Optimization Of Mixing Parameters To Produce PP - Enr Blend Via Response Surface Methodology.

(1)

UNIVERSITI TEKNIKAL MALAYSIA MELAKA

OPTIMIZATION OF MIXING PARAMETERS TO PRODUCE

PP/ENR BLEND VIA RESPONSE SURFACE METHODOLOGY

This report submitted in accordance with requirement of the Universiti Teknikal Malaysia Melaka (UTeM) for the Bachelor Degree of Manufacturing Engineering

(Engineering Material)

by

FAISAL FARIS BIN RAHIM B050910134

870116565273

FACULTY OF MANUFACTURING ENGINEERING 2012


(2)

UNIVERSITI TEKNIKAL MALAYSIA MELAKA

BORANG PENGESAHAN STATUS LAPORAN PROJEK SARJANA MUDA

TAJUK: Optimization of mixing parameters to produce PP/ENR blend via response surface methodology.

SESI PENGAJIAN: 2011/12 Semester 2

Saya FAISAL FARIS BIN RAHIM

mengaku membenarkan Laporan PSM ini disimpan di Perpustakaan Universiti Teknikal Malaysia Melaka (UTeM) dengan syarat-syarat kegunaan seperti berikut: 1. Laporan PSM adalah hak milik Universiti Teknikal Malaysia Melaka dan penulis. 2. Perpustakaan Universiti Teknikal Malaysia Melaka dibenarkan membuat salinan

untuk tujuan pengajian sahaja dengan izin penulis.

3. Perpustakaan dibenarkan membuat salinan laporan PSM ini sebagai bahan pertukaran antara institusi pengajian tinggi.

4. **Sila tandakan ()

SULIT

TERHAD

TIDAK TERHAD

(Mengandungi maklumat yang berdarjah keselamatan atau kepentingan Malaysia yang termaktub di dalam AKTA RAHSIA RASMI 1972)

(Mengandungi maklumat TERHAD yang telah ditentukan oleh organisasi/badan di mana penyelidikan dijalankan)

Alamat Tetap: No.100 Jalan TC 1/5

Taman Cemerlang, Gombak 53100 Kuala Lumpur

Tarikh: 1/06/2012

Disahkan oleh:

PENYELIA PSM

Tarikh: _______________________

** Jika Laporan PSM ini SULIT atau TERHAD, sila lampirkan surat daripada pihak berkuasa/organisasi berkenaan dengan menyatakan sekali sebab dan tempoh laporan PSM ini perlu dikelaskan sebagai SULIT atau TERHAD.


(3)

I hereby, declared this report entitled “Optimizing of mixing parameters to produce PP/ENR blend via response surface methodology” is the results of my own research except as cited in references.

Signature : ……….

Author’s Name : Faisal Faris Bin Rahim Date : 1st June 2012


(4)

This report is submitted to the Faculty of Manufacturing Engineering of Universiti Teknikal Malaysia Melaka (UTeM) as a partial fulfillment of the requirements for the degree of Bachelor of Manufacturing Engineering (Engineering Material). The member of the supervisory committee is as follow:

……… (Official Stamp of Principal Supervisor)


(5)

i

ABSTRAK

Termoplastik elastomer semakin mendapat perhatian kerana ciri-cirinya yang menyerupai getah tervulkan dan mudah difabikat seperti termoplastik. Kajian ini merupakan satu usaha untuk meneroka potensi polipropilena (PP) apabila digabungkan dengan getah asli terepoksida ENR. Polipropilena (PP) dan getah asli terepoksida(ENR) disediakan melalui kaedah penyebatian lebur menggunakan pencampur dalaman dan pematangan sulfur. Parameter pencampur seperti nisbah, suhu percampuran, masa percampuran dan kelajuan pemutar dioptimumkan dengan kaedah metodologi permukaan sambutan dengan bantuan perisian Expert 6.0.10. Suhu pencampuran dan terma interaksi telah dikenalpasti sebagai faktor tidak signifikan dengan nilai P lebih daripada 0.0500. Beberapa ujian dan analisis termasuk ujian ketumpatan, indeks kecairan aliran, ujian tegangan, ujian kekerasan, kemikroskopan elektron imbasan (SEM) dan pemeteran kalori pengimbasan kebezaan (DSC) dijalankan untuk mencirikan sifat-sifat PP/ENR. ENR berupaya meningkatkan keliatan dan kebolehlenturan polipropilena. Nilai kiraan optimum untuk pembolehubah yang dikaji (nisbah, suhu, kelajuan pemutar dan masa pencampuran) untuk memaksimumkan pemanjangan sebelum putus telah dikenalpasti sebagai ENR 16.33%, suhu 170oC, kelajuan pemutar 50rpm dan masa pencampuran 6 minit dengan pemanjangan yang dijangkakan sebelum terputus pada 11.7171%, berbanding 9% PP tulen.


(6)

ii

ABSTRACT

Thermoplastic elastomers have become important because they have combination properties of vulcanized rubbers and can be rapidly fabricated as thermoplastic. This research is an effort to explore the potential of polypropylene (PP) when incorporated with ENR. Polypropylene (PP) and epoxidized rubber (ENR) were prepared by melt blending with internal mixer and sulfur curing. Mixer parameter such as the ratio, mixing temperature, mixing time, and rotor speed were optimized with response surface methodology with the assistance of Design Expert 6.0.10

software. The mixing temperature and its interaction terms were identified as insignificant factors with a P value greater than 0.0500. Testing and analysis including density test, melt flow index (MFI), tensile test, hardness test, impact test, scanning electron microscopy (SEM) and differential scanning calorimetry (DSC) were performed to characterize the properties of PP/ENR. The ENR is proven to increase toughness and flexibility of polypropylene. The optimum calculated values of the tested variables (ratio, temperature, rotor speed and mixing time) for the maximum elongation to break was found to be at ENR of 16.33%, temperature of 170oC, rotor speed of 50 rpm and a mixing time of 6 min with a predicted elongation to break of 11.7171%, compared to 9% of pure PP.


(7)

iii

ACKNOWLEDGEMENT

I would like to offer my unreserved gratitude and praises to Almighty Allah for His generous blessing and the undying strength bestowed upon me during the course of this research.

Special thanks to my supervisor, Dr. Noraiham Mohamad who guide, assist and advice me all the way through this project.

Thanks to all my friends, who always give me the moral support and been there whenever I am in need.


(8)

iv

TABLE OF CONTENT

Abstrak i

Abstract ii

Acknowledgement iii

Table of Content iv

List of Tables viii

List of Figures xi

List of Abbreviations xiv

List of Symbols xv

1. INTRODUCTION 1

1.1 Background 1

1.2 Problem Statement 2

1.3 Objective 3

1.4 Scope 3

1.5 Chapter Overview 3

2. LITERATURE REVIEW 5

2.1 Polymer Blends 5

2.1.1 Thermoset Elastomer (TSE) 7

2.1.2 Thermoplastic Elastomer (TPE) 8

2.1.2.1 Thermoplastic 9

2.1.2.2 Elastomer 10 2.1.2.3 Current Development of Thermoplastic Elastomer 12

2.2 Compounding Process 14

2.2.1 Melt Blending 15

2.2.1.1 Internal Mixer 15

2.2.1.2 Twin-Screw Extruder 16

2.2.1.3 Two Roll Mill 17


(9)

v

2.2.2 Compressing Molding 19

2.3 Vulcanization/Curing Process 20

2.3.1 Sulfur Vulcanization 20

2.3.2 Peroxide Vulcanization 23

2.3.3 Mixed Vulcanization 24

2.4 Fabrication 24

2.4.1 Hot Press 24

2.4.2 Cold Press 25

2.4.3 Isostatic Press 25

2.5 Testing and Analysis 26

2.5.1 Physical Test 26

2.5.1.1 Density Test 26

2.5.1.2 Melt Flow Index (MFI) 26

2.5.2 Mechanical Test 27

2.5.2.1 Tensile Test 27

2.5.2.2 Izod Impact Test 28

2.5.2.3 Hardness Test 29

2.5.3 Morphological Study 31

2.5.3.1 Scanning Electron Microscopy (SEM) 31

2.5.4 Thermal Analysis 32

2.5.4.1 Differential Scanning Calorimetry 32

2.6 Optimization 32

2.6.1 Response Surface Methodology (SEM) 33

3. METHODOLOGY 38

3.1 Introduction 38

3.2 Raw Material 40

3.3 Characterization of Raw Material 40

3.3.1 Polypropylene 40

3.3.2 Epoxidized Natural Rubber 41


(10)

vi

3.4 Optimization of Internal Mixer Parameter using Response Surface

Methodology (RSM) 44

3.4.1 Design of Experiment 44

3.4.1.1 Screening Factor 44

3.5 Blending of PP/ENR Blends in Internal Mixer 46

3.6 Pelletizing 48

3.7 Hot Pressing 50

3.8 Testing and Analysis 52

3.8.1 Physical Test 52

3.8.1.1 Density Test 52

3.8.1.2 Melt Flow Index (MFI) 53

3.8.2 Mechanical Test 55

3.8.2.1 Tensile Test 55

3.8.2.2 Hardness Test 56

3.8.2.3 Izod Impact Test 58

3.8.3 Morphological Study 59

3.8.3.1 Scanning Electron Microscopy (SEM) 59

3.8.4 Thermal Analysis 60

3.8.4.1 Differential Scanning Calorimetry (DSC) 60

4. RESULT AND DISCUSSION 61

4.1 Introduction 61

4.2 Raw Material Characterization 62

4.2.1 Density 62

4.2.2 Melt Flow Index 62

4.3 Optimization of Physical and Mechanical Properties 63

4.3.1 Density Analysis 63

4.3.2 Hardness 70

4.3.3 Melt Flow Index 76

4.3.4 Impact Strength 82

4.3.5 Tensile Properties 89

4.3.5.1 Tensile Strength 90


(11)

vii

4.3.5.3 Young Modulus 101

4.4 Analysis 107

4.4.1 Scanning Electron Microscopy (SEM) 107

4.4.2 Differential Scanning Calorimetry (DSC) 110

4.5 Determination of the optimum formulation of PP/ENR using the Response Surface Methodology (RSM) 111

5. CONCLUSION AND RECOMMENDATION 114

5.1 Conclusion 114

5.2 Recommendation 115

REFERENCES 116 APPENDIX


(12)

viii

LIST OF TABLES

Table 2.1: Basic recipe for the sulfur vulcanization system 21

Table 2.2: Sulfur vulcanization system 23

Table 2.3: Compounding formulation for ENR 23 Table 2.4: 23 Factorial Design Matrix Used for the Screening Factors 35

Table 2.5: Levels of Variables Chosen for Trial 36

Table 2.6: Full Factorial Central Composite Design for the Optimization

of Machine Parameters in the ENRAN Composite Preparation 36 Table 2.7: Levels of Variables Chosen for Trial in the

Optimization Experiments 36

Table 3.1 General properties of polypropylene 40

Table 3.2 Thermal properties of polypropylene 41

Table 3.3: Properties of sulfur 43

Table 3.4: Properties of zinc oxide 43

Table 3.5: Properties of stearic acid 44

Table 3.6: Combination of parameters internal mixer machine for 24 factorial

designs for screening factor 45

Table 3.7: Level of variables for the screening factor 45

Table 3.8: Composition of ENR vulcanization 46

Table 3.9: Design matrix of process parameter PP/ENR blends 47

Table 3.10: Level of variables 48

Table 3.11: The standard test conditions sample weight and

testing time for materials. 55

Table 4.1: Density Average of PP and ENR 62

Table 4.2: Melt Flow Rate of PP and ENR 63 Table 4.3: Density Average with Mixing Parameters and Ratios 64 Table 4.4: ANOVA for the Selected Factorial Models 66 Table 4.5: Observed Responses and Predicted Values 67 Table 4.6: Regression Coefficients and P Values as


(13)

ix

Calculated from the Models 68

Table 4.7: Hardness with Mixing Parameters and Ratios 70 Table 4.8: ANOVA for the Selected Factorial Models 72 Table 4.9: Observed Responses and Predicted Values 73 Table 4.10: Regression Coefficients and P Values as

Calculated from the Models 74

Table 4.11: Melt flow rate with Mixing Parameters and Ratios 77 Table 4.12: ANOVA for the Selected Factorial Models 79 Table 4.13: Observed Responses and Predicted Values 80 Table 4.14: Regression Coefficients and P Values as

Calculated from the Models 80

Table 4.15: Impact strength with Mixing Parameters and Ratios 83 Table 4.16: ANOVA for the Selected Factorial Models 85 Table 4.17: Observed Responses and Predicted Values 86 Table 4.18: Regression Coefficients and P Values as

Calculated from the Models 87

Table 4.19: Tensile strength with Mixing Parameters and Ratios 90 Table 4.20: ANOVA for the Selected Factorial Models 91 Table 4.21: Observed Responses and Predicted Values 92 Table 4.22: Regression Coefficients and P Values as

Calculated from the Models 92

Table 4.23: Elongation to break with Mixing Parameters and Ratios 96 Table 4.24: ANOVA for the Selected Factorial Models 98 Table 4.25: Observed Responses and Predicted Values 99 Table 4.26: Regression Coefficients and P Values as

Calculated from the Models 99

Table 4.27: Young Modulus with Mixing Parameters and Ratios 102 Table 4.28: ANOVA for the Selected Factorial Models 104 Table 4.29: Observed Responses and Predicted Values 105 Table 4.30: Regression Coefficients and P Values as

Calculated from the Models 105

Table 4.31: Glass Transition Temperature of samples 110 Table 4.32: Properties and characteristics processing of the need for


(14)

x

optimizing the formulation PP/ENR 111 Table 4.33: Optimum formulation with the processing characteristics and

properties generated for PP / ENR based on the degree of


(15)

xi

LIST OF FIGURES

Figure 2.1: Structure of Polypropylene 10

Figure 2.2: Structure of cis-Polyisoprene 11

Figure 2.3: Structure of Epoxidized Natural Rubber (ENR) 12 Figure 2.4: Schematic representation of the two-roll milling method 18 Figure 2.5: Schematic representation of the compressing molding 19 Figure 2.6: Schematic illustration of injection molding 20 Figure 2.7: The mechanism of peroxide vulcanization 24

Figure 2.8: Cold Compression Molding 25

Figure 2.9: Schematic illustration of how a tensile load produces an elongation

and positive linear strain 28

Figure 2.10: SEM micrographs of dynamically cured 60/40 ENR-30/PP

TPVs with sulphur system 31

Figure 3.1: Flow chart of the research project 39

Figure 3.2: Polypropylene 41

Figure 3.3: Epoxidized Natural Rubber 42

Figure 3.4: Stearic Acid (a), Zinc Oxide (b) and Sulfur (c) 43 Figure 3.5: ENR vulcanization; scale: 20cent Malaysia Diameter 23mm 46 Figure 3.6: HAAKE RHEOMIX OS internal mixer machine 48

Figure 3.7: PP/ENR using crusher machine 49

Figure 3.8: Crusher machine 49

Figure 3.9: Pellet compound is placed in the mold. 50 Figure 3.10: Gotech (GT 7014 – A) hot press machine 51 Figure 3.11: Gotech (GT 7016 –H) Specimen cutter machine 51

Figure 3.12: Electronic densimeter. 53

Figure 3.13: Melt Flow Indexer MH-525 equipment 54

Figure 3.14: Autograph AG-IC floor universal testing machine. 56 Figure 3.15: Dog bone type specimen size for ASTM D-638 Type 1 56

Figure 3.16: Shore D Durometer 57


(16)

xii

Figure 3.18: Zeiss EVO-50 ESEM machine 59

Figure 3.19: DSC Perkin Elmer DSC-7 60

Figure 4.1: Half Normal Plot for Density 65

Figure 4.2: Effects of the ENR and temperature on the density

of the PP/ENR blend 68

Figure 4.3: Density of all samples 69

Figure 4.4: Half Normal Plot for Hardness 71

Figure 4.5: Effects of the ENR and temperature on the hardness

of the PP/ENR blend 74

Figure 4.6: Hardness of all samples 75

Figure 4.7: Half Normal Plot for Melt Flow Rate 78

Figure 4.8: Effects of the ENR and temperature on the melt flow rate

of the PP/ENR blend 81

Figure 4.9: Melt flow rate of all samples 82

Figure 4.10: Half Normal Plot for Impact Strength 84 Figure 4.11: Effects of the ENR and temperature on the impact strength

of the PP/ENR blend 87

Figure 4.12: Impact strength of all samples 88

Figure 4.13: (a) Dogbone for PP, (b) Dogbone for PP/ENR 70/30 and

(c) PP/ENR 40/60 89

Figure 4.14: Half Normal Plot for Tensile Strength 91 Figure 4.15: Effects of the ENR and temperature on the tensile strength

of the PP/ENR blend 94

Figure 4.16: Tensile strength of all samples 94

Figure 4.17: Half Normal Plot for Elongation to Break 97 Figure 4.18: Effects of the ENR and temperature on the elongation to break

of the PP/ENR blend 100

Figure 4.19: Elongation to break of all samples 100 Figure 4.20: Half Normal Plot for Hardness 103 Figure 4.21: Effects of the ENR and temperature on the Young modulus


(17)

xiii

Figure 4.22: Young modulus of all samples 106 Figure 4.23: (a) Scanning electron micrograph of unfilled PP at magnification

of 500x. (b) Scanning electron micrograph of PP/ENR 70/30 at magnification of 500x. (c) Scanning electron micrograph

of PP/ENR 40/60 at magnification of 500x. 108 Figure 4.24: (a) Scanning electron micrograph of unfilled PP at magnification

of 5000x. (b) Scanning electron micrograph of PP/ENR 70/30 at magnification of 5000x. (c) Scanning electron micrograph

of PP/ENR 40/60 at magnification of 5000x. 109 Figure 4.25: Fractional degrees of desire fulfilled the selection formula


(18)

xiv

LIST OF ABBREVIATIONS

ASTM - American Standard Test Method ENR - epoxidized natural rubber

TPNR - thermoplastic natural rubber

NR - natural rubber

NBR - nitrile butadiene rubber

PP - polypropylene

RSM - response surface methodology SEM - scanning electron microscopy DSC - differential scanning calorimetry FTIR - fourier transform infrared

EPR - ethylene propylene rubber TPO - thermoplastic polyolefin TPV - thermoplastic vulcanizate TPE - thermoplastic elastomer TSE - thermoset elastomer IR - synthetic isoprene rubber

BR - polybutadiene rubber

SBR - styrene butadiene rubber

IIR - butyl rubber

CIIR - chloro butyl rubber BIIR - bromo butyl rubber DOE - design of experimental rpm - rotation per minute


(19)

xv

LIST OF SYMBOLS

oC - Celsius

M/S - meter per second

% - percentage

kW - kilo watt

min - minute

kg - kilogram

mm - millimeter

μm - micrometer

s - second

nm - nanometer

g - gram


(20)

1

1.1 Background

Polyolefins are the largest group of thermoplastics, the two most important and common types of polyolefins are polyethylene and polypropylene. They are very popular due to their low cost and wide range of applications. Polyolefins are usually processed by extrusion, injection molding, blow molding, and rotational molding methods.

Polyolefin elastomers (POEs) are a relatively new class of polymers that emerged with recent advances in metallocene polymerisation catalysts. Representing one of the fastest growing synthetic polymers, POE’s can be substituted for a number of generic polymers including ethylene propylene rubbers (EPR or EPDM), ethylene vinyl acetate (EVA), styrene-block copolymers (SBCs), and poly vinyl chloride (PVC). Polyolefin elastomers are compatible with most olefinic materials, are an excellent impact modifier for plastics, and offer unique performance capabilities for compounded products.

Thermoplastic elastomers based on natural rubber and thermoplastic blends are classified as thermoplastic natural rubber (TPNR) blends. There are two types of thermoplastic natural rubber. Blending of NR with thermoplastic (i.e., polyolefins) to get co-continuous phase morphology is technologically classified as thermoplastic polyolefin (TPO). The other class is known as thermoplastic vulcanizate (TPV), which is prepared by blending NR with polyolefins and involve vulcanization process. In type two, the rubber phase is vulcanized during the mixing process at

INTRODUCTION

CHAPTER 1


(21)

2

high temperature, and the process is known as dynamic vulcanization. Dynamic vulcanization of epoxidized natural rubber (ENR) and polypropylene (PP) are also performed by using either a sulfur based system or peroxide. The sulfur cured system showed superior mechanical properties in term of tensile strength, elongation at break and tension set compared to the peroxide system due to the polypropylene degradation during dynamic vulcanization.

1.2 Problem Statement

Polypropylene (PP) is well-known of its outstanding dielectric properties under high voltage and high frequency condition up to 30 kHz (Khachen et al., 1992). Due to that, it is a suitable material for electrical insulator whether in interior or exterior cables. However, PP is less flexible when the thickness of the cable is increases. The epoxidized natural rubber (ENR) is a potential candidate to increase the flexibility of polypropylene. Malaysia is known as the world’s major natural rubber producer. ENR being a derivative of natural rubber is more readily available, and it has unique properties offering high strength due to their ability to undergo strain crystallization, along with increased glass transition temperatures and solubility parameter. These properties are reflected in vulcanizates with increased oil resistance, enhanced adhesive properties, high degree of damping and reduce gas permeation (Gelling, 1991). Response surface methodology (RSM) is reported to be an effective tool for optimizing a process, as highlighted by various workers (Yadav et al., 2007). RSM could save cost and time by reducing number of experiments required. The application of RSM to design optimization is aimed at reducing the cost of expensive analysis methods and their associated numerical noise. Originally, RSM was developed to model experimental responses (Box and Draper, 1987), and then migrated into the modeling of numerical experiments.


(22)

3

1.3 Objective

The main objectives on this research are:

i. To produce PP/ENR blend via melt blending using internal mixer.

ii. To determine the optimum formula and mixer parameter using response surface methodology

iii. To characterize the properties of PP/ENR blend through testing and analysis.

1.4 Scope

This research is focusing on optimization of formulation and mixer parameter to produce PP/ENR blend. Firstly, the experiment was designed using RSM. Then, samples were prepared in different combination of process parameters in an internal mixer followed by various physical and mechanical testing. Some analysis such as thermal and morphology were performed to support the data.

1.5 Chapter Overview

There are five chapters in this report;

i. Chapter 1 is the introduction of the research. That consists of research background, a problem statement, and objectives of the project, scope and chapter overview.

ii. Chapter 2 is the literature review and covers the fundamental of polymer blends, thermoplastic elastomer and also a general overview of the current development of polymer blends.


(23)

4

iii. Chapter 3 is the methodology of this research, response surface methodology and it discuss the raw material specification, equipment and experimental procedures used in this study.

iv. Chapter 4 is the results and discussions of laboratory and field research work described in this study.

v. Chapter 5 is formulate procurement review and list of potential research and also proposed future work.


(24)

5

2.1 Polymer Blends

Basic principles of polymer blends are either homogeneous or heterogeneous (He et al., 2004). In homogeneous blends, the final properties are often an arithmetic average of the properties of the blend components. In heterogeneous blends, the properties of all blend components are present. A deficiency in the properties of one component can be camouflaged to a certain extent by strengths of the others (He et al., 2004). Polymer blending is a convenient route for the development of new polymeric materials, able to yield materials with property profiles superior to those of the individual components (He et al., 2004). Blending of polymers is an effective way to obtain materials with specific properties. Most polymers are immiscible, therefore, blending usually leads to heterogeneous morphologies (Willemse et al., 1997). Most polymer pairs are immiscible, and therefore, their blends are not formed spontaneously. Moreover, the phase structure of polymer blends is not equilibrium and depends on the process of their preparation. Five different methods are used for the preparation of polymer blends are melt mixing, solution blending, latex mixing, partial block or graft copolymerization, and preparation of interpenetrating polymer networks (Anonymous, 2005).

Polymer blend constitute of 36 wt% of the total polymer consumption, and their pertinence continues to increase (Utracki, 2002). About 65% of polymer alloy and blend are produced by polymer manufacturer, 25% by compounding companies and the remaining 10% by the transformer (Utracki, 2002).

LITERATURE REVIEW

CHAPTER 2


(1)

xv

LIST OF SYMBOLS

oC - Celsius

M/S - meter per second

% - percentage

kW - kilo watt

min - minute

kg - kilogram

mm - millimeter

μm - micrometer

s - second

nm - nanometer

g - gram


(2)

1

1.1 Background

Polyolefins are the largest group of thermoplastics, the two most important and common types of polyolefins are polyethylene and polypropylene. They are very popular due to their low cost and wide range of applications. Polyolefins are usually processed by extrusion, injection molding, blow molding, and rotational molding methods.

Polyolefin elastomers (POEs) are a relatively new class of polymers that emerged with recent advances in metallocene polymerisation catalysts. Representing one of the fastest growing synthetic polymers, POE’s can be substituted for a number of generic polymers including ethylene propylene rubbers (EPR or EPDM), ethylene vinyl acetate (EVA), styrene-block copolymers (SBCs), and poly vinyl chloride (PVC). Polyolefin elastomers are compatible with most olefinic materials, are an excellent impact modifier for plastics, and offer unique performance capabilities for compounded products.

Thermoplastic elastomers based on natural rubber and thermoplastic blends are classified as thermoplastic natural rubber (TPNR) blends. There are two types of thermoplastic natural rubber. Blending of NR with thermoplastic (i.e., polyolefins) to get co-continuous phase morphology is technologically classified as thermoplastic polyolefin (TPO). The other class is known as thermoplastic vulcanizate (TPV), which is prepared by blending NR with polyolefins and involve vulcanization process. In type two, the rubber phase is vulcanized during the mixing process at

INTRODUCTION

CHAPTER 1


(3)

2

high temperature, and the process is known as dynamic vulcanization. Dynamic vulcanization of epoxidized natural rubber (ENR) and polypropylene (PP) are also performed by using either a sulfur based system or peroxide. The sulfur cured system showed superior mechanical properties in term of tensile strength, elongation at break and tension set compared to the peroxide system due to the polypropylene degradation during dynamic vulcanization.

1.2 Problem Statement

Polypropylene (PP) is well-known of its outstanding dielectric properties under high voltage and high frequency condition up to 30 kHz (Khachen et al., 1992). Due to that, it is a suitable material for electrical insulator whether in interior or exterior cables. However, PP is less flexible when the thickness of the cable is increases. The epoxidized natural rubber (ENR) is a potential candidate to increase the flexibility of polypropylene. Malaysia is known as the world’s major natural rubber producer. ENR being a derivative of natural rubber is more readily available, and it has unique properties offering high strength due to their ability to undergo strain crystallization, along with increased glass transition temperatures and solubility parameter. These properties are reflected in vulcanizates with increased oil resistance, enhanced adhesive properties, high degree of damping and reduce gas permeation (Gelling, 1991). Response surface methodology (RSM) is reported to be an effective tool for optimizing a process, as highlighted by various workers (Yadav et al., 2007). RSM could save cost and time by reducing number of experiments required. The application of RSM to design optimization is aimed at reducing the cost of expensive analysis methods and their associated numerical noise. Originally, RSM was developed to model experimental responses (Box and Draper, 1987), and then migrated into the modeling of numerical experiments.


(4)

3

1.3 Objective

The main objectives on this research are:

i. To produce PP/ENR blend via melt blending using internal mixer.

ii. To determine the optimum formula and mixer parameter using response surface methodology

iii. To characterize the properties of PP/ENR blend through testing and analysis.

1.4 Scope

This research is focusing on optimization of formulation and mixer parameter to produce PP/ENR blend. Firstly, the experiment was designed using RSM. Then, samples were prepared in different combination of process parameters in an internal mixer followed by various physical and mechanical testing. Some analysis such as thermal and morphology were performed to support the data.

1.5 Chapter Overview

There are five chapters in this report;

i. Chapter 1 is the introduction of the research. That consists of research background, a problem statement, and objectives of the project, scope and chapter overview.

ii. Chapter 2 is the literature review and covers the fundamental of polymer blends, thermoplastic elastomer and also a general overview of the current development of polymer blends.


(5)

4

iii. Chapter 3 is the methodology of this research, response surface methodology and it discuss the raw material specification, equipment and experimental procedures used in this study.

iv. Chapter 4 is the results and discussions of laboratory and field research work described in this study.

v. Chapter 5 is formulate procurement review and list of potential research and also proposed future work.


(6)

5

2.1 Polymer Blends

Basic principles of polymer blends are either homogeneous or heterogeneous (He et al., 2004). In homogeneous blends, the final properties are often an arithmetic average of the properties of the blend components. In heterogeneous blends, the properties of all blend components are present. A deficiency in the properties of one component can be camouflaged to a certain extent by strengths of the others (He et al., 2004). Polymer blending is a convenient route for the development of new polymeric materials, able to yield materials with property profiles superior to those of the individual components (He et al., 2004). Blending of polymers is an effective way to obtain materials with specific properties. Most polymers are immiscible, therefore, blending usually leads to heterogeneous morphologies (Willemse et al., 1997). Most polymer pairs are immiscible, and therefore, their blends are not formed spontaneously. Moreover, the phase structure of polymer blends is not equilibrium and depends on the process of their preparation. Five different methods are used for the preparation of polymer blends are melt mixing, solution blending, latex mixing, partial block or graft copolymerization, and preparation of interpenetrating polymer networks (Anonymous, 2005).

Polymer blend constitute of 36 wt% of the total polymer consumption, and their pertinence continues to increase (Utracki, 2002). About 65% of polymer alloy and blend are produced by polymer manufacturer, 25% by compounding companies and the remaining 10% by the transformer (Utracki, 2002).

LITERATURE REVIEW

CHAPTER 2