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Acrylic Based Thermoplastic Elastomers: Design and Synthesis for Improved Mechanical Performance

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Acrylic Based Thermoplastic Elastomers: Design and Synthesis for Improved Mechanical Performance University of Tennessee, Knoxville TRACE: Tennessee Research and Creative Exchange Doctoral Dissertations Graduate School 5-2017 All Acrylic Based Thermoplastic Elastomers: Design and Synthesis for Improved Mechanical Performance Wei Lu University of Tennessee, Knoxville, [email protected] Follow this and additional works at: https://trace.tennessee.edu/utk_graddiss Part of the Materials Chemistry Commons, Organic Chemistry Commons, Polymer and Organic Materials Commons, Polymer Chemistry Commons, and the Polymer Science Commons Recommended Citation Lu, Wei, "All Acrylic Based Thermoplastic Elastomers: Design and Synthesis for Improved Mechanical Performance. " PhD diss., University of Tennessee, 2017. https://trace.tennessee.edu/utk_graddiss/4411 This Dissertation is brought to you for free and open access by the Graduate School at TRACE: Tennessee Research and Creative Exchange. It has been accepted for inclusion in Doctoral Dissertations by an authorized administrator of TRACE: Tennessee Research and Creative Exchange. For more information, please contact [email protected]. To the Graduate Council: I am submitting herewith a dissertation written by Wei Lu entitled "All Acrylic Based Thermoplastic Elastomers: Design and Synthesis for Improved Mechanical Performance." I have examined the final electronic copy of this dissertation for form and content and recommend that it be accepted in partial fulfillment of the equirr ements for the degree of Doctor of Philosophy, with a major in Chemistry. Jimmy W. Mays, Major Professor We have read this dissertation and recommend its acceptance: Alexei P. Sokolov, Michael D. Best, Thomas A. Zawodzinski Accepted for the Council: Dixie L. Thompson Vice Provost and Dean of the Graduate School (Original signatures are on file with official studentecor r ds.) All Acrylic Based Thermoplastic Elastomers: Design and Synthesis for Improved Mechanical Performance A Dissertation Presented for the Doctor of Philosophy Degree The University of Tennessee, Knoxville Wei Lu May 2017 Copyright © 2017 by Wei Lu All rights reserved. ii ACKNOWLEDGEMENTS It would not be possible to complete either the work in this thesis and all my PhD work and life without the kindness and support from numerous people. First and foremost, I would like to thank Professor Jimmy Mays for his guidance, supervision, instructions, encouragement and full support of every aspect from research to life. His generous and patient help and various opportunities provided have made me acquainted with the panorama of polymer not only in academia but also in industrial applications. His passion, wisdom, and spirit of collaboration have greatly influenced my attitude toward my future career and life. I would like to thank my doctoral committee members: Dr. Alexei Sokolov for kind interpretations and suggestions on the theories and physics behind and beyond polymer chemistry, Dr. Michael Best for his valuable time and advising on synthetic chemistry, Dr. Thomas Zawodzinski for his explanations on the mechanism and engineering aspects of membrane applications. It is my great honor to have all these collaboration and support. I sincerely thank Dr. Nam-Goo Kang, and Dr. Kunlun Hong (ORNL) for all- sided help and sharing their knowledge, experience and insightful perspective, not only as friends but also as mentors through many difficult times. Throughout these five years’ graduate research and studies, it is my great fortune to have worked with and learned from many smart, kind, helpful, and iii selfless polymer scientists and engineers including: From ORNL: Dr. Panchao Yin for guidance on DLS, SAXS, self-assembly and solution characterizations; Dr. Yangyang Wang and Dr. Shiwang Cheng for mechanical tests, rheology and polymer physics; Dr. Jiahua Zhu for SAXS and TEM. From UT: Dr. Carlos Steren for guidance on theories and experiments of NMR; Dr. John Dunlap for AFM; Dr. Weiyu Wang for kind suggestions, experimental skills, and DMA; Tom Malmgren for GPC, Ms. Ting Wu from Dr. Binhu’s lab for spin coating techniques. I would also like to thank Dr. Mi Zhou (Zhejiang University of Technology, China) and Dr. Chunhui Bao (Solvay USA Inc) for their guidance on living radical polymerization; Dr. Xiaojun Wang (Novus International) for his sharing with rich research experience. I am also lucky to work with many lively and aspirant current and ex- group members in Mays’ group including: Dr. Kostas Mischronis, Dr. Beomgoo Kang, Dr. Priyank Shah, Dr. Andrew Goodwin, Dr. Sachin Bobade, Dr. Vikram Srivastava, Dr. Christopher Hurley, Hongbo Feng, Xinyi Lu, Huiqun Wang, and Benjamin Ripy. Finally, I want to express my great love and appreciation to my family: Thank my wife Yuecheng Fang for tireless support and encouragement, thank you for constituting a happy family with me and bringing me a cute baby! Thank my parents, Zhonghai Lu and Jinmei Huang, and parents in law, Xuehong fang and Xiaoping Tian for your trust and great concern, thank you for taking care of my baby and making the strong back for me! Finally, thank my little baby, Daniel iv Muyang Lu to give me the chance to be your father, thank you for all the laugh and precious moments you have brought to my life! Thus I exclusively dedicate this dissertation to my family, especially my little baby! v ABSTRACT Thermoplastic elastomers (TPEs) have been widely studied because of their recyclability, good processability, low production cost and distinct performance. Compared to the widely-used styrenic TPEs, acrylate based TPEs have potential advantages including exceptional chemical, heat, oxygen and UV resistance, optical transparence, and oil resistance. However, their high entanglement molecular weight lead to “disappointing” mechanical performance as compared to styrenic TPEs. The work described in this dissertation is aimed at employing various approaches to develop the all acrylic based thermoplastic elastomers with improved mechanical performance. The first part of this work focuses on the introduction of acrylic polymers with high glass transition temperatures. Poly(1-adamantyl acrylate) (PAdA) was studied including the anionic polymerization, molecular information, thermal properties, unperturbed chain dimensions and chain flexibility. The homopolymers exhibit a high glass transition temperature (133 oC) and decomposition temperature (376 oC). The polymer chain exhibits a comparable persistence length, diameter per bead, and characteristic ratio to those of poly(methyl methacrylate) and polystyrene. The outstanding properties of PAdA were utilized by the cooperation with poly(tetrahydrofurfuryl acrylate) (PTHFA) to make the PAdA-b-PTHF-b-PAdA (ATA) triblock copolymers. The resulting polymer showed distinct microphase separation behaviors and an upper service temperature at 123 vi oC, which is higher than that of both conventional styrenic TPEs and acrylic TPEs. The ATA triblock copolymers exhibited mechanical strength and elongation higher than those of commercial all acrylic TPEs. The second part involves the synthesis of poly(butyl acrylate)-g-poly(methyl methacrylate) (PBA-g-PMMA) graft copolymers. Secondary-butyl lithium/N- isopropyl-4-vinylbenzylamine (sec-BuLi/PVBA) initiation system was used to synthesize the PMMA macromonomer by anionic polymerization. By the combination of enhanced molecular weight and complex architecture, the resulting polymer showed exceptional microphase separation behavior, extraordinary mechanical strength and superelastomer characteristics with greatly improved elongation and exceptional recovery behavior. In the final chapter, other approaches to improve the mechanical properties of all acrylic based TPEs are discussed and prospected, including the introduction of extra driving forces, and the possible combination routes of all the approaches attempted. In addition, the great potential of PVBA to build complex architectures is proposed, including triarm stars, multigraft copolymers with tetrafuntional branch points, four arm stars and H-shaped copolymers. vii TABLE OF CONTENTS Chapter 1 Introduction to All Acrylic Based Thermoplastic Elastomers ................. 1 1.1 Thermoplastic Elastomers ........................................................................... 2 1.1.1 Advantages and Disadvantages of TPEs .............................................. 2 1.1.2 Classification of TPEs ........................................................................... 3 1.2 Styrenic Block Copolymers (SBCs) Thermoplastic Elastomers ................... 5 1.2.1 Mechanism of Function of TPEs ........................................................... 5 1.2.2 Styrenic Thermoplastic Elastomers (SBCs) .......................................... 8 1.3 All Acrylic Based TPEs ................................................................................ 9 1.3.1 Industrial Applications of Acrylic based TPEs. .................................... 11 1.3.2 Entanglement Molecular Weight (Me) ................................................. 12 1.3.3 Synthesis and Properties of PMMA-b-PBA-b-PMMA Triblock Copolymer TPEs ............................................................................................................ 18 1.4 Approaches to Improve the Performance of TPEs .................................... 24 1.4.1 Compounding ..................................................................................... 24 1.4.2 Glass Transition Temperature ............................................................ 26 1.4.3 Complex Architectures .......................................................................
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