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
2
Introduction
Literature review
Methodology
Results and Discussions
Conclusion and Recommendations
Content
Bio-based
polymer
Plant Oils
Polymeric composite
Eco-friendly
Triglycerides
Functionalization
Introduction
4
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
(Zlatani et al., 2004).
Green thermosetting resins were prepared using epoxidized palm
oil (EPO) and epoxy based petroleum (Mamauod et al., 2012).
Background of study
5

Due to the advantage of Malaysia as the producer of
palm oil, this research plans to explore the potential of
epoxidized palm oil (EPO).

Several studies have investigated about different ratio of
VE/AESO, UPE/ ESO and VE/nanoclay. However, the
EPO/VE/nanoclay ratios have not been developed.
Following are some of the questions that need to be
answered to expand this research area.

Problem Statement
6
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
7
To investigate the effect of composition of EPO/VE/nanoclay
on the mechanical properties of nanocomposite polymer
resin such as flexural, tensile, impact strength.

To characterize EPO/VE/nanoclay composite on thermal and
curing behavior of nanocomposite polymer resin as well as its
resistance to thermal decomposition compared to the parent
VE and EPO.

To determine the dispersion and morphology of nanoclay
inclusion in EPO/VE.
Objective
8
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 impact
test.

Characterization analysis on the thermal and curing behavior of
EPO/VE/nanoclay resin for using Fourier transform infrared (FTIR) and
differential scanning calorimetry (DSC).

Morphological study of EPO/VE/nanoclay resin using atomic force
microscopy (AFM).
Scope
9
Literature Review
10

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 cure
shrinkage
More expensive than
vinylesters.
(315/kg) Critical
mixing. Corrosive
handling
11
Resin Advantages Disadvantages
Polyester
Easy to use
Lowest cost of resins
available (12/kg)
Only moderate mechanical
properties. High styrene
emissions in open molds.
High cure shrinkage
Limited range of working
times
12
Resin Advantages Disadvantages
Vinylester
Very high
chemical/environment
al resistance.
Higher mechanical
properties than
polyesters
Postcure generally
required for
high properties. High
styrene content.
Higher cost than
polyesters (24/kg)
High cure shrinkage
13
Type of Vinyl Ester Resins
Epoxy vinyl ester resins
Non epoxy vinyl ester resins.

Curing Reaction
Initiator
Crosslinking

Vinyl ester resin

14
Schematic representation of free-radical crosslinking mechanism.

15
Vegetable Oils
R1 R2 R3fatty acid chain

Schematic of a triglyceride molecule
Synthesis of triglyceride
16
Vegetable Oils
a) Palm oil b) Epoxidized palm oil
17
Types of Nanocomposites
Conventional Composite
Intercalated Composite
Delaminated Composite or exfoliated


Nanoclay

Nanocomposites

18
Nanocomposites
Schematic representations of different types of composite
prepared from the layered silicates and polymers
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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20



METHODOLOGY
21
Bisphenol-A type epoxy Vinyl ester resin (VE)
Epoxidized Palm oil (EPO)
Methyl ethyl ketone peroxide (MEKP)
Organically modified montmorillonite
Cloisite 30B
Styrene
Materials
22
Sample Preparation
Formulations of VE/EPO/CALY
Formulation
Wt %
Vinyl ester
resin (wt%)
Wt %
Epoxidized
Palm Oil (wt%)
Wt %
Clay (phr)
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

23
Sonication
Clay (1Kg) +Acetone
(50L)
for 2 hours
Mixing
Sonicated
clay/Acetone+ VE
Acetone Removal
Heating on heater @
55
o
C for 3 hours
Styrene Addition
Add a lost amount of
styrene
Initiator Addition
(MEKP)1.5 wt %
Mixing
EPO+VE+clay
Stirring
Curing
@ room temperature
for 24 hours
Post curing
@ 120
o
C for 2 hours
24
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
25
Results and Discussion
26
Tensile Properties of VE/ EPO/ Clay
Nanocomposite

0
10
20
30
40
50
0 2.5 5 7.5 10 12.5
T
e
n
s
i
l
e

s
t
r
e
n
g
t
h

(
M
p
a
)

EPO wt%
0
0.5
1
1.5
2
2.5
3
0 2.5 5 7.5 10 12.5
t
e
n
s
i
l
e

M
o
d
u
l
u
s

(
G
P
a
)

EPO wt%


Effect of EPO content on tensile
strength of VE/EPO blend
Effect of EPO content on tensile
modulus of VE/EPO blends
27
Tensile Properties of VE/ EPO/ Clay
Nanocomposite

0
5
10
15
20
25
30
35
0 1 2 3
T
e
n
s
i
l
e

S
t
r
e
n
g
t
h

(
M
P
a
)

Clay Loading (phr)
0
500
1000
1500
2000
2500
3000
0 1 2 3 4
T
e
n
s
i
l
e

M
o
d
u
l
u
s

(
M
P
a
)

Clay loading (phr)
Tensile strength of VE/5 wt% EPO
with various clay loadings


Tensile modulus of VE/5 wt% EPO
with various clay loadings

28
Tensile Properties of VE/ EPO/ Clay
Nanocomposite

0
0.5
1
1.5
2
2.5
3
3.5
4
0 1 2 3
E
l
o
n
g
a
t
i
o
n

a
t

B
r
e
a
k

(
%
)

Clay Loading (phr)
Elongation at break of VE/5 wt% EPO with various clay loadings

29


Flexural Properties VE/EPO/ Nanoclay
Composite

0
5
10
15
20
25
30
35
40
0 0.5 1 1.5 2 2.5 3 3.5
f
l
e
x
u
r
a
l

s
t
r
e
n
g
t
h
(
M
p
a
)

Clay Loading (phr)
0
500
1000
1500
2000
2500
3000
3500
4000
0 1 2 3
f
l
e
x
u
r
a
l

m
o
d
u
l
u
s
(
M
p
a
)

Clay Loading (phr)
Flexural strength of VE/5 wt% EPO
with various clay loadings

Flexural modulus of VE/5 wt% EPO with
various clay loadings

30


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
f
l
e
x
u
r
a
l

s
t
r
a
i
n

EPO Loading (wt%)
Flexural strain of VE/EPO with various EPO loadings

31
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
I
m
p
a
c
t

s
t
r
e
n
g
t
h


(
J
/
m
)

EPO wt%
0
5
10
15
20
25
30
35
40
0 1 2 3 4
i
m
p
a
c
t

s
t
r
e
n
g
t
h


(
J
/
m
)

Clay Loading (phr)
Impact strength of VE/5 wt% EPO with
various clay loadings

Impact strength of VE/EPO with various
EPO content

32
X-Ray Diffraction VE/EPO/Nanoclay
Composite

0
50
100
150
200
250
300
350
400
450
500
0 10 20 30 40 50
I
n
t
e
n
s
i
t
y

2 ( )
a
g
h
0
50
100
150
200
250
300
350
400
450
500
0 10 20 30 40 50
I
n
t
e
n
s
i
t
y

2 ()
ab
ac
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

33
Fourier Transform Infrared spectroscopy
(FTIR)

FTIR spectrum of VE, EPO and VE/EPO blends

34
Differential Scanning Calorimetry Study of
VE/EPO Blends

DSC thermograms of VE and VE/EPO blends

35
Atomic Force Microscopy (AFM)
AFM 3D topography VE/EPO5% /Clay 2 phr AFM 3D topography VE/EPO 5%
/Clay 1 phr
36

Months



Activities

S O N D J F M A M J J
A
Literature
Study and
Writing
Proposal


Designing the
Process and
Materials
Preparation


Preparation of
Nanocomposite


Analyzing
Data


Writing
Dissertation 2


Writing Paper



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