Amir Ali Presentation

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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

    Your logo here

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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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