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A. Title : Zeolite Synthesis from Rice Husk Ash (RHA)

B. Objectives : Synthesize Zeolite from RHA
C. Literature Review
Zeolite crystals are hydrated aluminosilicates with an organized structure that
have cavities and channels up to 2 nm in size that allow a lot of molecules to flow
through. Numerous alkali and alkaline earth metal cations, as well as certain
organic cations, can counteract the negative skeletal charge caused by the
presence of aluminum atoms in the zeolite structure. K+, Na+, Ca2+, Ba2+, and
H+ are the cations that are a part of the zeolite structure[1]. When combined with
a particular channel system, the chemical makeup of zeolites determines their
characteristics. Zeolites are porous substances that have been thoroughly
researched and used in a number of industries, including the petrochemical
sector, oil refinery, the manufacturing of drying agents and detergents, the
separation of gas mixtures, in ecology, new high-tech fields such as electronics,
optics, and sensor technology[2].
Large amounts of kaolinite minerals can be found in nature. Since it has special
properties like platy structure (ground aggregates that form primarily along the
horizontal axis, layered and flaky), chemical inertness, and particle size that the
presence of silica and alumina in clay-based raw materials provides suitable
conditions for use as a starting material for zeolite synthesis, kaolin with kaolinite
as the primary phase is widely used on an industrial scale. Kaolinite comprises
one tetrahedral silica layer and one octahedral alumina layer[2]. By reacting
calcined kaolin, also known as meta-kaolin, with sodium hydroxide solution, this
kaolin can serve as the primary source for the hydrothermal synthesis of zeolites.
Treatment of kaolin at high temperatures changes kaolinite to meta-kaolin. This
substance's interaction with sodium Zeolite formation from hydroxide is influenced
by kaolin impurities, aging duration, crystallization time, and NaOH concentration.
Accordingly, attaining the proper structure depends in part on the purity of the
kaolin [1]. Activation temperature, contaminants like iron, Si/Al ratio, quartz
concentration, and the raw material's initial crystallinity are other factors that
influence the synthesis of zeolite from kaolin [3].
The application of TiO₂ impregnated with fly ash zeolite material is an effective
approach to enhance the photocatalysis method for degrading ammonia
compounds. This technique inhibits the recombination rate of holes and electrons,
minimizes the potential for agglomeration by maintaining catalyst dispersion,
improves the adsorption capacity for pollutants, and simplifies the catalyst
recovery process [4]. Coprecipitation is one of several synthetic techniques that
can be utilized to produce zeolite [7].
There are two types of zeolites: synthetic and natural. Chemical compounds
known as synthetic zeolites share the same physical and chemical characteristics
as their natural counterparts. Zeolites can be synthesized utilizing materials
containing Si and Al. Aluminum packaging as a source of alumina and rice husk
ash as a source of silica are two resources that can be utilized to create zeolites.
Because of its poor cellulose and sugar content, rice husk is generally not advised
for use as animal feed. Rice husk ash is utilized in industry as boiler fuel and for
power generation. The percentage of rice husk ash ranges from 18 to 20%. Silica,
which makes up 85–95% of rice husk, is its primary component [5].
throughout 1257, Mount Samalas had volcanic activity, leaving behind volcanic
deposits all throughout the mountain range. Mount Samalas, which is now more
commonly known as Mount Rinjani, has twice had significant eruptions. Large-
scale volcanic eruptions result in the production of igneous rock deposits. Pumice

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is one kind of igneous rock that results from this volcanic activity.
describe pumice [6].
Data on Indonesia's petroleum reserves (proven and probable) show that there
were 3.8 billion barrels in 2019 with a 9-year reserves to production ratio (R/P) [5].
Alternative energy can be used to combat fuel oil scarcity (BBM).
Biodiesel is one of the options that some nations have begun to develop as an
alternative energy source to address the issue.
The development of biodiesel production started because it is simple, affordable,
and renewable [4].
Recent research has also demonstrated that sludge synthesis from rice husk
ash lessens the negative environmental effects of agricultural waste. For instance,
this process can lessen the accumulation of rice husk ash, which frequently
contaminates soil and water. Furthermore, sludge derived from rice husk ash has
found application in various industrial fields, such as wastewater treatment, air
filtration, and even renewable energy. Therefore, in addition to producing new
products with added value, the process of turning rice husk ash into sludge aids
in the more sustainable management of agricultural waste. [8]
In the past, rice husk ash was mostly used in the building industry to make
cement and concrete, for example. Concrete is made stronger by the silica in rice
husk ash, which acts as a binder. Nevertheless, its potential has also been
acknowledged in the waste treatment industry, where sludge made from rice husk
ash can be used as an adsorbent to reduce soil and water pollution. [9]
Before 2020, the majority of research on rice husk ash's potential
applications was focused on how it might be used to produce concrete or
as a soil fertilizer in the building or agricultural sectors. However, initial Rice
husk ash has a relatively high silica (SiO2) content, according to study, and
can be used to create composite materials like sludge. The silica-rich rice
husk ash can be utilized to create sludge with potent adsorption capabilities
that can be used to absorb contaminants or hazardous substances from the
environment. [10]

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D. Methods
1. Experimental Tools and Materials
 Tools
No Tools Name Tools Picture Tools Tools
Function Category
1 Watch glass To weigh
samples of rice
husk ash. The
watch glass
was chosen
because it is
light and its I
slim shape
makes it easy
to fit onto the
scale.
2 Beaker glass Accommodate
samples of rice
husk ash and a
place to store
chemicals.
I

3 Measuring To measure the

cup volume of
liquids or
powdered
substances
I
with a fairly
good level of
accuracy.

4 Analytical Weigh
balance chemicals
accurately
without the
influence of
II
free air and
Weighing small
sample masses
with high
precision.
5 Drop pipette to transfer
liquid from one
container to
another in small I
amounts,
namely drop by

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drop.

6 Stirring rod Helps decant

solutions,
namely moving
solutions from
one container
I
to another while
leaving the
solids in the
original
container
7 Spatula for taking
materials in
small quantities
and small I
sizes.

8 Hot plate Heating

solutions or
chemicals,
Stirring
solutions or
II
chemicals,
Mixing or
homogenizing
chemical
solutions
9 Mortar to grind or
crush solid
materials into
powder or I
smaller shapes

10 Oven Ovens can be

used to heat at
various
temperatures II
with a high
degree of
accuracy

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11 Sieve (100 to filter

mesh) heterogeneous
solutions and
separate II
impurities in
laboratory
analysis
processes

 Materials
N Material Physical Chemical Categor
o s Name Properties Properties y
1 Samples - Thin flake - cellulose: 30- General
(Rice shape 50%
Husk
- The specific - hemi
Ash)
gravityof cellulose: 20-
rice husk is 25%
about 0,1-
- liginin: 10-
0,3 g/cm
15%
- The water
- silica content
content of
15-20%
rice husk is
8-12% - contains
minerals
- neutral rice
husk pH (6.5-
7.5)
2 KOH - Form: White - Nature: Special
crystalline Strong base,
solid. corrosive.
- Reactivity:
- Molecular Absorbs
Mass: 56.11 moisture
g/mol. from the air
- Melting and reacts
Point: About exothermicall
360°C. y with water.
- Reacts with
acids to form
water and
potassium
salts.
3 Al2(SO4)3 - Appearance - pH indicator: Special
: White, Changes
crystalline color
solid. depending on
- Solubility: the pH of the
Soluble in solution;

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water, forms colorless at

acidic pH below 8.2,
solutions. pink at pH 8.2
– 10, and red
- Melting
at pH above
Point:
10
Decompose
s before - Stability:
melting. Stable under
normal
conditions,
but may
decompose
when
exposed to
high light or
heat
- Does not
react with
water but
interacts with
hydroxide
(OH-) ions in
alkaline
solutions
causing
discoloration
4 Aquades - Liquid form - Chemically Special
- Colorless neutral (pH 7)
- Universal - Does not
solvent react except
- Boiling point with reactive
100°C at 1 compounds
atm - Used as a
pressure solvent in
- Freezing various
point 0°C chemical
reactions

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2. Experimental Work Scheme

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E. Result and Discussion

1. Result
Group 5
No Treatment Observation Result
1 Grinding rice husk ash using a Weight 7,5 grams
mortar and pastle, then
weighing it
2 Dissolve KOH(s) KOH(s) = 1,5 grams
Aquadest = 5 mL
3 Dissolve Al2(SO4)3 Al2(SO4)3 = 1,875 grams
Aquadest = 5 mL
4 - Mix the KOH solution - Foaming and emitting gas
with Al2(SO4)3 - After heating the sample
- Heated in a water bath thickers
while stirring until the
solution becomes thick
5 Then dried in the oven at 151oC Into activated charcoal wiyh a final
and observe the changes that weight after drying of 50,1089
occour grams

Group 6
No Treatment Observation Result
1 Grinding rice husk ash using a Weight 7,5041 grams
mortar and pastle, then
weighing it
2 Dissolve KOH(s) KOH(s) = 4,375 grams
Aquadest = 5 mL
3 Dissolve Al2(SO4)3 Al2(SO4)3 = 1,875 grams
Aquadest = 5 mL
4 Mixing KOH solution with Solution occurs slightly viscous the
Al2(SO4)3 and rice husk ash mixed
5 The solution is heated using a Solution becomes viscous
water
6 Drying the viscous mixture in an Sample mixture becomes dry and
oven af 150oC solid

Group 7
No Treatment Observation Result
1 Grinding rice husk ash using a Weight 7,5 grams
mortar and pastle, then
weighing it
2 Dissolve KOH(s) KOH(s) = 3,75 grams
Aquadest = 5 mL
3 Dissolve Al2(SO4)3 Al2(SO4)3 = 1,875 grams
Aquadest = 5 mL
4 Mixing KOH solution with Solution occurs slightly viscous the
Al2(SO4)3 and rice just ash mixed
5 The solution is heated using a Solution becomes viscous
water
6 Drying the viscous mixture in an Into rice husk ash charcoal weighing
oven af 155oC 58,9812 grams

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2. Discussion
- Group 5
First, the rice husk was weighed at 7.5 grams after being pounded with
a mortar and pestle. By reducing the rice husk's particle size, this procedure
makes it easier to employ in subsequent steps, particularly the chemical
process. Potassium Hydroxide Dissolution (KOH) 5 mL of distilled water was
used to dissolve 1.5 grams of KOH. A strong base solution is created when
KOH dissolves, and this solution will be utilized in the reaction with aluminum
sulfate (Al₂(SO₄)₃). The purpose of this step is to supply an appropriate reaction
media.
Aluminum Sulfate (Al₂(SO₄)₃) Dissolution 5 mL of distilled water was also
used to dissolve 1.875 grams of Al₂(SO₄)₃. In the following step, this solution
was ready to be combined with the KOH solution. The reaction's source of
Al2+ ions is aluminum sulfate.
KOH and Al₂(SO₄)₃ Solution Mixing A reaction that creates foam and gas
happens when KOH solution and Al₂(SO₄)₃ solution are combined. This
indicates that the aluminum sulfate salt and the base (KOH) are undergoing a
chemical reaction. Following that, a water bath was used to heat the liquid while
stirring it to thicken the solution. In order to produce a more concentrated
solution, the heating process speeds up the chemical reaction and water
evaporation.
Drying in the oven. After that, an oven was used to dry the reaction mixture at
151°C. At a final weight of 50.1089 grams, the mixture transformed into
activated carbon during the drying process. This method demonstrates that the
material has been transformed into activated carbon with a structure
appropriate for adsorbents and other specific uses.
The experimental findings demonstrate that rice husk ash carbon activation
effectively yields a substance with qualities appropriate for making activated
carbon. The structure and characteristics of the finished material are formed in
large part by the addition of KOH and Al2(SO4)3. The successful activation
procedure was indicated by the end weight's notable modifications.

- Group 6
Ash from rice husks used as the starting material for the carbon activation
procedure in this experiment. The first step was using a mortar and pestle to
ground the rice husk ash into smaller particles, increasing their surface area
and facilitating the subsequent reaction. The material weight as a result of this
grinding was 7.5041 grams.
The next step was to dissolve 4.375 grams of KOH had to be dissolved in 5
milliliters of distilled water as the next step. This KOH solution is utilized as an
alkaline substance that aids in chemical reactions that produce activated
carbon. Furthermore, 1.875 grams of Al2(SO4)3 were dissolved in 5 milliliters of
distilled water as an auxiliary substance to aid in the development of the
intended structure on activated carbon.
Drying the mixture at 150°C in an oven is the last stage. The viscous mixture
becomes solid and dry as a result of this drying. This procedure shows that a
stable structure was successfully produced in the activated carbon material.
Overall, this experiment shows that the use of KOH and Al 2(SO4)3 as supporting
chemicals, as well as the heating and drying methods applied, are effective in
producing activated carbon from rice husk ash. Observations at each stage
showed physical and chemical changes that support the process of activated
carbon formation.

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- Group 7
The rice husk ash was first ground with a mortar and pestle until it was
smooth, and then the weight of 7.5 grams was noted. In order for the
subsequent chemical process to proceed as smoothly as possible, it is crucial
that the ash has a consistent particle size.
Al₂(SO₄)₃ (aluminum sulfate) and KOH (potassium hydroxide) were then
dissolved. Five milliliters of distilled water were used to dissolve the 3.75 grams
of KOH and 1.875 grams of Al₂(SO₄)₃. The goal of this dissolution is to create
a uniform solution that will make mixing easier in the following stage.
The fourth step involved mixing the KOH solution, rice husk ash, and Al₂(SO₄)₃
solution. The substance that emerged from this mixing started to get a little
viscous. The mixture's elasticity or viscosity was probably brought on by
chemical reactions between these ingredients, specifically the creation of a gel
or binding substance.
Heating the mixture with water is the next step. It's believed that the purpose of
this heating is to speed up the chemical reaction or eliminate extra water to
make the mixture thicker. When the solution gets hotter, it gets more viscous,
which means that either the chemical reaction has advanced further or most of
the water has evaporated.
The last step involves drying the viscous mixture at 155°C in an oven. The
final weight of the charcoal made from rice husk ash after this drying process
is 58.9812 grams. The conversion of basic ingredients into a stable, dry final
product is indicated by this process.
Overall, this experiment shows a systematic method for using rice husk ash to
produce charcoal products by heating it and causing chemical reactions.
There is a noticeable shift in mass from the starting material to the finished
product, suggesting that the process is effective.

F. Conclusions
The process of converting the high silica in RHA into porous zeolites is
known as synthesizing zeolites from rice husk ash (RHA). Rice husks are used
to produce RHA contained in silica, and then this silica is examined using a
basic solution, such as sodium hydroxide (NaOH), to make a sodium silicate
solution. This solution is then compared with an acid, resulting in amorphous
silica.
In conclusion, this silica was formulated using an alumina source and a
basic solution to produce a zeolite precursor. This mixture was dissolved in
water (during the hydrothermal process) to form zeolite crystals. The results
are discussed, evaluated and characterized to ensure the quality and structure
of the zeolites. Zeolites from RHA are widely used as adsorbents, catalysts,
and ion exchangers, utilizing agricultural products to create high-quality
products.

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G. Bibliography

[1] Foroughi, M., Salem, A., & Salem, S. (2021). Characterization of phase transformation
from low gradekaolin to zeolite LTA in fusion technique: Focus on quartz melting and
crystallization inpresence of NaAlO2. Materials Chemistry and Physics, 258, 123892.
https://doi.org/https://doi.org/10.1016/j.matchemphys.2020.123892
[2] Kalvachev, Y., Todorova, T., & Popov, C. (2021). Recent Progress in Synthesis and
Application of Nanosized and Hierarchical Mordenite—A Short Review. In Catalysts (Vol. 11,
Issue 3).https://doi.org/10.3390/catal11030308
[3] Kirdeciler, S. K., & Akata, B. (2020). One pot fusion route for the synthesis of zeolite 4A
using kaolin.Advanced Powder Technology, 31(10), 4336–4343.
https://doi.org/https://doi.org/10.1016/j.apt.2020.09.012
[4] Setyaningsih, S., & Dewanti, B. A. (2022). Sintesis Dan Karakterisasi Zeolit Mordenit
(MOR) Secara Hidrotermal Menggunakan Kaolin Dan Abu Sekam Padi Sebagai Sumber
Silika. Molluca Journal of Chemistry Education (MJoCE), 12(1), 23-32.
[5] Ulfa, S. N. S., & Samik, S. (2022). Artikel review: pemanfaatan katalis zeolit alam teraktivasi
dalam sintesis biodiesel dengan metode esterifikasi dan transesterifikasi. UNESA Journal of
Chemistry, 11(3), 165-181.
[6] SINTESIS DAN KARAKTERISASI KOMPOSIT TiO2/ZEOLIT SEBAGAI FOTOKATALIS
PADA DEGRADASI AMONIA DI DALAM AIR LIMBAH
[7] Li, Y., & Xu, Z. (2021). Sustainable synthesis of adsorbent sludge from ricehusk ash:
Application of natural binders. Journal of Cleaner Production, 296,126601.
[8] Rahmawati, R., & Harsono, T. (2022). Potensi Sintesis Lumpur dari Abu Sekam Padi untuk
Pengolahan Limbah dan Aplikasi Industri. Jurnal Teknologi Lingkungan, 27(3), 88-96.
[9] Sudarno, D., & Santoso, M. (2016). Pemanfaatan Abu Sekam Padi dalam Industri
Konstruksi dan Lingkungan. Yogyakarta: Penerbit Gadjah Mada.
[10] Suryanto, A., & Purnomo, D. (2019). Pemanfaatan Abu Sekam Padi dalam Sintesis
Material Adsorben untuk Pengolahan Limbah Cair. Jurnal Teknik Lingkungan, 34(1), 45-53.

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H. Appendix
15 gr 7,5 gr ( sample )
Perbandingan Al2(SO4)3 : Aquades
1,875 : 5 mL
KOH : 5 mL
4,375 : 5 mL
3,75 : 5 mL

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