Mechanical and Thermal Properties of Hybrid Coating

HPI-FAPS International Conference on Innovation in Polymer Science and Technology 2013 (IPST2013) Inna Garuda Hotel, Convention & Business Yogyakarta - Indonesia, October 7 - 10, 2013

Preface We are very pleased to present the Proceedings of The International Conference on Innovation in Polymer Science and Technology 2013 (IPST2013) held in Yogyakarta, Indonesia during October 7 until 10, 2013. This conference was organised by the Indonesian Polymer Association (HPI) under the auspices of Federation of Asian Polymer Societies (FAPS). The conference aimed to be a platform on academic exchange for polymer scientists and practitioners from all over the world through invited talks and distinguish lectures series. In total, we received 98 manuscripts and all of them have been reviewed by the reviewers. Those manuscripts are covering of 6 topics in polymer science & technology meeting: Nanostructure Polymers, Blends and Composites; Fiber and Fibrous Polymer Materials; Smart and Functionalized Polymers; Green, Sustainable and Bio-polymers; Advanced Synthesis Polymers. Among those manuscripts, it has been decided by the Chief of Editors to publish 14 papers in Polymer-Plastic Technology and Engineering 2015, Vol. 54, Issue 3 by Taylor & Francis and 34 papers in Macromolecular Symposia 2015 (Wiley). Other manuscripts published in the Proceeding of the Innovation of Polymer Science and Technology 2013 (31 papers) and in the Indonesian Polymer Journal (Majalah Polimer Indonesia) 2014, Vol. 17, No. 1 (5 papers) and No. 2 (2 papers). We are also honored as the selected conference papers will be published in the special issues of high impact factor international journals, i.e. Polymer Plastics-Technology and Engineering (Francis & Taylor) and Macromolecular Symposia (Wiley). This achievement is showing the level of the international conference in Indonesia, organised by the profesional associations, i.e. the Indonesian Polymer Association (HPI). Here, we are delighted to acknowledge for incredible support from the State Ministry of Research and Technology (Kemenristek), Indonesia; the Ministry of Industry (Kemenperin), Indonesia; Indones ian Institute of Sciences (LIPI); National Nuclear Energy Agency of Indonesia (BATAN); the Agency of the Assessment and Application of Technology (BPPT), Indonesia; University of Gadjah Mada (UGM), Indonesia; and special thanks to PT Lab Sistematika Indonesia as a major sponsor in this event, PT JJ Executive International and PT LMS Indonesia. We hope that the present proceedings provide the valuable information to the readers in the field of polymer science and technology.

Eniya Listiani Dewi Chair of IPST2013

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CONFERENCE ORGANISATION

Chair Co-chair Secretary

: Eniya Listiani Dewi : Edy Giri Rachman Putra : Rike Yudianti

Members Agus Haryono Anung Syampurwadi Arie Listyarini Arum Patriati Chandra Wahyu Purnomo Devi Dewi Kusuma Erizal Guntarti Supeni Himawan Tri Bayu Murti Indriyati Jarot Raharjo Joni Prasetyo Koentari Adi Soehardjo Kurniawan Lies A. Wisojodharmo

Lucia Indrarti Maria Christina P. Mirah Yuliali Mochamad Chalid Muhammad Ghozali Myrtha Karina Nendar Herdianto Nuri Astrini Oka Pradipta Sulistioso G. Sukaryo Tita Puspitasari Tjutjuk Ismujanto Wiwik Pujiastuti Yualina Riastuti Partiwi Yuyun Irmawati Zulaicha

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Editor in Chiefs Dr. Mochamad Chalid Department of Metallurgy Engineering University of Indonesia [email protected]

Dr. Agus Haryono Research Center for Chemistry Indonesian Institute of Sciences [email protected]

Guest Editors Prof. Atsushi Suzuki Yokohama National University, Japan [email protected]

Dr. Eniya Listiani Dewi Agency for the Assessment and Application of Technology, Indonesia [email protected]

Dr. Hermawan Judawisastra Institute of Technology Bandung, Indonesia [email protected]

Prof. I Made Arcana Institute of Technology Bandung, Indonesia [email protected]

Prof. John Forsythe Monash University, Australia [email protected]

Prof. Jun-ichi Azuma Kyoto University, Japan [email protected]

Prof. Kell Mortensen Copenhagen University, Denmark [email protected]

Prof. William H. Starnes Jr. College of William and Mary, Williamsburg, USA [email protected]

Dr. Myrtha Karina Indonesian Institute of Sciences, Indonesia [email protected]

Prof. Rochmadi University of Gadjah Mada, Indonesia [email protected]

Prof. Satyendra Mishra North Maharashtra University, Jalgaon, India [email protected]

Dr. Yenny Meliana Research Center for Chemistry Indonesian Institute of Sciences [email protected]

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Organising Committees of IPST2013

Andrew Whittaker, University of Queensland, Australia Antonius Augustinus Broekhuis, University of Groningen, Netherland Atsushi Suzuki, Yokohama National University, Japan Buvanesh Gupta, Indian Institute of Technology, India Der-Jang Liaw, National Taiwan University of Science and Technology, Taiwan Fosong Wang, Chinese Academy of Sciences, China Hamdani Saidi, Universiti Teknologi Malaysia, Malaysia Hirohisa Uchida, Tokai University, Japan Hiroyuki Nishide, Waseda University, Japan John Forsythe, Monash University, Australia Jung-Il Jin, Korea University, Korea Lars Berglund, Royal Institute of Technology (KTH), Sweden Mikihito Takenaka, Kyoto University, Japan Mohamed Mahmoud El-Sayed Nasef, Universiti Teknologi Malaysia, Malaysia Olgun Guven, Hacettepe University, Ankara, Turkey Shigeo Hirose, Fukui University of Technology, Japan Suharto Honggokusumo, Indonesian Rubber Council, Indonesia Suminar Setiati Achmadi, Bogor Institute of Agriculture, Indonesia Tadahisa Iwata, University of Tokyo, Japan Unggul Priyanto, Agency for the Assessment and Application of Technology, Indonesia Wan Ramli Wan Daud, UniversityiKebangsaan Malaysia, Malaysia William H. Starnes Jr., College of William and Mary, USA Steering Committee Achmad Zainal Abidin, Institute Technology of Bandung, Indonesia Adiarso, Agency of the Assessment and Application of Technology, Indonesia Andika Fajar, Ministry of Research and Technology, Indonesia Anhar Riza Antariksawan, National Nuclear Energy Agency, Indonesia Anny Sulaswati, Ministry of Research and Technology, Indonesia Bambang Widiyatmoko, Indonesian Institute of Sciences, Indonesia Cynthia L. Radiman, Institute Technology of Bandung, Indonesia Dadan Kusdiana, Ministry for Energy and Mineral Resources, Indonesia Edy Haryanto Majlan, University Kebangsaan Malaysia, Malaysia Gunawan, National Nuclear Energy Agency, Indonesia Linar Zalinar Udin, Indonesian Institute of Sciences, Indonesia Masbah R.T. Siregar, National Research Council, Indonesia Ngakan Timur Antara, Ministry of Industry, Indonesia Nursyamsu Bahar, Ministry of Industry, Indonesia Panut Mulyono, University of Gadjah Mada, Indonesia Rochmadi, University of Gadjah Mada, Indonesia Rochmi Widjajanti, Ministry of Industry, Indonesia Sudirman, Indonesian Polymer Association, Indonesia Sunit Hendrana, Indonesian Institute of Sciences, Indonesia Wawas Swathatafrijiah, Agency of the Assessment and Application of Technology, Indonesia Wieke Pratiwi, Ministry of Industry, Indonesia

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Table of Content

Preface

i

Editor in Chiefs and Guest Editors

Ii

Organising Committees of IPST2013

iv

Table of Content

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Invited Papers Structure Analyses of Poly(styrene-ran-butadiene) Rubber Crosslinked by Sulfur with Small-Angle Neutron Scattering M. Takenaka, S. Nishitsuji, N. Amino, Y. Ishikawa, D. Yamaguchi, S. Koizumi, T. Kanaya Radiation Processing of Polymers for Medical and Pharmaceutical Applications D. Darwis, Erizal, B. Abbas, F. Nurlidar, D. Pribadi Thermally Conductive Adhesive from Chemically Modified Cellulose and Nanoparticle of Surfactant-doped Polypyrrole S. F. S. Draman, R. Daik, S. M. El-Sheikh, F. A. Latif Novel Epoxy Resins with Unsaturated Ester Chains Derived from Sodium Lignosulfonate S. Hirose

1

2

3

4

Nanostructure Polymer and Composites Nanoparticles formation of Poly(Styrene Acrylate) Emulsion by Two-stage Polymerization Process M. A. E. Hafizah, A. Manaf Effect of Blending Process Condition on Morphology and Properties of Oil Palm Trunk based Wood Plastic Composite Bahruddin, R. Efrizal, Zulfansyah, S. P. Utami Effect of Grafting with Maleic Anhydride on Interfacial Bonding of Rubber Wood Flour Filled Polypropylene Composite A. Zulfia, R. S. Mohar, A. W. Saptoraharjo Therapeutic-Polymer-Cyclodextrin Composite Processing with Dense Gas Antisolvent Technology F. Kurniawansyah, R. Mammucari, N. R Foster Electrical and Thermal Conductivity of Graphite-CNT-Polymer Hybrid Composites S. Radhakrishnan, A. Khare, I. Zope

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5

11

17

18

25


Effect of Electron Beam Radiation on the Mechanical Properties of Low-Density Polyethylene (LDPE)/Waste Tire Dust (WTD) Blends C. T. Ratnam, S. A. Rashid, Z. Mohamed, S. Ramrad Combustion Resistance and Tensile Strength of Recycled Polypropylene Modificated Multifungtional Agent Composites with Kenaf Fiber and in the Presence of Kaolin and Zinc Borate N. S. Suharty, H. Ismail, K. Dihardjo, E. G. R. Putra, D. S. Handayani, A. D. K. Nagari Super Heat Resistant Conductive Nanocomposites Based on Polysulfone-Carbon Nanofillers L. Nayak, T. K. Chaki, D. Khastgir The Effect Surface Treatment PEG 4000 of Natural Silica to Changes Mechanical Properties of Natural Rubber/Bromobuthyl Vulcanizates M. Hamzah, M. Anggaravidya, Siswanto, Fausiah The Making of Train Brake Lining Block from Non-Asbestos Polymer Composite Using Sintering Method K. A. Soehardjo, A. Basuki, S. S. Rahardi Insertion of Platinum Particles in Bacterial Cellulose Membranes from PtCl4 and H2PtCl6 Precursors H. F. Aritonang, D. Onggo, Ciptati, C. L. Radiman The Effect of Recorcinol-Formaldehyde (RF) Loading as Coupling Agent on The Physical Properties and Curing Characteristics of Starch/Natural Rubber Composite Adi Cifriadi The Influence of Natural Rubber (NR) – Butadiene Rubber (BR) and Type of Carbon Black Particle as the Filler on the Mechanical Properties of Track L. A. Wisojodharmo, Indriasari, D. K. Arti The Manufacture and Mechanical Properties of 5 wt%. MWCNT/Epoxy Composites by Using 2Aminoethanol Functionalization and Thermal Pre-curing Treatment D. Abdullah, B. Yahya, H. Judawisastra, M. Siswosuwarno, M. Karina The Effect of Organoclay on Curing Characteristics, Mechanical Properties, Swelling and Morphology of Natural Rubber/Organoclay Nanocomposites M. I. Fathurrohman, B. Soegijono, E. Budianto, S. Rohman, A. Ramadhan Effect of Nanofiller on Properties of Poly Vinyl Chloride/Teak Sawdust Nanocomposites Dwiwahini Nurhajati, Dodi Irwanto, Emiliana Kasmudjiastuti The Effect of Coarse Particle Size on the Properties of Recycled Copper Filled Epoxy Composites M. N. F. Pargi, P. L. Teh, H. Salmah, C. K. Yeoh Effect of Different Blend Ratios and Compatibilizer on Tensile Properties of Recycled Polypropylene/Recycled High Density Polyethylene Blends A. A. S. Mariam Atiqah, H. Salmah, Z. Firuz, D. N. U. Lan Effect of Crosslink Agent on Tensile Properties of Chitosan/Corn Cob Biocomposite Films C. M. Yeng, H. Salmah, S. T. Sam Synthesis of MMA-TPE and Lead Tetroxide Composites as Material for X-Ray Radiation Shielding Door M. Anggaravidya, Sudirman, R. Rarista, E. Budianto, B. Soegijono

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33

34

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39

48

58

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Effects of Corn Husk and LLDPE Ratio on the Properties by Thermo-pressing M. Dirgantara, M. Kurniati Characteristics of Composites from Recycled Polypropelene and Three Kinds of Indonesian Bamboos Fiber K. W. Prasetiyo, L. Astari, M. Y. Massijaya Effect of Amide Functionalization and Precuring on Tensile Properties of MWCNT/Epoxy Nanocomposites H. Judawisastra, C. Harito, A. H. D. Abdullah Oxygen Barrier Properties of Al2O3 and TiO2 Coated LDPE Films S. Lange, T. Arroval, R. Saar, I. Kink, J. Aarik Synthesis of Gold Nanoparticles with Polyamidoamine (PAMAM) Generation 4 Dendrimer as A Stabilizing Agent for CT Scan Contrast Agent I. Sutriyo, A. Mutalib, E. Anwar, M. Radji, Zhuisa, P. Purnamasari, A. Pujiyanto Optimizing Delignification of Distilled Vetiver Root by Soda Pulping for Cellulose Extraction F. A. Syamani, Subyakto , Sukardi, A. Suryani Effect of Carbon Fiber Loading in Mechanical Properties and Electrical Conductivity of Polyvinyl Alcohol Based Composites Ismadi, A. H. Yuwono, S. Astutiningsih, Subyakto Effect of Ultrasonication Process from Unbleach Empty Fruit Bunches Pulp Reinforcing with Polyvinyl Alcohol W. B. Kusumaningrum, Ismadi, S. S. Munawar Mechanical Properties of Natural Rubber-Organo Layer Silicate Nanocomposite Jayatin, S. Rohman, M. Irfan Failure Analysis on POM Product Using Scanning Electron Microscope Microscope, Thermal and Processing Analysis R. Wijaya, A. Rifathin, B. Afrinaldi The Use of Activated Carbon of Palm Shell and Chitosan from ‘Belangkas’ as Adsorbent to Reduce Metal Level of Hg M. Z. Siregar, Z. Alfian, H. Marpaung, H. Agusnar On the Tensile Properties of Polylactide (PLA)/Arenga pinnata "ijuk" Fibre A. Rahman, M. Chalid, R. Ferdian, Nofrijon, B. Priyono ETP Insertion Effect on Carbon Composite Natural Rubber SIR 20 E. Budianto, Sudirman, M. Anggaravidya, Nasruddin, A.Haryono

77

89

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103

108

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Fiber and Fibrous Polymer Materials Mechanical Properties and Chemical Changes of Mahoni Wood (Swietenia mahagoni) by Close System Compression Hot Press Machine W. Dwianto, T. Darmawan, D.S. Adi, Y. Amin, I. Wahyuni, M. Karina

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117


Smart Material and Specialty Polymer Polymer-ionic Liquid Networks for Stretchable Electronics P. G. Whitten, S. Saricilar (Zengin), D. Antioho, K. Shu, C. Wang, G. G. Wallace

124

Light Sensitive Molecule for Photonic Devices G. Hegde, P. Z. Fernandes, A W Mahrokh, A R Yuvaraj, M. R. Lutfor, M. M Yusoff

125

Effect of Phthalate Buffer on Drug Released from Chitosan Microspheres Cross-linked by Tripolyphosphate K. Mulia, E. Krisanti, M . I. S. Husain, S. Yosaputra Study of Bacterial Cellulose-PVA Nanocomposite as a Bone Tissue Scaffold A. Z. Abidin, U. Sukandar, H. P. R. Graha , F. Ahmad The Investigation of CuOx Anode Interlayer Effect in Working Performance and Charge Carrier Transport in Hybrid Solar Cells with Inverted Structure Tulus, R. Hidayat Hydroxyapatite Deposition on Modified Bacterial Cellulose Matrix F. Nurlidar, D. Darwis, E. Budianto, Sugiarto Fast Swelling Superabsorbent Hydrogels Starch Based Prepared by Gamma Radiation Techniques Erizal, D. P. Perkasa, Sudirman, E. Budianto, R. Yudianti Catalytic and Non-Catalytic Depolymerization of Mixed Plastic Waste to Fuel Using Spent RFCC Catalyst A. Z. Abidin, Adrian Characterization of Electrodeposited PEDOT Films for Electrochromic Applications M. F. Zainal, Y. Mohd

126

133

142

143

144

155

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Green, Sustainable and Bio-polymers New Innovation on Fresh Latex Processing Through Combination of Air Compressing and Heating Technique D. Suwardin, A. Vahlepi, S. Hanifarianty, M. Purbaya Effect of Cocopeat Addition to the Some Properties of Cassava Starch-based Foam T. C. Sunarti, H. Integrani, K. Syamsu Development of Particle Board from Oil Palm Frond Fibers Using Citric Acid and Sucrose as Adhesives Subyakto, Z. Zhao, K. Umemura, S. Kawai Hygrothermal Aging on Heat Treated Kenaf Mat-Unsaturated Polyester Composite made by Resin Transfer Molding Process D. Ariawan, Z. A. M Ishak, R. M. Taib, M. Z. A. Thirmizir Synthesis and Characterization of Carboxymethyl Derivatives of Sago (Metroxylon sagu) Starch O. Zainon, K. Hashim, K. Sabariah, M. H. A. Nasir, A. Hassan

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164

165

166

174

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Cellulose Palmitate Biopolymer for Composite: Preparation and Application D. K. Arti, L. A. Wisojodharmo, D. A. Winarto, S. Septiva

184

Chemical Modification of Palm Kernel Shell Filled Unsaturated Polyester Biocomposites S. Husseinsyah, A. W. N. Mazlina Improvements of Tensile Properties and Durability of Chitosan Fiber Using Methanol Drying Treatment H. Judawisastra, I. O. C.Hadyiswanto, R. D. R.Sitohang, W. Winiati Preparation and Characterization of Polyurethane-modified Epoxy with Various Types of Polyol M. Ghozali, E. Triwulandari Synthesis of Sunflower Oil Based Elastomer and Its Characterization by Using Spectroscopic Techniques M. Purbaya, H. M. Noor, D. Suwardin The Utilization of Microcrystalline Cellulose from Waste Coconut Bunches (Cocos nucifera linn) as Filler for Cassava Starch Edible Film with Glycerol as Plasticizer P. Purworini, Y. Muis, B. Wirjosentono Surface Modification of Bacterial Cellulose Sheet as 2,3-dialdehyde H. Shim, M. Karina, R. Yudianti, L. Indrarti, J. Azuma, H. Uyama Study of Metal Ions Removal from Aqueous Solution by Using Radiation Crosslinked Chitosan co Poly(Acrylamide)-based Adsorbent T. Puspitasari, Oktaviani, D. S. Pangerteni, E. Nurfilah, D. Darwis The Effect of Temperature on the Grafting of Acrylic Acid onto Carboxymethyl Cellulose L. Anah, N. Astrini, A. Haryono

The Influence of Succinyl Groups and Lithium Perchlorate on Chitosan Membranes as Electrolyte Polymers I. Fauzi, D. Wahyuningrum, I. M. Arcana Adsorption of Heavy Metal Ion from Aqueous Solutions by Using Cellulose Based Hydrogel Composite N. Astrini, L. Anah, H. R. Haryadi The Influence of Accelerated Stability Test to Physical Properties of Varied-stirring Speed Chitosan-based Nanoemulsion W. K. Restu, Y. Sampora, A. Haryono Radiation Copolymerization of Styrene Monomer onto Tapioca and Natural Rubber S. Iskandar Thermal Characterization of Crude Natural Polymer Recovered from Bioethanol Pretreatment Process A. Hanafi, H. Budiman Arrowroot Starch Nanoparticles Christina Winarti, Titi Candra Sunarti, Djumali. Mangunwidjaja, Nur Richana

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192

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195

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209

217

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Bonding Performance of Natural Rubber-based Aqueous Polymer Isocyanate As Plywood Adhesive E. Hermiati, L. Risanto, R. P. B. Laksana Influence of Methacrylic Acid Modification on Tensile Properties of Polypropylene/Cocoa Pod Husk Biocomposites S. C. Koay, H. Salmah, H. Osman Effect of Corn Hominy and Polyvinyl Alcohol on Mechanical Properties of Cassava Starch Baked Foam E. S. Iriani, T. T. Irawadi, T. C. Sunarti, N. Richana, I. Yuliasih Isolation and Characterization of Nanocrystalline Cellulose from Sugar Palm Bunch (Arenga pinnata (Wurmb) Merr.) Sumaiyah, B. Wirjosentono, Karsono, M. P. Nasution, S. Gea Study of Phenol and Acetic Acid Components in Liquid Smoke of Palm Redestilation and Microbial Activities Test on Escherecia coli and Staphylococcus aureus Using the Kirby-Bauer Method D. Ardilla, Thamrin, Eddyanto, B. Wirjosentono

242

251

252

253

261

Studies of Dielectric Properties and Conductivity of Chitosan–Lithium Triflate Electrolyte Sudaryanto, E. Yulianti, H. Jodi

268

Copolymerization of Acrylamide with 9– and 10 Acrylamidodecanoic Acid Desnelli, C. L. Radiman, D. Mujahidin, Y. Permana

269

Freeze-Thaw Treatment in 2% w/w NaOH-6 M Urea Enhanced Extraction of β-(1,3;1,4)-Glucan from Corn Pericarp T. Yoshida, Y. Honda, T. Tsujimoto, H. Uyama, J. Azuma The Effect of Filler Content and UltraPlast TP01 of Nypa Fruticans Fiber Filled Polylactic Acid/Recycled Low Density Polyethylene Biocomposites on Tensile Properties and Morphology. M. Syahmie Rasidi, H. Salmah, P.L. Teh Degradation of Chitosan by Hydrothermal in the Presence of Sonication Pre-treatment with Supercritical CO2 as Pressurized Fluid E. Savitri, Sumarno, A. Rosyadi Isolation of Natural Polymer from the By-product of Hydrolysis of Oil Palm Empty Fruit Bunch for Bioethanol Production H. Budiman, A. Hanafi

270

271

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273

Advanced Synthesis Polymers Application of Hydrazine Compound to Produce Constant Viscosity Rubber A. Vachlepi, D. Suwardin, M. Purbaya, S. Hanifarianty

274

Study of Synthesis and Properties of Novel γ -Valerolactone-based Polyurethanes M. Chalid, H. J. Heeres, A. A. Broekhuis

275

Synthesis and Characterization of kappa-Carrageenan-graft-acrylamide for Enhanced Oil Recovery Application M. G. Darmayanti, C. L. Radiman

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Cutting Techniques Chain Structure of Amylopectin as Macro-initiator for Biodegradable Copolymers by ATRP A. S. Handayani, M. Chalid, D. Priadi, I. S. Purwaningsih Mechanical and Thermal Properties of Hybrid Coating Product from Polyurethane and/or Polysiloxane Based on Acrylic Polyol and Tolonate E. Triwulandari, M. Ghozali Synthesis of LiFePO4 in the presence of Organic Reductant by Hydrothermal Method and its Characterization I. Gunawan, H. Wagiyo

277

285

296

Radiation Graft Copolymerization of Acrylic Acid onto Rice Straw Cellulose Rahmawati, M. Suhartini, E. Budianto

297

Fast Photoswitching Azo Dyes G. Hegde, A. R. Yuvaraj, W. S. Yam, M. M. Yusoff

298

Surface Coating of Acrylate Polymer on Sengon Wood (Paraserianthes falcataria) using UV Irradiation Darsono

Author Index

299

300

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The International Conference on the Innovation in Polymer Science and Technology 2013 (IPST2013) Yogyakarta, Indonesia, October 7 –10, 2013

Mechanical and Thermal Properties of Hybrid Coating Products from Polyurethane and/or Polysiloxane Modified Epoxy Based on Acrylic Polyol and Tolonate E. Triwulandari1,, M. Ghozali1 1

Research Center for Chemistry, Indonesian Institute of Science, Serpong, Indonesia; [email protected] Abstract. Hybrid coating products were synthesized from polyurethane and/or polysiloxane modified epoxy based on acrylic polyol and tolonate. Hybrid coating which synthesized were epoxy-polyurethane, epoxy-polysiloxane and epoxy-polyurethane-polysiloxane. Hybrid coating from epoxy-polyurethane was synthesized by reacting epoxy, acrylic polyol and tolonate. The second hybrid coating from epoxy-polysiloxane was synthesized by reacting epoxy and polysiloxane by using γ-aminopropyl triethoxysilane (γ-APS) as crosslinking agents. And the third hybrid coating from epoxy-polyurethanepolysiloxane was synthesized by reacting epoxy with monomer constituent of polyurethane and polysiloxane via simultaneous reaction. Characterizations of hybrid coating products were using FTIR and 1H-NMR spectroscopy. Curing process of hybrid coating products to obtain film sheets were done by adding versamid 140 as hardener. Characterizations of film sheets were conducted by determination of mechanical properties such as tensile strength and elongation at break and thermal properties by using thermogravimetric analysis (TGA). The mechanical and thermal properties of hybrid coating products have been compared with the unmodified epoxy. Mechanical properties of epoxypolyurethane and epoxy-polyurethane-polysiloxane hybrid coating were higher than the mechanical properties of unmodified epoxy. The highest thermal property was shown by the epoxy-siloxane hybrid coating thermogram. Keywords: Hybrid coating; epoxy; polyurethane; polysiloxane; acrylic polyol; tolonate

Introduction Epoxy and polyurethane are binders that usually used in the formulation of protective coating. Epoxy and polyurethane are used as multilayer in paint system, whether epoxy usually as primer or intermediate coat and polyurethane as the top coat [1,2]. Although epoxy has good mechanical properties and chemical resistant but it has some weakness. The weaknesses of epoxy are brittle, low impact strength and low elongation at break so it has limitation when applied for high performance applications [3-5]. Several researches about modified epoxy had been done to improve the characteristic of epoxy. One of the

285 © 2015 Published by IPST2013


methods for modification of epoxy is by reacting epoxy with another polymer (binder) and/or inorganic material to produce hybrid coating. Hybrid coating is a new technology in coating method. This technology develops a new binder system by combining two binders or more that have different properties to improve their characteristic as a coating for corrosion protection [3,6,7]. Polyurethane resin that usually used as the top coat in paint system can be used as modifier of epoxy resin because it has excellent properties. When the epoxy resin was modified with polyurethane it produces a new resin system, the process application of this coating can be done only using one layer and not multilayer again [3-5, 8-10]. It has been reported that modification of epoxy using polyurethane improved the toughness of epoxy, for example thermal resistant and mechanical property [4]. Modification of epoxy resin via organic-inorganic hybrid coating concept has also been studied. Modification of organic resin with polysiloxane has generally been recognized as a new class of high-performance coatings. Siloxane is an inorganic system, it is more resistant in degradation mechanism, and it is also based on that structure consists of a silicone resin with a stable polysiloxane backbone [- (Si-O) n-Si-]. The chemical bonding of Si-O is stronger than C-C chemical bond of the organic coating structure, where the strength of Si-O bond is 108 kcal / mole and the strength of C-C bond is 83 kcal / mole. It requires large energy to break the Si-O bonds therefore coating based on siloxane will have excellent properties such as thermal stability, weather and UV resistance, durability and chemical attack [1,11]. Epoxy-siloxane hybrid is a kind of organic-inorganic hybrid coating that has been studied and commercialized. This new resin combines the properties of epoxy as organic polymer and siloxane as inorganic polymer. It has been reported that epoxy-siloxane hybrid have anticorrosive performance in acid, saline and organic solvent environments in general and in alkaline environments [1, 11-15]. Another research about hybrid coating also has been reported by modified epoxy with other organic polymer and siloxane. Polyurethane is an organic polymer that can be used in modified epoxy with siloxane to produce hybdrid coating [3, 16]. Polyurethane is widely used as a coating material because it has excellent mechanical, physical and abrasion resistant properties. The addition of polyurethane in the process of modified epoxy with siloxane resin can improve the properties of the resulting resin respectively. It has been reported that the mechanical and thermal properties modified epoxy-polyurethane-siloxane hybrid coating increase [3, 4, 17]. Several researches about synthesis of hybrid coating based on epoxy-polyurethane-siloxane are 286 © 2015 Published by IPST2013


still limited and it needs further studies especially by using other constituent monomer of polyurethane. Different kind of constituent monomer will affect the properties and characteristic of polyurethane resin. The scope of this research is synthesis hybrid coating from polyurethane and/or polysiloxane modified epoxy by using acrylic polyol and tolonate as the constituent monomer of polyurethane. Comparison properties and characteristic between unmodified epoxy, epoxy-polyurethane, epoxy-polysiloxane and epoxy-polyurethane-siloxane hybrid coating also have been studied.

Experimental Materials Epoxy diglycidyl ether bisphenol A (epoxy YD 128 with Epoxy Equivalent Weight (EEW) = 180-190), acrylic polyol (Evercryl 2901 with a hydroxyl number = 47.28 mgKOH / g), Tolonate HDT (% NCO = 31.6155%), versamid 140 (curing agent), hydroxyl

terminated

polydimethylsiloxane

(HTPDMS,

Aldrich),

γ-aminopropyl

triethoxysilane (γ –APS, Merck). Synthesis of Epoxy-Polyurethane Hybrid Coating (Polyurethane Modified Epoxy) Epoxy-polyurethane hybrid coating was synthesized by reacting epoxy, acrylic polyols, and tolonate in the three-neck flask simultaneously. The ratio of NCO/OH of tolonate and acrylic polyol as the components of polyurethane used in this research is 2.5. The total weight of acrylic polyol and tolonate was 20% relative to the epoxy. The reaction was conducted at 50ᵒC for 30 min. Synthesis of Epoxy- Polysiloxane hybrid coating Epoxy-polysiloxane hybrid coating was synthesized by reacting epoxy with hydroxyl terminated HTPDMS (10%) and γ–APS (1%) as silane cross-linking agents. The reaction was conducted at 50ᵒC for 20 min. Synthesis of epoxy-polyurethane-polysiloxane hybrid coating Epoxy-polyurethane-polysiloxane hybrid coating was synthesized by reacting epoxy, acrylic polyols, tolonate and HTPDMS (10% relative to the epoxy) in the three-neck flask simultaneously. The ratio of NCO/OH of isocyanate and polyol as the components of polyurethane in this research is 2.5. The total weight of acrylic polyol and tolonate was 20% to the epoxy. The reaction was conducted at 50ᵒC for 30 min. Characterization



Before characterization, the resulting mixture was cured by using versamid 140 as curing agent with the composition 0.5w/w relative to the hybrid coating mixture to obtain film sheet. The film sheet product has cured for 7 d prior to analysis. Characterization of the hybrid coating products were conducting by using FTIR analysis (IRPrestige-21 Shimadzu) to determine the functional groups which were formed, and analysis of 1HNMR (JNM ECA-500 Brand JEOL) to determine the proton chemical shifts. The mechanical properties were analysis to determine the tensile strength and elongation at break properties using Universal Testing Machine, Orientec Co. Ltd, Model UCT-5T and thermal analysis using TGA Instrument Q50.

Results and Discussion Synthesis of Epoxy-Polyurethane Hybrid Coating Modification of epoxy with polyurethane can be done by reacting with the polyol and isocyanate as constituent monomer of polyurethane. Because of epoxy diglycidyl ether bisphenol A contain hydroxyl group in its structure, so it can act as a polyol which will react with isocyanates group in tolonate. Modification process of epoxy by using polyurethane was conducted via simultaneous reaction where epoxy, acrylic polyol and tolonate were reacted in one step. The reaction between epoxy, acrylic polyol and tolonate are shown in Fig. 1. O

OR

OH O

O

O

O

O

O

O

OH

n

+

+

C6H12 N

n C O

OH

OR

O

OR O

NH

C6H12

O

O

O

N

N

C6H12 C

O

NH

12

C O

O O

H

HN C6H 12

O

O

C

6

HN O

NH

N

N O C

O

C O

C

C6H12

O

C6H 12 N C

O

O O n

N O

tolonate

acrylic polyol O

O N

O

epoxy

C N C6H 12 N O

OR

O

N

O

C6H 12

N

N H

O

O

O C O

O

O O

O

O

n RO O

n

O O

RO

polyurethane modif ied epoxy

O

Figure 1. Synthesis of Epoxy-Polyurethane Hybrid Coating



Fig. 1 showed how epoxy and acrylic polyol can react with tolonate to form a new compound called epoxy-polyurethane hybrid coating (polyurethane modified epoxy). The isocyanate groups (two groups) from tolonate reacted with two hydroxyl groups from acrylic polyol and one hydroxyl group from epoxy. It is assumed due to the hydroxyl groups on the acrylic polyol is a primary alcohol while hydroxyl groups on the epoxy is a secondary alcohol, so it is suspected that acrylic polyol more reactive to form urethane bonds than the reaction with epoxy. Fig. 4 showed the FTIR analysis of raw material (epoxy and polysiloxane) and the hybrid coating products. Figure 4D is the unmodified epoxy before reaction. The FTIR spectra of the unmodified epoxy has wide absorption peak in the wave number 3500 cm-1 which is the absorption peak of the –OH group. While, The FTIR spectra of polyurethane modified epoxy (Fig. 4B) has sharper absorption peak in the wave number 3437 cm-1 from the absorption peak of –NH group. The appearance of –NH group in the polyurethane modified epoxy product indicates that the -OH groups from epoxy and polyol have reacted with isocyanate and formed urethane bond. Fig. 4B from the spectra of the polyurethane modified epoxy showed a new absorption peak appeared at wave number 1726 – 1722. This new peak is from C = O group absorption of the urethane bond (-NH-(C = O)-O-) which is formed from the reaction between isocyanate (N = C = O) with hydroxyl group (OH) of the epoxy and polyol. Fig. 5 showed the H-NMR analysis of unmodified epoxy (5A) as raw material and the hybrid coating products (5B and 5C). There were new chemical shifts at 2.3 ppm which indicated the –CH2 bonding from acrylic polyol and at 1.25 ppm from the –CH2 of tolonate. Synthesis of Epoxy- Polysiloxane hybrid coating Modification of epoxy with polysiloxane has been conducted by using hydroxyl terminated polydimethylsiloxane (HTPDMS) as polsiloxane and γ-aminopropyl triethoxysilane (γ-APS) as cross-linking agents. The reaction between epoxy and polysiloxane is shown by Figure 2.



OH O

O

O

O

O

O

+

n

NH2

O

O

(CH 2) 3

OH

Si(OEt)3

OH O

O

O

PDMS

HO

OH

OH O

HO

O

O

O

O

N n

n

(CH 2)3 Si

O

Si

O

Si

O Si

Figure 2. Synthesis of epoxy- polysiloxane hybrid coating. In this reaction, the oxirane ring of epoxy reacted with the amine group in γ-APS and the oxirane ring cleavage and produced hydroxyl group. The next reaction was the ethoxy groups in γ-APS reacted with hydroxyl group in HTPDMS to produce Si – O- Si linkage. According to the overlay data of FTIR spectra from unmodified epoxy (Fig. 4D) and epoxy-polysiloxane hybrid coating (Fig. 4C) can be figured that in the spectra of epoxypolysiloxane hybrid coating there is new absorption peak in the wave number 1099 cm-1 from the absorption peak of Si-O-Si. This new absorption peak from Si-O-Si showed that reaction between ethoxy groups in γ-APS and the hydroxyl group in HTPDMS has occurred. Reaction between oxirane ring of epoxy and the amine group in γ-APS was shown by the decreasing intensity of absorption peak from oxirane ring in the wave number 912 cm-1 because of the oxirane ring cleavage after reacted with amine group. Synthesis of epoxy-polyurethane-polysiloxane hybrid coating This synthesis process of epoxy-polyurethane-polysiloxane hybrid coating is similar with the synthesis process of polyurethane modified epoxy above. Where there was not addition of γ-APS as cross linking in this reaction. Because of hydroxyl terminated polydimethylsiloxane contain hydroxyl group in its structure, so it can act as a polyol which will react with isocyanates. Isocyanates which added in the process synthesis reacted with hydroxyl group of epoxy, polyol and HTPDMS. The reaction between epoxy, acrylic polyol, tolonate and HTPDMS are shown by Fig. 3. Urethane linkage that being produced from the reaction between N=C=O group of isocyanate and hydroxyl group of epoxy, polyurethane, and HTPDMS are shown by absorption peak in wave number 17241687 cm-1 from C=O group and 1581 cm-1 and 3433-3292 cm-1 from N-H group. Reaction between hydroxyl group of HTPDMS and N=C=O group of isocyanate produced (-NH-(C = O)-O-Si-) linkage which is shown by absorption peak in the wave number 1157 cm-1



(Figure 4A). From the 1H-NMR spectra there were new chemical shift at 2.3 ppm which indicated the –CH2 bonding from acrylic polyol and at 1.26-1.25 ppm from the –CH2 of the tolonate (Figure 5B).

O

O

OH O

O

O

OR O

O

C N C6H 12 N O

OR

O

O

+

OH

n

O

+ HO

PDMS OH

+

O

Hydroxy Terminated N Polydimethylsiloxane C6H 12

n

C

OH

N

N O

C6H 12 N C

O

acrylic polyol

epoxy

O

OR

O

OR

O

O O n

O

C

C O NH

N O

O

O

O C6H12 C NH O

N N

O C 6H

HN C6H 12

C

N

O

O

O O

NH

12

HN O

C6H12

O

C6H 12

O

C

O

tolonate

N

O N C O H

O

C6H 12

N O

PDMS OH

O O

n O O

Epoxy-Polyurethane-Polysiloxane Hybrid

Figure 3. Synthesis of epoxy-polyurethane-polysiloxane hybrid coating.



Figure 4. FTIR Spectra of Epoxy-Polyurethane-Polysiloxane Hybrid Coating (A), EpoxyPolyurethane Hybrid Coating (B), Epoxy-Polysiloxane Hybrid Coating (C), Unmodified Epoxy (D), and hydroxyl terminated polydimethylsiloxane (E).

Figure 5. 1H-NMR spectra of Unmodified Epoxy (A), Epoxy-Polyurethane-Polysiloxane Hybrid Coating (B), Epoxy- Polyurethane Hybrid Coating (C).



Mechanical Properties The mechanical properties of unmodified epoxy and modified epoxy have been conducted by using tensile strength and elongation at break analysis. Mechanical properties comparison between unmodified epoxy, epoxy-polyurethane, epoxy-polysiloxane and epoxy-polyurethane-polysiloxane hybrid coating films are shown at Table 1. The highest value of tensile strength and elongation are from epoxy-polyurethane hybrid product. This is due to the addition of polyurethane enhance the cross-link density of epoxy resin. Moreover the addition of polysiloxane into epoxy resin was not significantly affect the tensile strength of epoxy but affect the increasing of elongation at break value. It is suspected because of polysiloxane has flexible –Si–O–Si– linkage, therefore the siloxane moiety functioning can act as an internal plasticizer. The tensile strength of epoxypolyurethane-polysiloxane was smaller than epoxy-polyurethane hybrid but had the same elongation at break value. These data showed that the addition of polysiloxane into epoxypolyurethane hybrid decreases its tensile strength due to the flexibility of –Si–O–Si– linkage [3, 18]. Table 1. Mechanical Properties of Unmodified and Modified Epoxy Film Unmodified Epoxy Epoxy-Polyurethane Hybrid Epoxy-Polysiloxane Hybrid Epoxy-PolyurethanePolysiloxane Hybrid

Thickness (µm)

Tensile Strength (MPa)

Elongation at break (%)

283.53 239.22 280.2

6.82 11.29 6.62

2.29 2.92 2.5

263.925

10.8

2.92

Thermal Properties The thermal stability of unmodified epoxy and modified epoxy is illustrated in Figure 6. As seen in the figure, for all of the samples have similar degradation thermogram. The thermal stability of epoxy-polyurethane hybrid and unmodified epoxy overlap and has tendency to be similar. Therefore the addition of polyurethane into epoxy resin was not significantly affecting the mechanical properties. The thermal stability of epoxy resin improved when it was modified with polysiloxane and polyurethane-polysiloxane. At temperature 500ᵒC the weight loss of unmodified epoxy and epoxy-polyurethane hybrid is smaller than the weight loss of epoxy-polysiloxane hybrid and epoxy-polyurethane293 © 2015 Published by IPST2013


polysiloxane hybrid. At temperature 500ᵒC the weight of unmodified epoxy and epoxypolyurethane hybrid is 10%, the weight of epoxy-polyurethane-polysiloxane hybrid is 22% and the weight of epoxy-polysiloxane hybrid is 34%. Polysiloxane has ability to delay the thermal degradation process because of its high bond energy and thermal stability of –Si-O-Si linkage [3].

Figure 6. TGA curves of Unmodified Epoxy and Hybrid Coating

Conclusions The hybrid coating products from polyurethane and/or polysiloxane modified epoxy based on acrylic polyol and tolonate were successfully synthesized via simultaneous reaction and confirmed by FT-IR and 1H-NMR spectra. Modification of epoxy by using polyurethane and polyurethane-polysiloxane increased the tensile strength and elongation at break properties of epoxy. Whereas modification of epoxy by using polysiloxane have not significant effect on change in tensile strength, but increased the elongation at break and have highest thermal properties.

Acknowledgement This work has been financially supported by Competitive Program LIPI. The authors would like to thank Ir. Wiwiek Pudjiastuti, MSi, Yenni A.D and Hadidjah, for their help during this work.

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Author Index A Aarik, 91 Abbas, 2 Abdullah, 58, 90 Abidin, 133, 155 Adi, 117 Adrian, 155 Afrinaldi, 108 Agusnar, 109 Ahmad, 133 Alfian, 109 Amin, 117 Anah, 206, 208 Anggaravidya, 36, 116 Antiohos, 124 Anwar, 92 Arcana, 207 Ariawan, 174 Aritonang, 38 Arroval, 91 Arti, 48, 184 Astari, 89 Astrini, 206, 208 Astutiningsih, 101 Aziz, 74 Azuma, 204, 270

B Bahruddin, 11 Basuki, 37 Broekhuis, 275 Budianto, 64, 76, 116, 143, 144, 297 Budiman, 225, 273

C Chaki, 35 Chalid, 115, 275 Ciptati, 38

D Daik, 3 Darmawan, 117 Darmayanti, 276 Darsono, 299 Darwis, 2, 143 Desnelli, 289 Dihardjo, 34 Dirgantara, 77 Draman, 3 Dwianto, 117

E Efrizal, 11 El-Sheikh, 3 Erizal, 2, 144

F Fathurrohman, 64 Fausiah, 36 Fauzi, 207 Ferdian, 115 Fernandes, 125 Firuz, 74 Foster, 18

G Gea, 253 Ghozali, 193, 285 Graha, 133 Gunawan, 296

H Hadyiswanto, 192 Hamzah, 36 Hanafi, 225, 273 Handayani, 34 Hanifarianty, 164, 274 Harito, 90 Haryadi, 208 Haryono, 116, 206, 209 Hashim, 183 Heeres, 275 Hegde, 125, 298 Hermiati, 242 Hidayat, 142 Hirose, 4 Honda, 270 Husain, 126

I Indrarti, 204 Indriasari, 48 Integrani, 165 Irawadi, 252 Irfan, 103 Iriani, 252 Irwanto, 65 Iskandar, 217 Ismadi, 101, 102 Ismail, 34

J Jayatin, 103 Jodi, 268 Judawisastra, 58, 90, 192

K Karina, 58, 117, 204 Karsono, 253 Kasmudjiastuti, 65 300

© 2015 Published by IPST2013


Kawai, 166 Khare, 25 Khastgir, 35 Kink, 91 Koay, 251 Krisanti, 126 Kurniati, 77 Kurniawansyah, 18 Kusumaningrum, 102

L Laksana, 242 Lan, 74 Lange, 91 Latif, 3 Lutfor, 125

M M Ishak, 174 Mahendra, 76 Mahrokh, 125 Mammucari, 18 Marpaung, 109 Massijaya, 89 Mohamed, 33 Mohar, 17 Mohd, 163 Muis, 195 Mujahidin, 269 Mulia, 126 Munawar, 102 Mutalib, 92

N Nagari, 34 Nasir, 183 Nasruddin, 116 Nasution, 253 Nayak, 35 Nofrijon, 115 Noor, 194 Nurfilah, 205 Nurhajati, 65 Nurlidar, 143

O Oktaviani, 205 Onggo, 38 Osman, 251

P Pangerteni, 205 Pargi, 73 Perkasa, 144 Permana, 269 Prasetiyo, 89 Pribadi, 2 Priyono, 115

Pujiyanto, 92 Purbaya, 164, 194, 274 Purnamasari, 92 Purworini, 205 Puspitasari, 215 Putra, 34

R Radhakrishnan, 25 Radiman, 38, 269, 276 Radji, 92 Rahardi, 37 Rahman, 115 Rahmawati, 297 Ramadha, 64 Ramrad, 33 Rarista, 76 Rashid, 33 Ratnam, 33 Restu, 209 Richana, 252 Rifathin, 108 Risanto, 242 Rohman, 64, 103 Rosyadi, 272

S Saar, 91 Sabariah, 183 Salmah, 73, 74, 75, 251 Sam, 75 Sampora, 209 Saptoraharjo, 17 Saricilar (Zengin), 124 Savitri, 272 Septiva, 184 Shim, 204 Shu, 124 Siregar, 109 Siswanto, 36 Siswosuwarno, 58 Sitohang, 192 Soegijono, 64, 76 Soehardjo, 37 Subyakto, 93, 101, 166 Sudaryanto, 268 Sudirman, 76, 116, 144 Sugiarto, 143 Suhartini, 297 Suharty, 34 Sukandar, 133 Sukardi, 93 Sumaiyah, 253 Sumarno, 272 Sunarti, 165, 252 Suryani, 93 Sutriyo, 92 Suwardin, 164, 194, 274 Syamani, 93 Syamsu, 165



T Taib, 174 Takenaka, 1 Thirmizir, 174 Triwulandari, 193, 285 Tsujimoto, 270 Tulus, 142

U Umemura, 166 Utami, 11 Uyama, 204, 270

V Vachlepi, 274 Vahlepi, 164

W Wagiyo, 296 Wahyuni, 117 Wahyuningrum, 207 Wallace, 124 Wang, 124 Whitten, 124 Wijaya, 108

Winarto, 184 Winiati, 192 Wirjosentono, 195, 253 Wisojodharmo, 48, 184

Y Yahya, 58 Yam, 298 Yeng, 75 Yeoh, 73 Yosaputra, 126 Yoshida, 270 Yudianti, 144, 204 Yulianti, 268 Yuliasih, 252 Yusoff, 125, 298 Yuvaraj, 125, 298 Yuwono, 101

Z Zainal, 163 Zainon, 183 Zhao, 166 Zhuisa, 92 Zope, 25 Zulfansyah, 11 Zulfia, 17
