UNIVERSITI PUTRA MALAYSIA PREPARATION AND CHARACTERIZATION OF POLY(BUTYLENE ADIPATE-CO-TEREPHTALATE) /OIL PALM EMPTY FRUIT BUNCH FIBER BIOCOMPOSITES

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1 UNIVERSITI PUTRA MALAYSIA PREPARATION AND CHARACTERIZATION OF POLY(BUTYLENE ADIPATE-CO-TEREPHTALATE) /OIL PALM EMPTY FRUIT BUNCH FIBER BIOCOMPOSITES SAMIRA SIYAMAK FS

2 PREPARATION AND CHARACTERIZATION OF POLY(BUTYLENE ADIPATE-CO-TEREPHTALATE) /OIL PALM EMPTY FRUIT BUNCH FIBER BIOCOMPOSITES By SAMIRA SIYAMAK Thesis Submitted to the School of Graduate Studies, Universiti Putra Malaysia, in Fulfilment of the Requirements for the Degree of Master of Science February 2011 i

3 Abstract of thesis presented to the Senate of Universiti Putra Malaysia in fulfilment of the requirements for the degree of Master of Science PREPARATION AND CHARACTERIZATION OF POLY(BUTYLENE ADIPATE-CO-TEREPHTALATE)/OIL PALM EMPTY FRUIT BUNCH FIBER BIOCOMPOSITES Chair: Faculty: Science Nor Azowa Ibrahim, PhD By SAMIRA SIYAMAK February 2011 During the last years, the interest in renewable and biodegradable materials has tremendously increased in the global community. The global market for renewable and biodegradable materials increases immensely due to societal awareness of the climate situation and the problems arise from thermoplastics. In this research, the oil palm empty fruit bunch (EFB) fiber was used as an interesting source of lignocellulosic filler for preparation of the cost effective and biodegradable composites. The aliphatic aromatic co-polyester poly(butylene adipate-co-terephthalate) PBAT (Ecoflex TM ), a fully biodegradable thermoplastic polymer was used as matrix. The aim of this research is to fabricate a new class of biocomposite based on PBAT/EFB fiber and to improve the new biocomposites performance by chemical modification using succinic anhydride (SAH) as coupling agent in presence and absence of dicumyl peroxide (DCP) and benzoyl peroxide (BPO) as initiator. For the composite preparation, several blends were prepared ii

4 at different contents of filler and matrix using melt blending technique. The specimens for mechanical tests were prepared based on ASTM standards. The effects of fiber loading and coupling agent loading on thermal properties of biodegradable polymer composites were evaluated using thermal gravimetric analysis (TGA) and dynamic mechanical analysis (DMA). TGA was used to evaluate composite decomposition and stability whilst DMA was utilized to evaluate parameters such as the glass transition temperature, T g, storage modulus, E'and loss modulus, E". Scanning Electron Microscopy (SEM) was used for morphological studies. The chemical structure of new biocomposite was also analyzed using Fourier Transform Infrared (FTIR) Spectroscopy technique. The water absorption test was used for composite moisture absorption determination and the burial test was used to biodegradation studies. The PBAT biocomposite reinforced with 40 (wt%) of EFB fiber showed the best mechanical properties compared to the other PBAT/EFB fiber biocomposites. Biocomposites treatment with 4 (wt%) of succinic anhydride (SAH) and 1 (wt%) of DCP improved both tensile and flexural strength as well as tensile and flexural modulus, whereas the biocomposites impact strength improvement was only marginal. The FTIR analyses proved the mechanical test results by presenting the evidences of successful esterification using SAH/DCP in biocomposites spectra. The SEM micrograph of the tensile fractured surfaces showed the improvement of fiber-matrix adhesion after using SAH. The TGA results showed that chemical modification using SAH/DCP improved the thermal stability of PBAT/EFB biocomposite. The DMA results showed the improvements of storage modulus as well as loss modulus and T g of new composite modified by SAH. The water absorption test results indicated a decrease in moisture iii

5 absorption trend of new biocomposite affected by (SAH) coupling agent compared to the untreated biocomposite. The biodegradation test observations showed a moderate increase in biological resistance of the modified biocomposites compare to the unmodified one. iv

6 Abstrak tesis yang dikemukakan kepada Senat Universiti Putra Malaysia sebagai memenuhi keperluan untuk ijazah Master Sains PEMBUATAN DAN KARAKTERISASI POLI(BUTILENA ADIPAT- KOTEREFTALAT)/ MINYAKSAWIT BIOKOMPOSIT IKATAN BUAH SERAT KOSONG Pengerusi: Nor Azowa Ibrahim, PhD Fakulti: Sains Oleh SAMIRA SIYAMAK Februari 2011 Selama tahun terakhir, bunga di bahan terbarukan dan ramah lingkungan telah sangat meningkat dalam komuniti global. Pasar global untuk bahan terbarukan dan ramah lingkungan sangat meningkat kerana kesedaran masyarakat tentang situasi iklim dan masalah-masalah yang timbul dari termoplastik. Dalam kajian ini, kelapa sawit tandan buah kosong (TKS) serat digunakan sebagai sumber lignoselulosa menarik filler penyusunan kos komposit berkesan dan biodegradable. The alifatik aromatik copoliester (polibutylene adipat-co-terephthalate) PBAT (EcoflexTM), sebuah polimer termoplastik biodegradable sepenuhnya digunakan sebagai matriks. Tujuan dari penelitian ini adalah untuk membuat kelas baru biokomposit berdasarkan PBAT / serat TKS dan untuk meningkatkan prestasi biokomposit baru 'dengan pengubahsuaian kimia menggunakan esternya suksinat (SAH) sebagai agen kopling dalam keberadaan dan ketiadaan dicumyl peroksida (DCP) dan benzoil. peroksida (BPO) sebagai inisiator. Untuk penyusunan komposit, beberapa campuran kandungan yang berbeza v

7 disiapkan di filler dan matriks menggunakan teknik pencampuran mencair. Spesimen untuk uji mekanikal disusun berdasarkan standard ASTM. Kesan daripada serat dan loading loading kopling agen terhadap sifat terma komposit polimer biodegradable dievaluasi menggunakan analisis gravimetri termo (TGA) dan analisis mekanik dinamik (DMA). TGA digunakan untuk menilai dekomposisi komposit dan kestabilan sementara DMA ini digunakan untuk menilai parameter seperti suhu peralihan kaca, T, simpanan modulus, modulus E'dan rugi, E" Scanning Elektron. Microscopy (SEM) digunakan untuk kajian morfologi. Thestruktur kimia biokomposit baru ini juga dianalisis menggunakan Fourier Transform Infrared (FTIR) Spektroskopi teknik. Ujian penyerapan air digunakan untuk penyerapan kelembapan penentuan komposit dan uji pengebumian itu digunakan untuk kajian biodegradasi. The biokomposit PBAT diperkuatkan dengan 40 (% wt) serat TKS menunjukkan sifat mekanik terbaik berbanding / lain PBAT biokomposit serat TKS. perubatan biokomposit dengan 4 (% wt) dari esternya suksinat (SAH) dan 1 (% wt) dari DCP ditingkatkan baik kekuatan tarik dan lentur serta modulus tarik dan lentur, sedangkan kesan peningkatan kekuatan biokomposit 'hanya marjinal. Analisis FTIR membuktikan keputusan ujian mekanik dengan menunjukkan bukti-bukti sukses pengesteran menggunakan SAH / DCP pada spektrum biokomposit. The mikrograf SEM dari paras patah tarik menunjukkan peningkatan adhesi serat-matriks selepas menggunakan SAH. TGA Keputusan kajian menunjukkan bahawa pengubahsuaian kimia menggunakan SAH / DCP meningkatkan kestabilan terma PBAT / biokomposit TKS.Keputusan DMA menunjukkan perbaikan modulus simpanan serta modulus kehilangan dan Tg komposit baru diubahsuai oleh SAH. Keputusan uji penyerapan air menunjukkan trend penurunan vi

8 penyerapan kelembapan biokomposit baru dipengaruhi oleh (SAH) coupling agent dibandingkan dengan biokomposit tidak dirawat. Pemerhatian uji biodegradasi menunjukkan peningkatan sederhana dalam perlawanan biologi dari biokomposit buat kali terakhir berbanding dengan yang tidak diubahsuai pertama. vii

9 ACKNOLEDGEMENTS I would like to take this opportunity o express my utmost gratitude to the chairman of my supervisory committee Dr. Nor Azowa Ibrahim, for her invaluable guidance and advices through this research. Sincere thanks are due to Prof. Dato' Dr. Wan Md Zin Wan Yunus and Assoc. Prof. Dr. Mohamad Zaki Ab Rahman for their kind support and valuable guidance. Special thanks also to all the faculty staff members that have helped me throughout this period. It is a pleasure to acknowledge my brother Ali Siyamak for his kind support and encouragements. My sincerely appreciation also goes to my parents for their supports, understanding and sacrifices. Finally, I would like to dedicate this work to my beloved son, Mehryar, who is my every day s sun. viii

10 I certify that an Examination Committee has met on 23 February 2011 to conduct the final examination of Samira Siyamak on her Master of Science thesis entitled Preparation and characterization of Poly(Butylene Adipate-co-Terephthalate)/Oil Palm Empty Fruit Bunch Fiber Biocomposites, in accordance with Universiti Pertanian Malaysia (higher degree) act 1980 and Universiti Pertanian Malaysia (higher degree) Regulations The committee recommends that the student be awarded the relevant degree. Members of the examination committee were as follows: Prof. Madya Dr. Sidik Silong Faculty of Science Universiti Putra Malaysia (Chairman) Prof. Madya Dr. Mansor Ahmad Faculty of Science Universiti Putra Malaysia (Internal Examiner) Prof. Madya Dr. Abdul Halim Abdullah Faculty of Science Universiti Putra Malaysia (Internal Examiner) Prof. Madya Dr. Rusli Daik School of Chemical Science and Technology Faculty of Science and Technology Universiti Kebangsaan Malaysia UKM-Bangi Selangor (External Examiner) HASANAH MOHD.GHAZALI, PhD Professor and deputy dean School of graduate studies University Putra Malaysia Date: ix

11 This thesis was submitted to the senate of Universiti Putra Malaysia and has been accepted as fulfilment of the requirements for the degree of Master of Science. The members of the supervisory committee were as follows: Nor Azowa Ibrahim, PhD Senior Lecturer Faculty of Science Universiti Putra Malaysia (Chairman) Wan Md Zin Wan Yunus, PhD Professor Faculty of Science Universiti Putra Malaysia (Member) Mohamad Zaki AB Rahman, PhD Associate Professor Faculty of Science Universiti Putra Malaysia (Member) HASANAH MOHD. GHAZALI, PhD Professor and Dean School of Graduate Studies Universiti Putra Malaysia Date: x

12 DECLARATION I declare that the thesis is my original work except for quotations and citation, which have been duly, acknowledge. I also declare that it has not been previously, and is not currently, submitted for any other degree at universiti Putra Malaysia or at any other institution. SAMIRA SIYAMAK Date: 23 February 2011 xi

13 TABLE OF CONTENTS Page ABSTRACT ABSTRAK ACKNOWLEDGEMENTS APPROVAL DECLARATION TABLE OF CONTENTS LIST OF TABLES LIST OF FIGURES LIST OF SCHEMES LIST OF ABBREVIATIONS CHAPTER ii v viii ix xi xii xv xvii xxi xxii 1 INTRODUCTION Back Ground of Study Biodegradable Synthetic Thermoplastic Polymer (PBAT) Natural Fiber (Oil Palm Empty Fruit Bunch Fiber) Significance of Study Objectives of Research 8 2 LITERATURE REVIEW 2.1 Natural Fibers Natural Fiber: Source and Classification Oil Palm Empty Fruit Bunch Fiber (EFB) Issues Regarding the Use of Natural Fiber in Composites Biodegradable Polymers Biodegradable Thermoplastics: Source and Classification Poly Butylene Adipate-co-Terephthalate (PBAT) Natural Fiber/Biodegradable Thermoplastic Composites (Green Composites) Oil Palm EFB Fiber Filled Bio Thermoplastic Composite PBAT/Natural Fiber Reinforced Composite Methods to Improve the Properties of Biocomposites Coupling Agents: Classification and Actions Modification of Natural Fiber and Biopolymer Mechanical Properties of Green Composite Thermal Properties of Green Composites Biodegradation of Green Composites 51 3 MATERIALS AND METHODOLOGY Materials Methods Preparation of Oil Palm Empty Fruit Bunch Fiber 56 xii

14 3.2.2 Preparation of New Biodegradable Composites Fourier Transform Infrared Spectroscopy (FTIR) Mechanical Properties of Biodegradable Composites Tensile Test Flexural Test Impact Test Thermal Analysis of Biodegradable Composites Thermal Gravimetric Analysis (TGA) Dynamic Mechanical Analysis (DMA) Surface Morphology Study Water Absorption Study Biodegradation Study 68 4 RESULTS AND DISCUSSIONS Effects of Fiber Loading on Mechanical Properties of PBAT/EFB Composites Tensile Properties Flexural Properties Impact Properties Effects of Fiber Modification on Mechanical Properties of PBAT/EFB Fiber Composites Effect of Fiber Modification Using SAH and Initiator on Tensile Properties of PBAT/EFB Biocomposites Effect of Fiber Modification Using SAH and Initiator on Flexural Properties of PBAT/EFB Biocomposites Effect of Fiber Modification Using SAH and Initiator on Impact Properties of PBAT/EFB Biocomposites Effects of Matrix Modification Using SAH and Initiator on Tensile Properties of PBAT/EFB Biocomposites Effect of Matrix Modification Using SAH and Initiator on Flexural Properties of PBAT/EFB Biocomposites Effect of Matrix Modification Using SAH and Initiator on Impact Properties of PBAT/EFB Biocomposites FTIR Analysis Thermal Analysis of PBAT/EFB Fiber Biocomposites Thermal Gravimetric Analysis (TGA) Dynamic Mechanical Analysis (DMA) Morphological Study of PBAT/EFB Biocomposites SEM of PBAT/EFB Biocomposite at 40% Fiber Loading SEM of PBAT/EFB Biocomposite After Fiber Modification SEM of PBAT/EFB Biocomposite After Matrix Modification Water Absorption Study Effect of Fiber Loading on Water Absorption of PBAT/EFB Fiber Composite Effect of Chemical Threatment on Water Absorption of PBAT/EFB Fiber Composite Biodegradation Study 148 xiii

4.7.1 Effect of Fiber Loading on Biodegradation of PBAT and PBAT/EFB Fiber Composites 4.7.2 Effect of Chemical Treatments on Biodegradation of PBAT and BAT/EFB Fiber Composites 5 CONCLUSIONS AND RECOMMENDATIONS 155 5.

15 4.7.1 Effect of Fiber Loading on Biodegradation of PBAT and PBAT/EFB Fiber Composites Effect of Chemical Treatments on Biodegradation of PBAT and BAT/EFB Fiber Composites 5 CONCLUSIONS AND RECOMMENDATIONS Conclusions Recommendations 161 REFERENCES 163 BIODATA OF STUDENT xiv

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