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Title page
Abstract
국문요약
Contents
1. INTRODUCTION 16
2. THEORITICAL BACKGROUND 22
2.1. Free-radical Polymerization 22
2.1.1 Introduction 22
2.1.2 Chain Polymerization 22
2.1.3 Chemistry of Free-radical Polymerization 24
2.1.3.1 Initiation 25
2.1.3.2 Propagation 29
2.1.3.3 Termination 30
2.1.3.4 Chain transfer 31
2.1.3.5 Inhibition and retardation 35
2.1.4 Stereochemistry of Polymerization 36
2.1.4.1 Tacticity 36
2.1.4.2 Polymerization of 1,3-dienes 38
2.2 Heterogeneous System 40
2.2.1 Heterogeneous Polymerization techniques 40
2.2.1.1 Basic Principles 41
2.2.1.2 Suspension polymerization 44
2.2.1.3 Emulsion polymerization 46
2.2.1.4 Mini-and Microemulsion polymerization 47
2.2.1.5 Dispersion polymerization 50
2.2.1.6 Precipitation Polymerization 50
2.2.2 Mechanism of Dispersion polymerization 51
2.2.2.1 Scope and definition 51
2.2.2.2 Essential formulation component 52
2.2.2.3 A Typical Formulation and Process 57
2.2.2.4 Dispersion Properties 58
2.2.2.5 Copolymerization and crosslinking 68
2.2.2.6 Mechanism of Particle Formation 69
2.2.2.7 Kinetics 73
2.2.2.8 Applications 74
3. EXPERIMENTAL 76
3.1 PART A : Optimum Conditions for Preparing Micron-sized PMMA Beads in the Dispersion Polymerization using PVA 76
3.1.1 Materials 76
3.1.2 Polymerization 77
3.2. PART B : Effect of PVA in Dispersion Polymerization of MMA 78
3.2.1 Materials 78
3.2.2 Polymerization 79
3.2.3. Analysis 80
4. RESULTS AND DISCUSSION 82
4.1 PART A : Optimum Conditions for Preparing Micron-sized PMMA Beads in the Dispersion Polymerization using PVA 82
4.2 PART B : Effect of PVA in Dispersion Polymerization of MMA 97
5. CONCLUSIONS 114
5.1 PART A : Optimum Conditions for Preparing Micron-sized PMMA Beads in the Dispersion Polymerization using PVA 114
5.2 PART B : Effect of PVA in Dispersion Polymerization of MMA 115
6. REFERENCES 116
Table 2-I. Some dispersion polymerization systems 56
Table 2-II. Recipe for preparing PMMA in the Dispersion polymerization 58
Table 4-A-I. Effect of MeOH/water mixture composition on conversion (%), weight-average particle diameter (Dw), coefficient variation (Cv), weight average molecular weight 88
Table 4-A-II. Optimum conditions for obtaining micron-sized monodisperse particles in the dispersion polymerization in this study 89
Table 4-B-I. Recipe Used in Dispersion polymerization 104
Figure 2-1. The range of particle size covered by each technique 44
Figure 2-2. Schematic of particle growth in dispersion polymerization 70
Figure 4-A-1. SEM photographs of PMMA microspheres prepared at different stabilizer at 70 C in a water/MeOH (50/100, g/g) mixture ; (a) PVA 15wt%, (b) PVP 15wt% 90
Figure 4-A-2. Comparison of the FTIR spectra of the synthesized PMMA particles using 15 wt% PVA and PVP. (a) pure PVA, (b) PMMA with PVA, (c) PVP, and (d) PMMA with PVP 91
Figure 4-A-3. SEM photographs of PMMA microspheres prepared at MeOH(g)/water(g) mixture of (a) 120/30, (b) 110/40, (c) 100/50, (d) 90/60, and (e) 80/70 92
Figure 4-A-4. Effect of solvents on conversion and particles in the dispersion polymerization in methanol (100g)/water (50g) mixture at 70 C . (a) MeOH, (b) EtOH, (c) acetone 93
Figure 4-A-5. Effect on temperature on conversion and particles in the dispersion polymerization in a MeOH/water (100/50, g/g) m 94
Figure 4-A-6. H-NMR spectrum of the obtained PMMA 95
Figure 4-A-7. DSC data with polymerization time 96
Figure 4-B-1. H-NMR spectra of the polymerized PMMA particles using PVA 105
Figure 4-B-2. SEM micrographs of PMMA microspheres prepared by dispersion polymerization in a methanol (100g)/water (50g) mixtures at 70 C for (a) 0.5hr, (b) 1hr, (c) 2 hr, 106
Figure 4-B-3. Effect of polymerization time with average diameter (Solid Symbol) and Cv (Open Symbol) in the dispersion polymerization in methanol (100g)/water (50g) mixtures with 15 wt% PVA and 1 wt% AIBN at 70 C. 107
Figure 4-B-4. Effect of polymerization time on the molecular weight, conversion, and PDI using MeOH/water (100/50g) mixture with 15 wt% PVA and 1 wt% AIBN at 70 C. 108
Figure 4-B-5. Comparison of the FT-IR spectra of the synthesized PMMA particles by (a) soap-free emulsion polymerization, and dispersion polymerization using (b) PVP and (c) 109
Figure 4-B-6. Comparison of the FT-IR spectra of (a) pure PVA, (b) PMMA particles prepared using PVA, and (c) filtered PMMA (synthesized using PVA) solution after dissolved in 110
Figure 4-B-7. SEM photographs of PMMA microspheres prepared at initiator concentrations of (a) 0.5% w/w, (b) 1% w/w, (c) 2% w/w, and (d) 4% w/w relative to monomer. 111
Figure 4-B-8. SEM photographs of PMMA microspheres prepared at PVA concentrations as stabilizer of (a) 10% w/w (a), (b) 15% w/w (b), (c) 20% w/w (c), and (d) 25% w/w 112
Figure 4-B-9. SEM photographs of PMMA microspheres prepared at monomer concentrations of 3.3% w/w (a), 6.6% w/w (b), 10% w/w (c), and 13% w/w (d) relative to medium 113
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