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研究生： 周妤庭
Chou, Yu-Ting
論文名稱： 探討在深共熔溶劑中以可見藍光引發之可逆加成斷裂鏈轉移聚合對超高分子量聚甲基丙烯酸甲酯的高效聚合行為
Efficient Synthesis of Ultrahigh Molecular Weight PMMA via Visible Blue Light-Induced RAFT Polymerization Mediated by Deep Eutectic Solvent
指導教授： 游聲盛
Yu, Sheng-sheng
學位類別： 碩士
Master
系所名稱： 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年： 2023
畢業學年度： 111
語文別： 英文
論文頁數： 115
中文關鍵詞： 深共熔溶劑 、超高分子量 、甲基丙烯酸甲酯 、光引發之可逆加成斷裂鏈轉移聚合
外文關鍵詞： ultrahigh molecular weight, methyl methacrylate, photoinduced RAFT polymerization, deep eutectic solvent
相關次數： 點閱：38  下載：1 
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    • 本研究主要聚焦於在深共熔溶劑(deep eutectic solvent, DES)中之超高分子量(ultrahigh molecular weight, UHMW)聚甲基丙烯酸甲酯(poly(methyl methacrylate, PMMA))的高效聚合行為，並透過可見藍光引發可逆加成斷裂鏈轉移(reversible addition-fragmentation chain transfer, RAFT)聚合以達到控制分子量成長及分布的效果。與二甲基亞碸 (Dimethyl sulfoxide, DMSO)相比，UHMW PMMA在DES系統中的聚合速率及控制行為都更有效地提升。我們採用了多種聚合條件，包括不同溫度、光強度、鏈轉移劑(chain transfer agent, CTA)濃度和光誘導RAFT機制來探討各種變數對於反應的動力學影響。在其中發現了基於高分子量及高系統黏度所引發的凝膠效應，其進一步提升了反應速率，並在光誘導電子轉移(photoinduced electron/energy transfer-RAFT, PET-RAFT)反應中更為明顯。除此之外，若想成功控制聚合出UHMW PMMA，適當的光強、溫度及溶劑的選擇是至關重要的。而由於UHMW PMMA中的分子鏈糾纏強烈，其機械性質也呈現出比起低分子量PMMA更高的強度。簡而言之，本研究在相對較短的時間內於DES中以可見藍光引發RAFT聚合出具有控制行為的UHMW PMMA。

    This work focuses on the synthesis of ultrahigh molecular weight (UHMW) poly(methyl methacrylate) (PMMA) through visible blue light-induced reversible addition-fragmentation chain transfer (RAFT) polymerization in a deep eutectic solvent (DES) composed of tetrabutylammonium chloride (TBACl) and ethylene glycol (EG). Compared to dimethyl sulfoxide (DMSO), the DES system exhibited an enhanced polymerization rate and control behavior. Various polymerization conditions, such as temperature, light intensity, chain transfer agent (CTA) concentration, and photoinduced RAFT (photo-RAFT) mechanisms, were investigated to study the kinetics. Surprisingly, the presence of a gel effect, attributed to high molar mass and high viscosity, resulted in an improved polymerization rate and more pronounced effects in the photoinduced electron/energy transfer-RAFT (PET-RAFT) compared to the photoiniferter-RAFT (PI-RAFT) system. To achieve a well-defined UHMW PMMA, optimal conditions, such as appropriate light intensity, temperature, and solvent selection, were crucial. Using the PET-RAFT system in DES under 0.42 mW/cm2 blue light intensity at 30 ℃, well-defined UHMW PMMA was successfully synthesized within 4 hours. Additionally, the significant entanglements in the UHMW PMMA gel demonstrated enhanced mechanical properties compared to PMMA with lower molar masses. In short, this work presents an unprecedented rapid synthesis of well-defined UHMW PMMA through photo-RAFT polymerization in a DES system.

    ABSTRACT I 摘要 III 致謝 V LISTS OF CONTENTS VI LISTS OF FIGURES IX LISTS OF TABLES XVIII CHAPTER 1. INTRODUCTION 1 1.1 REVERSIBLE-DEACTIVATION RADICAL POLYMERIZATION 1 1.1.1 INTRODUCTION OF REVERSIBLE-DEACTIVATION RADICAL POLYMERIZATION 1 1.1.2 COMMON STRATEGIES OF RDRP 3 1.1.3 APPLICATION OF RDRP 5 1.2 RAFT POLYMERIZATION 8 1.2.1 MECHANISM OF GENERAL RAFT POLYMERIZATION 8 1.2.2 KINETIC OF GENERAL RAFT POLYMERIZATION 11 1.2.3 SELECTION OF CHAIN TRANSFER AGENT 13 1.2.4 PHOTOINDUCED RAFT POLYMERIZATION 17 1.3 DEEP EUTECTIC SOLVENT (DES) 21 1.3.1 INTRODUCTION OF DES 21 1.3.2 ADVANTAGES OF DES 23 1.3.3 RDRP WITH DES 24 1.4 ULTRAHIGH MOLECULAR WEIGHT POLYMER (UHMW) 26 1.4.1 INTRODUCTION OF UHMW 26 1.4.2 UHMW POLYMERS BY RDRP 28 1.4.3 SOME EXAMPLES OF UHMW POLYMERS BY PHOTO-RAFT 30 1.4.4 CHALLENGES AND PROSPECTS 34 1.5 OBJECTIVE 36 CHAPTER 2. MATERIALS AND METHODS 38 2.1 MATERIALS 38 2.2 INSTRUMENTS 39 2.3 GENERAL PI-RAFT POLYMERIZATION PROCEDURES 42 2.4 GENERAL PET-RAFT POLYMERIZATION PROCEDURES 42 2.5 IN SITU CHAIN EXTENSION USING A MACRO-CTA 44 2.6 MEASUREMENT OF MONOMER CONVERSION 44 CHAPTER 3. KINETICS OF UHMW PMMA WITH CTA-1 IN DES 46 3.1 PI-RAFT 46 3.2 PET-RAFT 68 CHAPTER 4. KINETICS OF UHMW PMMA WITH CTA-2 IN DES 72 4.1 PI-RAFT 72 4.2 PET-RAFT 73 CHAPTER 5. OXYGEN TOLERANCE 86 CHAPTER 6. APPLICATION 91 CHAPTER 7. CONCLUSION 99 REFERENCE 101

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