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DOCTORAT EN SCIENCES Par Mr. BAOUZ TOUFFIK THEME

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DOCTORAT EN SCIENCES Par Mr. BAOUZ TOUFFIK THEME REPUBLIQUE ALGERIENNE DEMOCRATIQUE ET POPULAIRE MINISTERE DE L’ENSEIGNEMENT SUPERIEUR ET DE LA RECHERCHE SCIENTIFIQUE UNIVERSITE FERHAT ABBAS - SETIF 1 UFAS (ALGERIE) THESE Présentée à La Faculté de Technologie Département de Génie des Procédés Pour l’Obtention du Diplôme de DOCTORAT EN SCIENCES Option : Génie des Polymères Par Mr. BAOUZ TOUFFIK THEME MODIFICATION DE RESINES POLYESTERS PAR DES ADDITIFS NATURELS ET/OU SYNTHETIQUES Soutenue le: 25 / 06 / 2015 devant un Jury composé de Président : Prof. DJAFER BENACHOUR Université Ferhat Abbas, Sétif 1 Rapporteur : Prof. FAROUK REZGUI Université Abderrahmane Mira, Bejaia Examinateurs : Prof. HOCINE DJIDJELLI Université Abderrahmane Mira, Bejaia Prof. AMAR BOUKERROU Université Abderrahmane Mira, Bejaia Prof. MOHAMED TAHAR Université Ferhat Abbas, Sétif 1 BENANIBA ABSTRACT The main objective of the present research study was to toughen poly(lactic acid) (PLA) using rubber-toughening technique without adversely affecting its stiffness and strength. PLA was melt blended in a twin screw extruder with an ethylene-methyl acrylate-glycidyl methacrylate (E-MA-GMA) impact modifier in the range 5-30 wt% in the presence of 2 wt% of an organomodified montmorillonite (OMMT) to minimize the loss of stiffness and strength of PLA. The first part of this work reports on the study and comparaison of PLA/E-MA-GMA blends and PLA/E- MA-GMA/OMMT ternary nanocomposites prepared by mixing all ingredients simultaneously in the hopper of the extruder. Scanning electron microscopy (SEM) revealed that PLA and E-MA-GMA form an immiscible blend in which the rubber formed sub-micron particles the size of which increased with increasing rubber content. Impact strength and ductility of the blends increased with increasing rubber content but at the expense of stiffness and strength. Ternary nanocomposites exhibited intercalated/partially exfoliated structure, whereas the ternary nanocomposites at 10 wt% rubber ratio showed complete exfoliation of OMMT as detected by x-ray diffraction (XRD) and confirmed by transmission electron microscopy (TEM) which thus resulted in balanced properties. The viscosity of the mixtures as measured by melt flow index was found to be highly influenced by the addition of the rubber and the OMMT. In the second part of this work and with the same aim of increasing further PLA toughness, the effects of four addition protocols of the components of the ternary nanocomposites were investigated. It was found that both clay dispersion and morphology were influenced by the blending method as detected by XRD and observed by TEM and SEM. The XRD results, which were also confirmed by TEM observations, demonstrated that the OMMT dispersed better in PLA than in E-MA- GMA. All formulations exhibited intercalated/partially exfoliated structure with the best clay dispersion achieved when the clay was first mixed with PLA before the rubber was added. According to SEM, the blends exhibited fine dispersion of the rubber in the PLA with differences in the mean particle sizes that depended on the addition order. Balanced stiffness-toughness was noticed at 10 wt% rubber content in the compounds without significant sacrifice of the strength. High impact toughness i was attained when PLA was first mixed with the clay before the rubber was added, and the highest tensile toughness was obtained when PLA was first compounded with the rubber, and then clay was incorporated into the mixture. Thermal characterization by DSC carried out in both parts of this research work confirmed the immiscibility of the blends, but in general, it was revealed that the thermal parameters and the degree of crystallinity of the PLA were not affected by the preparation procedure. Furthermore, both the clay and the rubber were found to decrease the crystallization temperature of the PLA by acting as nucleating agents. ii ORIGINAL CONTRIBUTION TO SCIENTIFIC KNOWLEDGE Peer-Reviewed Journal Publications: 1- Touffik Baouz, Farouk Rezgui, Ulku Yilmazer, Ethylene-Methyl Acrylate- Glycidyl Methacrylate Toughened Poly(lactic acid) Nanocomposites, Journal of Applied Polymer Science, Volume 128, pages 3193-3204, 2013. 2- Touffik Baouz, Eda Açik, Farouk Rezgui, Ulku Yilmazer, Effects of Mixing Protocols on Impact Modified Poly(lactic acid) Layered Silicate Nanocomposites, Journal of Applied Polymer Science, Volume 132, 2015. Conference Publications: Touffik Baouz, Farouk Rezgui, Ulku Yilmazer, “Impact Modified Poly(lactic acid)- Organoclay Nanocomposites Prepared by Twin Screw Extruder”, 3rd International Polymeric Composites Symposium, Exhibition and Workshop, 9-12 November 2012, Izmir-Turkey. iii ACKNOWLEDGEMENTS In the name of God, most Gracious, most Compassionate, and peace be upon his messenger Mouhamed who exhorted his followers to seek for knowledge from cradle to grave. It is of my duty to express, in this small allowed space, all my heartfelt gratitude to all who have contributed to the completion of the present modest work. I would like to express my sincere and deepest gratitude to my supervisor, Pr. Dr. Farouk Rezgui for his continuous technical guidance, constructive criticism, patience and insight throughout elaboration of this research work. I am also highly indebted to Pr. Dr. Ülkü Yılmazer from Chemical Engineering department of Middle East Technical University (METU-Ankara-Turkey) who trusted me and accepted me in his laboratory. I am forever grateful to him for his inspiring, guidance, valuable scientific contribution and critics and also for his endless support and warm care during my stay in Ankara. I am also grateful to Pr. Dr. Göknur Bayram from Department of Chemical Engineering (METU) for allowing me to use some of the instruments in her laboratory. Special thanks are also addressed to the committee members Pr. Dr. Djafer Benachour, Pr. Dr. M. Tahar Benaniba, Pr. Dr. Amar Boukerrou and Pr. Dr. Hocine Djidjelli who have accepted to review my thesis, to evaluate my research work and to attend the defense of the thesis. My beloved wife deserves special thanks for the unconditional sacrifices she made, her understanding and encouragement, and also for her moral support for which I was in great need all along the completion of this modest research work. Thanks are also due to my dear friend B. Elbirly and his wife Nimet for their encouragement, moral support and advices during may stay in Turkey. I also extend my heartfelt gratitude and thanks to all my lab fellows and friends in METU, especially Eda Açik, Ali Sinan Dike, Sengor Irem, Yuksel Sayin, Miray Yasar and Sertan Yeşil for their great help either scientific or social and also for their understanding and moral support which have made my stay in Ankara memorable. Also, I am very grateful to all the technicians of the Chemical Engineering Department of METU especially Mihrican Açıkgöz for her assistance with all thermal analysis. Last but not least, I wish to express my sincere thanks to all who have contributed either directly or indirectly to the fulfillment of this project. iv TABLE OF CONTENT TABLE OF CONTENT Page ABSTRACT i ORIGINAL CONTRIBUTION TO SCIENTIFIC KNOWLEDGE iii ACKNOWLEDGEMENTS iv TABLE OF CONTENTS v LIST OF FIGURES ix LIST OF TABLES xiv LISTE OF ABBREVIATIONS xv Chapter I - Introduction I-1 General Background 1 I-2 Problematic Associated with PLA 3 I-3 Motivations and Research Project Objectives 4 1-4 Thesis Overview and Organization 5 References 6 Chapter II - General Background and Literature Review II-1 Composites 9 II-2 General Aspects of Polymer Nanocomposites 11 II-3 Polymer Layered Silicate (PLS) Nanocomposites 15 II-3-1 Layered Silicates 16 II-3-2 Phyllosilicates: Types, Structure and Properties 18 II-3-3 Structure of Phyllosilicates 18 II-3-4 Cation Exchange Capacity (CEC) of Phyllosilicates 20 II-3-5 Hierarchical Organization of Phyllosilicates Structure 20 II-3-6 Organically Modified Layered Silicates (OMLS) 21 II-3-7 Montmorillonite (Smectite clay) 24 II-4 Structures of Polymer Layered Silicate Nanocomposite 26 II-4-1 Phase-Separated Composites (microcomposites) 27 II-4-2 Intercalated Nanocomposites 28 II-4-3 Exfoliated Nanocomposites 28 v II-5 Preparation Methods of PLS Nanocomposites 29 II-5-1 Intercalation of Polymers or Prepolymers from Solution 30 II-5-2 In Situ Intercalative Polymerization Method 31 II-5-3 Melt Intercalation Method 32 II-6 Biodegradable polymers 35 II-6-1 Introduction 35 II-6-2 Definition and Types of Biodegradable Polymers 36 II-6-3 Classification of Biodegradable Polymers 37 II-6-4 Biodegradable Polymers Production, Market and Applications 41 II-6-4-1 Biodegradable Polymers Production 41 II-6-4-2 Biodegradable Polymers Applications and Market 43 II-7 Biodegradable Polyesters 45 II-8 Poly(lactic acid): Synthesis, Structure, Properties and Applications 48 II-8-1 Poly(lactic acid) Precursor: Lactic Acid 48 II-8-2 Polyl(actic acid) Production Techniques 50 II-8-2-1 Direct Condensation Polymerization 51 II-8-2-2 Azeotropic Condensation Polymerization 51 II-8-2-3 Ring Opening Polymerization (ROP) 52 II-8-3 PLA Properties 55 II-8-3-1 Crystallization 55 II-8-3-2 Thermal Properties 56 II-8-3-3 Degradation 58 II-8-3-4 Solubility in solvents 58 II-8-3-5 Physical and Mechanical Properties 59 II-8-3-6 Rheology and Processing 60 II-8-3-7 Other Properties 61 II-8-4 PLA Applications 62 II-8-4-1 Medical, Biomedical and Pharmaceutical Applications 63 II-8-4-2 Packaging Applications 63 II-8-4-3 Fiber and Textiles 64 References 66 Chapter III - PLA Modifications : Litterature Survey and Previous Research Studies III-1 Introduction
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