which means is boiling stone. Zeolites are crystalline microporous
aluminosilicates or hydrated aluminosilicate which consist on three dimensional network of
aluminum and silicon atoms tetrahedral linked with oxygen atoms. Zeolite can be synthesize by
numerous sources of material such as fly ash which including coal, kaolinite, sugarcane
bagasse , nanofiber, lithium slag, rice husk, and palm oil fuel mill waste and red mud and etc.
The synthesis of zeolite from fly ash was carried out through multi-methods such as conventional
hydrothermal method, fusion method, pre-fusion method, microwave treatment, hydrothermal
proceeded by sonication, and molten salt and etc. The experimental zeolitic products is
characterized by the following techniques such as X-ray fluorescence (XRF), X-ray diffraction
(XRD), scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR),
and inductively coupled plasma mass spectrometry (ICP-MS). The type of zeolite synthesize
depends on the concentration of alkali mixed duration of the experiment temperature and some
time depends on PH of solution. By using multi-step zeolitization process we can convert
numerous amounts of fly ashes, which consist of alumina and silica into zeolite product. In this
review, the effects of sonication and microwave on the synthesis of different zeolites are also
observed. The modern technologies such as ultrasound, and microwave, reduce time period for
nucleation and crystallization growth and also improve crystallinity of the synthesized zeolite.
Besides, use of ultrasound and microwave are also altered morphologies and size of the particles,
and high purity zeolite produced which have good working efficiency between ninety to more
than ninety five percent.
1. Introduction;

1.1 What is zeolite and chemistry of zeolite;

Zeolites is a hydrated aluminosilicate minerals, which can be synthesize using numerous source
materials such as fly ashes (Chang & Shih, 1998; Inada et al., 2005; Querol et al.,1995; Belviso
et al., 2016; Querol et al., 2002; Berkgaut & Singer 1996; Belviso et al., 2016; Querol et al.,
1997; Querol et at., 2002; Belviso et al., 2015; Shigemoto et al.,1993; Molina & Poole, 2004;
Belviso et al., 2014; Belviso et al., 2009; Belviso et al., 2010; Belviso et al., 2012). and kaolinite
example (Murat et al., 1992; Garca et al., 2017; Heller & Lapides, 2007; Park et al., 2001;
Gualtieri et al., 1997; Rios et al., 2009; Du & Yang, 2010; Belviso et al., 2013). The general
formula for a zeolite is M2O.Al2O3.xSiO2.yH2O as M is alkaline or alkali earth metal, and the
value of x varies from two to ten and y varies from two to seven. The Al2O3 and SiO2 are the
structural cations because they form the tetrahedral framework with oxygen (Mumpton, 1985).

Zeolites are crystalline microporous aluminosilicates minerals which consist on three

dimensional networks of aluminum and silicon atoms tetrahedral linked with oxygen atoms
(Barrer, 1978; Breck, 1984). Zeolites are tectosilicates characterized by three dimensional
network of tetrahedral unit that form a system of consistent pores. The substitutions of silicon
with aluminium produce a net negative charge which is balanced with the existence of an extra
cation in the structure. Zeolites molecules confined in small spaces due to changes in their
structure and reactivity.

1.2. Applications of zeolite;

Due to three dimensional network and sorption property zeolite have wide range of application
like, cation exchange capacity (CEC), mobility tracing of toxic element and number of
environmental applications (Belviso et al., 2010; Belviso et al., 2012;Moreno et al., 2001;
Belviso et al., 2014; Can & lk, 2010; Medina et al., 2010; Visa et al., 2012) to enzymatic
model and catalysis (Corma 2003; Gayubo et al., 2004; Lanzafame et al., 2012; Van et al., 2014).
Zeolites due to their active sites, shape selectivity, frequent pores and thermal stability, are
extensively used as a catalyst in the petroleum industries, for example in fluid catalytic cracking
and hydro cracking (Burch & Scire, 1994; Byggningsbacka et al., 1998; Corma & Martnez,
1997; Corma et al., 1998; Hlderich et al., 1997; Kumar et al., 2000; Kumar et al., 2007; Tran et
al., 1998). The effectiveness of a zeolite is strictly connected to their typical structural
characteristics which assist as a pollutant adsorption and encapsulation. The magnetic zeolite
have been effectively used to remove contaminant particles from polluted water (Bourlinos et
al., 2003; Barquist & Larsen, 2010; Deng et al., 2009; Faghihian et al., 2013; Yamaura &
Fungaro, 2013; Liu et al., 2013; Cao et al., 2013; Oliveira et al., 2004).
 Zeolites also have high carbon dioxide (CO2) adsorption capacity and good desorption
characteristics (Choi et al., 2009; Jin et al., 2013; Wajima et al., 2010; Walton et al., 2006).
There have been numerous technique of the development of various types of zeolites for CO2
adsorption, example beta (You et al., 2013), Na-A (Ruen-ngam et al., 2009; Chen & Ahn, 2014),
Na-P1 (Bukhari et al., 2015), Na-X (Ruen-ngam et al., 2009; Chen et al., 2014; Liu et al., 2014;
Park et al., 2012), Na-Y (Cavenati et al., 2004). Zeolite X has appreciably higher adsorption
selectivity for CO2 as compared with methane (CH4) or nitrogen (N2) than numerous other types
of zeolite (Ruen-ngam et al., 2009; Cavenati S et al., 2004). Zeolites can be synthesized from
different materials among these in the most recent few years much research has been focused on
the use of coal fly ash (Shigemoto et al., 1993; Inada et al., 2005; Belviso et al., 2010; Belviso et
al., 2011; Belviso et al., 2012; Belviso et al., 2013; Belviso et al., 2015).

1.3. Why we needs to synthesis zeolite;

1.3.1. Organic compound issue;

Volatile organic compounds such as benzene, toluene and formaldehyde are dangerous to human
health and the environment (Zhou et al., 2014; Cosseronet al., 2013).Contemporary, the
management of volatile organic compounds is becoming a focus of the whole society
.Adsorption is the most useful way to get rid of or collect these harmful compounds. Zeolites and
activated carbons is the most common materials used for adsorption of volatile organic
compounds (Kim & Ahn, 2012).Zeolites used as adsorbents have the advantages of being non-
flammable, thermally stable and hydrophobic for adsorption of volatile organic compounds
(Anet al., 2011).Therefore, its necessary to develop economically possible techniques to prepare
zeolite materials as effective adsorbents for volatile organic compounds removal.

1.3.2. Inorganic compound issue;

i. Lithium slag issues;

Lithium slag is a solid waste by-product which is generated during the production of lithium
carbonate by using the sulfuric acid (H2SO4) method. During the production of lithium carbonate
a large amount of solid waste (lithium slag) is produced which is ten time greater than the
lithium carbonate about one ton of lithium carbonate produced ten tons of lithium slag. While on
the other hands small portion lithium slag is utilized as a raw material for building manufacturing
and construction purpose (Glukhovskii et al., 1983). The remaining solid waste is dispose in
open air or landfill, which causing environmental problems. To solve these environmental
problems lithium slag is used in zeolite synthesis.

i. Heavy metal issues;

The World Health Organization considers mercury as one of the top ten chemicals or group of
chemicals associated to public health concern (Attariet al., 2017). The discharge of effluent
contains of mercury in soil, sediments, and water can inflict an irreversible harm to the
environment. The major sources of mercury emissions besides the natural origins are ore mining,
burning of fossil fuels, and the industrial production processes, in common. The most dangerous
is the conversion of inorganic mercury into organic like, methyl mercury, and its
bioaccumulation in the aquatic species which is at the top of food chain. Because of this high
toxicity of mercury, the US Environmental Protection Agency (EPA) specifies the maximum
contaminant level of mercury at very low level of 0.2 ppb (0.2 mg/L). This has led to a great
inspiration for a growing number of researches on the treatment of wastewater for mercury
removal (Kulkarni, 2015; Manohar et al., 2002; Lee& Lee, 2012; Selin, 2009; Bernhoft, 2011).
Recently, there is a variety of techniques available for mercury removal, such as sulfide
precipitation, coagulation, co-precipitation, and reverse osmosis. Even though these techniques
are effective to some extent, most of them have disadvantages such as high cost, operational
difficulties, complicated industrial setups, and large toxic irreversible sludge (Gupta &
Bhattacharyya, (2011; Babel & Kurniawan, (2003); Kurniawan et al., 2006). Coal fly has been
effectively used for flue gas cleaning from mercury element (Li & Maroto-Valer, (2012); Xu et
al., 2013; Chunfeng et al., 2009; Papandreou et al., 2011; Wanget al.,2015). Recently,
researchers identified that the modification of coal fly ash can improve its adsorption properties
while reducing its leaching problem. The main method to modify coal fly ash involves
conversion of coal fly ash into zeolites that has been exposed to be effective in enhancing heavy
metal removal like mercury and etc. (Chunfeng et al., 2009; Jha et al., 2009; Hui et al., 2005).

ii. Fly ash issues;

Fly ash is a small dark spot produced by the burning of coal or other materials like cotton linter,
rice husk and etc. carried into the air. The disposal of fly ash is an economical problem for every
developed country, therefore the improper disposal of fly ash cause increase its concentration
every day. Fly ash particles as a result of combustion mean burning of fossil fuel sugarcane
bagasse and etc. and other materials are released into the environment. Fly ash particles impart
great environments for the interaction of variety of substance during the combustion of material.
Particles may cause inhalation of hazard workers. The emission of fly ash in open environment is
dangerous for human health because it contains carcinogenic compound and as a result of
inhalation alteration in immune system (Haugsten & Gustavson, 2000; Jala & Goyal, 2006). Fly
ash solid waste is classified as a hazardous waste because it contains inorganic oxides like oxides
of carbon, oxides of nitrogen, oxides of sulphur and etc. It also contains heavy metals and, some
time, toxic chlorinated organic content (Mangialardi, 2003). Disposal of fly ash into ordinary
landfill sites poses serious environmental problems, principally because this material contains
high concentrations of leachable heavy metals. Various technologies have been investigated in
order to reduce the hazardous characteristics of fly ash

2. Synthesis of zeolite;

The type of zeolite synthesize depends on the conditions which we are adopted during the
experiment. Its depends upon the ratio of fly ash, and concentration of base used, temperature,
pressure, some time depends on the Ph of the solution. By following all these parameter we can
synthesis different types of zeolites from same fly ash (Querol et al 2001; Blissett & Rowson,
2012). All techniques are based on the dissolution of alumina and silica bearing fly ash with
alkali solution (such as NaOH, KOH and LiOH solution) and consequent precipitation of zeolitic
material (Blissett & Rowson, 2012).

2.1. Raw materials using in zeolite synthesis;

i. Coal fly ash;

Coal is most naturally occurring fossil fuel in the world. Mostly it is used as fuel for the
production of electricity in many countries. The percentage of coal used in China is seventy nine
percent, in Poland is ninety two percent, in South Africa is ninety three percent, in United State
is forty nine percent, in India is sixty nine percent and in Pakistan is more than fifty percent
(Burnard & Bhattacharya, 2003). The amount of electricity production in 2006 from Coal fired
power plants is forty one percent while in 2030 forty four percent are expected globally
(Mehmoodet al., 2012). The consumption of coal has increased globally day by day form few the
decade years (www.eia.gov/cfapps/ipdbproject/IEDIndex3.cfm?tid=1&pid=1&aid=2).

Coal ash is produced as a solid waste product by burning of coal in coal fired power
plants (Querol et al., 2002; Blissett & Rowson, 2012). The amount of coal ash generated in Japan
is just about five hundred to six million tons per year respectively. It is predicted that its
concentration increase rapidly every day (Handbook C. A, 2000). There are two types of coal ash
is generated from coal fire power plant. One is fly ash and the other is slag or bottom ash. Coal
fly ash is collected from the top of a burner by using cyclones whereas the slag is collected from
the bottom of a furnace. More than eighty percent of fly ash in Japan is used as a raw material for
cement production. While the remaining material is disposed in land filled, and about only
fifteen percent of the fly ash is recycled. Coal fly ash consists on various hazardous heavy
metals, example lead, Cadmium, Arsenic, Tin, Antimony (Handbook C. A, 2000). Therefore it is
need to the development of new recycling process which is necessary for the removal of heavy
metals.

The inorganic residue produced from coal combustion process is recognized as coal
combustion by-product. However a large amount of fly ash is used by the construction industry.
There is still a proportion of fly ash which is disposed in landfills. The use of coal fly ash has
become significant environmental and economical problems. Therefore a ton of fly ash used to
replace a ton of cement saves the use of an corresponding of nearly one barrel of oil
(http://www.ecoba.com).

Coal fly ash mostly used as a raw material for pozzolana cement production (Heidrich et
al., 2013). Although fifty percent of coals fly ash in the world is disposed into landfills
(Ahmaruzzaman, 2010). The dumping of fly ash is a universal issue. As its massive production
play harmful effects on the environment (Twardowska &Szczepanska, 2002). To solve the
environmental and economical issues various approach have been studied in which coal fly ash is
used as starting material and convert it into valuable products. As the fly ash contain amorphous
aluminosilicate glass which represent as a reactive phase for the zeolite synthesis (Subotic &
Bronic, 2003; Boistelle &Astier, 1998).

In the past fifty years researchers have focused on using coal fly ash as a source of
aluminosilicate for manufacturing different types of synthetic zeolites such as Sodium-Y
(Kondru et al., 2011), zeolite X and sodalite (Querol et al., 2002), zeolite A (Bukhari et al., 2016;
Ojumu et al., 2016), and Sodium-P zeolite (Park et al., 2000; Berkgaout & Singer, 1996; Moreno
et al., 2001; Querol et al., 1997; Hollman et al., 1999; Querol et al., 2001; Moreno et al., 2002;
Inada et al., 2005; Wdowin et al., 2014; Waek et al., 2008). This synthetic zeolite have high ion
exchange capacity and can be used as following water softening, gas separation and removal of
heavy metal and etc. (Albert et al.,1998; Huo et al ., 2012). In addition, its high content of Si and
Al makes it as a good resource for the production of zeolitic materials (Hller &Wirsching,
1985; Moreno et al., 2001). Although the larger quantities of Alumina and Silica in fly ash are
reported to be entrapped in the amorphous phase of the ash, the crystalline phases such as quartz,
mullite, hematite and magnetite also contain significant quantities of these elements.
 (a) Characteristics of coal fly ash;

The most important chemical ingredient and properties of Coal fly ash are depends upon the
properties of coal being burned (Ahmaruzzaman, 2010; Zacco, 2014) by (i) combustion method
(ii) heating and cooling regime in coal boiler (Siddique, 2004). Coal fly ash may have inorganic
compounds (i) sulfates (ii) alumina (iii) silica (iv) mullite (v) quartz (Hower, 2012). Coal fly ash
is mostly composed of irregular solid (Zacco, 2014). There are two major classes of coal fly ash
one is F class and other is C class. Class C have greater than twenty percent of calcium oxides
for example lignite while on the other hands class F contains lesser than twenty percent of
calcium oxides example is anthracite (Hower, 2012; Franus, 2012). High calcium coal fly ash is
tri & tetra calcium aluminosilicates while low calcium coal fly ash are mullite & quartz
(Ahmaruzzaman, 2010). In spite of the variability of coal fly ash around the world have been
successfully used to synthesize zeolite in different countries including, Australia (Wang & Zhu,
2005), Bulgaria (Shoumkova& Stoyanova,2013) Nada (Behin et al.,2013; Bukhari et al., 2014),
Italy (Belviso et al., 2013), India (Chauhan & Talib, 2012), Japan(Inada et al., 2005; Fukui et al.,
2007; Fukui et al., 2006; Shigemoto et al., 2003; Jha et al., 2009), Poland (Franus , 2012; Franus
et al., 2014; Wdowin et al., 2014), South Africa (Woolard et al., 2000; Musyoka et al., 2012),
South Korea(Kim & Lee, 2009; Park et al., 2000; Park et al., 2000), Spain (Querol et al., 1997;
Moreno et al., 2003), and United States (Sakthivel et al., 2013).

ii. Rice husk ash; and its characterstics;

Traditionally, zeolites are synthesized from sodium silicate and aluminate (Barrer, 1982; Breck,
1974). However, other aluminosilicate rich materials like (i) coal fly ash (ii) rice husk ash (iii)
kaolin have also been used (Chareonpanich et al., 2004; Vempati et al., 2006; Wang et al., 2007).
Rice husk fly ash has the added advantage of being inexpensive and utilizing them as raw
materials alleviates environmental pollution challenges. Many researchers show that rice husk is
excellent source for the preparation of high class of hydrated aluminosilicates (Katsuki et al.,
2005).

Rice husk consist on both organic and inorganic compounds. The percentage of organic
compound is about seventy five to eighty percent and inorganic compound is about twenty to
twenty five percent (Kurama & Kurama, 2008; Mohamed et al., 2015). The percentage of
organic compound is greater than inorganic compound in rice husk but after the combustion
process organic content is removed, and only inorganic content like silica is present in rice husk
ash which have high purity about ninety percent (Sun &Gong, 2001). A large amount of the husk
produced during the processing of rice is also burnt or dumped as waste. Even some of this husk
is converted into end products such as feedstock (Maiti et al., 2006) and adsorbent (Mohamed et
al., 2015). The amount of rice husk burnt in open environment cause health problems especially
in poor and developed countries. Therefore, it is a necessary to find out proper pathways to fully
utilize the rice husk. Silica can be extracted from rice husk ash in the form of sodium silicate by
using a solvent extraction method (Pijarn et al., 2010).

The amorphous silica present in rice husk changed to crystalline silica when it is heated
at high temperature. The change in structure with temperature is affected its chemical purity and
particle size (Daffalla et al., 2010). Silica extract from rice husk is undesirable agricultural mass
residue (Seung et al., 2011; Mane & Babu, (2011) that contains metal ion impurities such as
Titanium oxides and Iron oxides is chemically treated with sodium hydroxide to prepare
amorphous silica (Mohamed et al., 2008).Today, zeolites are widely employed in industrial (Kurt
et al., 2017), environmental (Ng et al., 2009), biomedical (Pavelic et al., 2001) and intensive
agriculture (Li, 2003) applications. In order to reduce the cost of zeolite synthesis, attempts have
been made to use rice husk ash, an agriculture waste, as silica precursor in zeolite synthesis.

iii. Sugarcane straw ash;

Sugarcane straw is the material that is removed before the cane is crushed and comprises
the dried/fresh leaves and the top of the plant (Saad et al., 2010; Moriya et al., 2007).
Sugarcane is used worldwide as a feedstock for ethanol and sugar production
(http://www.unica.com.br) Sugarcane bagasse is a huge by product in the sugar mills when juice
is extracted from the cane (Balakrishnan & Batra, 2011). Sugarcane processing to produce sugar
and ethanol generate several agricultural residues, being straw and bagasse is considered as the
main among them. An amount of 1 ton of sugarcane generates 270 kg bagasse and 144 kg
trash/straw (Costa et al., 2013).

The disposal of large amounts of sugarcane bagasse ash and multilayer food packing has
become a serious environmental problem. However, these solid wastes can be used in the zeolite
synthesis process. Sugarcane bagasse is a hazardous solid waste generated in large amounts in
sugar mills. Combustion of sugarcane bagasse in boilers, used for steam and electricity
generation, produces a great amount of another solid waste, denominated sugarcane bagasse ash
(Balakrishnan & Batra., 2011).Employing this quartz abundant waste as a silicon source can
avoid its accumulation (Jha VK et al., 2009; Shigemoto et al., 1993; Moises et al., 2013).

It was already known that sugarcane straw ashes can be recycled in the manufacture of
commercial cements and other composites, as pozzolanic material (Hernandez et al., 1998; Frias
et al., 2007; Morales et al., 2009). One possibility for effective usage of those wastes is to
convert the sugarcane straw ash into zeolites for environmental uses. Sugarcane straw ashes have
aluminosilicates glass, mullite and quartz, which are the required building blocks of zeolite
formation (Hernandez et al., 1998; Frias et al., 2007; Morales et al., 2009). Some authors have
reported the conversion of bagasse fly ash into zeolites (Shah et al., 2011; Shah et al., 2011; Shah
et al., 2012; Worathanakul et al., 2011), but apart from one earlier study, are no reports on the
conversion of sugarcane straw ash into zeolites.

iv. Solid waste palm oil;

Typically solid waste palm oil sediment is used as a fuel to produce steam for electricity
generation in order to generate energy. After combustion, an ash is estimated about five percent
by weight of solid waste (Foo & Hameed, 2009). Palm Oil Fuel Mill Fuel Ash is a solid waste
residue which is produced by the combustion of palm nut and fiber of palm at high temperature
bout 800 o Cto1000 o C. The palm oil mill fuel ash has spongy & porous structure in nature with
angular and irregular component form (Yusuf, et al., 2015; Ho, et al., 2012; Chong, et al., 2009;
Chandara, et al., 2010;) The palm oil mill fly ash can also be utilized for the removal toxic gas
for example sulphur oxide nitrogen oxide and etc. The activated compound (zeolite) adsorbent
can also synthesis from palm oil mil fuel ash because it contains high concentration of silica,
alumina, potassium and etc. which is used for the removal of contaminants particles from water
(Yeliz, 2010; Moises., et al., 2013).

v. Cotton linter fly ash;

Cotton linter is also play an important role in the synthesis of zeolite. Mostly two types of zeolite
nanofibrous and ZSM-5 are synthesis by cotton ash. Zeolite socony mobil-5 due to its high
efficiency is used as a catalytic cracking for the conversion of methanol to gasoline (Ivanova et
al., 2007). Nanofiber zeolite has plenty of mesoporous with which special adsorption and
catalytic properties are expected (Zhang et al., 2011).

vi. Red mud;

Red mud is produced during production of alumina (Al2O3) from Bayer process by Bauxite ore.
It contains high levels of both (i) toxic heavy metal and (ii) alkaline metal therefore Red mud is a
hazardous solid/liquid waste of alumina industry. The amount of Red mud production depends
on the crude Bauxite ore which is 1 to 1.5 time greater than the volume of alumina. The liquid
Red mud from alumina processing plant is the major reason of environment pollution because it
is usually disposed into reservoirs (Liu et al., 2009). Red mud is nano particle. The particle size
of red mud is >1 millimeter. Due to small particles size dry red mud easily spread into the air and
causes dust pollution and its often cause irritation for skin and eyes. From the previous literature
it is show that red mud contains a large amount of oxides such as; Fe2O3, Al2O3, SiO2, TiO2,
NaO, K2O, CaO, and sometimes a high concentration metal elements like Vanadium and gallium
and some others radioactive elements (Liu et al., 2009; Yang & Xiao, 2008; Huizhi et al., 2009;
Muduli et al., 2010; Kavas, 2006; Kalkan, 2006; Acosta et al., 2002; Sglavo et al., 2000). Mostly
red mud is used as a raw material for the cement production industries to avoid its solid waste.
Due to high toxicity level Red mud is used in zeolite synthesis, because it contains high
alkalinity level which considered valuable raw material for zeolite synthesis. Zeolite is
economical method for the utilization of red mud waste.

2.2. Methods involved in the synthesis of zeolite;

A variety of methods such as hydrothermal reaction with pre-fusion method (Shigemoto

et al., 1993; Lizcano-Cabeza et al., 2015; Berkgaut & Singer, 1996; Rayalu et al., 2000; Belviso
et al ., 2015; Shigemoto et al., 1994; Belviso et al ., 2012; Belviso et al ., 2011; Chang & Shih,
1998), fusion method (; Molina & Poole, 2004; Chang et al., 2000; Yao et al 2009; Zhang et al.,
2011), hydrothermal and conventional method (Komarneni et al., 1992; Inada et al., 2005;
Molina & Poole 2004; Li et al., 2005; Alkan et al 2005; Cundy & Cox 2005; Loiola et al., 2012),
fusion and hydrothermal process (Holler & Wirsching, 1985; Querol et al., 2001; Shih & Chang,
1996; Querol et al., 1997; Murayama et al., 2002; Tanaka et al., 2003; Querol et al., 1995),
molten-salt method (Park et al., 2000; Park et al., 2000 ) and methods employing microwaves
are used for the synthesis of zeolite(Katsuki et al., 2001; Querol et al., 1997; Inada et al., 2005
Slangen et al., 1997). Recently modern technique ultrasonic wave has also been used in the
synthesis of zeolites (Wang et al., 2008; Park et al., 2001; Wu et al., 2006 Andac et al., 2005).

i. Pre fusion method;

In this method first of all fly ash sample pre-fused with NaOH (1:1.2 wt ratio) was stirred
for some hours at room temperature with a solution of [2,3,7,8,12,13,17,18-octakis(ethylthio)-
5,10,15,20-porphyrazinate] copper(II) in chloroform. Then hydrothermal treatment applies on it.
The crystallization is produced between 45 o C to 60 o C in 4 days. Temperature & time period
for the synthesis of different types of zeolite was given in the table 1 (Belviso et al., 2010;
Belviso et al., 2012). After heating we can separate solid and solution by using centrifugation
methods. At final stage solid particles washed with distilled water and dried in an oven at 80 o C
(Belviso et al., 2016). Zeolite of high purity product is obtained which has efficiency greater than
eighty percent and product is ready for usage.

ii. Fusion method;

 The fusion methods contain two stages (Molina & Poole, 2004). Typically one is alkaline
fusion and the second is alkaline hydrothermal process. High purity zeolite is obtained by this
method (Yao et al., 2015).

(a). Alkaline fusion method;

Alkaline fusion method was carried out at higher temperature greater than 500 C
(Shigemoto et al., 1993). In the first step alkali solution was mixed with fly ash ground with to
obtained homogeneous mixture. Then the homogeneous mixture was heated in a glass crucible
ceramic at high temperature at 980 C for 1 h.

(b). Alkaline hydrothermal method;

The resultant fused mixture was cooled to room temperature, ground again and dissolved
in LiOH/H2O solutions with solid to liquid ratio 1:2 of different concentrations varying from 1 to
3M were used to explore the influence on products. Then, the resulting mixture was put into
autoclave which is made of stainless steel and a hydrothermal treatment was conducted. The
temperature of the reaction is set between 80 to180 C for 12h. The crystallinity of the zeolite
product was observed between different times 2 to 24h. At the end of the process, the solid
zeolite particle is separated by filtration, washed with distilled water and then dried at overnight
at 100 C (Yao et al., 2009).

iii. Hydrothermal, conventional method;

It is simplest and common method used for the synthesis of zeolite. Zeolite which is
synthesized by this method has low yield and transformation efficiency (Murayama et al. 2002;
Shigemoto & Hayshi, 1993). A lots of research used different method for synthesizing zeolites
from fly ash by hydrothermal alkaline conversion. (Park. et al., 2000a,b; Querol et al., 1995;
Hller & Wrisching, 1985; Singer & Berkgaut, 1995; Kolousek et al., 1993; Kato et al., 1986;
Bergk et al., 1987; Larosa et al., 1992; Park & Choi, 1995; Shih et al., 1995; Querol et al., 1997a;
Lin & His, 1995; Querol et al., 2001; Rayalu et al., 2000; Rayalu et al., 2001; Mondragn et al.,
1990). The classical alkaline conversion use combination of fly ash with different molarity of
base solution (NaOH/KOH) for 3 to 48 hours at 80 t0 200 o C in open air synthesize up to 15
different zeolites from same fly ash. The industrial applications of the zeolite are depends on its
type, pore size and capacity of cation exchange with molecules. Zeolite with large pore size
(greater than 7 A o) and high cation exchange capacity (5 meq g-1) are widely used in molecular
sieving. On the other hand zeolite with small pore size (2.30 A o) example hydroxysodalite has
low cation exchange capacity and not more applicable for molecular sieving (Berkgaut & Singer,
1996; Park & Choi, 1995; Singer& Berkgaut, 1995).
 A series of experiments is conduct for fly ash in various alkali solutions such as sodium
carbonate, potassium hydroxide and sodium hydroxide to clarify the mechanism of zeolite
synthesis. The synthesizing time, temperature and type of zeolite is shown in the table 1. From
the experiment it is noted that the rate of zeolitic reaction is affect by the concentration of ions
like potassium and sodium ion present in the alkali solution. When sodium and potassium ion
exist at the same time in the alkali solution, then the rate of crystallization of zeolite is decrease
with an increase in concentration of coexisted ion. The following Three step dissolution,
condensation and crystallization are common in hydrothermal reaction for the synthesis of every
type of zeolite. In previous study example (Yao et al., 2013) it is evaluate that hydrothermal
process proceeds at a low temperature without much amount of energy utilization and produced
high valuable industrial materials for ion exchange and gas adsorbent, etc. (Inada et al., 2004). In
hydrothermal process the production of crystallization in zeolite has a few problems because the
reason is that the nucleation rate is difficult to control which cause larger crystal size. Another
problem in hydrothermal process is long crystallization period normally one day for complete
crystallization (Li et al., 2006). Recently the conventional method has been improved by using
advanced method,`` as well as an alkaline fusion followed by hydrothermal treatment (Rayalu et
al., 2000).

iv. 2-step method/Fusion, hydrothermal method;

The authors used two-step process and the fusion assisted method. A 2-step process for
the synthesis of zeolite from fly ash was customized by Hollman (Hollman et al., 1999) whereby
a mixture of alkaline solution and fly ash was subjected to the ageing step and later on followed
by the hydrothermal treatment step. During the ageing step the mass ratio of sodium hydroxide
pellets to fly ash is 1:1. The water content after ageing is keep at constant molar ratio of 0.49
(H2O/SiO2).

The 2-step process consists of an aging step operated at 48 o C for 24 to 48 hours followed by
hydrothermal method at 140 o C. In the fusion assisted process however, fly ash is first fused
with NaOH at 550 o C then silica and alumina is extracted from the fused ash followed by
hydrothermal method. The fusion assisted process makes use of an electrical furnace operating at
550 o C. The Crystallization of the zeolitic product is achieved by introducing the slurry in sealed
Parr bombs in a thermo stated Memmert hot-air oven for a predetermined time and temperature.
The crystallization formed at 80 o C for 12 to 24h as shown in the table. This energy intensive
process would be likely very expensive to operate on an industrial scale (Musyoka et al., 2012b;
Musyoka et al., 2011a; Musyoka et al., 2012).

v. Molten salt method;

 Recently the molten is a new and alternative method for the conversion of fly ash in to
zeolitic material (M. Park et al., 2000). The purpose of molten salt method employs a salt
mixture instead of an aqueous solution as the reaction medium unlike the hydrothermal method
(M. Park et al., 2000). By applying simple thermal treatment in molten salt mixture a variety of
mineral waste including fly ashes is easily converted into zeolitic materials. Salt mixtures like
NH4F-NH4NO3, NaOH-KNO3, KOH-NaNO3, and NaOH-NaNO3, lead to the formation of
cancrinite and sodalite zeolites. The product yield of molten salt method is twice and minor
elemental losses as compared to the hydrothermal method (Park et al., 2000). Zeolite synthesize
by molten salt method (cancrinite & sodalite) has few important applications like fertilizer
additives, wide range of cation exchange capacity and soil conditioners. In this review, NaOH-
NaNO3 mixed with fly ash without any addition of water because molten salt is in liquid form
increase the diffusion rate of reaction. Then the resulting mixture is heated at high temperature
about 500 to 1000 o C to achieve high crystallinity in the zeolite product mostly an alkali metal
halide is used as the flux in the molten salt method (Walton 2002).

vi. Membrane preparation;

Membrane method due to the low cost and high selectivity is one of the most attractive
separation methods. Because membrane is an intervening phase acting as a passive barrier
between adjacent phases to it under a driving force. Zeolitic membranes have gained
considerable attention during the last decade (Noble &Falconer, 1995; Bein, 1996; Exter et al.,
1996; Matsukata &Kikuchi, 1997; Coronas & Santamaria, 1999; Tavolaro & Drioli, 1999; Caro
et al., 2000).
First of all fly ash and NaOH in equal mass ratio is added in laboratory scale ball mill for 15 to
20 mints to obtained homogenous mixture. Then the homogenous mixture is transfer into a
muffle furnace which is set at high temperature 550 o C and left to fuse for 90mints. The sintered
granules of fused fly ash after high temperature fusion are again ground by using laboratory scale
ball mill for15 to 20 mints to obtain a fine powder. Then resulting mixture of fine powdered is
aged by dissolving it in deionize water and stirring it magnetically at room temperature for more
than two hours. At final stage we can separate crystalline compound by filtering the fused fly ash
slurry using a Buchner Funnel or filter paper under vacuum (Zhou et al., 2014).

vii. Microwaves methods;

Microwaves are low energy electromagnetic radiation (EMR) with wave length range from one
meter to one millimeter and frequency between three hundred megahertz (100 centimeter) to
three hundred gigahertz (0.1 centimeter) (Pozar & David, 1993; Hitchcock &Timothy, 2004;
Kumar et al., 2004; Jones et al., 2013). Its well-known that dipole rotation in water molecule is
produced due to directly absorption of microwave radiation, which causes rapid heating of the
solution. From the previous literature it is stated that dissolution of fly ash is accelerate by
microwave radiation (Sun et al., 2006).

Todays microwave one of the most widely used comprehensive technique as

hydrothermal method for synthesis of fine powder oxides (Somiya & Roy, 2000). Microwave
assist hydrothermal is an effective method for the synthesis of zeolite from alumina-silica gel
precursor (Jansen et al., 1992). From the previous studies it is indicate that using of microwave,
shortening in the reaction time of the zeolitization of coal fly ash (Querol et al., 1997). The low
energy electromagnetic radiation broke the hydrogen bonds present in solution. So shorter-time
zeolitization is more applicable for industrial production because the longer reaction time
consumes more energy (Enomoto et al., 2001). For the preparation of zeolite by using
microwave treatment, first of all alkali solution mixed with fly ash in 500 ml Teflon flask stirring
it continuously with magnetic stirrer and conventional heating for 2 h in open atmosphere at 100
o
C. After conventional heating microwave radiation is continuously applying for 15 mints to
solution using house hold microwave oven. We Conventional and microwave heating processes
are combined in this study for the short-time microwave irradiation, the solution was not stirred
because crystallization of the zeolite product is starting.

viii. Ultrasonic treatment;

Ultrasonic is a sound wave with frequencies greater than the upper limit capable of being heard
for humans that is greater than about 20 kilohertz (https://www.britannica.com). Acoustic
cavitation the most important fact happens in sono crystallization technique. Ultrasound as a
wave is radiated through any substances. When ultrasound wave exceed through solid liquid
system it cause of stirring effect, which decreases the diffusion layer thickness and as a result
mass transfer improves (Boels et al., 2010; Shah et., 1999). For the preparation of wide range of
micro or nano particles Ultrasound has been successfully used (Feng et al., 2004). From previous
studies it is show that sonication improving the formation of semi crystalline to crystalline
phases and also increase the compressive strength & thermal stability of geopolymers by
accelerating alumina-silica dissolution. Strengthening the bonds in solid particle to gel phase
interfaces, enhancing the poly condensation process. The most essential method for enhancing
crystallization is ultrasonic cavitation. The cavitation method is also enhancing nucleation rates
and mass transfer with the consequent increase in crystal growth rates. The result of cavitation is
described in terms of the hotspot (Suslick et al., 1990) and electrical theories (Margulis
&Margulis, 2002). Shock waves produced from a cavitational hotspot region which cause high
velocity inter particle collisions in a solid liquid system.

Brittle solids are fragment into pieces which make surface area larger. Thus increase in
the reactive surface area cause substantial increase in chemical reactivity. The phenomena of
electric cavitation are a result of the electric double layer formation on the surface of the
cavitation bubbles. The region between gas and liquid phase of the cavitation bubble are
transformed many times during the movement of the bubbles. The pulsation of cavitation
bubbles cause increase in resonance radii, deformation and fragmentation with considerable
enhancement of chemical reactivity. Therefore ultrasonic treatment is considered better as
compared with conventional methods because it requires lower temperature and the shorter time
required for the synthesis of zeolite. Moreover the degree of zeolite crystallinity increases
through the sonication treatment (Park al., 2001; O. Andac et al., 2005).

ix. Replacing fusion with sonochemical treatment;

The first step in replacing fusion with sonochemical treatment was to attain the optimal
sonication time that would dissolve maximum amounts of silica and alumina species from the fly
ash in a minimum amount of time. The fly ash was sonicated for varying time from 5 to 30 mints
as shown in the table 1. Clear solution is obtained after sonication treatment which is analyzed in
order to determine the degree of dissolution.

Its basically modern technique which has numerous applications. It decreases induction period
and meta stable width (Li et al., 2006), improvement in the particle size and crystallization
growth and etc. (Amara et al., 2001; Abbas et al., 2017; Boels et al., 2010; Dalas, 2001;
Dennehy, 2003; Dodds et al., 2007; Guo & Jones, 2006; Guo et al., 2005; Kakinouchi et al.,
2006; Kordylla et al., 2008; Li et al., 2003; Nishida, 2004; Kultanen et al., 2009; Castro &
Capote, 2007; Lyczko et al.,2002; Kordylla et al., 2009; Miyasaka et at., 2006; Virone et al.,
2006). Furthermore with an increase in the ultrasound power, the average crystal size decreases
(Li et al., 2006; Kordylla et al., 2008; Castro & Capote, 2007; Wohlgemuth et al., 2010; Wu et
al., 2008). The most important phenomenon occurs in sonocrystallization is acoustic cavitation
which is explain in above.

3 Types of zeolite;

There are two types of zeolite, natural zeolite and synthetic zeolite. But I am focus on synthetic
zeolite. Over the past few decades years approximately more than 170 unique zeolites have been
synthesized and identified by the International Zeolites Association (IZA) (Worathanakul et al.,
2011). Recently many researchers have devoted themselves to the synthesis of zeolites with
different morphologies since the properties and catalytic performances of zeolites were generally
influenced by their sizes and shapes (Ocampoa et al., 2010; Zhang et al., 2011; Kosanovic et al.,
2011; Gao et al., 2012). It can be predicted that the zeolites would reveal better catalytic
performance in many reactions when they present in nano-size, due to the shorter channels and
larger external surface in comparison with the counterpart in block-size. Ivanova and coworkers
have synthesized nanofibrous zeolite socony moblie-5 zeolite and found that it is more active for
catalyzing methanol converting to gasoline (Ivanova et al., 2007).
 In fact, various types of zeolite can be prepared using different fly ashes, these including
NaA (Wajima et al., 2009), faujasite-X (Dalai et al., 1985),mordenite (Bajpai et al., 1981), ETS-
10 (Ng &Jei, 2009), Beta (Prasetyoko et al., 2006), ZSM-5 (Vempati et al., 2006), ZSM-12 (S.
Loiha et al., 2009) andZSM-48 (Wang et al., 1998)zeolites. However, only a few types of zeolite
have been successfully synthesized in nanometer scale (<100 nm with at least one dimension is
considered (Valtchev &Tosheva, 2013) from rice husk ash e.g. (Wong et al.,
2012),hydroxysodalite (Ghasemi et al., 2011),NaA (Ghasemi &Younesi, 2012)faujasite-X
(Ghasemi &Younesi, 2012), and EMT(Ng et al., 2015).Thus, the synthesis of nanosized zeolite
from this cheap and renewable silica precursor is worth to be explored further (Moliner et al.,
2014).

4. Characterization of zeolite;

Zeolite which is synthesized is examined by the following techniques. All this techniques are
used to determine the composition of material, structure elucidation and the percentage purity of
the zeolite product and etc. As we know that no single technique can be suitable to fully
elucidate the key steps of zeolite crystallization therefore we used multiple techniques as shown
below.

4.1. XRF analysis;

Its most widely used non destructive analytical techniques used to determine the elemental
identification, quantification composition of the zeolitic material (Alberti et al., 2007; Janssens et
al., 2000). It is such type of analysis art (Janssens et al., 2000) which depends on the emission
and characteristic of excited photon energies from inner atomic shells by an external source. The
spectroscopic analysis of the excited photons can be achieved by means of a simple low-power
Roentgen tube (Romano et al., 2005; Khusainov et al., 1999; Redus et al., 996).

This technique is called elemental mapping because it allows in principle building a map
of the distribution of each element. An excitation X-ray beam is produced by a compact and low
power tungsten anode generator is focused by a poly capillary X-ray lens and reaches the zeolite
sample going through a hole laser cut in the centre of the ring-shaped array of detectors.
Detectors move around the excitation beam and provide information about the geometry and
composition of the sample (Alberti et al., 2007). The chemical compositions of fly ash samples
can be determined using an X-ray fluorescence spectrometer (XRF; Philips PW 148 (Belviso et
al., 2015). The X-ray fluorescence analysis of the raw material can be divided into major and
minor chemical constituents. These chemical constituents are SiO2 (37.92%), CaO (6.21%), K2O
(5.35%), Al2O3 (3.42%), Fe2O3 (3.19%), P2O5 (2.50%), MgO (1.76%), SO3 (0.73%), Cl (0.38%),
TiO2 (0.27%), ZrO2 (0.09%), MnO (0.08%), Na2O (0.04%), CuO (0.03%), SrO (0.02%), Rb2O
(0.02%), ZnO (0.01%), Cr2O3 (0.01%), V2O5 (12.39%), NiO (11.34%), Nb2O5 (8.97%) and
As2O3 (5.27%). Raw material mostly containing SiO2, Al2O3, CaO, etc. was also reported by
researchers (Salih et al., 2015; Sata et al., 2010; Aziz et al., 2014; Salih, et al., 2015), but
difference in chemical composition may be caused by various operating systems of the raw
material.

4.2. XRD analysis;

Zeolite which is synthesis by the multi-step method is later analyzed by the X-ray diffraction
(XRD). X-ray diffraction is very fast analytical tool which is mostly used for identification of
crystalline phase in material and unit cell dimensions (Suryanarayana & Norton, (2013). It is
based on constructive interference of monochromatic X-rays and a crystalline sample. Its
working according to Braggs Law n=2d sin (Trepczyska & Szykowny, 2015).The integrated
intensities of the selected diffraction lines of the zeolites sample is provide better information
about the amount formed from given starting materials at different times (Belviso et al., 2015;
Musyoka et al., 2012; Inada et al., 2005).

The quantification and identification of mineral phases present in the raw material
(example zeolitic products) is carried out using quantitative X-ray diffraction (XRD) and X-ray
qualitative diffraction (XRD) techniques respectively. In first step sample is initially ground to a
fine powder and then mounted into sample holders. The sample is scanned step wise at angle 4o<
2 < 60o at intervals of 0.02o and counted for 0.5 s per step. Crystalline mineral phases present in
the samples is identified with the help of High score Expert software by comparing spectra with
the standard line patterns from the powder diffraction file database supplied by International
Centre for Diffraction Data (Ojumu et al., 2006). X-ray diffraction (XRD) measurements were
made from 2o to 64o at 2, using corundum as an internal standard (Belviso et al., 2011). XRD
result is different for each type of zeolite.

i. Difference between XRF and XRD;

X-ray fluorescence is used to analyzes for Chemistry while, X-ray diffraction is used to
determines the mineralogy
4.3. SEM

The morphology and structure of the zeolite synthesized were examined by a scanning electron
microscope (Zhou et al., 2014). A scanning electron microscope is a sort of electron
microscope that produce images of the zeolite product by scanning the surface with a focused
beam of electrons (Stokes, 2008).A final beam diameter of 100 A o was claimed and recording
was carried out by allowing the beam to pass through the specimen (zeolite sample) and then to
strike photographic paper which was scanned mechanically in synchronism with the beam of
electron (Oatley et al., 1966).Each zeolite type have different scanning electron microscopy
images and geometry (Chen et al., 2012). Scanning electron microscopy images with different
time show simultaneous fracture and transformation of amorphous glassy fly ash material into
fine particles of zeolite (Choi et al., 2001).

4.4. FT-IR

Fourier transforms infra- red spectroscopy is an analytical technique which is used to obtain,
infrared spectrum of given sample. Fourier transforms infra- red spectroscopy (FTIR) is used to
determine the functional groups present in the zeolite sample (Pavia et al., 2008). When infrared
radiation fall on the zeolite sample, due to the vibrations modes of atom present in the zeolite is
absorbed some radiation while other radiations is emitted, and spectrum is obtained which
shows the functional group and its percentage purity in the zeolite molecule (Jansen et al., 1984;
Coudurier, et al., 1982).

4.5. ICP-MS

Inductively coupled plasma mass spectrometry (ICP-MS) is a modern powerful and more
advance analytical tool for analyzing zeolite sample. It trace very small amount of element
present in the sample. An ICP-MS is the combination of both high temperature inductively
coupled plasma source with a mass spectrometer. The very first step in inductively coupled
plasma mass spectrometry is the introduction of zeolite sample with the help of tungsten boat
furnace sample cuvette. The method of introduction of sample depends on its physical
characteristics. There are numerous ways of sample introduction. The atom present in the zeolite
sample is converted in to its ions, which is later detected by the mass spectrometer. Inductively
coupled plasma mass spectrometry (ICP-MS) is used for both qualitative and quantitative
analysis which is told about, strength, weakness and structure of the detected elements. From the
previous literature it is stated that the percentage purity of the sample is more than ninety,
because ICP-MS is a powerful and accurate analytical technique. Every types of zeolite sample
is analyze by this technique (Fabre et al., 2011; Fabre et al., 2017; Becker B & Dietze, 2000;
Aydin & Soylak, 2010).
Conclusion

Fly ash concentration increasing day by day and its rapid increasing in concentration greatly
attract research attention, because fly ash waste is an environmental hazard and its disposal is a
financial problem for every developed country. As fly ash consist on forty to sixty percent
alumina and silica components, so we can utilize this waste and convert fly ash into useful
material namely zeolite which have numerous applications in water treatment , heavy metal
removal dye degradation and etc. This review shows that the synthesis and characterization of
zeolite with multiple methods. In this review, zeolite materials be synthesized by acid solution
and mixed alkali such as NaOH, KOH, LiOH, and etc. solution pretreatment from the fly ash.
The formation of zeolite was critically affected by the following factor such as concentration of
the mixed alkali, time, temperature and, Ph of solution. In this review following techniques such
as XRD, SEM, XRF, FT-IR, and ICP-MS are used to characterize the zeolitic products. The
crystal strength of the synthetic products increased with increasing concentration of the mixed
alkaline with different time temperature and Ph of solution. In previous publication
Conventional, Hydrothermal, Fusion methods, are mostly used but Ultrasonic and Micro wave is
very rare. But in this review I m utilizes all the possible methods, such as molten salt method,
conventional hydrothermal method, fusion method, membrane preparation Microwave and
ultrasound wave treatment and etc. Microwave and Ultrasound wave method is more beneficial
because it reduce the crystallization time, increased the crystal growth and efficiency of the
zeolite products. Zeolite is work on the base of adsorption phenomena which can be explained by
the Freundlich isothermal model and Langmuir model. Different type of zeolite can be synthesis
from Fly ash by using different methods as shown in the table. Zeolite which is produced by
Microwave and Ultrasound wave has high purity and its working efficiency is more than 90%,
then the zeolite produced by other methods.
 Table.1 shows different characterization techniques & synthesis methods of zeolite

Characterization Hydrotherm Hydrotherma Micro Ultrasonic Base Time Zeolit References

Morphology and al l + fusion wave wave e
chemical
temp temp temp temp type

XRF, XRD, SEM, 140 c - - - - - - NaOH 8h NaP1 Zhou, L. et

BET al., 2014

XRF, CEC, SEM, 90 c - - - - - - 2 NaOH 96h X Bukhari, S. S.

FTIR , ICP, et al., 2015
- - High - - - NaOH 2h A&X
-

2.45
- - - - GHz - - 2M 30mint & X
and NaOH 2h
500 W.
- - - - 100c Room
1 to 5 M
NaOH P
-
-

XRF, XRD, 100 c - - - - - 1M 24h M Aldahri, T. et

SEM,TGA/DTA , - NaOH al., 2016
PSD, BET, CEC, - - - - - - 4h Na-P
UST 1M
- - - - Room Room NaOH 3h p

- - 1M
NaOH

XRF, XRD, SEM, - - - - Room - - NaOH 24 h M& Tanaka, H. et

FTIR, CEC, FA , to vary al., 2008
EDTA , LTA , FAU

XRF, XRD, SEM, 80 c - - - - - NaOH 4 days X Belviso, C. et

ICP-MS, TG/DTA - al., 2011
- - - - 240 W; 35
- - kHz
NaOH 1h
25 TO 60
C
XRF, XRD, SEM, 45c - - - - - NaOH 1 TO 216 Zk-5, Belviso, C. et
MAS-NMR, ICP-MS, - h X, A al., 2015
SEM-EDS, ZK-5

XRF, XRD, - - - - - 100c NaOH 2h A Ojumu, T. V.

SEM,QXRD, ICP- - et al., 2016
AES, ATR-FTIR

XRF, XRD, SEM, 25 to 40c - - - - - 1.2 M 4 day A,X, Belviso, C et

EDS, VNIR, SWIR, - NaOH zk-5 al., 2015
ZK-5

XRF, XRD, SEM, 40 to 60c - - - - - 1.2 M 4day Cu(OE Belviso, S. et

EDS - NaOH SPz)- al., 2016
Zeolite

XRF, XRD, SEM, 70c - - - - - 3M 12 h LTA- Attari, M. et

BET , CEC, TGA - NaOH zeo al., 2017

ECE, XRD, 80 to 48c - - - - - NaOH 3 to 48 h A,X,Y Querol, X et

- ,KoH , ,P1, F al., 2002
of linde,
different faujasi
molarity te ,k-
chabaz
ite and
etc.

ZK-19, XRD, SEM, Room to 175 - - - - - NaOH 4 to 7 day P-1 to Donahoe, R.

KM-3 c - of P-22, J, & Ltou, J.
different zk-19 G, 1984
molarity

CEC, XRD, PVE, 80 to 200 c - - - - - 3M 3 to 48 h NaP1, Querol

ICP, AES , ICP-MS - NaOH A, X, Carceller, X.
KM, et al., 2007
chabaz
ite,
faujasi
te)

CEC, XRD, SEM, 180c - - - - - NaOH, 12 h A,X Yao, Z. T. et

- KOH, al., 2015
Na2CO3
,
NaOH/K
OH and
Na2CO3
 /KOH)

HR-TEM, FEI, BET, 80c - - - - - NaOH 24h 13 X Kongnoo, A.

SEM, ETD, XRD - different et al., 2017
molarity

- - 550 to 750c - - - 60 to 120

- - mint
-

XRF, XRD, SEM, - - Room temp - - - NaOH 12 to 24 h NaA Ameh, A. E.

ICP-MS, LTM-2 , - et al., 2016
LTM-4, FAU,
silicate1-ZSM-5,
MFI, MOR, CHA,
AFI, MIF

XRF, SEM, XRD 130 to 150c - - - - - 0.35 to 36 to 60 h Na-P1 Musyoka, N.

- 0.71M M.et al.,2012
NaOH

MTO, XRD, SONA- Vary - - - - - NaOH 24h SAPO Askari, S. et

SAPO-34, SEM, - -34 al., 2013
MCM-22, MCM-19, - - - - 200 c NaOH 1.5h SAPO
MCM-49, ZSM-5, - - -34
BZMS-5

XRF, XRD, SEM, - - 550c - - - NaOH 90 min A,X Du Plessis,

ATR-TTIR, AES - P. W. 2014

XRF, XRD, SEM, 80c - - - - - NaOH 12h X Belviso, C. et

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