CHARACTERIZATION AND

PERFORMANCE ANALYSIS OF
COMPOSITION BIOPLASTIC
SYNTHESIS USING POTATO PEEL AND
CELLULOSE FROM PROSOPIS JULIFLORA

Submitted by

SANKAR D (REG NO: 312818203033)

KISHORE SINGH M (REG NO: 312818203701)

JEEVITHA D (REG NO: 312818203014)

In partial fulfilment for the award of the degree

Of

BACHELOR OF TECHNOLOGY

IN

CHEMICAL ENGINEERING

AGNI COLLEGE OF TECHNOLOGY,

THAZHAMBUR

ANNA UNIVERSITY, CHENNAI 600025

JUNE 2022
 BONAFIDE CERTIFICATE

Certified that this Report titled CHARACTERIZATION AND

PERFORMANCE ANALYSIS OF COMPOSITION
BIOPLASTIC SYNTHESIS USING POTATO PEEL AND
CELLULOSE FROM PROSOPIS JULIFLORA is the bonafide
work of SANKAR D (312818203033), KISHORE SINGH M
(312818203701), JEEVITHA D (312818203014) who carried out
the work under my supervision. Certified further that to the best of my
knowledge the work reported herein does not form part of any other
thesis or dissertation on the basis of which a degree or award was
conferred on an earlier occasion on this or any other candidate.

SIGNATURE SIGNATURE

Dr.P.Murugan Mrs. C.D Karthika

Assosiate Professor and Head of, Assistant chemical
engineering department,
Agni College of Technology, Agni College of Technology,
Thazhambur, Chennai-6000130 Thazhambur, Chennai-6000130.

Submitted for the project viva-voce held on

INTERNAL EXAMINER EXTERNAL EXAMINER

ii
 ACKNOWLEDGEMENT

We would like to express our deepest gratitude to the management of

AGNI COLLEGE OF TECHNOLOGY and would like to thank our
respected principal Dr.SRINIVASAN ALAVANDAR for his words
of inspiration and for providing necessary facilities to carry out on our
project work successfully. We are especially grateful to
Dr.MURUGAN, Head of the Chemical Engineering, for her words of
wisdom and her constant source of inspiration. We would like to thank
our Internal guide and our project coordinate Ms. C.D KARTHIKA
Assistant Professor, Department of Chemical Engineering who molded
us accordingly and gave valuable suggestion for completing our project
work successfully and also for guiding us at each stage of progress. We
extend our warmest thanks to all the faculties of our department for
their assistance and we also thank all our friends who helped us in
bringing out our project in good shape and form. Finally, we express
our sincere benevolence to our beloved parents for their perceptual
encouragement and support in all endeavors.

SANKAR D (Reg No:312818203033)

KISHORE SINGH. M (Reg No:3128183701)

JEEVITHA. D (Reg No:312818203014)

iii
 DEPARTMENT OF CHEMICAL
ENGINEERING AGNI COLLEGE OF
TECHNOLOGY, CHENNAI-600130
PROJECT WORK

Name of the student : SANKAR D

KISHORE SINGH M
JEEVITHA D

Register number : 312818203033

312818203701
312818203014

Degree and branch : B.Tech Chemical Engineering

Month and year of submission : JUNE 2022

Title of the project : CHARACTERIZATION

AND PERFORMANCE ANALYSIS OF COMPOSITE
BIOPLASTIC SYNTHESIS USING POTATO PEEL
STARCH AND CELLULOSE FROM PROSOPIS
JULIFLORA.

Name & Designation of the : Mrs.C.D. Karthika

Supervisor Professor ,
Chemical Engineering Department,
Agni college of Technology,
Chennai- 600130.

PLACE: CHENNAI
DATE:

iv
 ABSTRACT
Recently, environmental problems caused by petroleum-based
plastics have been increasing. Therefore, researchers have begun to
investigate new materials that may be alternatives to plastics.
Bioplastics are considered as green materials biodegradable plastic
can meet these needs and can easily be disposed to the
environment.

In this study, the bioplastic was produced from potato peel as the
food industry waste. Also, some properties of our bioplastic such
as water absorption capacity, strength and biodegradability were
analysed.

Therefore, to reduce food industry waste, potato peel can be used

in biodegradable bioplastic production. Also to enhance the
production cellulose from prosopis juliflora were used.

XRD, SEM, FTIR, and surface roughness analyses were used to

characterize, the mechanical properties, thermal properties and the
morphology of the starch bioplastics and composite bioplastic.

KEYWORD :

v
biopolymer, potato peel, cellulose, plasticizer, preservative,

vi
 TABLE OF CONTENTS

ACKNOWLEDGMENT
ABSTRACT

TABLE OF CONTENT

SYMBOLS AND NOTATION

1.INTRODUCTION 1

1.1 GENERAL

1.2 SOURCES AND THREATS

1.2.1 PLASTIC 2
1.2.2 PROSOPIS JULIFLORA 2

1.3 PROSOPIS JULIFLORA 2

1.4 TECHNIQUES INVOLVED IN BIOPLASTIC

SYNTHESIS 4

1.5 TYPES OF PLASTIC

1.5.1 Polyethylene Terephthalate (PET or 4
PETE)
1.5.2 Polyvinyl Chloride (PVC or Vinyl) 4
1.5.3 Polyethylene (PE) 5
1.5.4 Polypropylene (PP) 5
1.5.5 Polystyrene (PS or Styrofoam) 5

2.LITERATURE REVIEW 6

vii
3. MATERIALS WITH PROCESSE 9
3.1 RESOURCES USED IN EXTRACTION OF STARCH
3.1.1 POTATO PEEL 9
3.1.2 DEIONISED WATER 10

3.2 CHEMICALS USED AND PROCESSES IN

EXTRACTION OF CELLULOSE 11

3.2.1 ALKALI TREATMENT

13
NaOH
3.2.2 DELIGNIFICATION
13

H2O2
3.2.3 ACID HYDROLYSIS
13
HCL
H2SO4
HNO3
CH3COOH

4. BIOPLASTIC
16
4.1 INTRODUCTION TO BIOPLASTIC
16
4.2 TYPES OF BIOPLASTIC
16
4.3 RECENT ADVANCES IN BIOPLASTIC
17
4.4 SELECTION OF NANOPARTICAL
18
4.5 CHEMICAL USED IN BIOPLASTIC:
18
VINEGAR

viii
GLYCEROL
HCL
STARCH
CELLULOSE
TIO2
ZnO

ix
5. METHODOLOGY 21

5.1 APPARATUS USED USED 21

5.2 SAMPLE COLLECTION AND PREPARATION 21
5.3 PREPARATION OF STARCH 22
5.4 PREPARATION OF CELLULOSE 24
5.5 SYNTHESIS OF BIOPLASTIC 25

6. RESULTS AND DISCUSSION:

6.1 FTIR ANALYSIS 28
6.2 SEM ANALYSIS 32
6.3 XRD ANALYSIS 35
6.4 STRESS AND STRAIIN ANALYSIS 36
6.5 DEGRADEABILITY 37
6.6 WATER ADSORPTION 38

7. CONCLUSION 39
8. REFERENCE 40

x
SYMBOLS AND NOTATIONS:

Poly Propylene – pp
Poly Styrene - PS
Indian Institute of Bioplastics and Biocomposites – IIBB
Pol Lactic Acid – PLA
PolyButylene Adipatic Terephthalate – PBAT
PolyButylene Succinate – PBS
PolyCaprol Actone –PCA
Prosopis Juliflora -- PJ
PolyHydroxy Butyrate – PHB
PolyHydroxy Valerate – PHV
PolyHydroxy Hexanoate –PHH
Business Communication Company –BCC
Low Density Polyethylene – LDPE
High Density Polyethylene – HDPE
X-Ray Diffraction – XRD
Fouirer Transform Infra Red – FTIR
Scanning Electron Microscopy – SEM
 CHAPTER 1

INTRODUCTION

1.1 GENERAL INTRODUCTION

• We utilize the food waste as Bioplastic products because in
recent research for the first time following a study that detected
microplastics have been found in the human blood and High
concentrations of waste plastics have been found on seafloor
and snowclad areas In the arctic by transported through oceans.
• Our aim is to use Bio-plastics to replace the conventional
plastics in different sectors such as food packing, plastic plates,
cups, cutlery, plastic storage bags etc., and therefore can help in
making environment sustainable.
• Cellulose is also a essential constituent for our bio plastic which
can be extracted from Prosopis juliflora, the plant that sucks
more underground water, for the water conservation and
environmental protection that plant can be deforested.
• Potato peel is rich in starch which contains 25% starch and
also easy to access because of high production of potatoes
nearly 376million tones worldwide annually.

• Nano science and nanotechnology are the study and application

of extremely small things and can be used across all the other
science fields, such as chemistry, biology, physics, materials
science, and engineering.
• The present work green synthesis of TiO2 and ZnO nanoparticles
is based on the Prosopis Juliflora plant extract. Prosopis Juliflora
is also a recent medicinal plant ever known and a, which is also a
large mass plant species, the species is frequently cited in near
water resources.

xii
1.2 SOURCES AND THREATS
1.2.1 Plastic Threats:
The main sources of plastic debris found in the ocean are land
based, coming from urban and stormwater runoff, sewer overflows,
littering , inadequate waste disposal and management, industrial
activities, tyre abrasion , construction and illegal dumping.
Pure plastics have low toxicity and due to their non dissolving in
water property, and also they have a large molecular weight, they are
biochemically inert and some plastic contains some additives which
are highly toxic . For example, Polyamides, Polyesters,
Polypropylene, And Acrylonitrile Butadiene Styrene Copolymer to
make alloy in the plastic and Methacrylate Butadiene Styrene
polymers added to bottles to improve impact strength.
Bisphenol A (BSA) is a additive which is a cause for Harmone
Imbalance , and some of the chemicals which disturbs endocrine can
cause around 80 diseases like birth defect, tuberculosis, cancer and
obesity.
1.2.2 Prosopis Juliflora:
They reported that the introduced tree P. juliflora has become a
serious threat to native species of the Brazilian Caatinga vegetation
threatening native biodiversity and rural sustainability due to its
superior ability to adapt and establish itself in the given environment.

1.3 PROSOPIS JULIFLORA :

Prosopis juliflora is an invasive plant species available in the hot
region. It was introduced in many countries for 150 years. It is
widely used as fuelwood in many developing countries such as India.
Prosopis juliflora is hard and withstands different environmental
conditions such as temperature, water/soil quality, humidity, etc.
They are growing at a faster rate as they have a higher success rate of
germination success. They also prevent the growth of other plants.
They extract more amount of water from the ground and hence kill
other plants. The intrusive growth of Prosopis juliflora would affect
biodiversity and many other impacts.
Researchers have extracted fibers from Prosopis juliflora and analyzed
their properties . The characterization of Galactomannan from

13
 Prosopis juliflora was studied and the impact grinding machine with a
high-speed domestic grinder was used to seclude the Endosperm by
eliminating the seed coat and germ

They reported that the introduced tree P. juliflora has

become a serious threat to native species of the Brazilian
Caatinga vegetation threatening native biodiversity and rural
sustainability due to its superior ability to adapt and establish
itself in the given environment.

Fig 1.3.1 Prosopis Juliflora Fig 1.3.2 PJ wooden bark

14
1.4 TECHNIQUES INVOLVED IN SYNTHESIS OF
BIOPLASTIC:

1.5 TYPES OF PLASTICS:

Type of plastic
1) Polyethylene Terephthalate (PET or PETE)
2) Polyvinyl Chloride (PVC or Vinyl)
3) Polyethylene (PE)
4) Polypropylene (PP)
5) Polystyrene (PS or Styrofoam)

1.5.1 Polyethylene Terephthalate

Polyethylene terephthalate (or poly (ethylene terephthalate),

PET, PETE, or the obsolete PETP or PET-P ), is the most common
thermoplastic polymer resin of the polyester family and is used in
fibres for clothing, containers for liquids and foods, and
thermoforming for manufacturing, and in combination with glass fibre
for engineering resins .

1.5.2 Polyvinyl Chloride (PV)

Chlorine is the basic building block of our most infamous toxic

problems: CFCs which destroyed the ozone layer, the dioxin
contamination at Love Canal and Times Beach, Agent Orange, PCBs
and DDT pesticides. Hundreds of chlorine-based toxins are building
up in the air, water and food chain.

15
1.5.3 Polyethylene (PE)

Polyethylene is toxic if its components leak into

beverages and products that could cause health risks.
Polyethylene may be toxic through different manipulations of
the plastic

1.5.4 Polypropylene (PP)

Polypropylene (PP) is a thermoplastic ìaddition polymer”
made from the combination of propylene monomers. It is used
in a variety of applications to include packaging for consumer
products, plastic parts for various industries including the
automotive industry, special devices like living hinges, and
textiles.

1.5.5 Polystyrene (PS or Styrofoam)

Polystyrene is a synthetic aromatic hydrocarbon polymer made
from the monomer known as styrene. Polystyrene foam
contains the chemical styrene, which has been linked to cancer,
vision and hearing loss, impaired memory and concentration,

16
 CHAPTER 2
LITERATURE REVIEW
Characterization and Md. Ruhul Amin, The composite
performance analysis of Mohammad Asaduzzaman Bioplastics is stronger
composite bioplastics Chowdhury * than starch bio plastic
worth increased tensile
synthesized using , Md. Arefin Kowser(2019)
strength and reduced
titanium dioxide
elongation
nanoparticles with corn
starch

Extraction and M.K. Marichelvam a To use the prosopis

development of starch- juliflora which affects
, P. Manimaran
based bioplastics from bio diversity as a
Prosopis , S. Siengchin c Bioplastic and various
K. Kandakodeeswaran a tests were conducted to
Juliflora Plant: Eco-
evaluated the properties
friendly and , Pawinee Boonyasopon e, of Bioplastic film.
sustainability aspects Sergey Gorbatyuk (2022)

Synthesis of bio- Jaya Bharathi Jayabalan1, a), To improve the shelf

polymers from Prosopis Senthilkumar Kandasamy1
juliflora ,Manjula Palanisamy,
Naveen Kumar Manickam1
Elizabeth Nirmala John
Gerard Roya (2020)
life of food by using
cellulose for increase
strength of Bioplastic.
Dur good can be
preserved using this
Bioplastic

Evaluation of Coconut Omoniyi A. Babalola1,a and By adding 10 % of fiber

(Cocos nucifera) Husk Fibre Abel O. content could result in
as a significant improvement

17
 Potential Reinforcing Olorunnisola2,b*(2019) in the tensile strength
Material for Bioplastic and modulus of
Production elasticity.

Production of bioplastic Ezgi Bezirhan Arıkan a,* and To identify the

from potato peel waste and H. Duygu Bilgen a(2019) degradation time of a
investigation of its bio plastic
biodegradability

Microalgae starch-based Charlie Mathiot, Pauline Normal temperature

bioplastics: screening of Ponge, Benjamin Gallard, required for drying corn
ten strains and Jean-Franc¸ois Sassi, Florian and potato based
plasticization of Delrue, Nicolas Le Moigne bioplastics
unfractionated microalgae (2009)
by extrusion

Material characterization Anagha Ashoka, R. investigates starch

of starch derived bio Abhijitha, C. R. Rejeesh bioplastics for
degradable plastics and its (2017) biodegradability and
mechanical property mechanical properties
estimation like hardness and
impact strength.

Lignocellulosics as Malin Brodin, María Methodology for data

sustainable resources for Vallejos, Mihaela Tanase collection, selection and
production of bioplastics – Opedal, María Cristina Area, review
a Gary Chinga-Carrasc
(2017)

Thermal degradation of Satyanarayan Patnaik, Thermal degradation of

18
corn starch based Achyut K. Panda, Sachin starch based
biodegradable plastic Kumar biodegradable plastic
plates and determination
(2019) determination of kinetic
of kinetic parameters by
parameters by
isoconversional methods
isoconversional
using thermogravimetric
methods
analyzer

19
CHAPTER 3
MATERIALS WITH PROCESSES

3.1RESOURCES USED IN EXTRACTION OF

STARCH

3.1.1 POTATO PEEL

The bioplastic was produced from potato peel as the food

industry waste. Also, some properties of the produced
bioplastic such as water absorption capacity and
biodegradability were analyzed. Furthermore, water absorption
capacity and biodegradability of a commercial bioplastic were
also determined in order for the comparison with the one
produced from potato peel waste in different conditions.

FIGURE 3: GRAPHICAL REPRESENTATION OF BIOPLASTIC

It was found that the produced potato peel bioplastic (PPB) had
higher water absorption capacity than commercial bioplastic (CB).

20
Therefore, PPB may not be used in the food service industry but can
be used as packing material. Biodegradability tests showed that PPB
biodegraded at about 71% in moist soil and 100% in vermicompost
within four weeks.

On the other hand, it was determined that CB was not

degraded in the soil or in the compost in four weeks. Therefore, as a
food industry waste, potato peel can be used in biodegradable
bioplastic production. We need 1.9kgs of potato peel to extract
20grams of potato starch.

Fig 3.1.1 POTATO STARCH

3.1.2 DEIONISED WATER :

Deionised water, or DI water, is sometimes called
demineralised water, or DM water. It is water which has had (most
of) the ions removed. Ions are atoms or molecules which have either
more electrons than protons, making a negative ion (an anion) or
fewer electrons than protons, making a positive ion (called a cation).

Normal tap water is full of ions derived from the natural

environment, the pipes and other sources. Typically these might
include Sodium (Na), Calcium (Ca), Iron (Fe) and Copper (Cu). The
deionisation process removes these mineral ions and is an important
aspect of water purification for various applications.

21
 Deionised water is not the same as distilled water, although they
are both forms of purified water. While the deionisation process
produces high purity water by removing mineral ions it will not
significantly remove any uncharged organic molecules. Whereas the
distillation process boils water and then condenses the vapor which
leaves both solid, mineral contaminants and organic contaminants
behind. Deionised water is used in various applications which require
water of high purity.

Chemistry and Laboratory Applications

Water of known purity is often required in chemistry
and laboratory applications. Accurate test results can only be
obtained when the purity of the water used in experiments is
reliably known. Adequately pure water is also needed for
cleaning lab equipment and sterilisation.
Water purity levels are are classified from Type I to
Type IV, where Type I is defined as ëultrapureí.
Water purity is assessed using various characteristics including:
i. Resistivity
ii. Conductivity
iii. TOC (total organic compounds) for Type I water.

3.2 CHEMICALS USED AND PROCESSES

INVOLVED IN EXTRACTION OF
CELLULOSE:

There are various acid were used with a base NaOH and the
processes involved in the extraction process were Alkali treatment and
Delignification and Acid hydrolysis.

3.2.1 ALKALI TREATMENT

Alkaline treatment is a process where natural fiber is immersed
in a strong aqueous solution, such as NaOH, LiOH, or KOH to
create great swelling with resultant changes in the fine structure,
dimension, morphology, and mechanical properties

22
 Effect of alkali treatment on Cellulose was evaluated using
5%, 10%, 15%, and 20% volume fraction of GCW. The
cellulose were characterized using structural (Fourier
transform infrared spectroscopy (FTIR) and scanning
electron microscopy (SEM)), X-Ray Diffraction (XRD),
mechanical (tensile and impact test) properties, and water
absorption. FTIR spectrum indicated the eradication of
lipids, hemicellulose, lignin, and impurities after the
treatments lead to an improvement of the filler/matrix
interface adhesion. This is confirmed by SEM results.

Fig 3.2.1 ALKALI TREATMENT HEATING

NaOH
Sodium hydroxide (NaOH) is a chemical reagent often
used to treat both wooden and non-wooden fibres to improve
the mechanical properties of composites strengthened by these
materials

23
3.2.2 DELIGNIFICATION

Delignification, the process of extracting lignin from plant

sources, can be done using a variety of methods. Its aim is the
disintegration of the lignocellulosic structure into its fibrous
components . The delignification processes can be divided into two
major classes

H2O2
Hydrogen Peroxides can degrade cellulose as well as decolorize
it and remove stains. it is used as an oxidizer, bleaching agent, and
antiseptic, usually as a dilute solution in water for consumer use, and
in higher concentrations for industrial use.

3.2.3 ACID HYDROLYSIS

24
In organic chemistry, acid hydrolysis is a hydrolysis process in
which a protic acid is used to catalyze the cleavage of a
chemical bond via a nucleophilic substitution reaction, with the
addition of the elements of water (H2O). For example, in the
conversion of cellulose or starch to glucose.
Breakage of the β-1,4-glycosidic bonds by acids leads to the
hydrolysis of cellulose polymers , resulting in the sugar
molecule glucose or oligosaccharides Mineral acids, such as
HCl and H2SO4, have been used in the hydrolysis of cellulose.

HYDROCHLORIC ACID (HCL)

Hydrochloric acid [H+(aq) Cl−(aq) or H3O+ Cl−], also
known as muriatic acid, is an aqueous solution of hydrogen
chloride (chemical formula: HCl). It is a colorless solution with
a distinctive pungent smell. It is classified as a strong acid.

SULPHURIC ACID (H2SO4)

Sulphuric acid or sulfuric acid known in antiquity as oil
of vitriol. Sulphuric acid is a mineral acid composed of
elements sulphur, oxygen, and hydrogen. The molecular
formula is H2SO4.sulphuric acid is strong acid with hygroscopic
and oxidizing properties. Sulphuric acid is also known as
mattling acid that is made from burning sulphur and oxygen.
The sulphuric acid is highly corrosive. It is a colourless,
odourless and viscous liquid that is miscible with water.
Boiling point is 337@c and melting point is 10@c. Acidity is
1.01mM.

NITRIC ACID (HNO3)

Nitric acid is the inorganic compound with the formula is
HNO3. It is highly corrosive mineral acid. The compound is
colorless. But poles sample tend to be yellow cast ti
decomposition in to oxides of nitrogen. Most commercially
available nitric acid gad a concentration of 68% in water.
Boiling point is 83@c. Melting point is -42@c. The ph value of
nitric acid is 2.04

25
 ACITIC ACID (CH3COOH)
Acetic acid is also Known as ethonoic acid, ethylic
acid, vinegar acid and methane corboxylic acid. Acetic acid
systematically named ethonoic acid. Is an acidic, colorless
liquid and organic compound with chemical formula
CH3COOH. Vinegar is at least 4%. Acetic acid y volume
making acetic acid the main component of vinegar apart from
water and other trace element. The boiling point is 118@c and
melting point is 16.6@c. The classification of acetic acid is
corboxylic acid.

Fig 3.2.2 Maintaining Ph after the acid hydrolysis process

26
 CHAPTER 4
BIOPLASTIC
4.1 INTRODUCTION TO BIOPLASTIC

Bioplastics are considered as a promising alternative to

plastics since they may diminish the dependency on fossil fuels
and the certain environmental problems.

Fig 4.1 The products of various variations of bioplastic

4.2 TYPES OF BIOPLASTIC

The types of bioplastic are classified below:

a. Category 1: polymers directly

extracted/removed from biomass.
Examples are polysaccharides (starch
and cellulose) and proteins (casein and
gluten).

b. Category 2: polymers produced by

classical synthesis using renewable bio-
based monomers. A good example is poly
acetic acid, a bio polyester polymerized
from lactic acid monomers. The monomers

27
 themselves maybe produced via
fermentation of carbohydrate feedstock.

c. Category 3: polymers produced by

microorganisms or genetically modified
bacteria. To date, this group of bio-based
polymers consists mainly of the polyhydroxy
alkenoate, but development with bacterial
cellulose is in progress.

4.3 RECENT ADVANCES IN BIOPLASTIC

 .Landfilling has been widely employed for the end-of-life

management” of plastic waste. Not only does it require vast amounts
of space, negative consequences related to the contamination of
surrounding soils and ground due to by-products such as phalates and
bisphenols associated with plastic physical deterioration leaking into
the surrounding groundwater and soil have been reported.
Additionally, since none of the material is recovered, this waste
management” system is entirely linear and does not reduce virgin
resource utilisation, stifling the vision of a circular economy.
 Global economic growth and the improvement in living standards has
resulted in an increase in purchasing power by individuals, and so has
contributed to the increase in plastic production. While traditional
petrochemical plastic products have improved the quality of everyday
life, their mainly single use, durable, and recalcitrant nature has led to
a substantial increase as a fraction of municipal solid waste. Currently,
plastic packaging makes up approximately 40% of the plastic market,
of which most is destined for single use.
 Biodegradable polymers have been at the forefront of research for
biomedical applications in the last 50 years. The advancements have
been seen in the areas of using biodegradable polymers as delivery
vehicles for controlled drug release and development of therapeutic
devices , including implants and three-dimensional scaffolds for tissue
engineering.

4.4 SELECTION OF NANOPARTICLES

28
 Selection based on various factors such as preparation methods, cost of
the nano particles, shape, size and thermal performance of the nano particles.
The increasing of that ratio promotes the surface atoms of the material to
dominate over its material performance.

Nanoparticles have been increasingly incorporated into food packaging

to control the ambient atmosphere around food, keeping it fresh and safe from
microbial contamination. Such composites use nanoflakes of clays and
claylike particles, which slow down the ingress of moisture and reduce gas
transport across the packaging film.

Nanoparticles are also used among different types of environmental

preservation processes. These particles make good sense over here.

 ZnO
 TiO2

4.5 CHEMICAL USED

VINEGAR :

By adding a small amount of vinegar, you break up some

of the polymers chains, making the plastic less brittle.
Vinegar, a 6% in volume solution of acetic acid liberates
acetate ions and hydrogen ions in solution.
This is important, because ions react with the starch
polymers and make them be disordered more easily in the
solution. This disorder, resulting from the disruption by the
water and the ionization by the acetic acid, makes the resulting
cast film more homogenous.

GLYCEROL

29
 The glycerin acts as a plasticizer which ìlubricates” the
plastic. Adding more glycerin to make theplastic more pliable
Glycerin is a hygroscopic liquid with a high viscosity. It has 3
hydroxyl groups which make it be soluble in water. Glycerin
makes the biolastic more flexible.

HYDROCHLORIC ACID:
The 7.6 % of hydrochloric acid containing mixture gives
the plastic with the best homogeneity. The 9 % plastic smells of
the acid, which means that there was acid in abundance.

STARCH:
We used potato starch for our research because we
reflected about a sustainable use of potato peel, which is often
degraded to waste and potato starch is easily accessible in
every grocery. Plants store starch in special organelles called
amyloplasts which are present in the cells in form of granules
to save the energy produced by photosynthesis. The glucose
produced by photosynthesis forms bonds to grow to a
macromolecule following the equation:
n C6 H12O6 => (C6 H10O5 ) n + (n-1) H 2O

CELLULOSE
Cellulose-based bioplastics make for the second most
common type of bioplastics used today. As the name suggests,
these bioplastics are made from a blend of cellulose derivatives
(like celluloid) and cellulose esters. These are all products
derived from natural cellulose, the main substance of a plant
cell wall.
Cellulose can potentially be extracted from several types
of biomass and used to make biofilms. This will generate

30
extra income for farmers,” Janaswamy said. Using cellulose
to create biodegradable products that can replace petroleum-
based plastics will reduce the impact these packaging materials
have on the environment.
Structure of Cellulose (C6 H10 O5)n

31
 Fig 4.5.1 POWDERED CELLULOSE

TITANIUM DIOXIDE (TiO2)

The addition of titanium dioxide improved the tensile
strength of the bioplastics from 3.55 to 3.95 MPa and decreased
elongation from 88% to 62%. The degree of nano-composite
crystallinity was formed by the strong interfacial interaction
between the titanium dioxide nanoparticles and the amorphous
region of the chain.
The decomposition temperature of starch bioplastic was
increased by mixing with titanium dioxide nanoparticles.

ZINCOXIDE (ZnO)
Zinc oxide (ZnO) nanoparticle as a lightweight material
that is biocompatible, nontoxic, cost-effective and exhibit
strong antibacterial activity can be considered as nano
reinforcement of starch-based bioplastic. The ZnO enhances
some reinforcing effects like the physical, mechanical and
antibacterial properties of starch-based bioplastic. Moreover,
the decomposition temperature of bioplastic with ZnO
increased slightly which indicated the higher stability.

32
CHAPTER 5

METHODOLOGY

5.1 APPARATUS USED:

Conical flasks, beakers, test tubes were used to acquire the right
amount materials require for the synthesis and preparation of the
products we desired . we used 300ml conical flasks for titration in acid
hydrolysis and 200 ml to 500 ml beakers for the main purpose of
mixing, heating, neutralising, and synthesis.
Hot plate heater were used to heat the mixtures for the long
time autoclave process.
Hot air oven were used in the process of drying the samples for
several days and Muffle furnace is used to get fine product of
cellulose powder from the wood dust. Weighing machine is the most
important used in the whole process to get the precise amount of
materials required for project.

Fig 8 APPARATUS USED

5.2 SAMPLE COLLECTION AND PREPARATION

Potato starch was a one of the essential material required for
the synthesis of Bioplastic . We extract potato starch from potato peel
instead of using raw potatoes to reduce food waste and also to avoid

33
using fresh vegetables for manufacturing instead of eating. We
collected potato peels from from a food business centre who throw
the potato peels to garbage.

Cellulose were extracted from a very dangerous plant named

Prosopis Juliflora which is available near many water streams and
plain grounds and rivers. All the process held to extract cellulose
from PJ were diluted acids only.
And other analytical grade chemicals were highly
available in all the chemicals and drugs centers .

5.3 PREPARATION OF STARCH

The potato peels were Covered with warm water. Scoop the
potato peels into a pot, then cover them with warm water. How much
water we end up using will vary, but about 4 cups (700 to 950
milliliters).
Strain the potato peel, reserving the water. Place a strainer or
colander onto another pot. Line it with cheese cloth, then pouring
the potato peel into it.
Bundle the potato peel up in the cheese cloth, then squeeze it to
get as much water out as possible.
Repeat the watering and straining process until the water
runs clear. Placing the potato peel back into the empty pot. Cover
them with more warm water, then pour them back into the cheese
cloth-lined strainer or colander. Squeezed the cheesecloth to drain
more water. Repeated this step until the water runs mostly clear.
Save the strained water and set the potato peel aside. cover them
with water, add a squirt of lemon juice, and keep them in the cooler.
Allow the starch to settle for about 20 minutes. As time goes on,
the water will start to turn clear-ish again. The starch will settle at the
bottom of the pot. Pour out the excess water. The starch will be
mostly stuck to the bottom of the pot,. Still, avoid stirring or sloshing
the water around as much as possible. Discarded the excess water.

34
 Add fresh water to the container and wait another 20
minutes. Pour some more water into the container (try to use
the same amount that we used to poured out). Let the starch
settle to the bottom another 20 minutes. Pour the water off and
save the starch.
Use the wet starch as-is to thicken sauces, soups, and stews.
Allow the starch to dry and harden. You can cover the
starch with a sheet of paper, wax paper, or parchment paper to
we want to Avoid using plastic wrap, however, or we will trap
the moisture. It can take up to 24 hours for the starch to dry,
depending on how thick or thin it is.[

Break the dried starch up. We can do this with a fork, a

whisk, or even a spoon. Don't worry about getting all of the
clumps out; the next step will fix that. Grind the starch into
a powder. but we used a blender. This will break up any
remaining clumps and make it fine and powdery, just like the
kind we get in a store.

Fig 5.3.1 adding a squirt of lemon Fig 5.3.2 Rinsing potato peel
juice and deionised water to let it with fresh water
strained

35
Fig 5.3.3 the sediment from the wet Fig 5.3.4 Let it to
 5.4 PREPARATION OF CELLULOSE
The wood, after removing the outer bark, was cut into
small pieces and dried in the open air for 24 h. .The size of the
dried wood was further reduced to a chip like size. These chips
were washed with water, filtered, and dried in an oven at 105
degree Celsius for 1 day .
The chips were grinded again with electric grinder to convert it
to sawdust size. Finally, the powder sized P. juliflora wood
samples were stored in airtight containers for further use.

Figure 5.4 Cellulose Extraction Process

5.4.1 PRETREATMENT
Alkaline + Hydrogen peroxide pretreatment (Method II): ten
grams of the sawdust particles were placed in a 2L container where
100 ml of 2w/v% NaOH and 2.5 g H2O2 were added. This oxidizing
agent is very important to make the cellulose of the biomass sample
reachable to the acidic medium. The mixture was then autoclaved,
washed and dried

36
 5.4.2ACID HYDROLISIS
In this step, the effect of acid type (H3PO4, HCl, H2SO4 and
HNO3), acid concentration (4.0%, 6.0%, 8.0%, and 10.0v/v%) and
time (15 min 150 min) on the %conversion of cellulose to reducing
sugar content was investigated. Ten grams of the pretreated solid
samples by method IV, 200 ml of the required acid(type and con-
centration) was added and the whole mixture was gently stirred for the
required time.
All of the hydrolysis experiments were conducted at 120 degree
Celsius. Once the hydrolysis step is completed, the solid was filtered
and the pH of the supernatant was adjusted to 5.25 ± 2.5 using NaOH
solution.

After all this process the sample filtered and dried using hot air
oven and muffle finance. Anthe final product weighed and noted

5.5 SYNTHESIS OF BIOPLASTICS

To fabricate the starch bioplastic, 50gm of corn starch was added

into a beaker together with 300ml of distilled water. Next, 10gm.
Glycerol and 10 ml of white vinegar were added into the beaker. Then
the beaker is Placed on the” Hot-plate-magnetic-stirrer” and the mixture
is stirred for 5 Min. During heating, stirrer should be turned on. This
process occurs Quickly, so the mixture must be stirring until thickens.
Once the mixtnot Is completely ready, it will have to be stir several
times and then the Mixture should be poured into aluminum foil or dye.
Depending on the Thickness of the plastic it requires time may be less
or more during drying. Then the plastic will be kept in a cool, dry place.
After 10 days, bioplastic . In sheet form was obtained as shown in Fig.
1. Composite bioplastic made In the same process has just been added
extra 5gm. Titanium dioxide. And the mention is that composite
bioplastic is not transparent.
Last batch bioplastic was cellulose based nanocomposite
bioplastic. It was prepared by adding 3 gms of extracted
cellulose from PJ batch 2 ratio to make a good quality product.

37
 PROCESS FLOWSHEET:

(i) (ii)
(iii)

(vi) (v) (iv)

Fig 5.4.2 process flowsheet of

synthesis of bioplastic
(vii)

(i) Chemicals and raw materials required have

taken
(ii) The solvents used vinegar and glycerol
(iii) Perfectly weighed every materials
(iv) Mixing all the chemicals and solvents with
distilled water
(v) Stirred it well to mix a perfect level pf
composition
(vi) And also stirring while heating the mixture

38
 (vii) Finally, apply it in polished surface or mold to
let it dry

INTIAL AND FINAL IMAGE OF BIOPLASTIC FROM LIQUID

TO SOLID

Fig A preparation of normal bioplastic and its final product

Fig B preparation of nanocomposite bioplastic and its final product

Fig C preparation of cellulose based nanocomposite bioplastic and

its final product

39
CHAPTER 6

RESULTS AND DISSCUSSION

6.1 FTIR ANALYSIS:

6.1.1. FTIR ANALYSIS OF CELLULOSE POWDER:

The FTIR analysis is used to determine the wavelength of the

chemical compounds present in the bioplastic film. The FTIR spectra
of cellulose powder is given in the below figure. In the spectrum of the
cellulose powder bioplastic
The broadband at 3272.6 cm-1 was the OH stretching . A small
peak near 1638.2 cm-1 was due to C=O stretching and a there is no
peak further which confirms that there is absence of carbonyl group.
The peak at 2935.3 cm-1corresponded to the C-H stretching . The
bands from 851.7 to 1019.4 cm -1corresponds to the C- O bond of
stretching.

40
FIGURE 6.1.1 FTIR OF CELLULLOSE POWDER

41
 6.1.2 FTIR ANALYSIS OF CELLULOSE
STARCH BIOPLASTIC:

The FTIR measures were carried out on a Perkin Elmer Spectrum

One spectrometer coupled to an Auto Image light microscope. These
analyses were performed on samples of starch bioplastic and
composites
bioplastics. In the FTIR spectrum of Cellulose starch bioplastic, the
absorption peaks at 3360.11 cm_1 is determined to stretching
vibrational band of free OH groups. It indicates an increase in the
number of hydrogen bonds between
TiO2 and hydroxyl groups of the plastics components. The other
probable reason was the electrostatic interactions between OH groups
of starch and Ti2˛ atoms. The absorption band of the CH and
COH bending are shown at the wavenumbers 2812.092 and
1165.62cm_1 respectively, Similarly the difference in the absorption
peak intensity of CH and COH at the wavenumbers 2968 and 1136
cm_1, it is confirming the possible electrostatic interaction between
the starch chains and titanium dioxide..

FIGURE 6.1.2 FTIR ANALYSIS OF CELLULOSE BASED

NANOCOMPOSITE BIOPLASTIC

42
 6.1.3 FTIR ANALYSIS OF STARCH BIOPLASTIC:

The result of FTIR analysis of synthesized bioplastic from potato

starch was depicted in figure 2. The result of FTIR analysis of the
sample showed that FTIR spectrum of the sample was obtained at the
wavelength in the range of (400-4000nm). The results of the study
also showed that the peak at 716cm-1 was due to primary amine that
produce 2 N-H stretch absorptions, peak at 857cm-1 was attributed to
the alkane C-H bonds, stretching at 2096 cm-1 was due to carboxylic
O-H stretch(3).

FIGURE 6.1.3 FTIR ANALYSIS OF STARCH

BIOPLASTIC

43
6.2 SEM ANALYSIS:
6.2.1 SEM ANALYSIS OF CELLULOSE
POWDER:

The SEM(Scanning Electron microscope) is used to determine the

surface topology,size,shape and composition of the nanoparticles in
the sample by passing a strong beam of light on the surface of the
sample material. The SEM images of the cellulose powder are shown
in the below figures. The figure A represents SEM image at 10um ,
figure B at 100um, figure C at 5 um and figure D at 50 um. The
shape observed from the SEM analysis is that the cellulose powder
exhibits sheet like structure under 10,100,5 and 50 um size with
clustered and agglomerated particles .

Fig.A 10um sem image of cellulose powder

44
Fig.B 100um sem image of cellulose powder

Fig . c 5um sem image of cellulose powder

Fig . D 50um sem image of cellulose powder

45
 6.2.2 SEM ANALYSIS OF CELLULOSE BIOPLASTIC

The surface microstructure of CELLULOSE based nanocomposite

bioplastics was studied with SEM. The SEM images of the starch bioplastic
are shown in the below figures. The figure 1 represents SEM image at 10um
, figure 2 at 100um, figure 3 at 5 um and figure 4 at 50 um. The shape
observed from the SEM analysis is that the cellulose powder exhibits sheet
like structure under 10,100,5 and 50 um size with clustered and agglomerated
particles . Analyses of starch bioplastics surface reveal that the starch
bioplastics have an irregular structure, with ridges and grooves. SEM images
show that the starch bioplastics surfaces exposed to air are rough with some
grooves and presence of non-gelatinized TiO2 granules. This morphology is
typical of incompatible blends, resulting in a poor tensile property. The
morphology structure of Starch nanoparticles and glycerin bioplastic has not
given homogeneous morphology structure. Few voids, edge, holes and poor
interfacial adhesion observed in the morphologies of the surface. Few crack
propagations in the starch bio-plastics indicates poor bonding between the
components. The starch bioplastic presented a uniform and smoother surface
than starch bioplastic. The presence of the remaining part of the starch
particle and non-gelatinized TiO2 granules is higher in composite bioplastic
than starch bioplastic. The surface roughness starch bioplastic increased and
the uniformity decreased by the TiO2 nanoparticles. Fewer voids, holes, and
crack shows better compatible morphologies in starch composite bioplastic
compared to starch bioplastic.

Fig.a 50um of cellulose based nano composite bioplastic

46
 FIG .A

Fig.b 10um of cellulose based nano composite bioplastic

Fig .c 100um of cellulose based nano composite bioplastic

Fig.d 30um of cellulose based nano composite bioplasti

47
6.2 XRD ANALYSIS:

The XRD known as X-Ray Diffraction method is a experimental

science which determines the atomic and molecular structure of
chemical substance or compound in which the crystalline structure
causes a beam of incident X-Rays to diffract into all directions . The
XRD pattern of bioplastic with strong diffraction peaks is shown in
the below figure 6.3. The XRD studies gives us the information on the
intercalation and exfoliation process of the prepared bioplastic. The
XRD results shows us the various diffraction peaks of various
compounds which are used in the preparation of the bioplastic
compound. The results show that the diffraction peak in 2 at 15o and
24o for bioplastic material. The XRD of normal starch in the presence
of glycerol and Titanium dioxide and zinc oxideshow the peak angles
and d-spacing were about 16o and 26.1o armstrong respectively which
states that the bioplastic structure changes due to the use of TiO2 and

glycerol .

Fig 6.2.1 XRD analysis of cellulose powder

48
 6.3 STRESS AND STRAIN ANALYSIS:

The mechanical properties of Starch bioplastic and cellulose

bioplastic are compared and given in the below figure.. The results
of cellulose bioplastics have greater mechanical strength than
starch-bioplastics but less flexibility. The elongation of starch
bioplastic is decreased from 88 to 62 when it changed at cellulose
bioplastic by TiO2 nanoparticles. The reason for this behavior can
be anti-plasticization. Similar findings were reported such that for
the starch bioplastic and cellulose bioplastics tensile strength 2.66
MPa and 3.86 MPa and elongation 86.70% and 68.43%
respectively. By increasing interactions, reducing the free volume
between the biopolymer chains with decreasing the flexibility of the
bioplastic, titanium dioxide nanoparticles act as an anti- plasticizer
.
Mechanical properties of starch bioplastic and
cellulose bioplastic. Tensile strength (MPa)
Elongation (%)
Starch Bioplastic 3.55 _ 0.035 88.1
Cellulose Bioplastic 3.95 _ 0.039 62.5

FIGURE 6.4 STRESS AND STRAIN CURVE OF STARCH AND

CELLULOSE NANOCOMPOSITE
BIOPLASTIC

49
 6.4 BIODEGRADABILITY TEST ANALYSIS

cellulose bioplastic was landfilled in natural soil at a

depth of 10 cm and left for a month and the biodegradation
behaviour of the bioplastic was investigated. After biodegradability
tests, any materials attached to the surface of the bioplastic were
removed by washing in running water. Microscopy observations
and analysis of weight loss is carried out after drying the samples
at 50 °C for 2 hours. The weight loss of composted samples was
evaluated using the following equation:

where W0 and W1 were sample weights before and after

biodegradability test, respectively.
DAY 1 DAY 15 DAY 30

Starch
Bioplastic
6.5

Weight loss 0% 54% 92%

Nano
Composite
Bioplastic

Weight loss 0% 32% 64%

Cellulose based
Nanocomposite
Bioplastic

Weight loss 0% 43% 79%

50
WATER ADSORPTION TEST

Dried sheets were weighed for the initial weight and then placed
in a bath of distilled water at room temperature. The sheets were
removed after 24 hours where water on the surface of the sheets was
wiped off and weighed the sheets again.

where Wi is initial weight (g) before immersion in water and Wf is

final weight (g) after immersion in water. The sheets were cut into 100
mm x 25 mm, with the gauge 50 mm, and conducted with the speed of
2 mm/min. Based on starch content and cellulose addition absorption
differed.

51
CHAPTER 7

CONCLUSION

In this study, it can be ascertained that starch-based bioplastics and

composite cellulose nanocomposite bioplastic have been successfully
characterized52 | P a g e by various analysis. The composite bioplastic is
stronger than starch bioplastic with increased tensile strength and reduced
elongation. From FTIR analysis , which is confirmed the electrostatic
interaction between the starch chains and titanium dioxide. SEM images
show that Composite bioplastics have a better consistent surface in the
compared to starch bioplastics for less void, hole and crack. Composite
bioplastics have higher heat stability than the starch bioplastics. Soil burial
biodegradation test indicates the biodegradability of starch bioplastic is
more than composite bioplastic and also both plastics are highly
biodegradable. By adding TiO2 to starch bioplastics, its properties have
been improved. So it will be very useful in food packaging systems. The
preparation of starch bioplastic and composites bioplastic with better
thermal, mechanical and chemical properties is a significant achievement.
These products can be a appropriate alternative for the existing
conventional plastics for its high biodegradable properties with suitable
thermal and mechanical properties. Also starch is a renewable resource,
cheap and easy to modify. Titanium dioxide and zinc oxide nanoparticles
have antimicrobial properties and composite bioplastics can be considered
suitable for the food and pharmaceutical industry considering the
experimental results. It will reduce reliance on petroleum polymers and
environmental problems like today will not be intense anymore.

52
CHAPTER 8

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