Development of composite structure from recycled material

Development of Composite Structure
from Recycled Material
Under Guidance of
Dr. Jawahar Paulraj
(Assistant Professor)
Submitted By
Name: Pradeep Kumar
Enrollment no: 19PME005
M.Tech in Manufacturing Technology
National Institute of Technology,
Agartala-799046
&
Dr. Manish Bhargava
(Associate Professor) 1
Subject name: Project and Thesis (PME24P02)

AIM
To develop a commercial component using recycled plastic.
To decrease the burden of plastic in our NITA campus and Regeneration of plastic
into helpful product for daily use with low investment
Study the influence of calcium carbonate and natural lac resin on the developed
composite structure
To Contribute in the circular economy
2

Global plastic production and its fate
3

Case study
In India, annual per capita cost of municipal solid waste management ranges from
Rs 204 to Rs 900 for capital investment and from Rs 113 to Rs 269 for operation and
maintenance. 6

Literature review
Author’s Published Year Title Journal Inference
Biplob Nandy et al. 2015 Recovery of consumer
waste in India – A mass
flow analysis for paper,
plastic and glass and
the contribution of
households and the
informal sector
Resources,
Conservation and
Recycling
 The total waste
management data
shows that only 4.6
billion kg per year
out of the 10.7 to 12
billion kg per year
of plastic, rubber,
leathers and
synthetics waste
generated are
collected and
disposed off in the
form of mixed
municipal solid
waste.
7

LITERATURE REVIEW
A.M. Al-Sabagh et al. 2015
Greener routes for
recycling of polyethylene
Terephthalate
Egyptian journal of
petroleum
Compared to chemical
recycling routes, physical
recycling of PET by melt
reprocessing is relatively
simple, requires low
investments and has little
adverse environmental
impact
Eiji B Hosoda 2012 Recycling of waste and
downgrading of
secondary resources in a
classical type of
production model
Journal of
Economic
Structures,
Springer
Recycled product
quality obtained by
downgrading is entirely
depends on the choice of
method and process
selected for recycling
According to ISO 15270
downgrading or secondary
recycling is also referred
as mechanical recycling
Literature review
8

LITERATURE REVIEW
Ranjit N. Turukmane
et al.
2018 Recycling of PET
Clothes and Bottles
International Journal
of Research and
Scientific Innovation
Thermal recycling is
the best method of
polyester recycling in
which the waste PET
bottles are initially cuts
into small pieces,
washed and processed
into desired polyester
filaments, which
further converted into
fabric and garments
Duane M. Juriga 2008 Tufted PET fiber for
automotive carpet
application
United States Patent
Application
Publication
It has also been
observed that self
reinforced recycled
PET offers high
strength and light
weight exterior panels
of a heavy truck and
could be good
substitute for non-
recyclable composites
Literature review
9

LITERATURE REVIEW
S. Bandla et al. 2010 Microstructure and
elastic tensile behavior
of polyethylene
terephthalate-exfoliated
graphene
nanocomposites
Journal of material
science,
Springer
Graphene nano-platelets
were effective in achieving
an improved elastic
modulus for poly (ethylene
terephthalate)
Injection molding
process can help improve
the PET composite
properties.
Silvio Canonica et al. 2001 change the material and
content of polyethylene
terephthalate (PET)
bottles?
Journal of Water
Supply: Research
and Technology
PET bottles are
excellent containers for
soft drinks quite often
exposed to sunlight over
extended periods of time.
Photochemical ageing
of the bottles does not
change the quality of the
water stored in the bottles
with regard to aldehyde,
organic photoproduct,
additive or phthalate
concentrations
Literature review
10

LITERATURE REVIEW
R. S. Kognole et al. 2019
Utilization of Plastic
waste for Making
Plastic Bricks
International Journal
of Trend in Scientific
Research and
Development
50 gm crushed PET
waste plastic bottle
along with 50 gm red
soil, develop Bricks of
affordable rates and
satisfies all the basic
criteria of standardized
brick in terms of shape,
durability, soundness
and hardness.
 Water absorption of
this plastic sand brick
is zero percent.
Wan Mohd Nazmi
Wan Abdul Rahman
et al.
2013
Green Pavement Using
Recycled Polyethylene
Terephthalate (PET) as
Partial Fine Aggregate
Replacement in
Modified Asphalt
Procedia Engineering
Recycled PET
modified asphalt gives
more advantages
compared to the
conventional asphalt
mixture especially in
term of permanent
deformation
Reduce cost of road
construction
Literature review
11

LITERATURE REVIEW
Muhammad Akmal
et al. 2019
Flammability, Thermal
and Mechanical
Properties of
Polybutylene
Terephthalate (PBT)/
Dolomite composites
Journal of Physical
Science
 Addition of dolomite
into PBT has improved
flammability and
thermal properties of
the PBT/dolomite
composites
Enhanced the
flexural properties,
tensile strength and
Young’s modulus.
Literature review
12

LITERATURE REVIEW
Emy Aizat Azimi,
Mohd Mustafa Al Bakri
Abdullah,
Petrica Vizureanu,
Mohd Arif Anuar Mohd
Salleh,
Andrei Victor Sandu ,
Jitrin Chaiprapa,
2020
Strength Development
and Elemental
Distribution of
Dolomite/Fly Ash
Geopolymer Composite
under Elevated
Temperature
Materials
 The dolomite has the
potential to be used as a
raw material for
geopolymer and produces
a low reactivity in the
geopolymerisation
process, which leads to
slow strength
development
 A high amount of Ca
in geopolymer usually
produces a good setting
time.
13
Literature review

LITERATURE REVIEW
Noel Deepak Shiri
P. Varun Kajava
Ranjan H. V
Nikhil Lloyd Pais
Vikhyat M. Naik
2015
Processing of Waste
Plastics into Building
Materials Using a Plastic
Extruder and
Compression Testing of
Plastic Bricks
Journal of
Mechanical
Engineering and
Automation
 The compression
testing results
reveals that 70% PP
when effectively
mixed with 20%
Rubber powder and
10% Calcium
Carbonate by wt/wt
% ratio gives the
highest compressive
strength and sustains
high compressive
load.
14
Literature review

LITERATURE REVIEW
Adesakin A.O,
Ajayi O.O,
Imosili P.E,
Attahdaniel B.E
2013
Characterization
and Evaluation of
Mechanical
Properties of
Dolomite as Filler in
Polyester
The International
Institute for
Science,
Technology and
Education (IISTE)
 Revealed the
importance of
reinforcement on
modulus and
hardness of
polyester.
 It was observed
that there was an
increase in hardness
and modulus from
moving 20% to 30%
calcium carbonate
composition in
mass/mass ratio.
15
Literature review

LITERATURE REVIEW
K. K. Sharma
A. Roy Chowdhury
S. Srivastava
2020
Chemistry and
Applications of Lac
and Its By-Product
Springer nature
 Its ability to produce
smooth, decorative and
durable films from
alcoholic solutions,
which dry rapidly.
capable of yielding
laminated products, Good
thermal plasticity,
Ability to absorb large
amount of fillers
Rebecca j. Stacey
et al. 1998
The Chemistry,
Archaeology, and
Ethnography of a
Native American
Insect Resin
Journal of
California and
Great Basin
Anthropology
Lac resin softens on
heating at around 121° C
and becomes sticky and
darker in color and also
observed that lac does
not melt below 221° C.
 The resin has a
property of regaining the
hardness very rapidly
upon cooling which
directs it strong bonding
property.
Literature review
16

Inference
17
PET has been used at various occasion for developing a composite
Lac resin regains it hardness upon cooling thus acting as bonding agent
Lac resin softens on heating at around 121 ºC and does not melt below 221ºC
Calcium carbonate helps to reduce shrinkage , improve stiffness and impact strength
Injection molding process can help improve PET composite property.
Composite produced from recycled PET are cost effective and sustainable if the process and
additive composition is carefully controlled.

Minimum properties requirement for PET recycling
Sr. No. Properties Range
1 Viciousness Greater than 0.7 Pa-s
2 Melting temperature Above 240 ºC
3 Flake Size Diameter range should be
between
0.4mm to 8mm
4 Polyolefin percentage Less than 10 ppm
5 Moisture content Less than 0.02 wt % 20

Selection of filler
CALCIUM CARBONATE SILICA FLY ASH
Chemical formula
Ca(CO₃)₂
• M.P = 120- 130⁰C
• Mg Impurities present in it
provide refractory property.
• CaCO₃ offers:-
(a). Faster cooling rate
(b). Reduce shrinkage
• Improves – Impact strength,
stiffness & thermal
conductivity
• It is easy to exploit and
process so their prices are
very cheap.
Chemical formula
SiO₂
• M.P = 1710 ⁰C
• Prevents cracking,
• Causes shrinkage and wrapping
• Contains moisture
• Excess silica destroys the
cohesion between particles
Consist of oxides of
silicon, aluminum and Iron.
• Different ranges of M.P from
480 ⁰C to 1231 ⁰C depending
on type of ashes.
• Light weight
• Fire resistance
• Resist salt and other sulphate
• Lower water absorption
• Mechanical bonding strength
of fly ash is weak.
• Limitation of size
21

Calcium carbonate as a filler
• CaMg(CO3)2 is the primary component of a sedimentary rock and a mineral,
composing of Calcium Magnesium Carbonate [CaMg(CO3)2] generally found in
crystalline form. The calcite product of dolomitic limestone is used to
manufacture of calcium carbonate filler.
WHY CaCO3 ?
 It is easily available
 Higher surface hardness.
 Good weathering resistance
 Higher strength
Application
 Filler in cement industry
 Refractories
 Plastic & glass industry
22

Chemical composition of CaCO3 used in the experiment
Chemical composition Percentage
Ca(CO₃)₂ 88%
Mg(CO₃)₂ 8.65%
Impurities Alumina < 2- 3.5
Silica < 1%
Total CaMg(CO₃)₂ 96.65%
23

LAC Resin
• Secreted by Indian lac insect, Kerria lacca (Kerr), which lives on the
tender twigs of specific host trees.
• Lac resin softens on heating at around 121° C and becomes sticky
and darker in color and also observed that lac does not melt below
221° C.
WHY LAC ?
 Non-toxic
 Biodegradable
 Natural
 Major constituent of lac is resin, followed by two important by- products, dye
and wax.
Application
 Paint and varnishes
 Glue for joining metal with glass, isolator coating, sockets of electrical lamps,
PCB coating, etc.
 Adhesive for crystals, precious stones, lenses 24

Selection of Lac resin- Seedlac
WHY SEEDLAC ?
Obtain by grinding and washing the sticklac.
Highest percentage of resin out of all other variant
of lac resin.
Require unskilled labor for processing
Contain minimum quantity of gluten protein
26

Terpenenic acid and Aleuritic acid are two main chemicals found in lac
1. Terpenenic acid - Class of hydrocarbons.
Terpenoids Property :- Antimicrobial, antifungal, antiviral, antiparasitic, anti-
inflammatory, antioxidants.
2. Aleuritic Acid - containing 3 hydroxyl groups and can soluble in the lower alcohols
such as methyl, ethyl and isopropyl alcohols.
It has found its application in plastics with good adhesive properties
27

Seedlac resin
Sr.No Constituents Percentage
1 Resin 86-92 %
2 Dye 2.5 %
3 Wax 6 %
4 Gluten 2 %
5 Impurities < 2 %
6 Moisture 2 % 28

Waste PET
material
collection
Segregation
of waste
Cleaning
Mixing the
plastic with
additives
and filler
Blending at
elevated
temperature
Cutting the PET
bottles into
granules
Molding Testing
Analyzing the
mechanical
property
Methodology and process
29

Plastic is such a necessity that its use in near decade is not going to stop, to curve its harmful
effect on environment what we can done is recycling.
Growing plastic pollution in NITA campus
Though plastic has high strength to weight ratio, with PET material no investigation has been
carried out with the natural lac resin for developing the composite
To evaluate the effect of calcium carbonate filler and lac on the physical and chemical
properties of composite produced using PET
30
Motivation and Objectives

Proportion of constituent for developing composite
structure through injection molding in w/w %
SL No. PET Calcium
carbonate
Seedlac
SAMPLE 1 90% 10% -
SAMPLE 2 80% 20% -
SAMPLE 3 70% 30% -
SAMPLE 4 60% 30% 10%
SAMPLE 5 70% 10% 20%
SAMPLE 6 60% 10% 30%
31

Developed Composite structure using Injection molding
Sample 1 Sample 2 Sample 3 Sample 4 Sample 5
32

Proportion of constituent for developing composite
structure through casting
SL No. PET [ Wt %] Ca(CO₃)₂ [ Wt %] Seedlac [ Wt %]
SAMPLE 1
70% 10% 20%
SAMPLE 2
60% 20% 20%
SAMPLE 3
90%
-
10%
SAMPLE 4
80%
-
15%
SAMPLE 5
70%
-
20%
33

Developed Composite structure using Casting
(a) & (b) PET/Lac blend
(c)
(c) & (d). PET/Lac/ CaCO3 blend 35
(d)
(a) (b)

Microstructure for casting molded specimen
@ 50 x magnification
(a) PET (90%) + Lac(10%) (b) PET (85%) + Lac (15%)
36
 Surface texture improved
Promotes bonding with PET.
 Improvement in adhesion between both incompatible phases
(a) (b) (c)
(c) PET (90%) + Lac(20%)
36

Microstructure comparison for blend of (70 PET, 10 CaCO3 and 20 lac)
w/w % @ 50 X Magnification
(a). Injection molded (b). casting
In image (a),CaCO3 filler is uniformly distributed.
In image (b), CaCO3 filler is not uniformly distributed but the bonding between lac and PET can
be easily distinguished
(a) (b)
37

Scanning electron microscopy (SEM) Analysis Of casting molded
specimen
 Non- uniform grain  Large cracks Weak bonding 38
(b)
(a)

Scanning electron microscopy (SEM) Analysis Of Injection molded
specimen
 Uniformly distributed
Grain boundary  Small Voids  Better adhesion 39
(b)
(a)

Energy Dispersive X-ray (EDX) analysis
Element Weight % Atomic %
C K 46.52 65.36
N K 0.56 0.67
O K 26.77 28.23
MgK 2.78 1.93
SiK 3.05 1.83
CaK 0.70 0.30
AuL 19.62 1.68
 Presence of Silica impurities can be
identified. This presence of silica impurities is
due to the processing of calcite raw material
into CaCO3.
 No other impurities inclusion is observed.
Chemical composition of the Injection molded specimen using EDX for (PET/ CaCO3 /Lac) blend
composite
40

Energy Dispersive X-ray (EDX) analysis
Chemical composition of the casting molded specimen using EDX for (PET/ CaCO3 /Lac) blend
composite
Element Weight % Atomic %
C K 37.48 60.09
N K 0.00 0.01
O K 21.54 25.93
Mg K 6.23 4.94
Si K 8.05 5.52
Ca K 2.36 1.14
Au L 24.33 2.38
Presence of more Silica impurities No other foreign element inclusion in casting
41

Barrier study
1321.02
1202.02
754.23
859.8 872.85
1316.37
1185.647
742.31
797.62
827.54
1307.8
1167.6
736.12 745.351
805.85
Casting 1 Casting 3 casting 5 Injection molding 3 Injection molding 5
0
200
400
600
800
1000
1200
1400
Weight
(in
mg)
Sample no.
Initial weight (in mg)
weight after 7 Days ( in mg)
Weight after 28 days (in mg)
Effect of concentrated Sodium hydroxide solution on specimen
 Degradation of composite material
The rate of degradation of material was higher for first seven days
Rate of degradation of casting specimen was less than injection molded specimen 42

Barrier study
Effect of Acetic acid solution on specimen
Increase in the weight of specimens
The increase in weight indicates porosity behavior of the specimens.
Both casting and injection molded specimen shows increase in weight of the composite
1120.3
1604.79
573.63
737.94
693.44
1134.271
1618.942
582.36
743.85
702.43
1141.5
1626.2
587.4
745.351
704.2
Casting 1 Casting 3 casting 5 Injection molding 3 Injection molding 5
0
200
400
600
800
1000
1200
1400
1600
1800
weight
(in
mg)
Sample no.
Initial weight (in mg)

Shore A Hardness value for injection molded specimen
44
 Specimen lies in medium hard range in shore A scale.
Hardness decreases by incorporation of lac resin
Maximum hardness value is obtained with the blend of (80 PET/20 CaCO3) wt/wt %

Conclusion
Injection molding turns out to be the optimum process than casting for developing
the composite structure.
In casting, if the temperature is not well controlled PET produces dripping of the
melted flaming material that could spread the fire.
Casting developed recycled composite structure specimen has porosity which can be
visible with the naked eyes.
It was also observed that increasing the lac content to 30% w/w during injection
molding process led to decrease in the fluidity of PET and CaCO3 filler blend.
CaCO3 provides opacity and increases stiffness.
45

Conclusion
Lac offers better surface finish when blend with PET but was unable to Produce
composite structure with 20 w/w % CaCO3 filler during casting.
Adhesive nature of lac has somewhat added advantage in both the process
(injection molding and casting) in binding PET and filler.
From the barrier testing, it was observed that concentrated sodium hydroxide
solution degrade the developed recycled composite structure and changes the
colorless solution of conc. NaOH to brownish color.
There was little increase in the weight of the specimen that may indicate the
porosity behavior of the developed composite structure.
Shore A hardness value for injection molded specimen refers that the specimen
ranges in medium hard polymeric material.
46

Future Scope
47
Using injection molding or extrusion lot many household product
could be developed such as decorative items, pots, outer layer
cover for mirrors, toothpaste stand, pen or mobile holder, hanger
for clothes, switch panels because of its dielectric nature etc.
High scope for contributing in circular economy.
Further mechanical study is required to know the actual tendency
of these blends for different applications.

REFERENCES
1. S. Singh, Solid Waste Management in Urban India: Imperatives for Improvement. Urban
India, Observer Research Foundation , 2020, pp. 1-44.
2. Our world in data, https://ourworldindata.org/plastic-pollution
3. Plastic Waste Management Institute, An Introduction to plastic recycling, Tokyo, vol. 2,
2019, pp. 1-36.
4. Chiyoda corporation, Overview of the Petrochemical and Chemical Industry, Japan,
https://www.chiyodacorp.com/en/service/chemistry/
5. Irina Slav, Oilprice.com, 2019, https://oilprice.com
6. Rajarapu Bhushaiah, Shaik Mohammad, D. Srinivasa Rao, Study of Plastic Bricks Made from
Waste Plastic, International Research Journal of Engineering and Technology , vol. 6 (4),
2019, pp. 1122-1126.
7. J. Hopewell, R. Dvorak, E. Kosior, Plastics recycling: challenges and opportunities. Biological
Sciences , 2009, pp.2115-2126
8. Amcor, 2009, https://www.amcor.com/insights/blogs/what-is-closed-loop-recycling
9. Eiji B Hosoda , Recycling of waste and downgrading of secondary resources in a classical
type of production model, Journal of Economic Structures, Springer , 2012, pp. 01- 22.
48

REFERENCES
• Houssame Limami, Asmae Khaldoun, A., Imad Manssouri and Khalid
Cherkaoui, Study of the suitability of unfired clay bricks with polymeric HDPE &
PET wastes additives,Elsevier - Journal of Building Engineering, Vol. 27, 100956,pg.
1-10, 2020.
• K. K. Sharma, A. Roy Chowdhury, and S. Srivastava, Chemistry and applications of
Lac and Its By-Product, Springer Nature Switzerland ,2020.
• Rebecca j. Stacey, Carl heron, Mark Q. Sutton, The Chemistry, Archaeology, and
Ethnography of a Native American Insect Resin, Journal of California and Great
Basin Anthropology,1998.
• Muhammad Akmal, Ahmad Saidi, Farah Syazwani Mazlan, Azman Hassan,
Rashita Abd. Rashid,Abdul Razak Rahmat, Flammability, Thermal and Mechanical
Properties of Polybutylene Terephthalate (PBT)/ Calcium carbonate composites,
Journal of Physical Science, Vol. 30(3), 175–189, 2019.
• Adesakin A.O, Ajayi O.O, Imosili P.E, Attahdaniel B.E, Characterization and
Evaluation of Mechanical Properties of Calcium carbonate as Filler in Polyester,
The International Institute for Science, Technology and Education (IISTE), Vol.3
No.8, Pg. 36-40, 2013. 49

REFERENCES
• Noel Deepak Shiri, P. Varun Kajava, Ranjan H. V., Nikhil Lloyd Pais, Vikhyat M.
Naik , Processing of Waste Plastics into Building Materials Using a Plastic Extruder
and Compression Testing of Plastic Bricks ,Journal of Mechanical Engineering and
Automation, August 2015.
• R. S. Kognole, Kiran Shipkule, Manish Patil, Lokesh Patil, Udaysinh Survase,
Utilization of Plastic waste for Making Plastic Bricks, International Journal of Trend
in Scientific Research and Development (IJTSRD), June 2019.
• Rajarapu Bhushaiah, Shaik Mohammad, D. Srinivasa Rao ,Study of Plastic Bricks
Made From Waste Plastic ,International Research Journal of Engineering and
Technology, Apr 2019 .
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Technology (IRJET), Vol. 07 Issue: 06, 2020, pg. 3545-3551.
50

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• Firas Awaja, Dumitru Pavel, Recycling of PET, European Polymer Journal , Elsevier,
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• John Scheirs, Polymer Recycling:Polymer Science & Technology, 1998, pp. 01-614.
• M. Wegelin, S. Canonica, A. C. Alder, D. Marazuela, M. J.-F. Suter, Th. D. Bucheli,
O. P. Haefliger, R. Zenobi, K. G. McGuigan, M. T. Kelly, P. Ibrahim , M. Larroque,
Does sunlight change the material and content of polyethylene terephthalate
(PET) bottles?, Journal of Water Supply: Research and Technology, 2001, pp. 125-
133.
• Biplob Nandy, Gaurav Sharma, Saryu Garg, Shweta Kumari, Tess George,
Yengkhom Sunanda, Barbel Sinha, Recovery of consumer waste in India – A mass
flow analysis for paper, plastic and glass and the contribution of households and
the informal sector, Resources, Conservation and Recycling, 101,2015, pg. 167–
181.
• Vannessa Goodship, Plastic recycling, Science Progress, Vol. 4, 2007, pg. 245–268.
51

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