Zeolite synthesis from low-cost materials and environmental applications.

Under supervision of
Prof. Firasat Hussain

Submitted by:
Ankita
Examination roll no. - 22217746024
Department of Chemistry
University of Delhi
New Delhi - 110007

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 • Zeolites are hydrated aluminosilicate minerals made from
interlinked tetrahedra of [SiO4]4- and [AlO4]5-.
• three-dimensional crystal structure built from the elements
aluminium, oxygen, and silicon, with alkali or alkaline-Earth
metals (such as sodium, potassium, and magnesium) plus
What is water molecules trapped in the gaps between them.
zeolite? • General formula: -
• Ma/b[(AlO2)a(SiO2)y]. w H2O
Where a and y represent the total number of [SiO4]4- and[AlO4]
5-.

• Currently there are more than 200 type of zeolites which can
identifies by their Si/Al ratio in atomic structure of zeolite.
• When the Si/Al ratio of zeolite increase, thermal stability also
increases.
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 • Synthetic zeolites are highly pure with uniform crystal
size.
• Natural zeolite takes several days to decades to create,
while synthetic zeolites can be prepared in the laboratory
from a few hours to a few days with controllable pore
size.
Properties of • Tunable Pore Size: Synthetic zeolites offer the advantage
of tunable pore size, allowing for customisation to suit
synthetic specific applications.

zeolites • High Surface Area: Synthetic zeolites typically have a

high surface area per unit volume, providing ample
active sites for adsorption, catalysis, and ion exchange
reactions.
• Thermal Stability: Synthetic zeolites are thermally stable
materials, capable of withstanding high temperatures
without significant structural degradation.

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Methods used in
zeolite synthesis

1. Direct method
a) Hydrothermal method:-
most widely used method,
b) Solvothermal method
c) Ionothermal method

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 2. Alkali fusion method
It involves treating a source material containing silica and
alumina, such as kaolin, a strong alkali, typically sodium
hydroxide. This treatment leads to the formation of a fusion
mixture which is then heated to high temperature.
3. Microwave method
It uses microwave radiation to accelerate the synthesis of
zeolites. In this method, raw material and mineralizing agent
(NaOH) mixture exposed to microwave radiation.
It leads to faster heating rate.

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 Raw material for synthetic zeolite synthesis

• In contrast to natural zeolite, the use of industrial waste as a raw material for
zeolite synthesis has huge environmental significance.
• Some industrial wastes such as rice husk ash, coal fly ash, lithium slag, paper
sludge ash and so many can be used as raw materials for the zeolite ssynthesis
as they have a significant amount of silica/alumina content intheir composition.
• The main benefit of using different industrial wastes is that it can reduce
environmental pollution.
• Zeolites from kaolin and coal fly ash were found to be promising material and
potential for versatile applications.

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 1) Material required:- coal fly ash (source of alumina and
silica), NaOH, distilled water
2) Synthesis:-
• coal fly ash is used as the raw material

Synthesis of • no additional silicon-aluminium source is required

• Add 0.33 g NaOH and 3 mL distilled water to 1 g coal
zeolite NaP fly ash to adjust SiO2:Al2O3:Na2O:H2O =
5.2:1.0:5.0:100. The mixture was then transferred to a
from coal fly 100 mL stainless steel autoclave. The autoclave was
sealed and placed in an oven at 80–130 degrees for 6-72
ash hours.
3) Materials used for characterisation :-
• XRD:- D8 advance type diffractometer used.
• FTIR:- Spectrum Two type spectrometer using KBr
tablets.
• SEM:- JSM-7500F used

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 4) Result and discussion
XRD :-
Influence of SiO2/Al2O3 Molar Ratio
• SiO2/Al2O3 = 1.00, the crystallinity of the
NaP zeolite is insufficient.
• As the ratio increases the crystallainity also
increases.
Influence of Crystallization Temperature
• Crystallinity below 80 degree is insufficient
• As temperature increases, characteristics
peak of zeolite NaP appears.
Influence of Crystallization Time
• At 6 h, Coal fly ash does not react and
remains amorphous.
• When the crystallization time is 12–48 h,
NaP zeolite becomes the main crystalline
phase.
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 SEM Images FTIR results
• The morphology and average • band 3444 cm-1 is due to
particle size of the samples the vibration of Oh
were slightly different at group of absorbed water.
different SiO2/Al2O3 molar • In product spectrum,
ratios. 1644 and 3448 cm-1 is
• At a lower magnification, a assigned to vibration of
honeycomb crystal polymer OH groups.
can be observed • 438 cm-1 peak is of
• When the magnification is asymmetry stretching of
increased, about 4–7 μm Si-O or Al-O bonds
“cauliflower-like” aggregates • Peaks near 673 and 740
can be observed with an cm-1 is of symmetric
average diameter of less than vibration T-O-T ( T is Si,
1 μm. Al)

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 1) Material used:- kaolin (as source of aluminium and
silicon), NaOH, distilled water
2) Synthesis:- Hydrothermal reaction was performed at
115°C for 20 hours, the synthesis gel was prepared, by
mixing 2.53g of kaolin waste, NaOH and sodium
Synthesis of metasilicate. And series of experiments being done.
3) Material used for characterisation:-
zeolite NaP • XRD- diffractometer model X’Pert Pro used
from kaolin • SEM- a Philips SEM brand, model XL30, was used
• FTIR-Thermo-Nicolet Magna equipment 560 with 400
to 4000 cm-1

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 4) Results
XRD :-
Influence of SiO2/Al2O3 Molar Ratio
As the ratio increases, the characteristic
peak of zeolite NaP was seen.
Influence of Crystallization
Temperature
• At 100 C peak of zeolite NaP was seen.

Influence of Crystallization Time

• At 6h, no zeolite phase is form. By
increasing reaction time upto 48h,
characteristic reflection of zeolite NaP
are observed.

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 SEM Images FTIR results
• Kaolin consist predominantly • Strectching peakof OH at
particle with stacking booklet type 3697 cm-1 characteristic of
and pseudo hexagonal crystals. kaolin,.
(a&b) • 3420 and 1646 cm-1 band of
• Synthesized sample of zeolite vibration of OH group,
NaP identified by pseudo which describe to water in
spherical form, which form zeoliteic nature.
polycrystal with an average size • 435 cm-1 peak is of
of 7-9 μm. (c&d) asymmetry stretching of Si-
O or Al-O bonds
• Peaks near 680 and 745 cm-
1
is of symmetric vibration
T-O-T ( T is Si, Al)

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 Application of synthetic zeolites
1. Removal of ammonia nitrogen
from waste water (using NaP)
It mainly depends on the ion
exchange performance.
• Effect of absorbent dosage :-
When the amount of zeolite was
increased from 0.5 g/L to 40 g/L,
the ammonia nitrogen removal rate
increased and the adsorption
amount decreased.
• Effect of pH:- ammonia nitrogen
removal rate is proportional to the
pH from 3 to 7, and inversely
proportional to the pH from 7 to 10.

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 2) In agriculture
• The mercury adsorption by plants and its subsequent entry into the food chain can be
restricted using zeolites.
• Dealuminated zeolite Y helps in the removal of alcohol from beer while fatty acids
present in edible oil can be eliminated using zeolite X.
3) Removal of radioactive substances
• zeolites have the ability to accept some radionuclide such as 90Sr, 137Cs, 51Cr, 45Ca, and
60
Co. Zeolites such as Mordenite, has effectively removed 137Cs and 90Sr found in
contaminated soils
4) In detergents
• The growing awareness of the environmental damage created by the use of
polyphosphate-containing detergents caused detergent manufacturers to seek less
hazardous replacements. Zeolite A has proved to be a suitable substitute, and its current
application as a detergent builder represents a major success in direct use of zeolites as
ion exchangers.

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 Conclusion

• It was found that zeolites have versatile applications, although the

discussion was limited in environmental applications only.
• Cheap raw materials have been proven to produce good quality zeolites
compared to the use of relatively expensive materials.
• However,different methods have some limitations which need to be
control properly in future.

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 Thank You

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