PROJECT

“SYNTHESIS AND CHARACTERIZATION OF ZEOLITE FROM WASTE

AND NATURAL MATERIALS”

Group 1:

1. Akhirunnisa Audina (4201131018)

2. Annisa Rahayu (4203131045)

3. Evaline (4203131036)

4. Gracia Kristy Tarigan (4201131003)

5. Miranda A. Sihite (4203131031)

6. Safirda Hasanah (4201131006)

Class : CESP 2020

Course : Physic Inorganic Chemistry

Lecturer : Lisnawaty Simatupang, M.Si

CHEMISTRY EDUCATION STUDY PROGRAMS 2020

FACULTY OF MATHEMATICS AND SCIENCE

STATE UNIVERSITY OF MEDAN

 FOREWORD
Assalaamualaikum Warahmatullahi Wabarakatuh

First of all, the author would like to thank and thank Allah SWT, who has provided health
and opportunity for the author to complete this project assignment paper. Shalawat and greetings
are also delivered by the author to our great prophet Muhammad SAW who has brought us from
the labeling era to this bright era.

The author also wants to express his gratitude to Ms. Lisnawaty Simatupang, M.Sc as a lecturer
in Physical Inorganic Chemistry who has guided the author in completing this paper. The
purpose of making this paper is to fulfill one of the mandatory IQF tasks for students of the
Chemistry Department, Medan State University. The project paper entitled "Synthesis and
Characterization of Zeolite from Waste and Natural Materials" is expected to add insight to
anyone who reads it.

The author realizes that there are still many shortcomings in writing this paper, so
constructive criticism and suggestions are really needed by the author. That's all that the author
can convey, more and less the author apologizes. Thank you for your attention and hopefully
useful.

Wassalaamualaikum Warahmatullahi Wabarakatuh

Medan, 25th May 2023

Author,

Group 1

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 TABLE OF CONTENTS
FOREWORD ............................................................................................................................................................ I

TABLE OF CONTENTS.............................................................................................................................................. II

CHAPTER I .............................................................................................................................................................. 1

INTRODUCTION ..................................................................................................................................................... 1

A. BACKGROUND ...........................................................................................................................................................1
B. PURPOSES.................................................................................................................................................................2
C. FORMULATION OF THE PROBLEMS ................................................................................................................................2

CHAPTER II ............................................................................................................................................................. 3

LITERATURE REVIEW .............................................................................................................................................. 3

CHAPTER III ............................................................................................................................................................ 5

PROCEDURE AND DISCUSSION ............................................................................................................................... 5

A. APPARATUS AND MATERIALS .......................................................................................................................................5

B. PROCEDURES .............................................................................................................................................................6
C. DISCUSSION ..............................................................................................................................................................6

CHAPTER IV.......................................................................................................................................................... 11

A. CONCLUSION ...........................................................................................................................................................11
B. SUGGESTION ...........................................................................................................................................................11

REFERENCES......................................................................................................................................................... 12

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 CHAPTER I
INTRODUCTION
A. Background
Zeolite is a solid in the form of hydrated aluminosilicate crystals composed of SiO 4 and
AlO4 bonded to one another. This arrangement forms a three-dimensional framework structure
that is tetrahedral due to the use of oxygen atoms together, causing the formation of
intracrystalline cavities. Synthetic zeolite is more frequently used because of the uniformity of
particle size and higher level of purity compared to natural zeolite. Various types of zeolite such
as zeolite X, A, P1, Y or ZSM-5 have been successfully synthesized from commercial or waste
silica sources with high silica content. Because zeolites are crystalline compounds composed of
microporous crystalline aluminum silicates, which are composed of tetrahedral TO4 (T=Si, Al)
with O atoms as neighboring tetrahedral links. To improve the silicate structure, the combination
of TO4 units (T=Si) in this way leads to silica (SiO2) which is an uncharged solid. At the joining
of Al in the silica framework, the +3 charge on Al forms a framework that has a negative charge,
thus requiring the presence of other cations (namely organic and inorganic cations) to produce a
neutral framework. Zeolite is a compound that can be synthesized from natural minerals with a
SiO2/Al2O3 molar ratio varying from 2.0 to 4.5. M2O.mAl2O3.nSiO2. Zeolites have various
applications in the environment such as heavy metal removal and photocatalytic degradation of
several organic compounds such as metronidazole, benzophenone, eriochrome blackT, and p-
nitrophenol. Natural zeolite has a high silica content, most likely occurs in the form of
amorphous and crystalline phases.

The use of zeolite requires a relatively high cost for the synthesis of zeolite. Therefore it
is necessary to have an alternative raw material for making zeolite, which can reduce preparation
costs and zeolite synthesis. One alternative for zeolite synthesis is derived from waste and
natural materials. Based on the journal, several materials use different materials and different
methods and parameters but also show significant synthesis results in the manufacture of
synthetic zeolite which can be applied to the environment as an adsorbent.

In research that utilized the remaining carbonation by-products which were waste
disposal, then synthesized into zeolite, it was found that the zeolite synthesis using carbonation
by-products produced the same type of porous and highly crystalline zeolite P, and the
conversion rate of the zeolite was also similar 65- 87% (based on TGA data). So that this
technology can be said to be a technology that is more economical and environmentally friendly.
Other waste materials such as coal fly ash (CFA), biomass ash (rice husk, bagasse ash), steel and
glass waste originating from industry and other sources can be used as basic materials in the
synthesis of zeolite.

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B. Purposes
1. To knowing the effectiveness is the synthesis of zeolite using waste and natural materials.

2. To knowing the disadvantages and dangers if zeolite synthesis using waste and natural
materials.

C. Formulation Of The Problems

Based on the background above, it can be formulated the formulation of the problem is :

1. How effective is the synthesis of zeolite using waste and natural materials?

2. What are the advantages, disadvantages and dangers of zeolite synthesis using waste and
natural materials?

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 CHAPTER II
LITERATURE REVIEW
Increased human activity in various industries so that in line with it a large amount of
wastewater is generated and discharged to environmental agencies. Wastewater often contains
pollutants including dissolved metals, organic and inorganic contaminants. Currently, adsorption
is considered as a simple and effective method for water treatment and wastewater treatment.
Various adsorbents including zeolites have been widely used to remove contaminants in water
and wastewater. The large adsorption capacity and high cation exchange capacity have made
zeolite a promising material for removing contaminants and environmental pollution. Today on
an industrial scale, zeolites are used as adsorption media, catalysis and as ion exchange as well as
removing metal ions from waste.

Zeolite is also one of the most frequently used adsorbents and can be used for various
purposes including color reduction and environmental pollution. Zeolite is a hydrated
aluminosilicate mineral with a structure characterized by a linked tetrahedral network, each
consisting of four oxygen atoms surrounding a silicon or aluminum cation. The structural
arrangement of these compounds gives rise to their many intermolecular channels and cavities,
so that their molecular dimensions allow species to migrate into the interparticle spaces. Zeolite
has excellent physical properties such as excellent hydration capacity, low density, and high
purity after water removal. Another characteristic of zeolite is that it has a stable crystal structure
and has a high cation exchange capacity, this is because the pores of the zeolite are almost
uniform.

Zeolites have various applications in the

environment such as heavy metal removal and
photocatalytic degradation of several organic
compounds such as metronidazole, benzophenone,
eriochrome blackT, and p-nitrophenol. Zeolite is
defined as a microporous aluminosilicate crystal with
a 3D framework consisting of [SiO4]4- and [AlO4]5- ,
connected by sharing of oxygen atoms. The general
chemical formula is M2/n: Al2O3: XSiO2:yH2O,
where M represents the cation. The following figure
is a zeolite structure.Zeolite is an inorganic material with a porous microstructure that has been
widely developed and used in many applications. The zeolite structure consists of a tetrahedral
network of [SiO4]4 and [AlO4] tetrahedrons, which are connected via oxygen spherical bonds to
form an open structure with empty holes. Various types of zeolite such as zeolite X, A, P1, Y or
ZSM-5 have been successfully synthesized from commercial or waste silica sources with high
silica content. Because zeolites are crystalline compounds composed of microporous crystalline

3
aluminum silicates, which are composed of tetrahedral TO4 (T=Si, Al) with O atoms as
neighboring tetrahedral links. To improve the silicate structure, the combination of TO4 units
(T=Si) in this way leads to silica (SiO2) which is an uncharged solid. At the joining of Al in the
silica framework, the +3 charge on Al forms a framework that has a negative charge, thus
requiring the presence of other cations (namely organic and inorganic cations) to produce a
neutral framework. Zeolite is a compound that can be synthesized from natural minerals with a
SiO2/Al2O3 molar ratio varying from 2.0 to 4.5. M2O.mAl2O3.nSiO2. The use of zeolite or
geopolymer as an adsorbent has been widely studied, this is because zeolite is environmentally
friendly and has high efficiency, stability, simple preparation method, excellent binding
properties, and low cost. Zeolites have various applications in the environment such as removal
of heavy metals and photocatalytic degradation of several organic compounds such as
metronidazole, benzophenone, eriochrome blackT, and p-nitrophenol. Natural zeolites have a
high silica content, most likely to occur in the form of amorphous and crystalline phases.

In addition, zeolite can be used as a medium to harden asphalt, stabilize soil, and remove
metal ions from waste. Silicon and/or aluminum from solid wastes can be used to synthesize a
number of useful zeolites, including Na-P1, Na-X, and Na-A. Natural zeolites have a high silica
content, most likely to appear in the form of amorphous and crystalline phases. The use of zeolite
requires a relatively high cost for the synthesis of zeolite. Therefore it is necessary to have an
alternative raw material for making zeolite, which can reduce the cost of preparing and
synthesizing zeolite, one of which comes from waste and natural materials. Another advantage of
using natural materials and waste is as an alternative to solving environmental problems.
Currently there are many researches on the synthesis of zeolite from waste, combustion residue
and natural materials. In the study which utilized the remaining carbonation by-products which
were waste waste, then synthesized into zeolite, it was found that the zeolite synthesis using the
remaining carbonation by-products produced the same type of porous and highly crystalline P
zeolite, and the zeolite conversion rate was also similar 65-87% (based on TGA data). So that
this technology can be said to be a technology that is more economical and environmentally
friendly. Other waste materials such as coal fly ash (CFA), biomass ash (rice husk, bagasse ash),
steel and glass waste originating from industry and other sources can be used as basic ingredients
in the synthesis of zeolite. Other basic materials that can be used are waste from the
optoelectronics industry. Silicon and/or aluminum from solid wastes can be used to synthesize a
number of useful zeolites, including Na-P1, Na-X, and Na-A.

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 CHAPTER III
PROCEDURE AND DISCUSSION
A. Apparatus And Materials
Apparatus:

 Beaker Glass

 Magnetic stirrer

 Ultrasound Electric Heater

 Microwave Electric Heater

 Whatman Filter Paper

 Measuring cup

 Stopwatch

 Drop pipette

 Stirrer

 Hydrothermal Reactor

 Porcelain cup

 Sieve mesh 80-100

 Pycnometer

 Watch glass

 Erlenmeyer pumpkin

Materials:

 Rice husk

 Sodium hydroxide

 Aluminum oxide

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  Hydrochloric acid

 Gypsum

 Aquades

B. Procedures
Work Procedures:

1. After obtaining the husk ash

2. Then the next process is the synthesis of zeolite with microwave.

3. Sodium silicate solution is prepared by mixing husk ash, water and NaOH.

4. The sodium aluminate solution is added to the sodium silicate solution

5. Then put it in the microwave at various temperature and time variations.

6. washing and filtering process until the pH of the solution is close to 7.

7. The characteristic test of this synthetic zeolite from rice husk ash includes a crystal
structure test with XRD

C. Discussion
Zeolite is a type of natural or synthetic material with a porous crystal structure that has
the ability to absorb and exchange ions. Zeolite is used in various applications such as water
purification, heavy metal removal, gas adsorption, oil and gas recovery, catalysis and so on.
Making zeolite from waste is an interesting approach because it can convert waste materials into
materials that have added value. Glass waste, for example, contains silica which is the main raw
material in the manufacture of zeolite. Therefore, the use of silica precursors from glass waste
can be an environmentally friendly and economical alternative in the synthesis of zeolite.

The process of synthesizing zeolite from waste generally involves several stages such as
initial waste treatment, silica extraction, and further processing to form the zeolite structure. The
initial effluent treatment stage involves separating, milling, and drying the waste glass to obtain a
form suitable for silica extraction. Furthermore, silica is taken from waste glass through an
extraction process using a suitable acid or base solution. The silica obtained is then used as a
precursor in the synthesis of zeolite via the hydrothermal or sol-gel method.

6
 The characterization of the synthesized zeolite is very important to ensure the quality and
properties of the resulting zeolite. Several characterization techniques commonly used include
XRD (X-ray diffraction) analysis to identify the crystal structure of zeolite, SEM (electron
microscopy) analysis to view morphology and particle size of zeolite, BET (Brunauer-Emmett-
Teller) analysis to measure surface area and distribution zeolite pores, and so on.

In the context of manufacturing zeolite from waste using silica precursor from waste
glass, the potential is in reducing waste glass discharged into the environment, reducing
dependence on natural raw materials, and reducing environmental impacts associated with
manufacturing zeolite from conventional raw material sources. In addition, the resulting zeolite
can also be used in the various applications mentioned earlier, giving significant benefits in a
variety of industries and environments.

In addition to these benefits, the use of waste glass as a silica precursor in zeolite
synthesis can also provide added economic value. By using waste as a raw material, the cost of
zeolite production can be reduced because waste glass is usually available in abundance and
cheap. In addition, the use of waste as a raw material can also help reduce the use of valuable
natural resources.

However, in developing a process for making zeolite from waste, several technical
challenges may arise. One of them is the purification of silica from waste glass which may
require an efficient and selective extraction process to obtain silica of adequate quality. In
addition, selecting the right zeolite synthesis method and controlling the reaction conditions is
also important to obtain high quality zeolite with the desired structure and properties.

Rice husk ash (RHA) is a byproduct of rice milling and is rich in amorphous silica, which
can be utilized as a precursor for zeolite synthesis. The process of manufacturing zeolite from
rice husk ash typically involves several steps, including pre-treatment of the ash, extraction of
silica, and the synthesis of zeolite.

1. Pre-treatment of Rice Husk Ash: The raw rice husk ash may undergo pre-treatment steps
to remove impurities, such as organic matter and carbon. This can be done by washing,
calcination, or acid leaching. The purpose is to obtain a purified ash with a higher silica
content.

2. Extraction of Silica: The silica is extracted from the rice husk ash through a dissolution
process. Acid leaching is commonly used, where the ash is mixed with an acid solution,
typically hydrochloric acid (HCl) or sulfuric acid (H2SO4), to dissolve the amorphous
silica. The resulting solution is filtered to separate the soluble silica from the insoluble
impurities.

3. Synthesis of Zeolite: The extracted silica solution is then used as a precursor in the
synthesis of zeolite. The process can be performed using various methods, including

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 hydrothermal synthesis or sol-gel synthesis. In hydrothermal synthesis, the silica solution
is mixed with appropriate sources of alumina and alkaline or alkaline earth metal ions,
followed by heating in an autoclave at elevated temperatures and pressures. This
promotes the crystallization of zeolite with a specific structure. In sol-gel synthesis, the
silica solution is mixed with a templating agent and other precursors, and the mixture is
allowed to undergo hydrolysis and condensation reactions to form a gel. The gel is then
aged and calcined to obtain the zeolite.

4. Characterization of Zeolite: The synthesized zeolite is characterized using various

techniques to determine its structure, composition, and properties. Common
characterization methods include X-ray diffraction (XRD) analysis to identify the crystal
structure of the zeolite, scanning electron microscopy (SEM) to examine the morphology
and particle size, nitrogen adsorption-desorption analysis (BET) to measure surface area
and pore size distribution, and Fourier-transform infrared spectroscopy (FTIR) to study
the chemical bonding in the zeolite.

The manufacture of zeolite from rice husk ash offers several advantages, including the
utilization of a waste material, reduction in environmental impact by recycling a byproduct, and
the potential for cost-effective production. Zeolites have diverse applications, including catalysis,
adsorption, ion exchange, and separation processes, making them valuable in various industries.
Zeolites can be synthesized using a variety of natural materials and waste sources, offering
several advantages in terms of sustainability and cost-effectiveness.

1. Natural Materials as Precursors: Zeolite synthesis can involve the use of natural materials
rich in silica and alumina, such as clays, diatomaceous earth, and volcanic ash. These
materials contain amorphous silica and alumina, which can be converted into zeolite
through appropriate synthesis techniques. Natural materials as precursors offer the
advantage of being abundant, widely available, and potentially lower in cost compared to
synthetic chemicals.

2. Waste Materials as Precursors: Utilizing waste materials as precursors in zeolite synthesis

presents an opportunity for waste valorization and environmental sustainability. Various
waste sources, such as coal fly ash, rice husk ash, municipal solid waste ash, and
industrial byproducts, can be rich in silica, alumina, or other elements needed for zeolite
synthesis. By converting these waste materials into zeolite, not only can their disposal be
reduced, but valuable products with applications in various industries can also be
obtained.

3. Synthesis Methods: The synthesis of zeolite from natural materials and waste typically
involves processes such as dissolution, gel formation, and crystallization. The specific
synthesis method employed depends on the properties of the precursor material and the
desired zeolite type. Common techniques include hydrothermal synthesis, sol-gel

8
 synthesis, and microwave-assisted synthesis. These methods provide control over factors
such as temperature, pressure, reaction time, and composition to achieve desired zeolite
characteristics.

4. Characterization and Applications: After synthesis, the resulting zeolite is characterized

using techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM),
nitrogen adsorption-desorption analysis (BET), and Fourier-transform infrared
spectroscopy (FTIR) to assess its structure, morphology, surface area, and chemical
properties. Zeolites have diverse applications, including adsorption, catalysis, ion
exchange, gas separation, and wastewater treatment. The specific application of zeolite
depends on its unique properties and the requirements of the intended use.

The utilization of natural materials and waste in zeolite synthesis offers the potential for
sustainable and cost-effective production. By converting abundant and often underutilized
resources into valuable materials, this approach contributes to waste management, resource
conservation, and environmental sustainability.

Zeolite is an inorganic material with a porous microstructure that has been widely
developed and developed used in many applications. The structure of the zeolite consists of a
tetrahedral [SiO4]4 and [AlO4] network tetrahedrons, which are linked via oxygen spherical
bonds to form open structures empty hole. Various types of zeolite such as zeolite X, A, P1, Y or
ZSM-5 have been successfully synthesized from commercial silica sources or wastes with a high
silica content. Because of the zeolite a crystalline compound composed of microporous
crystalline aluminum silicate, which is composed of tetrahedra TO4 (T= Si, Al) with an O atom
as a tetrahedral link. To perfect the structure silicate, the combination of TO4 units (T=Si) in this
way produces silica (SiO2) which is a non-metallic solid loaded.

On incorporation of Al in the silica framework, the +3 charge on Al forms a possessive

framework negatively charged, thus requiring the presence of other cations (i.e. organic cations
as well inorganic) to produce a neutral framework [9] Zeolite is a compound that can be
synthesized a natural mineral with a SiO2/Al2O3 molar ratio varying from 2.0 to 4.5.
M2O.mAl2O3.nSiO2. The use of zeolite or geopolymer as an adsorbent has been widely studied,
this is because zeolite is environmentally friendly. as well as high efficiency, stability, simple
preparation method, excellent binding properties, and low cost. Zeolite has various
environmental applications such as removal heavy metals and photocatalytic degradation of
several organic compounds such as metronidazole, benzophenone, eriochrome blackT, and p-
nitrophenol. Natural zeolite has the highest silica content It may appear as an amorphous or
crystalline phase.

In addition, zeolite can be used as a medium to strengthen bitumen, stabilizing it soil, and
remove metal ions from the waste. Silicon and/or aluminum from solid waste can be used to
synthesize a number of useful zeolites, including Na-P1, Na-X, and Na-A. Natural zeolites have

9
a high silica content, most likely occurring in amorphous and amorphous phase forms crystal.
The use of zeolite requires a relatively high cost for zeolite synthesis. Therefore it is necessary to
have an alternative raw material for making zeolite which can reduce costs manufacture and
synthesis of zeolite, one of which comes from waste and natural materials.

Another advantage of using natural materials and waste is as an alternative solve

environmental problems. Currently there are many studies on the synthesis of zeolite from waste
disposal, combustion residues and natural materials. In research that utilizes by-product waste
the result of carbonation in the form of waste disposal, then synthesized into the obtained zeolite
data that zeolite synthesis using residual carbonation by-products yields the same type zeolite P
is porous and highly crystalline, and the zeolite conversion rate is also similar 65-87% (based on
data TGA). So this technology can be regarded as a technology that is more economical and
friendly environment. Other waste materials such as coal fly ash (CFA), biomass ash (rice husk,
bagasse ash), steel and glass waste originating from industry and other sources can be materials
basis in the synthesis of zeolite.

10
 CHAPTER IV
A. Conclusion
Zeolite is a solid in the form of hydrated aluminosilicate crystals composed of SiO 4 and
AlO4 bonded to one another. This arrangement forms a three-dimensional framework structure
that is tetrahedral due to the use of oxygen atoms together, causing the formation of
intracrystalline cavities. Zeolite is also one of the most frequently used adsorbents and can be
used for various purposes including color reduction and environmental pollution. Zeolite is a
hydrated aluminosilicate mineral with a structure characterized by a linked tetrahedral network,
each consisting of four oxygen atoms surrounding a silicon or aluminum cation. The process of
synthesizing zeolite from waste generally involves several stages such as initial waste treatment,
silica extraction, and further processing to form the zeolite structure. The process of
manufacturing zeolite from rice husk ash typically involves several steps, including pre-
treatment of the ash, extraction of silica, and the synthesis of zeolite. Zeolites can be synthesized
using a variety of natural materials and waste sources, offering several advantages in terms of
sustainability and cost-effectiveness. The utilization of natural materials and waste in zeolite
synthesis offers the potential for sustainable and cost-effective production. By converting
abundant and often underutilized resources into valuable materials, this approach contributes to
waste management, resource conservation, and environmental sustainability. Another advantage
of using natural materials and waste is as an alternative solve environmental problems. Currently
there are many studies on the synthesis of zeolite from waste disposal, combustion residues and
natural materials.

B. Suggestion
Suggestions for readers, the application in this study still requires further research and
requires tools and materials that are not easily available and requires adequate laboratory space
in its manufacture. suggestions for future researchers to make variations that are easier to apply
in everyday life. the synthesis of zeolite compounds from waste is certainly a good innovation to
save our earth from the increasing dangers of waste.

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 REFERENCES
Fitriyah., and Krisnandi, Y.K. (2023). Review : Sintesis Zeolit dari Bahan Alam dan Limbah
Buangan. Jurnal Serambi Engineering. 8(3): 6200-6207.

Kafillah, M., Nurlina., and Alimuddin, A.H. (2018). Sintesis Dan Karakterisasi Zeolit Analsim
Menggunakan Prekursor Silika Dari Limbah Kaca. JKK. 7(1): 73-78.

Syaifie, P.H., Wardhani, Kusumah, G.A.P., and Taufiq, A. (2019). Synthesis and
Characterization of Zeolite from Karawang Rice Husk Ash. Sains dan Terapan Kimia.
13(2): 89-98.

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