Salipur autonomous college, salipur

DSE- (IV) PROJECT YEAR -2022

TOPIC :- SYNTHESIS OF NANO SCALE BIOCOMPOSITES DERIVED

FROM AGRICULTURAL BIO WASTES

BY-_______________________

CLASS - +3 3rd YEAR, SCIENCE

ROLL NO -: _________________

AUTONOMOUS ROLL NO – ________________

PROJECT UNDER GUIDANCE OF:-

DR. ASIT PARIJA

READER IN CHEMISTRY

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HOD CERTIFICATE:
DR. PRADYUMNA CHOUDHURY, READER IN CHEMISTRY

HEAD OF HE DEPARTMENTOF CHEMISTRY

SALIPUR AUTONOMOUS COLLEGE, SALIPUR, CUTTACK

ODISHA

HOD CERTIFICATE

This is certified that , a student of +3 3 rd year science, chemistry (hons.) of Salipur

Autonomous College has successfully prepared the project on the topic “SYNTHESIS OF
NANO SCALE BIOCOMPOSITES DERIVED FROM AGRICULTURAL WASTE”. Under my guidance
and supervision for the academic year 2021-22.

Signature

Date:

Dr. Pradyumna Choudhury,

Reader In Chemistry

Head of Department of Chemistry

Salipur autonomous college, Salipur

2
 GUIDE CERTIFICATE
DR. ASIT PARIJA, READER IN CHEMISTRY

DEPARTMENT OF CHEMISTRY

SALIPUR AUTONOMOUS COLLEGE, SALIPUR

CUTTACK, ODISHA

This is certified that _________________ of 3rd year B.Sc. Chemistry

(Hons.) has prepared the report on the project entitled “SYNTHESIS
OF NANO SCALE BIOCOMPOSITES DERIVED FROM AGRICULTURAL
BIO-WASTE” is a bonafied work done under my supervision and
embodies the result of his contribution. The work has been done as
per the curriculum of B.Sc degree. This is testimony work done by
him. I personally wish him to get success in his life.

SIGNATURE:

DATE:

D R. ASIT PARIJA,

R EADER IN CHEMISTRY

D EPARTMENT OF CHEMISTRY

SALIPUR AUTONOMOUS COLLEGE, SALIPUR

3
 DECLARATION
Myself,____________________ , a student of +3 3 rd year science, chemistry(hons.) bearing
the Roll. No.___________ hereby declare that the project work entitled “SYNTHESIS OF
NANO SCALE BIOCOMPOSITES DERIVED FROM AGRICULTURAL BIO-WASTE ” submitted by
me for the partial fulfillment of the graduate degree in chemistry under SALIPUR
AUTONOMOUS COLLEGE is if original work and has not been submitted earlier either to
SALIPUR AUTONOMOUS COLLEGE or to any other institution for the fulfillment if any course

of study.

Name-___________________

Roll No.-_____________

Class: 3rd year B. Sc.

Chemistry (Hons.)

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 ACKNOWLEDGEMENT
It gives me great pleasure to express my gratitude towards our
chemistry teacher Dr. ASIT PARIJA for his guidance support and
encouragement throughout the duration of project. Without his
motivation and help, the successful completion of the project would
not have been possible.

I also pay my deep sense of gratitude to our beloved Principal,

Sangita Mishra and hardworking Head of Department,
Dr.Pradyumna Choudhury, for their permission to carry out the
project .I also thank Dr. Baishnab Charan Prusty, Mrs. Rina Swain
and Dr. Bhagyashree Pani for their timely help.

Above all I thank the Almighty for his blessing and my Father and
Mother for their support.

Name -

Roll No. -

Class –

Honors -

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 CONTENTS
SUBJECTS PAGE NO

1. Introduction………………………………………………………………7-8

2. Literature Review………………………………………………………9-10

3. Methodology…………………………………………………………….11-14

4. Characterization……………………………………………………….15-17

5. Analysis…………………………………………………………………….18-21

6. Conclusion………………………………………………………………..22-23

7. References……………………………………………………………….23-24

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 1. INTRODUCTION

 The word Nano comes from the Greek term “nanos” meaning a dwarf. More than

thousands of products based on nanotechnologies are already being used in

everyday life and many new nanoproducts are been expected to appear on the

market within the next few years. Since past couple of decades, numerous products

related to nanoparticles have been fabricated through various methods and are used

in many advanced technologies. There are different methods for nanoparticles

synthesis like chemical assisted, sonochemical reduction, pulse laser method and

green synthesis. [1]

 It has been shown that in the last decade nanotechnology plays a key role not only
in science but more and more often in industry as well. Recent researches have
shown that agricultural waste is a possible feedstock to produce nanocellulose which
can be used for different applications, such as a biosensor, semiconductor and
reinforcing agent. The use of agro-waste as a precursor not only offers advantages
for raw material costs, but also for the climate, low processing costs, availability and
convenience. It also helps to address environmental issues, such as illness, foul
odour and concerns with indoor use. Different processes, such as chemical
treatment, mechanical treatment and chemo-mechanical treatment, have been used
to extract nanocellulose from agro-waste. This article highlights the latest green
technologies used to acquire agro-waste nanocellulose, as well as existing advances
in and applications of nanocellulose technologies.[2]
 Nano-sized particles are characterized by their high surface-to-volume ratio, which
confers exceptional features on them. They are synthesized through physical,
chemical, or biological methods, that are classified into top-down and bottom-up
synthesis regarding whether the reagents are inorganic or are generated from the
break-down of a macroscopic material by some external agent. Several physical and
chemical methods like hydrothermal, sol-gel synthesis, laser ablation, or lithography,
among others, require special equipment and skilled labour.[3]

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 In addition, some of these techniques involve the use of toxic reagents that pose
health and environmental hazards. For instance, silver nanoparticles (AgNPs) can be
obtained by the reduction of a silver salt using strong reducers such as sodium
borohydride, which is an extremely irritant and corrosive agent with high
flammability risk.[4]
 Nowadays, green chemistry aims at the total or partial elimination of chemical waste
and the implementation of nontoxic reagents, environmentally acceptable solvents
and renewable materials, obtaining products with high thermal stability, low
volatility, and cost-effective production. Not only do these eco-friendly techniques
reduce the use of hazardous substances, but also employ natural renewable
compounds like polysaccharides, proteins, or those derived from vegetable extracts
(mainly leaves, roots, and flowers) and microorganisms like bacteria, fungi, and
algae, as reducing or capping agents.[5]
 Therefore, the three main concepts of nanoparticles green synthesis are the choice
of the solvent (preferably water); the use of an ecological reducing agent, GRAS
(substances generally recognized as safe), or natural reagents; and a nontoxic
material for nanoparticles stabilization (i.e., biopolymers). Products of natural origin
contain in their structure phenolic compounds, reducing sugar and nitrogen
compounds that can reduce metal cations to generate nanoparticles and, in certain
cases, can also act as stabilizers. In turn, the implementation of these compounds is
also advantageous from the economic point of view since they do not require high
temperatures conditions and reduce energy consumption.[6]

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2. LITERATURE REVIEW
Our goal is to find a way to deal with the problems mentioned above up to a certain extent,
with the literature review we carried out we are able to synthesize nano composites in a
green method from the sources of agro- waste like rice husk, rice straws, bagasse, coconut
coir, banana, pineapple leaf etc.

Agricultural residues for energy sources: a) rice husk, b) rice straws, c) baggase, d) coconut
coir, e) banana, g) pineapple leaf

Most of the chemical-mechanical methods are expensive & unaffordable. Hence, there are
not feasible at commercial level. There is a requirement of an effective method which can
be readily employed in laboratories as well as in industries.

Characterization methods like Transmission Electron Microscopy (TEM) analysis & Scanning
Electron Microscopy (SEM) of can show the formation of nano composites.

1) Florencia Ortega et. al. (Biobased composites from agro-industrial wastes and
by-products, 2021) in their study found that academic studies on composites obtained
from biopolymers, natural fillers and active agents, as well as green-synthesized
nanoparticles. In-depth discussion of biobased composites structures, properties,
manufacture, and life-cycle assessment (LCA).

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2) Shaik Rubeena Yasmin et. al. (Biowaste-derived Nanoparticles and Their Preparation: A
Review, 2021) their review deals with the synthesis of green synthesized nanoparticles
from various agricultural wastes. These NPs (Nanoparticles) transition between bulk
materials and atomic or molecular structures.
3) Anuj kumar et. al. (Characterization of Cellulose Nanocrystals Produced by Acid-
Hydrolysis from Sugarcane Bagasse as Agro-Waste) their study investigates the surface
morphology, topography, structural, elemental and thermal properties of cellulose
nanocrystals (CNCs) extracted by acid-hydrolysis.
4) Asghar Zamani et. al. (Agricultural waste biomass-assisted nanostructures: Synthesis and
application) Metal oxide nano porous materials and nanoparticles have main potential
uses in several different fields, such as nano electronics, biomedical science, renewable
solar energy, drug-gene delivery, thermal insulation, and so on. Agricultural waste
biomass-assisted synthesis is less costly, environmentally friendly and renewable
strategy, and therefore ideal resources for production of nanostructures.
5) Nur Athirah Abdullah et. al. (Nanocellulose from agricultural waste as an emerging
nanotechnology material for nanotechnology applications) concluded that use of agro-
waste as a precursor to nanocellulose offers advantages for raw material costs and
environmental concerns. Different processes, such as chemical treatment, mechanical
treatment and chemo-mechanical treatment, have been used. Their article highlights
the latest technologies used to acquire agro waste.
6) Nuraliah Ahmad Diah et al. (Processing and Characterisation of Banana Leaf Fibre
Reinforced Thermoplastic Cassava Starch Composites) studied that biocomposites
prepared by incorporating 10 to 50 % wt. of banana leaf fibre into the matrix of
thermoplastic cassava starch. The results showed significant increments in the tensile
and flexural properties of the materials, with the highest strength and modulus values
obtained at 40%.

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3. METHODOLOGY
(3.1) From Bamboo leaf

From ancient times bamboo was considered to have many applications such as food source
and building material. Bamboo species are native to warm and humid climates especially
areas in China, Japan, Korea, India, and Australia. Because of silica content of acid washed
bamboo leaf ash, it has also been used successfully as silica source in synthesizing of 13.8
nm sized SiO2 NPs by Venkatachalam and Rangaraj[8]. Based on nontoxicity nature of
bamboo leaf-derived SiO2 NPs, it has been proposed that these nanoparticles can be
considered as a potential candidate for drug delivery and other medical applications. In
2017, aluminosilicate zeolite A has been synthesized from bamboo leaf ash by Ng and co -
workers. The catalytic activity of biomass-derived zeolite A was tested in cyanoethylation of
methanol with 82% conversion and 100% product selectivity (Scheme 1). The recovered
catalyst could be reused at least nine times without significant loss in activity.[9]

Scheme 1.Zeolite A catalyzed cyanoethylation of methanol

(3.2) From Banana peel

In 2014, 20-50 nm Mn 3O4 nanoparticles have been synthesized using banana peel extract by
Yan and co-workers [10]. It is believed that banana peel extract plays a dual role, reducing
KMnO4 to form Mn3O4 and preventing the agglomeration of nanoparticles during the
preparation. Also 20 nm SiO2 NPs have been synthesized by addition of banana peel extract
to an alkaline solution of tetraethylorthosilicate in ethanol followed by calcination of
precipitate. These nanoparticles can be employed for the adsorption of methylene blue.[11]

Scheme 2. SiO2 NPs-catalyzed synthesis of pyrano[2,3-c]pyrazole derivatives.

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(3.3) From Coconut shell
In 2016, Asefa and co-workers prepared magnetic activated carbon by carbonization of
coconut shell in the presence of ferric chloride (FeCl 3⋅6H2O) under an inert atmosphere with
different FeCl3/coconut shell ratios [12]. The BET surface area, total pore volume and
average pore size of the resulted porous materials were 238-372 m 2/g, 0.118-0.210 cm3/g,
and 1.98-2.26 nm, respectively. Authors proposed that Fe 3O4 was formed via formation of
Fe2O3 and reduction of Fe (III) by carbon. It was shown that these nanomaterials are efficient
adsorbents for toxic dyes such as Sunset yellow. 10-100 nm sized Iron oxide nanoparticles
synthesized from coconut husk extract and ferric chloride by Sebastian and co-workers have
been used to remove Ca and Cd from aqueous media [13].

(3.4) From Wheat straw

Recently Patel and co-workers prepared 100-200 nm silica nanoparticles by calcination of

acid-washed wheat straw followed by treatment with NaOH solution and neutralization by
HCl [14]. This catalyst was studied in the synthesis of pyrano[2,3-c]pyrazole derivatives by
one-pot, four-component process of benzaldehydes, hydrazine hydrate, ethyl acetoacetate,
and malononitrile in an aqueous medium. In a separate study, Chen et al. described the use
wheat straw and Fe(NO3)3·9H2O to preparation of porous carbon-supported Fe 2O3 ultrathin
film by calcination of KOH-containing wheat straw under inert atmosphere followed by
addition of Fe(II) solution to aqueous mixture of calcined powder and annealing at 200°C
[15].

(3.5) From Egg shell

The eggshell is 95-97% calcium carbonate crystals, stabilized by a protein matrix and may be
considered as calcium source [16, 17]. In this regard, Jayasankar and co-workers prepared
Dy3+-doped calcium silicate (Ca2SiO4) nanoparticles by calcined waste egg shell and rice husk
through solid-state reaction technique at 1250 oC[18]. Dysprosium (III) ions-doped materials
are used in making laser materials, optical sensors and solar energy harvesting [19, 20].
Luminescence and excitation spectra of Dy 3+-doped calcium silicate were investigated and
the results indicate that the Dy3+-doped calcium silicate phosphors are appropriate for
production of low cost white light emitting devices. Hen egg shell has also been used

12
successfully to synthesize calcium oxide nanoparticles by Fulekar and Pandit [21]. Crushed
egg shell was decomposed to CaO above 800°C. Resulted calcium oxide was refluxed in
water and again calcined in furnace. The average size of calcium oxide nanoparticles were
found 75 nm based on XRD pattern. This nanomaterial was then studied as catalyst in the
transesterification of dry microalgae biomass (A. Obliquus) into biodiesel.

(3.6) From Sugar cane bagasse and leaves

Sugar cane bagasse (SCB) is the agricultural waste biomass of sugar and ethanol industries
that is abundantly available. Pereira and co-workers in 2015 reported a simple and low-cost
technique for modifying the textural properties and stability of mesoporous gamma-alumina
using bayerite as aluminum source and SCB as sacrificial template [22]. The effect of waste

biomass was evaluated by changing the template/ bayerite ratio. The presence of biomass as
a template improved surface area and pore volume up to 209 m 2/g and 0.44 cm3/g,
respectively. In addition, mean pore diameters are adjusted from 5.2 to 7.9 nm by varying
the template/bayerite ratio.

Due to high content of silica in SCB, Norhasyimi and co-workers prepared SBA-15 using acid
washed SCB ash as silica source and P123 as neutral template [23]. The BET surface area and
total pore volume of synthesized.

Pd NP @Si-C catalyzed carbonylative Suzuki reaction.

SBA-15 are 466 m2/g and 0.14 cm3/g, respectively. In a separate study, SCB has been used
for tuning the size of titanium oxide nanoparticles (TiO 2NPs) where the amount of biomass
template played an important role in size controlling [24]. TiO 2 sol from titanium
tetraisopropoxide in pH=4 was calcined under 200°C for 5 h resulted in TiO 2 powder gel.
Various amounts of SCB was added to this gel and stirred for 2 h at room temperature. SCB-

13
supported TiO2 NPs are in the range from 5–20 nm. The photocatalytic activity of SCB-

supported TiO2 NPs was tested in the degradation of azo dye methyl orange under visible
light. In 2018, Jabasingh and co-workers prepared 50-200 nm magnetic iron oxide
nanoparticles by co-precipitation of Fe(III)/Fe(II) in the presence of ammonia and sugar cane
bagasse under inert atmosphere followed by calcination in furnace [25]. This magnetic
material can be used as supports for adsorption of Cr 6+. Also, MgO hybrid sponge-like
carbonaceous composite has been synthesized using magnesium acetate and sugarcane
leafy trash as a sacrificial template by thermal decomposition method under N 2 flow [26].
This nanomaterial is comprised of nano-size magnesium oxide flakes and nanotube-like
carbon sponge with surface area and pore volume up to 40.61 m 2/g and 0.323 cm3/g,
respectively.

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4. CHARACTERISATION
(4.1)Fourier Transform Infra-red (FTIR) Spectroscopy

FTIR is a fascinating technique to evaluate structural variations on samples due to the

chemical treatments. The structural changes from SCB to CNCs were investigated by FTIR
spectroscopy using a Nexus Thermo FTIR (Thermo Nicolet, USA) spectrophotometer. The
samples were oven dried at 105°C for 4-5 h, mixed with KBr in a ratio of 1:200 (w/w) and
pressed under vacuum to form pellets. The FTIR spectrum of the samples was recorded in
the transmittance mode in the range of 4000-500 cm-1.

(4.2)X-ray Diffraction (XRD)

The structural (physical) analysis of the samples was evaluated by X-ray diffraction (XRD)
using a (Bruker AXS D8 Advance) diffractometer with a scanning rate of 5°C per min with Cu
Kα radiation source (λ = 1.54060 Å) operating at 40 kV and 30 mA. The XRD patterns were
obtained over the angular range 2θ = 5–60o. The Scherrer equation was used to calculate
the crystal size t (nm) of cellulose I structure in respect of (200) plane:

Where K is the correction factor and usually taken to be 0.91, λ is the radiation wavelength,
θ is the diffraction angle, and β1/2 is the corrected angular width (in radians) at half
maximum intensity.

(4.3)Thermal Analysis

TG (Thermo Gravimetry), DTG (Derivative Thermo Gravimetry) and DTA (Differential

Thermal Analysis) were carried out simultaneously by using EXSTAR TG/DTA 6300 thermo
gravimetric analyzer. The resolution of this instrument is 0.02μg as a function of
temperature. Runs were carried out at heating rates 10°C min−1 from ambient temperature
to 900°C (however 600°C shown in figures) under high purity nitrogen at a flow rate of
200ml min−1.Thermal analysis techniques such as thermo gravimetry (TG),

15
Derivative thermo gravimetry (DTG) and differential thermal analysis (DTA) were widely
used to measure the thermal stability and pyrolysis behaviour of polymers in different
conditions.

Figure 1. FE-SEM images of (a) sugarcane bagasse as raw-material; (b) de-lignified sugarcane bagasse; (c)
chemically purified cellulose fibres

Morphology and topography of cellulose nanocrystals: (a) field emission-scanning electron micrograph (FE-
SEM, 500 nm scale); (b)transmission electron microscopy image (TEM, 500 nm); (c) Atomic Force Microscopy
(AFM, 2 μm scale)

(4.6) Fourier Transform Infrared Spectroscopy (FT-IR)

FT-IR spectroscopy was used to detect the functional groups and chemical characteristics of
the material. The specimens used were in the measurement of 1mm(L) _ 1 mm (W) _ 3 mm
(T).The spectra of the samples were collected within a range of 4000 to 400 cm -1.

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(4.7) Field Emission Scanning Electron Microscopy (FE-SEM)

The surface morphology of cellulosic fibres and CNCs was examined using field emission
scanning electron microscopy (FE-SEM) (FEI Quanta 200 F, Netherland) microscope with an
accelerating voltage of 15–20 kV. Images showing surface morphologies of the cellulose
fibres and nanocrystals were taken at various magnifications. Before examination, a fine
layer of gold was sprayed on samples by an ion sputter coater with a low deposition rate.
Energy dispersive x-ray (EDX) diffraction attached with FE-SEM unit was used for elemental
analysis of CNCs.

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5. ANALYSIS
Figure 1 shows that the FE-SEM micrographs of the as received ground (30 mess screen) SCB
fibres having surface layers of a high percentage of extractives (waxes, pectin, oil etc.) Figure
2a, the de-lignified SCB with cleaner surface which confirms removal of lignin with some
other extractives after de-lignification with acidified sodium chlorite Figure 2b and the CPC
fibrils after the removal of hemicellulose with other residual extractives due to alkali
treatment Figure 2c and finally the CNCs extracted by acid-hydrolysis of the CPC fibres (as
shown in Figure 3a). Here, diameter and size of fibrils of purified cellulose was reduced to
great extent due to removal of all amorphous region of semi-crystalline cellulose leaving
nano-scale rod-like crystals. Figure 2c clearly shows the presence of fibres which are not
seen in Figure 2a and 2b. Figure 3(b) and 3(c) show the TEM and AFM micrographs of a very
dilute suspension of CNCs showing agglomerated ‘rod-like’ nanocrystals. The diameter of
nanocrystals has wide range of distribution but the size of most of the ‘rod-like’ nanocrystals
lies within the range 250-480 nm in length and 20-60 nm in diameter.

FT-IR Test
FT-IR spectroscopy is a technique of measuring the frequencies and intensities that a sample
absorbs based on the interaction between the IR radiation and samples that can be in the
solid, gaseous, or liquid state. These frequencies detect the chemical functional groups that
are responsible for the radiation absorption at different frequencies. FT-IR testing was
carried out to investigate the effect of reinforcing agents’ addition on the thermoplastic
starch. This also functioned to analyse the interaction between starch, fibre and glycerol.
Figure 2 displays the FT-IR data for TPCS reinforced with banana leaf fibre composites from
0 to 50% wt. of fibre content. In general, all the spectra of TPCS composites showed the
same pattern of bands. This finding exhibited that the amount of banana leaf fibre added to
the composites did not change or chemically affect the TPCS. A similar finding was reported
with the study by Sanjay et al. who reported that the native sugar palm starch (SPS) had a
similar spectrum with the agar spectrum. The stronger interaction between the components
of the polymer blends can be identified at a lower wave number. Based on Figure 2, both
pure TPCS and TPCS with banana leaf reinforcement displayed the same broad bands from
3200 to 3500 cm-1, which indicated the presence of O–H groups due to the hydroxyl groups

18
found in lignin, cellulose, and hemicellulose in the banana fibre. This finding showed that
the starch had high sensitivity towards water molecules due to the presence of hydroxyl
groups, and was also attributed to the hydroxyl groups stretching due to hydrogen bonding
between the molecules. However, it was noticeable that the O–H bond peak shifted to a
lower wave number when the fibre content was increased. Specimen with 0% fibre peaked
at 3288 cm-1, while specimen with 30% fibre peaked at 3281 cm -1. A similar O–H trend was
found in a previous study performed by Prachayawarakorn et al. [86] for both TPCS/kapok
fibre and TPCS/jute fibre. The O–H groups that appeared at 3300 to 3500 cm􀀀1 were
slightly shifted to lower wave numbers, which was attributed to the free, intra, and
intermolecular bound hydroxyl groups. This finding revealed that the formation of new
hydrogen bonds between the TPCS matrix and fibre existed. Thomas et al. [87] reported a
similar finding by indicating the presence of a hydrophilic O–H group at 3300 cm -1 which
proved the hygroscopic nature of cellulose.

Figure 2. FT-IR spectra of TPCS + banana leaf fibre.

Meanwhile, the presence of C–H stretching was recorded with the strong band within the
range of 2850–3000 cm−1 due to the vibrations of cellulose. This C–H band also
corresponded to the natural fibre components, which were cellulose and hemicellulose.
Other than that, the presence of anhydroglucose ring C–O stretching was found in the range
of 1000–1200 cm−1. This band was also attributed to the stretching of the C–O group from

19
lignin in the natural fibre. This finding was in agreement with a study by Hassan et al. (2019),
who also recorded a similar outcome with symmetric and asymmetric C–H stretching
vibrations at 2849 and 2917 cm−1, respectively, and the presence of C–O stretching between
980 and 1160 cm−1 in TPS/cellulose composite reinforced with PLA. Another study by
Jumaidin et al. also showed C–H stretching vibrations at 2900 cm −1 in cellulose and
hemicellulose, and also resembled the vibration from CH 2 and/or CH3 in a TPCS/CGF
composite.

The presence of C=O stretching can be found in the range of 1630–1740 cm −1. However, this
C=O peak could only be found in TPCS reinforced with banana leaf fibre samples and was
absent in the pure TPCS sample. According to Sgriccia et al. who obtained a similar outcome
with the kenaf and hemp fibre composites, the presence of C=O stretching might be
attributed to the presence of hemicellulose in the fibre. Another related finding in a study
by Lomelí-Ramírez et al. indicated the presence of carbonyl group vibration (C=O) at 1720
cm−1 in biocomposites of cassava starch with green coconut fibre reinforcement, and was
absent in the native starch sample.

FTIR ANALYSIS OF SCB

Direct information about changes in chemical functionality can be obtained by FTIR

spectroscopy which has been extensively used for structural analysis of the material before
and after chemical treatments. FTIR spectra of SCB as raw material, CPC and the CNCs
obtained by acid-hydrolysis. The spectral bands at 3175-3490 cm-1 (O-H stretching intra
molecular hydrogen bonds for cellulose I), 2850-2970 cm-1 (C-H stretching), 1730 cm-1 (C-O
stretching vibration for the acetyl and ester linkages in lignin, hemicellulose, pectin etc.),
1620-1649, 1512, and 1595 cm-1 (associated with the aromatic ring present in lignin and
absorbed water), 1250 cm−1 (C–O out of plane stretching due to the aryl group in lignin),
which are associated with the SCB before the chemical treatments. After chemical
treatment with acidified sodium chlorite and alkali treatment, these bands are not observed
in the FTIR spectrum of CPC. The effect of this chemical purification can be observed
through main spectral bands which must be emphasized at 1512 and 1250 cm−1. The band
at 1512 cm−1 is absent and the band at 1250 cm−1 is reduced drastically in the FTIR
spectrum of CPC.

20
21
However, FTIR spectra of CNCs having sharp bands but similar to that observed in CPC. The
spectral band observed in the spectra of CPC and CNCs in the region 1649–1634 cm−1 are
due to the O–H bending due to adsorbed water, 1430-1420 cm-1 is due to CH 2 scissoring
motion in cellulose), 1382-1375 cm-1 (C-Hbending), 1336 (O-H in plane bending) 1317 cm-1
(CH2wagging), 1054 cm−1 (C–O–C pyranose ring stretchingvibration), 902-893 cm−1
(associated with the cellulosic β-glycosidic linkages), ∼1155 cm−1 (C–C ring stretchingband) ,
and at 1105 cm−1 (the C–O–C glycosidic etherband ). The spectral bands observed at
1427cm-1 and 897 cm-1 shows significant cellulose I content. Incase of CNCs, spectral band
at 1375 cm-1 was very strongwhile spectral band at 1335, 1315 cm-1 overlap and and
diffused and other spectral band 1278-1285 cm-1 is weak and diffused. On comparing these
spectral data which revealed that CNCs are composed of crystalline cellulose I while content
of amorphous cellulose is negligible. These FTIR spectral peaks can be applied to analysis of
crystallinity of the samples consisting cellulose I or Cellulose II or mixture of both
components, andamorphous cellulose. According to ref. [46] 850-1500cm-1 region is
sensitive to crystal structure of the cellulosic material. Spectral bands at 1420-1430 cm-1
and 893-897 cm-1 are very important to elucidate to the crystal structure of cellulosic
material and its (1420/893 cm-1) spectral ratio and (1375/2900 cm-1) spectral ratio show
index of crystallinity [46] or lateral order index (LOI) and total crystallinity index (TCI)
respectively. In cellulosic samples, the spectral ratio (1430/897 cm-1) gives the evidence of
containing cellulose I fraction.

22
6. CONCLUSION
In this present study work we use agro waste material to synthesize novel nano bio
composites. These nano bio composites are characterized by using standard analytical
techniques. The synthesized nano bio composites was used in the treatment of water
contaminated with heavy metal ions and the result of our study clear indicate that our
synthesized nano bio composites was effective in the removal of chromium ion from waste
water.

The use of biomass and phytochemicals in the design and synthesis of nano bio composites
creates a significant connection between plant sciences and nanosciences that referred to
as “green nanotechnology”. Green nanotechnology emphasizes use of green chemistry
principles to the design and synthesis of nanostructure products and the application of
these nanomaterials. Many synthesis methods of nanomaterials include toxic chemicals, low
conversions, high energy necessities, and difficult, wasteful purifications; thus, there are
multiple opportunities to improve greener procedures for the synthesis of nanomaterials.
Many of the green chemistry principles apply readily to the synthesis of nanostructure
product. Advancement of clean and bio-based approaches to nanomaterials is one of the
most attractive fields of scientific and industrial researches in the recent years for the
growth of green technologies, namely bio-derived nanostructures that are compatible with
environmental necessities. Biomass derived materials with related uses (e.g., separation,
adsorption, catalysis, sensing, semiconductor materials and thermal insulation), will be
absolutely necessary for research and development for renewable resources based
fabrication especially non-extracted agricultural waste derived material synthesis. However,
recent developments in the environmentally friendly nano synthesis opened a novel
window to innovate new routes in large scale synthesis of thoroughly purified,
morphologically well-defined, and metal or organo-functionalized nanostructures. In this
article, an overview of the synthesis of agricultural waste biomass-assisted metal oxide
nanostructures, and their potential uses in different fields were presented. Despite the
growth over recent decades, substantial challenges exist that must be addressed to achieve
optimal efficiency and deliver maximum benefits from the complete and comprehensive
application of these agricultural waste biomass-assisted metal oxide nanostructures.

23
Sugarcane bagasse (SCB) can be utilized as source of cellulose for producing CNCs. The
preparation of CNCs was done in two steps of chemical treatments by chemical purification
and acid-hydrolysis. The chemical purification process through acidic sodium chlorite and
alkali treatment gives the white coloured chemically purified cellulose which was further
acid-hydrolyzed to extract CNCs. The morphology and topography of the nanocrystals were
characterized by FE-SEM, TEM and AFM. FE-SEM and AFM studies which showed supporting
evidence with TEM analysis for CNCs of nano-scale range. The CNCs were with average size
of ‘rod-like’ nanocrystals ranging from 250-480 nm for length and 20-60 nm for diameter.
Elemental analysis (EDX) showed 0.72 % wt sulfur impurity in CNCs along with other main
components. The structural changes were measured by FTIR and XRD, and thermal analysis
was measured by TG-DTG-DTA which revealed that CNCs showed lower thermal stability
and higher crystallinity (72.5%) as compared to native cellulose (63.5%). This investigation
shows that this chemical approach may be promisingly very efficient process for the
preparation of CNCs from SCB.

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