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CHARACTERIZATION AND MECHANICAL
PROPERTIES OF VINYL ESTER
RESIN/EPOXIDIZED PALM OIL/CLAY
NANOCOMPOSITE
Presented by: AmirAli Khalili
Supervisor: Assoc.Prof. Dr Abdul Razak Bin Rahmat
March 03, 2014
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Introduction
Literature review Methodology
Results and Discussions
Conclusion and Recommendations
Content
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Bio-basedpolymer
Plant Oils
Polymeric composite
Eco-friendly
Triglycerides
Functionalization
Introduction
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Nowadays, biodegradable vegetable oils have attracted more
attention due to oil crises (raw material with relative high cost and
low production), biodegradability and environmental friendly.
There are several techniques and various types of catalyst that have
been used by researchers to cure epoxidized vegetable oils and
hence produced thermosetting polymer resin such as epoxy
(Zlataniet al.,
2004).
Green thermosetting resins were prepared using epoxidized palm
oil (EPO) and epoxy based petroleum (Mamauod et al., 2012).
Background of study
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Due to the advantage of Malaysia as the producer ofpalm oil, this research plans to explore the potential ofepoxidized palm oil (EPO).
Several studies have investigated about different ratio ofVE/AESO, UPE/ ESO and VE/nanoclay. However, theEPO/VE/nanoclay ratios have not been developed.Following are some of the questions that need to beanswered to expand this research area.
Problem Statement
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What are the effects of loadings of EPO/VE/nanoclay composite on
thermal characteristic and curing behavior of composite resin as well as its
resistance to moisture absorption?
What are the effects of loadings of EPO/VE/nanoclay composite on the
mechanical properties of the composite resin such as tensile, flexural and
impact strength?
What are the dispersion and morphology of nanoclay inclusion in EPO/VE
resin composite resin?
Problem Statement
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To investigate the effect of composition of EPO/VE/nanoclayon the mechanical properties of nanocomposite polymerresin such as flexural, tensile, impact strength.
To characterize EPO/VE/nanoclay composite on thermal andcuring behavior of nanocomposite polymer resin as well as itsresistance to thermal decomposition compared to the parentVE and EPO.
To determine the dispersion and morphology of nanoclayinclusion in EPO/VE.
Objective
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Preparation of EPO/VE/clay at various ratio of VE/EPO 100/0, 95/5,92.5/7.5and 90/10-wt % respective and clay at various amounts of 1,2and 3 phr.
Mechanical testing of EPO/VE/clay using tensile, flexural and impacttest.
Characterization analysis on the thermal and curing behavior ofEPO/VE/nanoclay resin for using Fourier transform infrared (FTIR) anddifferential scanning calorimetry (DSC).
Morphological study of EPO/VE/nanoclay resin using atomic forcemicroscopy (AFM).
Scope
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Literature Review
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Type of Resin Advantages Disadvantages
Epoxy
High mechanical and thermal
properties. High water
resistance. Long working times
available. Temperature
resistance can be up to 140C
wet/220C dry. Low cureshrinkage
More expensive than
vinylesters.
(315/kg) Critical
mixing. Corrosive
handling
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Resin Advantages Disadvantages
Polyester
Easy to use
Lowest cost of resins
available (12/kg)
Only moderate mechanical
properties. High styreneemissions in open molds.
High cure shrinkage
Limited range of working
times
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Resin Advantages Disadvantages
Vinylester
Very high
chemical/environmental resistance.Higher mechanicalproperties thanpolyesters
Postcure generally
required forhigh properties. Highstyrene content.Higher cost thanpolyesters (24/kg)High cure shrinkage
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Type of Vinyl Ester Resins Epoxy vinyl ester resins
Non epoxy vinyl ester resins.
Curing Reaction
Initiator
Crosslinking
Vinyl ester resin
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Schematic representation of free-radical crosslinking mechanism.
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Vegetable Oils
R1 R2 R3fatty acid chain
Schematic of a triglyceride molecule
Synthesis of triglyceride
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Vegetable Oils
a) Palm oil b) Epoxidized palm oil
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Types of Nanocomposites Conventional Composite
Intercalated Composite
Delaminated Composite or exfoliated
Nanoclay
Nanocomposites
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Nanocomposites
Schematic representations of different types of composite
prepared from the layered silicates and polymers
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Autor Blend Year Result
Miyagawa UPE/EMS 2006 High elastic
modulus, Constant
Tg, HDT and E
decreased
Haq UPE/ESO/silicate 2009 Thermo-Physical
properties improved,
Karger VE/AESO 2010 Modulus, Strength
and Tg decreased but
ductility and
Fracture toughness
increased
Gefu VE/MMT 2008 Mechanical
properties improved
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METHODOLOGY
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Bisphenol-A type epoxy Vinyl ester resin (VE)
Epoxidized Palm oil (EPO)
Methyl ethyl ketone peroxide (MEKP)
Organically modified montmorilloniteCloisite 30B
Styrene
Materials
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Sample PreparationFormulations of VE/EPO/CALY
Formulation Vinyl ester
resin wt%
Epoxidized
Palm Oil wt%
Clay (phr)
VE/EPO 100 0 0,1,2,3
VE/EPO 95 5 0,1,2,3
VE/EPO 92.5 7.5 0,1,2,3
VE/EPO 90 10 0,1,2,3
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SonicationClay (1Kg) +Acetone
(50L)
for 2 hours
Mixing
Sonicatedclay/Acetone+ VE
Acetone Removal
Heating on heater @55 oC for 3 hours
Styrene Addition
Add a lost amount ofstyrene
Initiator Addition
(MEKP)1.5 wt %
Mixing
EPO+VE+clay
Stirring
Curing
@ room temperaturefor 24 hours
Post curing
@ 120 oC for 2 hours
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Fourier Transform Infra-red Spectroscopy (FTIR)
X-ray Diffraction (XRD)
Differential scanning calorimetry (DSC)
Atomic Force Microscopy (AFM)
Flexural Test
Tensile Test
Impact Testing
Characterization
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Results and Discussion
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Tensile Properties of VE/ EPO/ Clay
Nanocomposite
0
10
20
30
40
50
0 2.5 5 7.5 10 12.5
Tensilestrength(Mpa)
EPO wt%
0
0.5
1
1.5
2
2.5
3
0 2.5 5 7.5 10 12.5
tensileModulus(GPa)
EPO wt%
Effect of EPO content on tensilestrength of VE/EPO blend
Effect of EPO content on tensilemodulus of VE/EPO blends
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Tensile Properties of VE/ EPO/ Clay
Nanocomposite
0
5
10
15
20
25
30
35
0 1 2 3
TensileStrength(MPa)
Clay Loading (phr)
0
500
1000
1500
2000
2500
3000
0 1 2 3 4
TensileModulu
s(MPa)
Clay loading (phr)
Tensile strength of VE/5 wt% EPOwith various clay loadings
Tensile modulus of VE/5 wt% EPOwith various clay loadings
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Tensile Properties of VE/ EPO/ Clay
Nanocomposite
0
0.5
1
1.5
2
2.5
3
3.5
4
0 1 2 3
ElongationatBreak(%)
Clay Loading (phr)
Elongation at break of VE/5 wt% EPO with various clay loadings
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Flexural Properties VE/EPO/ Nanoclay
Composite
0
5
10
15
20
2530
35
40
0 0.5 1 1.5 2 2.5 3 3.5
flexuralstrength(M
pa)
Clay Loading (phr)
0
500
1000
1500
2000
2500
3000
3500
4000
0 1 2 3
flexuralmodulus
(Mpa)
Clay Loading (phr)
Flexural strength of VE/5 wt% EPOwith various clay loadings
Flexural modulus of VE/5 wt% EPO withvarious clay loadings
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Flexural Properties VE/EPO/ Nanoclay
Composite
0
0.01
0.02
0.03
0.04
0.05
0.06
0 2.5 5 7.5 10 12.5
flexuralstrain
EPO Loading (wt%)
Flexural strain of VE/EPO with various EPO loadings
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Impact Properties VE/EPO/ Nanoclay
Composite
0
5
10
15
20
25
30
35
40
45
50
0 2.5 5 7.5 10 12.5
Impactstr
ength(J/m)
EPO wt%
0
5
10
15
20
25
30
35
40
0 1 2 3 4
impactstren
gth(J/m)
Clay Loading (phr)
Impact strength of VE/5 wt% EPO withvarious clay loadings
Impact strength of VE/EPO with variousEPO content
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X-Ray Diffraction VE/EPO/Nanoclay
Composite
0
50
100
150
200
250
300
350
400
450
500
0 10 20 30 40 50
Intensity
2 ( )
ag
h
0
50
100
150
200250
300
350
400
450
500
0 10 20 30 40 50
Intensity
2 ()
abac
ad
X-Ray Diffraction (XRD) pattern of (a) clay;(g)VE; (h) VE/5 wt% EPO
X-Ray Diffraction (XRD) pattern of(ab) clay; (ac) VE/5 wt% EPO; (ad)VE/5 wt% EPO/1 phr clay
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Fourier Transform Infrared spectroscopy
(FTIR)
FTIR spectrum of VE, EPO and VE/EPO blends
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Differential Scanning Calorimetry Study of
VE/EPO Blends
DSC thermograms of VE and VE/EPO blends
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Atomic Force Microscopy (AFM)
AFM 3D topography VE/EPO5% /Clay 2 phr AFM 3D topography VE/EPO 5%/Clay 1 phr
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Months
Activities
S O N D J F M A M J J A
Literature
Study andWriting
Proposal
Designing theProcess and
MaterialsPreparation
Preparation ofNanocomposite
AnalyzingData
WritingDissertation 2
Writing Paper
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