1.

Synthesis and characterization of silica nanoparticle and their

application in waste water treatment

A Minor Project in partial fulfilment of the

Requirements For the degree of

BACHELOR OF TECHNOLOGY

IN

CHEMICAL ENGINEERING

Submitted by

S.NO SCHOLAR NO. NAME

1 201117004 ANUBHAV KUMAR
2 201117054 RAVENDRA
3 201117063 LOVEKUSH MEHTA
Supervisor

Dr. Jay Mant Jha

Department of Chemical Engineering

MANIT, BHOPAL

DEPARTMENT OF CHEMICAL ENGINEERING

MAULANA AZAD NATIONAL INSTITUTE OF TECHNOLOGY, BHOPAL

APRIL 2023
DECLARATION BY THE CANDIDATES
We hereby declare the project work entitled is our own work conducted under the guidance of Dr
Jay Mant Jha Sir, Department of Chemical Engineering, MANIT, Bhopal.

We further declare, to the best of our knowledge that the thesis does not contain any part of any
work that has been submitted for the award of any degree either in this institute or in any other
university without proper citation.

S.NO SCHOLAR NO. NAME

1 201117004 ANUBHAV KUMAR
2 201117054 RAVENDRA
3 201117063 LOVEKUSH MEHTA

This is to certify that the declaration made above by the candidate is true to the best of our
knowledge.

Dr. Jay Mant Jha (Department of

Chemical Engineering)
ACKNOWLEDGEMENT
Our deepest thanks to Dr. Jay Mant Jha Sir, the guide of the project for guiding and correcting us
at all stages of development of this project with attention and care.

Beside our guide we would like to thank our faculty members for providing us the much-needed
support and encouragement.

Lastly, we would also like to express our deep appreciation towards our classmates without
whom this project would have been a distant reality.
CERTIFICATE
This is to certify that following students has satisfactorily carried out some research at home and
submitted the report of ‘Synthesis and characterization of silica nanoparticle and their application
in waste water treatment’ in final year of Bachelors of Technology in Chemical engineering. It is
a genuine piece of work, carried out by them under my supervision.

S.NO SCHOLAR NO. NAME

1 201117004 ANUBHAV KUMAR
2 201117054 RAVENDRA
3 201117063 LOVEKUSH MEHTA

Dr. Jay Mant Jha

(Department of

Chemical Engineering)
Content

1 INTRODUCTION
2 MATERIAL & METHOD
3 RESULTS & DISCUSSION
4 CONCLUSION
5 REFERENCES
Synthesis and characterization of silica nanoparticle and their
application in waste water treatment

1. Introduction
In the recent times, with the ever growing technological progress comes an increase in
environmental concerns[1], [2]. contaminated water is one of the world's most serious
health and environmental issues, especially in poor and developing countries. Infectious
disorders such as typhoid, dysentery, diarrhea, cholera, hepatitis A, and polio are all
linked to the unavailability of clean water supplies. Across much of
the United States (U.S.), contaminated water remains a big issue. Contaminants in
drinking water such as disinfection byproducts, nitrate, arsenic, and radioactive
contaminants can increase the risk of birth defects and cancer[3], [4]. Nitrogen is an
essential nutrient for crops and is often added to agricultural fields for optimum crop
growth and yield[5]. However, the addition has its own environmental risks. In case of
limited crop growth due to environmental and chemical factors the influx of excess
nitrogen can cause residue of high amount of nitrogen in soil effecting next batch of
crops. Most of the residual inorganic N, especially that in the form of
nitrates, is water soluble and can be leached through the soil entering lakes or streams.
High nitrate levels in drinking water may lead to methaemoglobinemia (blue
baby syndrome) which can cause stomach cancer[5]–[7].

Pharmaceutical contaminant have become a major concern globally more specifically

active pharmaceutical ingredients(API) can have adverse effect on not just environment
but also on aquatic life and humans[8], [9]. Discarded unused drugs and releases from
factories can result in distribution of API in sewage water. In environment API can not
only effect but can also cause bacteria to develop resistances due to antibiotics in the
environment. Environmental bacteria are the origin of all known resistance mechanism,
we can conclude that driving force behind antibiotic resistance in human is mobilization
and selection of antibiotic resistance in the environment[10]–[13]. For example, in India,
Bangladesh and Pakistan three different vulture species were found to be extinct due to
Diclofenac and its metabolites. This decline was caused due to consumption of
Diclofenac by animals from waste streams who were then consumed by vultures causing
them to be infected as well[8], [14]. Conventional waste water treatment processes are for
macropollutants such as organic carbon, nitrogen, suspended solid, carbon and pathogens
from wastewater but are ineffective for removal of micropollutants such as API. Their
efficiency varies for such compound from negative to complete removal depending on
various factors such as physiochemical property, environmental condition and Influent
mass flow of the compound[8], [15].

As we discussed concern of emerging contaminant that is antibiotics because of its

potential danger due to bacteria resistance on humans and ecosystem there are some
antibiotic that are used for multiple benefits, one such widely used antibiotic is
tetracycline(TC) which is generally used medicines ranging 300 – 1000 mg/day[16], [17].
They are widely used as a veterinary antibiotic in aquafarms and farms for betterment of feed
efficiency and animal growth. TC are the second most produced and used antibiotic in the world
due to its low price and used. But as we know overdose of anything can have severe
consequences overuse of TC too has its cons which can lead to TC-resistant microorganism
which are dangerous for human health[18]–[20]. Since most veterinary antibiotics are soluble in
water, 17-90% of antibiotics ingested by animals are excreted through feces and urine, which are
used in several countries as fertilizer for agriculture. TC contamination of soil can be genotoxic
inhibiting seed germination of wheat plants. Hence TC has become a major concern for the
impact it can have on not just the ecosystem and aquatic life but also on human health as it can
cause several health risk such as liver damage allergy and teeth discoloration. Many novel
analytical method are developed by advanced research for detection of TC such as voltammetry,
luminescence, liquid chromatography and recently, carbon dots sensing[18], [21], [22].

Over the past few years there have been revelation that besides antibiotics there are unintentional
presence of pharmaceutical and personal care products (PPCP) at high concentration can have
adverse effect on aquatic organism. Personal care product helps us improve our daily lifestyle
quality whereas pharmaceuticals are used for treatment and prevention of human and animal
diseases[23], [24]. Both are used extensively in our day-to-day life which results in increase in its
release which has become a major concern. Organization such as European Union (EU) and
United States Environmental Protection Agency (USEPA) have been developing priority
 pollutant list for identification of different chemicals present in storm water and waste water
which can cause harmful effect on different water bodies which receive them including surface
water. Just detection on some chemical compound does not necessarily mean it will be harmful in
nature but when there is evidence that it can cause harm to the aquatic life then it becomes a
major concern. PPCPs are persistent and are not easily removed due to their physiochemical
properties which becomes a problem as without complete removal there are still risk present[24],
[25]. Many PPCP are biologically active which can have an impact on aquatic organism. The
biggest concern when dealing with PPCP in contaminated water is that they have toxic
implications and are designed specifically to maximize their biological activity and target certain
enzymatic or cell signaling mechanism. Besides aquatic life many PPCP find their way into the
environment after which it is possible for long range transport depending on characteristic of
environment and physiochemical property of compound. PPCPs are highly hydrophilic in nature
and have low volatility and are highly polar so they are they are mostly distributed through
aqueous transport and food chain dispersal[24], [26].

In India there is a rule that no water law can be enacted nationally the Constitution of India gives
the states the power to manage water hence the central Government task is limited to formulation of plans
for management and coordination of water resources only across state only. The only exception of this
rule is the Water (Prevention and Control of Pollution) act,1974 which prevents and control the
pollution of water by prohibiting the discharge of pollutants into the water system in excess of standard. It
also provides for setting up State Pollution Control Board (SPCB) and Central Pollution Control Board
(CPCB). IN 1975, the Water (Prevention and Control of Pollution) Rules,1975 was enacted as a sub-
regulation of the Water Act. The water (Prevention and Control of Pollution) Cess Act,1977 (the
“water tax act”) is another major law which govern the taxation of water consumed by municipalities and
industrial entities and the collection thereof. Under this act water meters must be installed by industrial
entities and municipalities and taxes must be paid on the basis of the amount of water used. In 1978, The
water (Prevention and Control of Pollution) Cess Rules, 1978 was enacted as a sub-regulation.

Some states and Union Territory have enacted their own regulation for groundwater resources
since there are no National regulation for the management of groundwater resources.
Seeing this the “Model Bill to Regulate and Control the Development and Management of
Groundwater” was enacted by the central government as a model for states and the Union
Territory to enact groundwater regulations. This model bill was amended in 1992,1996 and 2005.
According to this bill the state government should establish Ground water Authority and also
 recommends introduction of a permit system for ground water extraction and a registration
system of a well.

In this work we will extract and characterize silica nanoparticles using the acid leaching method
which will then be used for determining its application in waste water treatment.

2. Material And Method

Material: -
For the extraction of Silica nanoparticle from sugarcane bagasse we will require a
laboratory dryer for removal of moisture post soaking. A Grinder mixer for size
reduction. Muffle furnace for calcination. 62.5 ml 0.8M HCL for leaching. Distilled
water, deionized water. Filter paper for filtration. Agate mortar and pestle for
characterization.

Method: -
For extraction of silica nanoparticle from sugarcane bagasse we will use acid leaching
method. For this method we first washed the sugarcane bagasse and let it soak for 12hr
this will the contaminations such as sugar and soluble solids. After 12hrs we used a
laboratory dryer to dry the feedstock. This feedstock was then grinded in a mixer grinder
to obtain the bagasse in powdered form. This obtained powder was then calcinated in
muffle furnace (model 7013, Jung, BR) a 250°C for 3hrs, with heating rate of 5°C. From
this we will obtain ashes of sugarcane bagasse. This ash will then be leached with 0.8M
HCL using 5gm ash in 62.5ml of acid solution. The solution obtained was then washed
with distilled water and deionized water followed by filtration using a filter paper (filter
paper unifil C41) several times till PH7 is achieved after which the obtained silica was
then dried using laboratory dryer at nearly 100°C give or take 5°C
For 24hrs. the obtained powder was then crushed in a agate mortar and pestle so that it
can be further characterized. Fig. 1 shows a brief overview of the process for synthesis of
silica nanoparticle acid leaching method.
 Fig. 1.- Flow chart for synthesis of silica nanoparticle using acid leaching method.

3. Results and discussion

Fig. 2 shows The N2 adsorption/desorption isotherms of the silica prepared by acid

leaching method. The isotherms obtained were classified according to the presence or
absence of hysteresis between the adsorption and desorption curves[27], [28]. For both
prepared materials the isotherms were similar and typical of porous solids, presenting an
isothermal curve of type IV behavior. BJH was used to determine the pore size
distribution, presenting mean pore diameter values of 17 nm for the silica obtained by
method 1 and 4 nm for the silica obtained by acid leaching method[29].
Fig. 2 N2 adsorption–desorption isotherms of the powders prepared by acid
leaching method

Fig. 3 shows the XRD patterns of the raw materials, as well as the
materials prepared by the different purification methods. It is possible
to observe that in the different temperatures used in the preparation of
the raw materials (ash 1 850 °C and ash 2 600 °C), led to the formation
of materials with halos characteristic of amorphous materials, as well as
some crystalline peaks. Fig. 3 present broad halos characteristic of predominantly
amorphous materials, with some crystalline peaks concerned to K2O and at P2O5 oxides
(JCPDS 00-011-0526 and JCPDS 00-023-1301, respectively). After preparation via
different methods (method 1 and 2) the XDR analysis indicated that the
materials obtained by both procedures are predominantly amorphous.
 Y
3500

3000

2500

2000

1500

1000

500

0
12.1621
14.5487
16.9352
19.3218
21.7084

26.4816
28.8681
31.2547
33.6413
36.0279
38.4145

43.1876
45.5742
47.9608
50.3474
52.7339
55.1205
57.5071
59.8937
62.2803
64.6669
67.0534

71.8266
74.2132
76.5998
78.9863
81.3729
83.7595
86.1461
88.5327
90.9192
93.3058
95.6924
5.0023
7.3889
9.7755

24.095

40.801

98.079
69.44
Fig. 3 XRD patterns of the materials prepared by acid leaching method.

Fig. 4 shows the SEM images performed on materials obtained by different preparation
methods. In the sample obtained in the process it is possible to observe the structure of
biogenic silica, formed by the presence of agglomerates of irregular shapes, favored by
the raw material processing, as well as the presence of some spherical particles
distributed in a porous structure.
Fig. 4 SEM images of powders prepared by acid leaching method

Transmission electron microscopy (TEM) images of the silica powders obtained by the
different methods are shown in Fig. 5. In the sample obtained by leaching in HCl, Fig. 5 ,
the same morphology of the disordered three-dimensional network of silica nanoparticles
(agglomerates of nanoparticles) exhibiting a typical biogenic fibrous structure of the
sugarcane bagasse. Comparing the micrographs, it is possible to observe that the samples
present typical characteristics of the synthesis method. The samples prepared by acid
leaching show typical characteristics of the biogenic precursor, resulting in a lower
specific surface area.
 Fig. 5 TEM images of SiO2 nanoparticles prepared by acid leaching method.

4. Conclusion
The results obtained in this study indicate that the protocols developed for the
purification of the sugarcane bagasse ash is a successful approach to obtain SiO2.
whereas the silica nanoparticles obtained by acid leaching method (direct calcination and
leaching in HCl), exhibiting a biogenic structure characteristic of the sugarcane bagasse.
The microstructural characterization showed that nano-Si present similar morphology of
silica xerogel as well as additional characterization indicated that the prepared material
exhibit highly silicon rich with well-defined crystalline structure.

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