臺灣博碩士論文加值系統

本研究以含有醚鏈段的分枝狀高分子(HBP6)與含有矽氧烷分枝狀高分子(S10)為基礎，改變其聚二甲基矽氧烷(polydimethylsiloxane)與聚醚胺(poly(oxythylene)diamine)莫耳數比例，已知醚鏈段的分枝狀高分子(HBP6)因本身具有增韌性質，而含有矽氧烷分枝狀高分子(S10)則是具有阻燃性質，利用不同的配比，期待獲得具有較佳阻燃及機械性質之材料。研究期間，利用滲透色層分析儀(GPC)測量其分子量，微差掃描熱卡計(DSC)及熱重分析儀(TGA)分析其熱性質，傅立葉轉換紅外線光譜儀(FT-IR)與核磁共振儀(NMR)鑑定其結構，並使用錐-平板式流變探討高分子流變性質之影響，部分含矽氧烷分枝狀高分子其損失模數(G’)對頻率(f)之斜率小於2，有別於一般的線性高分子。藉由塑譜儀以熔融混煉法製備出聚乳酸/含矽氧烷/醚胺分枝狀高分子之複合材料分析阻燃及增韌性。機械性質有明顯改善其增韌拉伸從1.5%上升至32.3%，而耐衝擊從5.5 kJ/m2上升至15.1 kJ/m2 ；其阻燃性最佳LOI值可達31.5%且UL-94為V-0等級。

Blends of the polylactide (PLA) and branched polymer (S series and BD100) were prepared via direct melting compounding by using a brabender. The flame-retardant and thermal properties of the PLA blends were examined by limiting oxygen index (LOI), UL-94, thermogravimetric analysis (TGA), and infrared (IR) thermography analysis. The results showed that the limiting oxygen index (LOI) of the blends can be further raised to 31.5% for the PLA with addition of the polydimethylsiloxane branched polymer, which could also reach V-0 rating under UL-94 test. Furthermore, incorporated the silicon-containing branched polymer into the PLA increased the elongation at break to 32%, and impact strength to 15.1 kJ/m2 from 1.5% and 5.5 kJ/m2 of the neat PLA sample, respectively.

摘要 i
Abstract ii
誌謝 iii
目錄 iv
表目錄 ix
圖目錄 xi
第一章 緒論 1
1-1 前言 1
1-2 研究動機 3
第二章 文獻回顧 4
2-1 聚乳酸 4
2-1.1 聚乳酸之簡介 4
2-1.2 聚乳酸之合成 4
2-2 矽氧烷高分子簡介 6
2-3 分枝狀高分子簡介與特性 7
2-4 高分子混摻原理與加工方式 9
2-5 高分子韌化 10
2-5.1 增韌機制的發展 10
2-5.2 剪切屈服理論 11
2-5.3 屈服與冷拉現象 12
2-6 阻燃劑 17
2-6.1 阻燃劑之種類與發展 17
2-6.2 聚矽氧烷分枝狀高分子之阻燃機制 19
2-7 穩態剪切行為 27
2-8 高分子的剪切稀薄特性 28
2-9 動態流變行為 29
第三章 實驗方法 30
3-1 實驗藥品 30
3-2 實驗儀器 34
3-3 實驗流程 37
3-4 實驗配方與製備 39
3-4.1 分枝狀聚二甲基矽氧烷高分子合成 39
3-4.2 混煉及摻合物之製備方法 41
3-5 實驗方法 42
3-5.1 傅立葉轉換紅外線光譜儀 42
3-5.2 高分子分子量測量 42
3-5.3 核磁共振儀 42
3-5.4 環氧當量滴定 43
3-5.5 熱裂解性質 43
3-5.6 玻璃轉移溫度量測 43
3-5.7 流變性質 44
3-6 阻燃性質測試 45
3-6.1 垂直燃燒檢測(UL-94) 45
3-6.2 限氧指數檢測(Limiting Oxygen Index，LOI) 47
3-6.3 熱重分析儀(Thermogravimetric Analysis, TGA) 49
3-7 材料機械性質(Mechanical Properties) 50
3-7.1 萬能拉力機測試 50
3-7.2 耐衝擊測試(Impact test) 52
3-8 掃描式電子顯微鏡(Scanning Electron Microscope) 52
3-9 紅外線熱像分析(Infrared thermography analysis) 53
第四章 結果與討論:含矽氧烷分枝狀高分子 54
4-1 含矽氧烷分枝狀高分子合成 54
4-2 分枝狀高分子分析 55
4-2.1 分子量測量 55
4-2.2 FT-IR結構分析 55
4-2.3 滴定分析(計算轉化率) 57
4-2.4 核磁共振儀(結構分析) 58
4-3 分枝狀矽氧烷高分子熱性質分析 60
4-3.1 玻璃轉移溫度分析(DSC) 60
4-3.2 熱重分析儀(TGA) 60
4-4 分枝狀矽氧烷高分子之流變性質 62
4-4.1 穩態流變性質 62
4-4.2 動態流變性質 68
第五章 結果與討論:以不同含矽分枝狀高分子/聚乳酸摻合物 73
5-1 聚乳酸摻合物之熱分解性質分析 73
5-2 聚乳酸摻合物之機械性質探討 75
5-2.1 拉伸性質分析 75
5-2.2 耐衝擊分析 77
5-3 SL聚乳酸摻合物之燃燒性質探討 79
5-3.1 垂直燃燒(UL-94)及限氧指數(LOI)檢測分析 79
5-4 聚乳酸摻合物之DSC分析 81
5-4.1 冷卻速率(-5℃/min) 81
5-4.2 快速冷卻 83
5-5 紅外線熱影像分析 86
第六章 結果與討論:以相同含矽分枝狀高分子/聚乳酸摻合物 87
6-1 聚乳酸摻合物之機械性質探討 87
6-1.1 拉伸性質分析 87
6-1.2 耐衝擊分析 88
6-2 聚乳酸摻合物之燃燒性質探討 89
6-2.1 垂直燃燒(UL-94)及限氧指數(LOI)檢測分析 89
6-3 紅外線熱影像分析 90
6-4 聚乳酸摻合物之DSC分析 91
6-4.1 冷卻速率(-5℃/min) 91
6-4.2 快速冷卻 93
第七章 結論 95
圖集 96
References 167
Appendix A 含矽分枝狀高分子其他圖集 177
Appendix B 酸酐型高分子合成 185
B-1 合成相關藥品 185
B-2 反應條件與實驗結果 187
B-2.1 D.E.R. 732系列 187
B-2.2 DMS-E09系列 188
B-2.3 PEGDE系列 188
B-3 相關數據 189
B-3.1 GPC圖 189
B-3.2 DSC圖 190
B-3.3 IR圖 191
B-3.4 流變圖 191
B-3.5 機械性質測驗 197
B-3.6 13C NMR 圖 198
符號彙編 199

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