Group 3 Practicum Report

A. Title : Zeolite Synthesis from Rice Husk Ash

B. Objective : Students are able to synthesize Zeolite from Rice Husk Ash
C. Literature Review
The synthesis of zeolite from coal fly ash from PLTU Tanjung Jati Japara has
been carried out with hydrothermal alkali. Preparation is carried out on fly ash which has
been refluxed with 1M HCl and without reflux. NaOH solutions with certain
concentrations (2, 3, and 4 M) are mixed with coal fly ash with a ratio of 10 ml of solution
per 1 gram of fly ash into a 100 ml Teflon tube in an autoclave stainless steel. The
autoclave is then heated in an oven at a temperature of 120-1600C. The synthesized zeolite
was then tested qualitatively using Infrared Spectroscopy, X-ray Diffraction and SEM.
The results showed that NaOH concentration, temperature and time of hydrothermal alkali
process of coal fly ash affected the characteristics of zeolite products produced. Adequate
temperatures for the optimal hydrothermal process are in the range 140–160oC. The
increase in temperature causes the crystallinity of the resulting zeolite product to increase.
Hydrothermal synthesis products from fly ash are silica-alumina compounds, which are a
mixture of several crystals such as P zeolite, Y zeolite, Sodalite, Mullite and quartz [1].

Zeolite is an Aluminosilicate with a porous skeletal structure that is related to all

directions which causes the surface of the zeolite to be very wide so that it can be used as
an absorbent. In addition, the price of zeolite is relatively affordable, which is IDR 650 /
Kg. so that the application of zeolite as an absorbent material is very possible.
Experimental design or experimental design is an experimental design (with each step of
action that is truly defined) in such a way that information relating to or needed for the
problem being studied can be collected. In addition, experimental design is also defined
as a test or series of tests that aim to make changes to the input variables of the process or
system so that it can examine and identify the causes of changes in output [2].
Environmental pollution that occurs is mostly caused by waste from heavy metals
of an industry, especially the metal coating industry. Heavy metals such as cadmium
(Cd) are waste from metal coating which has a negative effect on living things. to
determine the effect of the use of zeolite in reducing levels of cadmium (Cd) waste from
the metal coating process. This study material is the ability of zeolite to reduce cadmium
(Cd) waste in the metal coating process. to optimize the mix of existing parameters and
variables and matters relating to the determination of waste quality standards so that they
can be disposed of into the environment. so this result suggests that zeolite provides
significant benefits for decreasing cadmium (Cd) metal coating waste [3] 

Interest in copper nanoparticles arises from the useful properties of this metal
such as the good thermal and electrical conductivity at a cost much less than silver, for
example. This leads to potential application in cooling fluids for electronic systems and
conductive inks.Due to plasmon surface resonance, copper nanoparticles exhibit
enhanced nonlinear optical properties, which could result in many applications in optical
devices and nonlinear optical materials, such as optical switches or photochromic glasses
metal when it has the form of nanoparticles In this work, we carry out the synthesis of
copper nanoparticles with specific attention to their future use in conducting inks [4].
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It is recommended for companies to overcome the problems that occur in

overcoming this waste, there must be the use of alternative materials that can be used to
overcome cadmium waste so that it can be disposed of into the environment and
according to the provisions of the ministry of environment without causing pollution and
damaging the ecosystem of other living things [5]

A common method has been carried out to reduce sulfur in fuel by conventional
hydrodesulfurisation (HDS) desulfurization techniques that require high investment to
reduce bound sulfur as aromatic organosulfur. Alternative technology for reducing sulfur
using zeolite adsorbents is quite promising due to ambient operating conditions and
simple technology [6]
The sulfur reduction experiments were carried out in batches with a temperature of
around 25oC and contact time of about 2 hours by shaking with a magnetic strirer with a
speed of 100 RPM and adding a number of zeolite weights to 100 mL of diesel fuel. The
use of Lampung and Malang natural zeolites in a sulfur reduction experiment in diesel
added as much as 1 g shows the sorpi capacity (q) of poor zeolite (0.58-0.60) greater than
float zeolite (0.12) which is in line with the decrease in sulfur (h) poor zeolite (7.17%) is
greater than Lampung zeolite (1.48%). The treatment of adding Ni metal into zeolite
increases the capacity of adsorption in decreasing sulfur in diesel fuel. The highest
increase in sorbsi capacity in addition was 0.5 g of Malang Ni-zeolite which was equal to
1.72 [7]
Crystaline silica is recognized as a material tahat can cause damage to respiratory
track and other tissues, and cancer according to the international agency for research on
cancer (IARC) announced in 1997.findding an appropriate utilization of the ash is
necessary to protect the environment and to decrease [8]
Rice husk ash (RHA), a by-product of rice mill industry, is one of the alternative
sources with high silica content and can be used for production of valuable materials and
chemicals. The silica in RHA is amorphous and transforms to crystalline silica when it is
heated at high temeratures. [9]
Have been done and this proved that ferrierite has a potential economical values.
The uses of low cost material such as rice husk ash in producing ferrierite will lower the
production cost of the product [10]
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D. Methode
1. Tools and materials
- Tools

No Name Figure tool Function Category

1. Lumping and pestle To smothing a rice husk ash I

2. Measuring cup To measure the volume of solution I

3. Sieve Used to sift the sample to get a finer I

powder

4. Watch glass Used to place substance to be weigh I

5. Analytic balance To Weigh samples and chemicals II

6. Oven To heathing samples II

7. Hot plate To heathing solution to thick II

8. Pipette drops To take small amounts of solution I

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9. Stirring rod To stir the solution I

10. Beaker glass As a forum solution and aquadest I

11. Spatula To take sample and chemicals powder I

- Materials

No Name Category Physical Properties Chemical

properties

1. Aquades General - Colorless clear liquid - Polar solvent

- Boiling point 1000 C - Is an Hion+, associated with
- Melting point 00 C OH-

2. KOH (kalium Spesific - Boiling Point 3270C - Solid Shape

hidroksida) - Melting Point 3600 C - Flammable
- Boiling Point 8200 C - Corrosive
- Density 90,5 gr / ml

3. Al2 (so4)3 Specific
- Density 2,672 gr / ml. - Not soluble in alcohol
Aluminium sulfate
- Melting point: 77,00C - Easy to dissolve in hot water
-Sweetness : Rather - Soluble in cold water
Heavy

4. Rice Husk Ash General - Fly ash contains chemical

- Whitish gray Ask
- Elements including : silica
- Very smooth which is (SiO2) Alumina (Al2o5),
aroun 100-200 mesh ferrous oxide (Fe2O3) an
calcium oxide (Cao)

2. Working Scheme

Start

- Considering 15 grams of Rice Husk Ash sample on the watch glass

- Considering KOH as much as 10 gr, 8.75 gr, 7,5 gr. In gach watch
glass and dissowed in 10 mL of distiled water
- Weight Al (SO4)3 3,75 gr for 3 comparisons above the watch glass
and dissolve in 10 mL aquadest
Group 3 Practicum Report

the sample turns into a

gel

Finish

E. Result and Discuss

1. Result

No Treatment Observations
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1. Weighing 5 grams of Rice Husk Ash with 3 5 grams each with 3 variants
compararisons

2. Weighing Al2 (SO4)3 as mush as 3,75 grams Weighs 3,75 grams in each variant

3. Dissolve with 10 mL aquades Hard to dissolve in distilled water

4. Weighing KOH as mush as 8,75 grams 7,5 Each with weight 8.75, 7,5 and 10
grams, and 10 grams grams

5. Dissolve into 10 mL aquadest Each is easily soluble in water

6. Mix the solution AL (SO4)3 and KOH with Initially white after adding Rice Husk
husk ash Ash to black

7. Heat the mixture a bath at 800C until it Black thickened solution

thickens

8. Dry in the oven -KOH 7,5 gr dried

-KOH 8,75 gr and 10 gr half a dried

2. Discuss
In the experiment of making calcium sulfate from limestone or limestone (CaCO3)
aims to obtain calcium sulfate (CaSO4) contained in limestone or limestone. Limestone or
limestone contains calcium sulfate (CaSO4) which is quite high.
Before filtering on limestone, the sample used must be finely ground first so that it is
easier at the moment of the earthing process. There is limestone used 60.4 mesh.
Limestone or limestone is easily evaporated because the magnitude of the particle radius
can affect the evaporation speed. The method used is to reduce the stone particles, the
function of ejection in this experiment is to remove carbon dioxide (CO2compounds) and
water (H2O)contained in limestone. So that the remaining solids are calcium oxide solids
(CaO).
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This experiment consists of several stages, namely the stages of sampling,

preparation, synthesis and qualitative testing. The sampling stage is the sampling activity
from the sampling location. Sampling is attemted to be taken in a representative area, which
is representative of all sampling sites. In this experiment sample were taken from Donggala
Village, West Distric, Gorontalo City.

Picture 1.The Maps Of Sampling

At the preparation stage, the sample is smoothed and sifted and then heated in the
furnace. Smoothing and sifting aims to reduce the sample particle size, so that the area of
the touch field or surface area is larger. So that it simplifies the synthesis process. The
function of size variation is to study the effect of size and surface area on the synthesis of
CaCO3 from limestone. The purpose of supplying is to eliminate the content of
H2Omolecules and compounds of CO2. So that the remaining solids are solids of calcium
monoxide or CO. According to the reaction equation as follows :
CaCO3(s) CaO(s) + CO2

In the experiment, 2 grams of samples were heated in a furnace at a temperature 900ºC for
one hour. Be heating by the high temperature because the melting point of calcium
carbonate is more than 800-900ºC .

Picture 2. After addition of Aquadest and HCl

Reactions that occur after the addition of distilled water and HCl :
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 Ca(OH)2 + 2HCl → CaCl2 + 2H2O

 CaO + 2HCl + H2O → CaCl2 + 2H2O

The function of adding HCl is to accelerate collisions between particles so that the
faster it reacts or dissolves. When adding HCl and distilled water which is insoluble with SiO 2
(silica) and MgO, t the reaction is:

CaO + SiO2 + H2O → Ca(OH)2 + SiO2

CaO + MgO + H2O → Ca(OH)2 + MgO

When the sediment is formed, then the sediment is filtered and the resulting filtrate is
concentrated using a bath not to form precipitates (picture 3). When precipitate is formed
stop heating and the drops with water reach no more deposits. After the evaporation
process, the filtrate is added with H2SO4 (while stirring)until the white precipitate is formed
(picture 4). The white precipitate formed is calcium sulfate deposits, where the reactions that
occur are:

                     Picture 3. The process of evaporation or heating

Picture 4. After adding H2SO4

After the screening process.Then the filtrate is added with H 2SO4 drop by drop until
white sediment is formed. The white precipitate formed is calcium sulfate. This process of
controlling is the last stage of the filtrate concentrated with H2SO4can be seen in picture 4
where the reaction that occurs is :
CaCl2 + H2SO4 CaSO4 + 2HCl

By using quantitative analysis methods based on the principle of weighing.

Gravimetric analysis is used in several fields including to find out a species of compounds
and the content of certain elements or molecules of a pure compound known to be based on
weight changes. Factors that cause the lack of yields of this sediment are the length of the
process of drying and the length of the process of drying the sediment, because the more
heated a sediment is heated, the less substance that is present in the solid, and will affect
the mass of the substance produced.

CaCl2 + H2SO4 → CaSO4 + 2HCl

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Picture 5. Calcium Sulfate produced

Then the sedimentis dried in the oven. This is intended to get calcium sulfate free
from hydrate.

Picture 6.Drying Calcium Sulfate and Calcium Sulfate

The deposite obtained from Calcium Sulphate are 7.3483 grams, the results are more than
previously weighed. This is because we weigh Calcium Sulfate that has not been completely
dried because the practicum time is up. And we also do not carry out this qualitative test of
this Calcium Sulfate.

F. Appendix
1. Conclusion
From the experiments that have been carried out in this practicum some conclusions
are obtained, namely:CaCO3 is heated with high temperature to produce CO2 and
CaO.and we make calcium sulfate from limestone with a deposit of around 7.3483
grams.
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G. Reference

[1] Merry Siska and Rudi Salam, (2012), Design Experiments on the Effect of Zeolite
on Decreasing Cadmium Waste, Industrial Engineering Scientific Journal,
Vol, 11, No, pp. 23-25.
[2] Winarno, F.G. 1997. Chemical Food and Nutrition. PT. Gramedia Main Library,
Jakarta
[3] Setiadji, A. H. B. 1996. Zeolites for Future Materials. Paper in the National
Chemistry Workshop, Yogyakarta
[4] Tsitsislivili, G.V., T.G. Andronikashvili, and G.N. Kirov. L.D. Filizova. 1992.
Natural Zeolites. Ellis Harvard, New York
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[5] Ahmahdi, (2013), Performance of Activated Natural Zeolites in Purification of Used

Frying Noodles in Tempe Chips, National Journal, Vol. 10, No. 2, pp. 34-
36
[6] Barrer, R.M (1982), “Hydrothermal chemistry of zeolites” london, academic press
[7] Bonnic, K.M.and cormier, E. (1999) “ Going green with zeolites”, Chemical
engineering progress
[8] Jamick, J.A. (1982), “Purifications of Rice Husk As a source of grade silicon for
cells” Journal of electrochem society
[9] Davis, M.E. (1998), “Zeolite-Based Catalyst For Chemical Synthesis”. Microporous
and Materials

[10] Rawtani, A.V, and Rao, M.S. (1989). “Synthesis Of Zeolite Using From Rice Husk
Ash”. Ind.Eng.Chem.Res

ATTACEHMENT
Group 3 Practicum Report