GDCA Siddipet Chemistry 31-03-2024 1
GDCA Siddipet Chemistry 31-03-2024 1
GDCA Siddipet Chemistry 31-03-2024 1
Submitted
In the partial fulfillment of the requirements for
JIGNASA –STUDENT STUDY PROJECT
in
CHEMISTRY
By
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CERTIFICATE
This is to certify that the Student Study Project “ECO FRIENDLY-RECYCLING OF WASTE PET
BOTTLES Via RECOVERY OF TEREPHTHALIC ACID (TPA) USING AMBERLITE IR-120[H+]
RESIN AS A REUSABLE CATALYST” that is being submitted by B.Sc STUDENTS in partial fulfillment
for the JIGNASA STUDENT STUDY PROJECT in CHEMISTRY is a record of bonafide work carried out by
them under my guidance and supervision for the Academic Year 2023-24.
The results embodied in this student study project have not been submitted to any other
University or Institute for the award of any degree or diploma.
Dr.VASAM SREENIVAS
This is to certify that the student study project “ECO FRIENDLY-RECYCLING OF WASTE PET
BOTTLES Via R E C O V E R Y OF TEREPHTHALIC ACID (TPA) USING AMBERLITE IR-
120[H+] RESIN AS A REUSABLE CATALYST” that is being submitted by B.Sc STUDENTS in
partial fulfillment for the JIGNASA STUDENT STUDY PROJECT2024 in CHEMISTRY to is a
record of bonafide work carried out by them under the guidance and supervision of Dr.Vasam
Sreenivas, Associate Prof. of. Chemistry, GDC(A), Siddipet for the Academic Year 2023-24, by the
students S. Sandya, G. Srilaxmi, G. Anuja, A. Bharath, Sana kouser and Ishrath Jahan.
We hereby declare that the contents presented in the student study project entitled
“ECO FRIENDLY-RECYCLING OF WASTE PET BOTTLES Via RECOVERY OF
TEREPHTHALIC ACID (TPA) USING AMBERLITE IR-120[H+] RESIN AS A REUSABLE
CATALYST” that is being submitted in partial fulfillment for the JIGNASA STUDENT
STUDY PROJECT in Chemistry is a record of original work investigated by us under the
supervision of Dr.Vasam Sreenivas, Department of Chemistry, Government Degree College
Siddipet (Autonomous), for the Academic Year 2023-24
Further this is to state that the results embodied in this dissertation have not submitted to any
other university or institution for the award of any degree or diploma.
We are thankful to Commissioner sir Sri Burra Venkatesam , IAS for encouraging
students in research program at undergraduate level.
It has been our proud privilege to undertake and complete present study under the able
guidance, sympathetic and encouraging attitude, ever inspiring influence and scholarly supervision
of Dr. Vasam Sreenivas, Associate Professor of Chemistry, Head Department of Chemistry,
Government Degree College Siddipet (Autonomous). It gives us great pleasure in expressing our
indebtedness and deep sense of gratitude to her. Without her valuable guidance, it was not possible
to complete the present work.
We also thank our Jignasa co-ordinator Dr. P. Pallavi, Assistant Professor of Microbiology
and Thank full to Department faculty members sri K.Anjaneyulu Assistant Professorof Chemistry,
Dr.G.Ravi Kumar Assistant Professorof Chemistry, Dr.P.Sumalatha Assistant Professor of
Chemistry, Sri.M.Shyamsunder Assistant Professor of Chemistry, Sri Md.Saleem Pasha Assistant
Professorof Chemistry, Dr.V. Balakishan Assistant Professor of Chemistry and Dr.K. Ravi kumar
Lecture in chemisty.
We are thankful to other faculty members, staff of Government Degree College Siddipet
(Autonomous), for their cooperation during this period.
Title Page No
Introduction 1
Hypothesis 3
Review of literature 5
Methodology 6
Findings 15
Photo Gallery 17
Government Degree College Siddipet (Autonomous)
INTRODUCTION
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What is PET?
PET (Polyethylene terephthalate) is versatile polyester with diverse applications, and
its synthesis involves poly condensation of teripthalic acid (TPA) with ethylene glycol
(EG).
The disposal of plastic waste has become a significant environmental problem that
requires effective solutions for its management and sustainable use. Despite the
increasing importance of recycling, there is still a need to explore advanced methods
for the recovery of plastics, especially for polyethylene terephthalate (PET).
For PET recycling mechanical and chemical methods are currently in the usage but
chemical recycling methods got advantage over mechanical recycling because
mechanical recycling involves high energy and pollution. There is also a loss of
quality in the recycled product. In chemical methods hydrolysis is the most facile
method for PET treatment that comprises its depolymerization to teripthalic acid
(TPA) and ethylene glycol (EG). These monomers are the basic raw material for the
re polymerization into PET.
Generally, the hydrolysis o f PET is promoted by a n acid and base catalysts such as
H2SO4, HNO3 and NaOH. Unfortunately large amounts of strong acids or alkali
waste water are produced in these reaction system. Recovery and reuse is difficult
resulting in waste of resources. So for hydrolysis of PET to TPA monomer we have
chosen reusable catalysts like Amberlite IR-120[H+] resin or eco-friendly Lewis’s acid
NiCl2. Hydrolysis treatment by depolymerization with Amberlite IR-120[H+] resin or
Lewis’s acid NiCl2 in polar solvents at moderate to high temperature is a promising way
to recover PET (Scheme-1).
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Government Degree College Siddipet (Autonomous)
Reaction times and temperatures on the weight changes in PET and the subsequent
recovery of the valuable monomer terephthalic acid (TPA). Furthermore, a
comparative analysis of the efficiency of Amberlite IR-120[H+] resin and
NiCl2catalyst in PET recovery is essential.
HYPOTHESIS
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during hydrolysis and contribute to the development of optimized methods for the
conversion of plastic waste into high-value end products. These findings have the
potential to Support sustainable practices in plastic waste management and facilitate
the transitionto a circular and environmentally friendly approach to plastic recycling.
AIMS
The present study aims at investigating the effects of different hydrolysis conditions
on PET in presence of Amberlite IR-120[H+] resin and Lewis acid NiCl2 catalyst with
a focus on recovery of TPA a valuble chemical used in various industrial applications.
The comparison between Amberlite IR-120[H+] resin and Lewis acid NiCl2 catalyst
will provide crucial insights into the effectiveness of different catalyzed hydrolysis
agents under boiling polar solvent conditions. The results of this research will
contribute to the development of sustainable processes for the recycling of PET
plastic waste, reducing the environmental impact associated with plastic disposal.
OBJECTIVES
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REVIEW OF LITERATURE
Plastic waste has become a global environmental problem, which has led to extensive
research into new ways for its recovery and long-term management. This study looks
at the national and international literature to provide an overview of the current state
of research on plastic waste recovery, with a focus on polyethylene terephthalate
(PET) and hydrolysis treatment.
Geyer and colleagues (2017). Production, use, and disposal of all plastics ever
created. Science Progresses, this major international study provides an in-depth
examination of global plastics production, consumption and fate in the environment.
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It emphasizes the crucial importance of appropriate systems for the disposal of plastic
waste. Achilias and Karayannidis (2004) state. Hydrolysis of poly (ethylene
terephthalate) in the molten state. Polymer, This global study examines the hydrolysis
of PET in the molten state and provides insights into the chemical mechanisms
involved. The work provides useful information on the depolymerization of PET,
which is an important part of plastic waste recycling. The occurrence of microplastics
in the marine environment. Marine pollution by A. L. Andrady (2011).
While not directly related to hydrolysis, this international study raises awareness of
the global problem of microplastics and highlights the importance of sustainable
plastic waste management practices. Jambeck and colleagues (2015). Plastic waste
from land ends up in the sea. Published in the journal Science, this nationwide study
examines the import of plastic waste into the ocean, highlighting the importance of
land-based sources. It emphasizes the importance of appropriate waste recycling
systems, particularly hydrolysis processes, to reduce marine pollution. According to
Salem et.al,(2010). A overview of the recycling and recovery routes for plastic solid
waste (PSW). Management of Waste, This nationwide assessment, which focuses on
solid plastic waste, examines alternative recycling and recovery strategies, including
hydrolysis. The work sheds light on the feasibility of hydrolysis as a method of PET
recovery. Plastic waste to liquid gasoline by hydrolysis: An overview. Das et al.
(2018), Materials Today: Proceedings.
This national assessment looks at the hydrolysis of waste polymers to produce liquid
fuel and offers insights into the wider applications of hydrolysis in plastic waste
management. Worldwide literature highlights the global scale of the plastic waste
dilemma, while national research offers insights into specific areas of plastic waste
recycling, such as hydrolysis. The cited publications contribute to the growing body
of knowledge aimed at developing sustainable practices for plastic waste
management. Amberlite IR-120[H+] resin is an efficient catalyst for chemical
transformations such as condensation reactions and has attracted considerable
attention due to its recyclability (Sharma et al., 2009). NiCl 2 is a Lewis acid catalyst
that can also be useful for the saponification reaction Khan et al. (2003).
MATERIAL AND METHODS
Primarily a meticulous cleaning process was implemented for the experiment. The
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Collection of
Collection of PET
PET Bottles
Bottlesfrom
from College
College Ground
Ground and
and Basil
Basil foundation
fondation
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Two different hydrolysis agents, Amberlite IR-120[H+] resin and NiCl2 were
employed in the hydrolysis process in separate reaction setups. For the general
procedure, 5 g of PET flakes, 50.00 mL methanol or EG was weighed in analytical
balance or measured using volumetric pipette and placed into a 250 mL round-
bottom distilling flask. An amount of 3 g of the catalyst to be optimized was also
added to the flask. The flask was then equipped with a Claisen head, a reflux
condenser, a thermometer, and a magnetic stirrer. The mixture was heated up to its
boiling point with constant agitation using an oil bath placed in a magnetic-stirring hot
plate. A reflux condenser was placed to avoid loss of volatile products and reagents in
the reaction as much as possible. The reaction time was then optimized.This
experimental setup was adapted from the methodology outlined by Hanaoka et al. in
2021.
The part was to determine the optimal depolymerization parameters that would allow
the production of the highest yield of TPA and EG (ethylene glycol). For the TPA, at
the end of each run, the heat source was removed, and the mixture obtained was
filtered to separate the unreacted PET residue with catalyst. The residue was then
washed with distilled water, dried for 105 °C for 4 h, cooled, and weighed. Dilute
hydrochloric acid (1 M) was added drop wise to the filtrate obtained with constant
stirring to form the white precipitate, TPA. Afterwards, the TPA was digested at
70°C for 30 min to increase particle size, cooled, and then filtered. The TPA solid
was washed using distilled water to remove water soluble impurities, filtered again,
dried at 105 °C, and then finally weighed, and stored in a clean container.The
following parameters optimized were the catalyst used and reaction time. Then, the
TPA obtained was characterized together with their corresponding standards using
Fouriertransform-infrared spectroscopy (FT-IR).
Chemical Equations
Depolymerization of PET:
PET →TPA+ Ethylene Glycol(EG)
This reaction breaks down the PET polymer into its monomer units, TPA, and Ethylene
Glycol, through hydrolysis.
Recovery of TPA using Amberlite IR-120[H+] Resin
TPA+AmberliteIR-120[H+]→TPA-Amberlite ComplexTPA+Amberlite
Complex+Base(e.g., NaOH)→TPA+ Regenerated Amberlite IR120TPA-Amberlite
Complex+Base (e.g., NaOH)→TPA+Regenerated Amberlite IR-120
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In this process, Amberlite IR-120[H+] resin acts as a catalyst to facilitate the reaction
and separation of TPA from the reaction mixture. The resin forms a complex with TPA,
which can then be regenerated by treating the complex with a base, yielding TPA and
regenerated Amberlite IR-120 resin for reuse.
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Characterization of TPA:
The TPA is well characterized by elemental IR, 1HNMR spectral analysis. Fig. 3
shows the schematic diagram for the isolation of TPA. Fig. 4 is showing the
correlated FT-IR of TPA generated from depolymerization with reference TPA. Fig. 5
is showing the correlated 1HNMR of TPA generated from depolymerization with
reference TPA. We further checked optimum heating studies with different catalyst
and we find the TPA yields were improved with reflux temperatures with 24hrs
reaction time (Table-1). We also recovered catalyst along with PET traces which can
be re-used up to four cycles; we see barely any difference in the isolated yields.
Similar reaction condition was applied using NiCl2.6H20 catalyst and in this case,
catalyst was not recovered. We also conducted similar experiment in EG as solvent at
its boiling temperatures and wefound improved yields with TPA synthesis.
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Figure 4:FT-IR spectra of (a) TPA product in black and (b) TPA standard in green.
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FINDINGS
In this experiment with longer reaction times and at high temperature around 180 C
nearly 80% monomer (TPA) is recovered. From our experiment it was found that
hydrolysis in presence of either Amberlite IR-120[H+] Resin or NiCl2 is more
effective and green method compare to acid.
Amberlite IR-120[H+] Resin is reusable catalyst and can be used upto four cycles.
But taking cost into consideration we preferred NiCl2 catalyst and considered that it
is more convenient for experiment than Amberlite IR-120[H+].
CONCLUSION
Recycling of PET depolymerisation by hydrolysis is the most promising technology
which results in production of key monomer Terpthalic acid (TPA).The process that
we demonstrated involving Amberlite IR-120[H+] resin and NiCl2 is a sustainable and
eco-friendly approach to plastic waste management. This process not only helps in
reducing environmental impact but also contributes to resource conservation, energy
efficiency. It lowers energy consumption compared to producing TPA from virgin
petrochemical sources.
SUGGESTIONS
• Plastics in the environment pollute our water, harm wildlife and have
largely unknown health impacts on us.
• As citizens of society, we have a responsibility to manage our waste for
sustainable life.
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REFERENCES
3. Cˇolnik M, Knez Z and Škerget M 2021 Sub- and supercritical water for
chemical recycling of polyethylene terephthalate waste Chemical Engineering
Science 233 Article 116389
4. Das, B., Sarkar, D., Deka, D., & Baruah, D. C. (2018). Waste plastics to liquid
fuel through hydrolysis: An insight review. Materials Today: Proceedings,
5(1), 2390-2395.
5. Geyer, R., Jambeck, J. R., & Law, K. L. (2017). Production, use, and fate of
all plastics ever made. Science Advances, 3(7), e1700782.
7. Jambeck, J. R., Geyer, R., Wilcox, C., Siegler, T. R., Perryman, M., Andrady,
A., ... & Law, K. L. (2015). Plastic waste inputs from land into the ocean.
Science, 347(6223), 768-771.
8. Khan, A. T., Mondal, E., Sahu, P. R., & Islam, S. (2003). Nickel (II) chloride as an
efficient and useful catalyst for chemoselectivethioacetalization of
aldehydes. Tetrahedron letters, 44(5), 919-922.
PUBLICATION
Eco Friendly-Recycling Of Waste PET Bottles Via Recovery Of Terephthalic Acid (TPA)
Using Amberlite IR-120[H+ ] Resin As A Reusable Catalyst. Sandhya. S, Srilaxmi. G and
Anuja. G (B.Sc. FZC-III) Bharath. A (B.Sc. MbZC III), Sana Kouser (B.Sc. BZC-II). Ishrath
Jahan (B.Sc. BTBC-I) *Dr. Vasam Sreenivas, Head & Associate Professor Department of
Chemistry Govt. Degree College, Siddipet-International Journal of creative Research
thought(IJCRT) 2024 IJCRT | Volume 12, Issue 3 March 2024 | ISSN: 2320-2882.
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PHOTOGALLERY
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