Study In The Effect Of Compatibilizer On The Properties Of Oil Palm Shell Powder Filled Polypropylene.

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UNIVERSITI TEKNIKAL MALAYSIA MELAKA

Study in the Effect of Compatibilizer on the

Properties of Oil Palm Shell Powder Filled

Polypropylene

Thesis submitted in accordance with the partial requirements of the Universiti Teknikal Malaysia Melaka for the Degree of Bachelor of Engineering (Honours) Manufacturing (Materials Engineering)

Khairun Nasuha bin Ambar

Faculty of Manufacturing Engineering April 2008

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UTeM Library (Pind.1/2005)

SULIT

TERHAD

TIDAK TERHAD

(Mengandungi maklumat yang berdarj ah keselamat an at au kepent ingan Malaysia yang t ermakt ub di dalam AKTA RAHSIA RASMI 1972)

(Mengandungi maklumat TERHAD yang t elah dit ent ukan oleh organisasi/ badan di mana penyelidikan dij alankan)

(TANDATANGAN PENULIS)

Alamat Tet ap: No 19 Jln Pasu

Rumah Murah Macap, 86200 Spg Renggam, Johor.

Tarikh: _______________________

Disahkan oleh:

(TANDATANGAN PENYELIA)

Cop Rasmi:

Tarikh: _______________________

* Tesis dimaksudkan sebagai t esis bagi Ij azah Dokt or Falsaf ah dan Sarj ana secara penyel idikan, at au disert asi bagi pengaj ian secara kerj a kursus dan penyel idikan, at au Laporan Proj ek Sarj ana Muda (PSM). ** Jika t esis ini SULIT at au TERHAD, sil a l ampirkan surat daripada pihak berkuasa/ organisasi berkenaan dengan menyat akan sekali sebab dan t empoh t esis ini perl u dikel askan sebagai SULIT at au TERHAD.

BORANG PENGESAHAN STATUS TESIS*

JUDUL: STUDY IN THE EFFECT OF COMPATIBILIZER ON THE PROPERTIES OF OIL PALM SHELL POWDER FILLED POLYPROPYLENE

SESI PENGAJIAN: 2/ 2007-2008

Saya _____________________________________________________________________

mengaku membenarkan t esis (PSM/ Sarj ana/ Dokt or Falsaf ah) ini disimpan di Perpust akaan Universit i Teknikal Malaysia Melaka (UTeM) dengan syarat -syarat kegunaan sepert i berikut :

1. Tesis adalah hak milik Universit i Teknikal Malaysia Melaka.

2. Perpust akaan Universit i Teknikal Malaysia Melaka dibenarkan membuat salinan unt uk t uj uan pengaj ian sahaj a.

3. Perpust akaan dibenarkan membuat salinan t esis ini sebagai bahan pert ukaran ant ara inst it usi pengaj ian t inggi.

4. **Sila t andakan (√)

KHAIRUN NASUHA BIN AMBAR

√

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APPROVAL

This thesis submitted to the senate of UTeM and has been accepted as partial fulfillment of the requirements for the degree of Bachelor of Manufacturing Engineering (Engineering Material).

The members of the supervisory committee are as follow:

……… Main Supervisor

(Official Stamp and Date)

……….. Co – Supervisor

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DECLARATION

I hereby, declared this thesis entitled “Study in the Effect of Compatibilizer on the Properties of Oil Palm Shell Powder Filled Polypropylene.” is

the results of my own research except as cited in references

Signature : ………

Author’s Name : ………

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DEDICATION

“Thanks to my parent, my family, my friends and all people that involve in this study for their support and guidance”

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ACKNOWLEDGEMENTS

In the Name of Allah, The Beneficent, The Merciful, thanks for His guidance to accomplish this project. I would like express my profound appreciation to all persons and group of persons that involve, lend a hand and contribute idea in accomplishing this project especially to Mr. Edeerozey bin Abd Manap, my supervisor that guide me during two semesters of PSM 1 and PSM 2 and he also assist me during all important part in this project. I also would like to offer a special thank you to all my friends under same supervisor that lend a hand in this project specially Wan Mazuwan bin Wan Azhal, Mohamed Asyraff bin Rafeek Ahmad, and Mohd Hafiz bin Abd Rahman. I wish to express my appreciation to Mr. Mazlan bin Ahmad, technicians at Ceramic and Polymer laboratory at Universiti Teknologi Tun Hussein Malaysia, also to Mr. Azhar Shah, Mr. Hisham and all technicians that guide me during all process related to this project. My appreciation goes to Universiti Teknologi Tun Hussein Malaysia (UTHM) and my colleagues in the Faculty of Manufacturing Engineering for their understanding and supportive towards my study. The working environment here was very supportive and student friendly. I also want to thanks to my parent and family that give their fully support to me and encouragement for me to become more successful and concern more on this study. And lastly I would like to express special thanks to my dearest roommate Muhammad Affendi that give me full support, advise and idea that really useful and that is very important reinforcement for me to complete this study.

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ABSTRACT

The main goal of this research is to fabricate a lightweight composite material using environmentally friendly natural particulate reinforcement, to characterize the mechanical properties of oil palm shell powder filled polypropylene and to investigate the effect of AMPS on its mechanical properties. This research is conducted to recycle oil palm shell; oil palm shell powder will be used as a reinforcement of oil palm shell powder/polypropylene composite. The mechanical properties of this composite will be determined and compared with same composite but with existence of Aminopropyltriethoxysilane (AMPS). Processing involve to produce this composite is crushing, mixing, and hot pressing. The purpose of doing process above is to make sure oil palm shell powder mix well and homogenously with polypropylene, this is because bonding between oil palm shell powder and polypropylene still can be improved to upgrade it properties. Mechanical properties that will be determined are a flexural strength, tensile strength and impact strength, while physical properties determined is water absorption test. All tests for this material is referred and followed under American Standard Materials Testing (ASTM) for composite material. As the results, all mechanical properties and physical properties of oil palm shell filled polypropylene with compatibilizer is better than oil palm shell powder filled polypropylene without compatibilizer, that mean compatibilizer can improve properties of this material.

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ABSTRAK

Tujuan utama kajian ini adalah untuk menghasilkan komposit dari bahan terpakai dan mesra alam sekitar, serta mengenal pasti sifat-sifat serta kesan AMPS terhadap komposit ini.Kajian ini dilakukan untuk mengitar semula tempurung kelapa sawit di mana tempurung ini dijadikan bahan penguat dan diproses bersama polypropylene untuk dijadikan komposit. Sifat-sifat mekanikal komposit ini akan dihitung dan dibuat perbandingan dengan komposit dari bahan yang sama tetapi diproses dengan menggunakan bahan campuran Aminopropyltriethoxysilane (AMPS). Proses terlibat dalam menghasilkan komposit ini termasuklah proses menghancurkan tempurung kelapa sawit (crushing), menyebatikan tempurung kelapa sawit hancur dengan polypropylene (mixing) dan membentuk kepingan komposit pada suhu dan tekanan tinggi (hot pressing). Tujuan kesemua proses tadi dibuat adalah untuk memastikan serbuk tempurung kelapa sawit ini dicampur dan diadun sebati dengan polypropylene, ini kerana ikatan antara serbu tempurung kelapa sawit dengan polypropylene dapat diperbaiki dan sifat-sifat fizikal dan mekanikalnya dapat ditingkatkan. Ujian kelenturan, ujian terikan, ujian impak and kadar serapan air akan dilakukan mengikut American Standard Materials Testing (ASTM) untuk bahan komposit. Dan keputusan ujian-ujian ini menunjukkan komposit serbuk kelapa sawit dan polypropylene yang dicampur AMPS mempunyai sifat-sifat fizikal dan mekanikal yang lebih baik berbanding komposit yang tidak dicampur AMPS. Ini menunjukkan bahan AMPS ini dapat memperbaiki sifat-sifat bahan ini.

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TABLE OF CONTENTS

DECLARATION i

DEDICATION ii

ACKNOWLEDGEMENT iii

ABSTRACT iv

ABSTRAK v

TABLE OF CONTENT vi

LIST OF TABLE x

LIST OF FIGURES xi

LIST OF SYMBOLS xiii

LIST OF APPENDICES xv

1. INTRODUCTION 1

1.1 Background 1

1.2 Problem Statements 2

1.3 Objectives of the study 2

1.4 Scope of Study 3

1.5 Hypothesis 3

2. LITERATURES REVIEW 4

2.1 Composite 4

2.1.1 Matrix 4

2.1.2 Reinforcement 5

2.2 Particulate reinforced composite 6 2.3Polymer matrix composite 6

2.4Oil palm 8

2.4.1 Oil palm plantation in Malaysia 10

2.5 Polypropylene 13

2.5.1Application of Polypropylene 14 2.6 Aminopropyltriethoxysilane (AMPS) 15

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2.7 Variable Speed Rotor Mill 17

2.8 Extrusion 18

2.8.1 Materials 20

2.8.2 Tolerances 21

2.8.3 Advantages of extrusion 21

2.8.4 Defects in Extrusion 21

2.9 Universal testing machine 23

2.10 Impact machine 25

2.10.1 Charpy and Izod test 25

2.10.1.1 Charpy test 25

2.10.1.2 Izod test 26

3. METHODOLOGY 27

3.1 Introduction 27

3.2 Material preparation 28

3.2.2 Extrusion moulding process 28

3.2.3 Crushing 30

3.2.4 Hot press 30

3.3 Material testing 31

3.3.1 ASTM for flexural properties C 393 31 3.3.1.1 Apparatus for flexural test 31

3.3.1.2 Test specimen 31

3.3.1.3 Three point bending 32 3.3.1.4 Testing calculation 32 3.3.2 ASTM for tensile testing D 3039M 34 3.3.2.1 Apparatus of testing 34

3.3.2.2 Test specimen 34

3.3.2.3 Test procedure 35

3.3.3 ASTM for water absorption of core material C272 36 3.3.3.1 Apparatus of testing 36

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3.3.3.3 Test procedure 37

3.3.3.4 Calculation 37

3.3.4 Impact Test ASTM D 256 38

3.3.4.1 Test specimen 38

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4.0 RESULT 39

4.1Material preparation 39

4.2ASTM for flexural properties C 393 40 4.3ASTM for tensile testing D 3039M 43 4.4ASTM for water absorption of core material C272 45

4.5Impact Test ASTM D 256 46

5.0 DISCUSSION 48

5.1Effect of Aminopropyltriethoxysilane on flexural properties 48

5.2Tensile strength 50

5.3Water absorption 52

5.4Impact Test 53

6.0 CONCLUSION AND RECOMMENDATION 56

6.1Conclusion 56

6.2Suggestion and recommendation 57

REFERENCES 58

APPEDICES 60

A Gantt chart B Graphs C Pictures

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LIST OF TABLES

NO TITLE PAGE

2.1 Typical Physical Properties 15 4.2 Flexural modulus for 15% oil palm shell powder 41

filled pp without compatibilizer

4.3 Flexural modulus for 15% oil palm shell powder 42 filled pp with compatibilizer

4.4 Tensile strength for 15% oil palm shell powder 44 filled pp without compatibilizer

4.5 Tensile strength for 15% oil palm shell powder 44 filled pp with compatibilizer

4.6 Value of water absorption for 15% oil palm shell 45 powder filled pp with compatibilizer

4.7 Value of water absorption for 15% oil palm shell 45 powder filled pp without compatibilizer

4.8 Impact value for 15% oil palm shell powder filled 46 pp without compatibilizer

4.9 Impact value for 15% oil palm shell powder filled 47 pp with compatibilizer

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LIST OF FIGURES

NO TITLE PAGE

2.1 Structure of palm fruit 9 2.2 Cross section of a fruitlet 9

2.3 Fresh fruit bunch 10

2.4 Fresh fruit (on the left cut fruit) 10 2.5 Polypropylene produce from propylene monomer 13 2.6 Isotactic polypropylene 13 2.7 Atactic polypropylene 14 2.8 Aminopropyltriethoxysilane chemical structure 15 2.9 Picture of Aminopropyltriethoxysilane in polymer lab 16 2.100 Picture of rotor mill machine 17 2.11 Sieves ring and rotor blade 18 2.112 Plasticizing single screw extruder 19 2.123 Engineering Stress-Strain Diagram depicting 23

important mechanical properties for metals

2.134 Anatomy of a universal hydraulic testing machine 24 2.145 Picture of impact tester machine 25 3.1 Flow chart processes 27 3.2 Extrusion machine in polymer lab 29 3.3 Crusher and hot press machine 30 3.4 Three point bending 32

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4.15 Picture of oil palm shell powder with different 39 powder sizes

4.16 Extruded oil palm shell powder and polypropylene mixture 40 4.17 Specimen after hot pressed 40 4.4 Example of graph obtained from for flexural tests 41 4.5 Example of curve stress vs. strain during tensile strength 43 4.6 Example of table from Trapezium2 software for flexural 43

test

5.18 Graph shows maximum force for 15% oil palm shell 49 filled polypropylene with compatibilizer

5.2 Three type of stress/strain graph 50 5.3 Stress vs. strain graph for 15% oil palm shell powder filled 51

polypropylene

5.3 Picture shows how silane reacts between matrix and 50 reinforcement

5.4 Graph impact value vs. specimen 53 5.5 Bar chart that show comparison of impact strength value 54

between both composite

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LIST OF SYMBOLS

σ Tensile strength

σf Stress in outer fibers at midpoint, [MPa]

εf Strain in the outer surface, [%]

Eb Modulus of elasticity in bending,[MPa] AMPS Aminopropyltriethoxysilane

ASTM American standard testing material

b Width of test beam, [mm] C Carbon

CMC Ceramic matrix composite CPO Crude palm oil

d Depth of tested beam, [mm]

D maximum deflection of the center of the beam, [mm] E Flexural Modulus PP Polypropylene

L Support span, [mm]

m Slope of the tangent to the initial straight-line portion of the load deflection curve, [N/mm]

MAPP Maleic Anhydride Polypropylene MMC Metal matrix composite

P load at a given point on the load deflection curve, [N] PE Polyethylene

PMC Polymer matrix composite R&D Reasearch and development Rp Radius the plastic zone Si Silicon

UTeM Universiti Teknikal Malaysia Melaka UTHM Universiti Teknologi Tun Hussein Malaysia UTM Universal Testing Machine

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LIST OF APPENDICES

APPENDIX TITLE PAGE

A1 Gantt Chart for semester 1 59 A2 Gantt Chart for semester 2 59 B Stress strain curves for flexural and tensile test 60 C Pictures

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CHAPTER 1 INTRODUCTION

1.1Background

Natural fiber composites have attracted the attention of scientists and engineers due to their low cost, low density an environmentally harmless properties. Many attempts have been made to prepare and evaluate natural fiber composites for various applications.

Polypropylene (PP) and oil palm shell powder are used to produce polymer composite in this project. The processes involved in producing this composite are a crushing of oil palm shell, extrusion moulding process, hot pressing and some cutting process. The purpose of crushing is to produce particulate form of oil palm shell, while the using of extrusion moulding machine is to produce a compound of oil palm shell powder and PP with a good blend. The extruded oil palm shell powder/PP composite will then crushed into crusher into small granules.

After the panel of oil palm shell/PP composite is prepared, it will be cut into specific dimension that required by its testing, in this research, 4 type of testing i.e. flexural strength, tensile strength, impact strength and water absorption will be conducted. All testings follow the American Standard Testing Material (ASTM) and the details about these testing will be elaborated in Chapter 2.

As a method to improve the compatibility between particulate reinforcement and the matrix, compatibilizer will be used in this project. By improving the compatibility between oil palm shell and PP, the mechanical properties also will be improved. The mechanical properties of the composite will be characterized by studying the flexural strength, impact strength, Young modulus, water absorption and effect of the compatibilizer on the properties of the composites itself.

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The main bottlenecks in the broad use of natural particulate reinforcement in various polymer matrixes are poor compatibility between the particulate and the matrix, and the inherent high moisture absorption, which brings in involvement of compatibilizer in the composite. The efficiency of a particulate reinforce composite depends on the reinforcement/matrix interface and the ability to transfer stress from the matrix to reinforcement. In this project, in order to improve the compatibility between oil palm shell powder and PP granule, Aminopropyltriethoxysilane compatibilizer is used. Effect of compatibilizer on the properties of oil palm shell powder filled polypropylene will be studied (Callister Jr., 2003).

1.3Objective of the project

• To fabricate a lightweight composite material using environmentally friendly natural particulate reinforcement

• To characterize the mechanical properties of oil palm shell powder filled polypropylene

• To investigate the effect of Aminopropyltriethoxysilane compatibilizer on the bonding properties between oil palm shell powder filled polypropylene

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1.4 Scope of the project

In this project, the effect of Aminopropyltriethoxysilane compatibilizer on the mechanical properties of oil palm shell powder/ polypropylene composite will be discussed. The mechanical properties studied in this project are flexural strength, impact strength, tensile strength and water absorption. However this report will not cover on effect of other compatibilizer on this composite.

1.5 Hypothesis

In this research, it is expected that the use of the compatibilizer will improve the mechanical properties of oil palm shell powder/PP composites such as its tensile strength, flexural strength, impact strength, and water absorption.

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CHAPTER 2 LITERATURE REVIEW

2.1 Composite

Composite is a multiphase material and the constituent phase must be chemically dissimilar and separate by a distinct interface. It can be divided into 3 groups that is Fiber reinforced composite, particulate reinforce composite and structural composite.

2.1.1 Matrix

The phase in composite that continuous and surround the other phases that is reinforcement. Matrix is being melted and that mean some of their properties are changed. The problem of brittleness in reinforcement can be solved by using matrix. The reinforcement is bonded to matrix means any loads applied to a composite are carried by both constituents. Usually the reinforcement is the stiffer and stronger constituent while the matrix is supposed to transfer the load to the reinforcement.

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2.1.2 Reinforcement

Reinforcement is discontinuous phase that surrounded by matrix phase. It is often a strong, stiff material the problem of this material is brittleness; although able to sustain a high stress. It’s not melted and in solid and monolithic form, mechanical properties and chemical properties not change.

Many composites used today are applied especially in aircraft and spacecraft, with very good performance appropriate costs. But the idea of using composite to produce better properties actually has been used by nature for millions of years. Ancient society, imitating nature, used this approach as well, for example using straw to reinforce mud in brick making, without which the bricks would have almost no strength. Fibers used in modern composites have strengths and stiffnesses far above those of traditional bulk materials. The high strengths of the glass fibers are due to dispensation that circumvents the internal or surface flaws which normally weaken glass and the strength and stiffness of the polymeric aramid fiber is a significance of the nearly perfect alignment of the molecular chains with the fiber axis.

These materials are not generally functional as fibers alone, and naturally they are infusing by a matrix material that acts to transfer loads to the fibers, and also to defend the fibers from abrasion and environmental attack. The matrix dilutes the properties to some degree, but even so very high specific (weight-adjusted) properties are available from these materials. Metal and glass are offered as matrix materials, but these are now very expensive and largely limited to R&D laboratories. Polymers are much more commonly used, with unsaturated styrene-hardened polyesters having the majority of low-to-medium performance applications and epoxy or more sophisticated thermosets having the higher end of the market. Thermoplastic matrix composites are increasingly eye-catching materials, with processing difficulties being perhaps their principal drawback (Matthews and Rawlings, 1999).

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2.2 Particulate reinforced composite

To produce particulate reinforcement is much simpler an easier than fiber and because of that, many material can be produce into particulate form. Roughly all material can be produced into powder, there have many method can be used to produce this powder for example bulk processing, precipitation from solution, gas atomization and sol-gel processing. Particulate reinforcements have dimensions that are approximately equal in all directions. The shape of the reinforcing particles may be spherical cubic, platelet or any irregular shape. The arrangement of particulate reinforcement may be random or with a preferable orientation, however for practical purpose it is made in random orientation.

2.3 Polymer matrix composite

Polymeric material is the most common composite material; firstly it is because the strength and stiffness are low compared to metals and ceramics. So, its mechanical properties are not adequate for many purpose of application, and this can be compensated by the use of reinforcement. Secondly the processing of PMC (polymer matrix composite) is easier than CMC (ceramic matrix composite) or MMC (metal matrix composite) because high temperature and pressure are not required. Equipment for this processing also simpler and less cost. For this reason, PMC is being used widely in structural application. PMC can be classified into three categories that are thermosetting, thermoplastics and rubber.

Over three quarters of all matrices of PMC’s are thermosetting polymers, thermosets have cross-linking bonding that stronger than bonding in thermoplastic, but the limitation of cross-linking bonding is it cannot be melted because it can cause it lost it properties; compare than thermoplastic, it can be melted and after solidification it gain it properties. That why thermosetting process not applied high temperature (not reach melting point) and pressure. On the other hand, thermosets have their own advantages; it can be used at high temperatures and better creep properties than thermoplastics. They are also more resistance to chemical attack than most thermoplastics.

While thermoplastic should be melted during processing to allow them to fabricate into required shape after it solidified. This type of polymer can be melted repeatedly after fabricated and solidified; however it may degrade if it was melted too many times or heated too much temperature above melting point. As mentioned before, thermosets is a cross linking polymer

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and regain its properties through that type of bonding, while thermoplastic has linear or branches structure because they not cross linking to network. Even though it can be branches, it is still different with network in thermosets. The bonding between chains in thermoplastic is weak van der Waals forces that not strong against combined action of thermal activation and applied stress. This is why the thermoplastic flow at elevated temperatures.

Rubbers composite include in group of PMC, natural rubber is latex from Havea Brasiliensis and contain more than 98% polyisoprene. Polyisoprene can be cis and trans but the cis form is the main constituent of natural rubber. To gain suitable properties of rubber for structural purpose, it has to be vulcanized or in the more clear word it is a process to make the long molecule of rubber to become cross linking. The agent in vulcanized is usually sulphur and the stiffness and the strength increase is depending on the amount of cross linking.

There are many type of PMC processing such as hand lay-up, spray up (almost same with hand lay-up but use spray method), Match die moulding, forming methods employing gas pressure, Low pressure closed mould system, Pultrusion, Filament winding and many more. We use hands method in this experiment because it is easier, low cost and knowingly as effective method to introduce students in producing PMC.

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