臺灣博碩士論文加值系統

聚對苯二甲酸碳酸丁二酯(Poly(butylene carbonate-co-terephthalate)，PBCT)屬於半結晶聚合物且特性類似於低密度聚乙烯，為一新型之生物可分解高分子，本研究透過兩階段製程將碳酸二甲酯、對苯二甲酸二甲酯以及1, 4丁二醇合成出三種比例PBCT，分別為PBCT85、PBCT50以及PBCT25，並利用共沉澱法製備辛酸與硬脂酸改質層狀雙氫氧化物(OA-LDH與SA-LDH)，以擴大層間距及提升無機物與高分子之相容性，藉由XRD鑑定其層間距由原本之0.84 nm分別增加至2.21 nm 與3.16 nm。由FTIR圖譜觀察到改質後LDH增加了波數2925 cm-1、2854 cm-1以及1558 cm-1，同時也發現1384 cm-1之消失，表示改質劑烷基鏈段成功插層進入LDH層間。經由溶劑插層法製備1、3及5 wt%之PBCT/OA-LDH與SA-LDH奈米複合材料，由XRD圖譜及TEM影像顯示出改質LDH以少部分插層與大部分剝離型態分散在PBCT基材中，而添加改質LDH並不會改變PBCT之結構。由TGA分析PBCT及其奈米複合材料之熱穩定性，發現所有材料皆出現PBC獨特的裂解機制，在升溫過程BC單元鏈段發生分子內酯交換進而造成兩階段重量損失，而其中添加OA-LDH及SA-LDH皆導致PBCT之熱穩定性下降，由於鎂鋁金屬具有催化裂解效果。藉由DMA分析探討其機械性質，結果顯示添加OA-LDH及SA-LDH皆提升了PBCT之剛性，且隨著含量比例增加而隨之上升，由於剛性LDH板層之增強效應。透過SAXS分析以了解PBCT及其奈米複合材料之微結構，結果顯示添加OA-LDH及SA-LDH造成結晶板層變薄，由於PBCT分子鏈排列堆疊時受到改質LDH阻礙而無法形成完整結晶層，導致整體結晶情形下降。利用假單胞菌脂肪酶酵素進行生物降解測試，其結果顯示出材料之結晶度、高分子組成比例與表面親疏水對PBCT及其奈米複合材料之降解速率造成了顯著之影響。也進行了細胞存活率測試以探討其生物相容性，結果可知PBCT85及其奈米複合材料相對較適合細胞生長，而OA-LDH及SA-LDH對細胞存活率影響不大。

致謝 i
摘要 ii
Abstract iii
目錄 v
表目錄 ix
圖目錄 xii
第一章 續論及簡介 1
1.1 前言 1
1.2 生物可分解高分子 4
1.3 有機/無機奈米複合材料 6
第二章 文獻回顧及基礎理論 8
2.1 聚對苯二甲酸碳酸丁二酯共聚合物(poly(butylene carbonate-co-terephthalate)，PBCT) 8
2.2 層狀雙氫氧化合物(Layered double hydroxide，LDH) 15
2.2.1 層狀雙氫氧化合物(Layer double hydroxide，LDH)之改質 17
2.3 高分子/層狀雙氫氧化合物(LDH)奈米複合材料 20
2.4 高分子小角度X光散射(SAXS) 30
2.5 可分解高分子及其複合材料之生物降解性 33
2.6 細胞存活率測試(MTT) 40
2.7 研究動機與方向 42
第三章 實驗方法與步驟 43
3.1 實驗材料 43
3.2 實驗儀器 45
3.3 實驗架構 47
3.4 實驗方法與步驟 48
3.4.1 聚對苯二甲酸碳酸丁二酯共聚合物之製備 48
3.4.2 鎂鋁層狀雙氫氧化物之製備 49
3.4.3 有機改質鎂鋁層狀雙氫氧化物之製備 49
3.4.4 聚對苯二甲酸碳酸丁二酯共聚合物/有機改質鎂鋁層狀雙氫氧化物之奈米複合材料製備 50
3.4.5 高分子之生物降解實驗 51
3.4.6 高分子之細胞存活率測試 52
3.5 實驗儀器分析 53
3.5.1 超導磁場核磁共振儀(Nuclear Magnetic Resonance，NMR) 53
3.5.2 廣角X光繞射儀(Wide Angle X-Ray Diffraction，WAXD) 53
3.5.3 膠體滲透層析儀 (Gel Permeation Chromatography，GPC) 54
3.5.4 傅立葉轉換紅外線光譜儀 (Fourier Transform Infrared Spectrometer，FTIR) 54
3.5.5 示差掃描式熱分析儀 (Different scanning calorimeter，DSC) 55
3.5.6 熱重分析儀 (Thermogravimetric analysis，TGA) 55
3.5.7 小角度X光散射(Small-Angle X-ray Scattering，SAXS) 55
3.5.8 動態力學分析儀 (Dynamic Mechanical Analysis，DMA) 56
3.5.9 場發射掃描式電子顯微鏡 (Field-emmision Scanning electronic microscopy，FE-SEM) 56
3.5.10 穿透式電子顯微鏡 (Transmission Electron Microscope，TEM) 56
3.5.11 接觸角量測儀 (Contact Angle Meter) 57
第四章 結果與討論 58
4.1 有機改質MgAl-LDH之結構分析 58
4.2 有機改質MgAl-LDH之熱性質分析 64
4.3 聚對苯二甲酸碳酸丁二酯共聚合物PBCT85與其奈米複合材料之特性研究探討 67
4.3.1 聚對苯二甲酸碳酸丁二酯共聚合物PBCT85之組成與結構鑑定 67
4.3.2 PBCT85/OA-LDH奈米複合材料之分散性研究 70
4.3.3 PBCT85/SA-LDH奈米複合材料之分散性研究 72
4.3.4 PBCT85/OA-LDH奈米複合材料之熱穩定性 73
4.3.5 PBCT85/SA-LDH奈米複合材料之熱穩定性 75
4.3.6 PBCT85/OA-LDH奈米複合材料之機械性質 78
4.3.7 PBCT85/SA-LDH奈米複合材料之機械性質 79
4.3.8 PBCT85/OA-LDH奈米複合材料之微結構探討 81
4.3.9 PBCT85/SA-LDH奈米複合材料之微結構探討 85
4.3.10 PBCT85/OA-LDH奈米複合材料之生物降解性 88
4.3.11 PBCT85/SA-LDH奈米複合材料之生物降解性 93
4.4 聚對苯二甲酸碳酸丁二酯共聚合物PBCT50與其奈米複合材料之特性研究探討 98
4.4.1 聚對苯二甲酸碳酸丁二酯共聚合物PBCT50之組成與結構鑑定 98
4.4.2 PBCT50/OA-LDH奈米複合材料之分散性研究 101
4.4.3 PBCT50/SA-LDH奈米複合材料之分散性研究 103
4.4.4 PBCT50/OA-LDH奈米複合材料之熱穩定性 105
4.4.5 PBCT50/SA-LDH奈米複合材料之熱穩定性 107
4.4.6 PBCT50/OA-LDH奈米複合材料之機械性質 110
4.4.7 PBCT50/SA-LDH奈米複合材料之機械性質 112
4.4.8 PBCT50/OA-LDH奈米複合材料之微結構探討 114
4.4.9 PBCT50/SA-LDH奈米複合材料之微結構探討 117
4.4.10 PBCT50/OA-LDH奈米複合材料之生物降解性 120
4.4.11 PBCT50/SA-LDH奈米複合材料之生物降解性 125
4.5 聚對苯二甲酸碳酸丁二酯共聚合物PBCT25與其奈米複合材料之特性研究探討 130
4.5.1 聚對苯二甲酸碳酸丁二酯共聚合物PBCT25之組成與結構鑑定 130
4.5.2 PBCT25/OA-LDH奈米複合材料之分散性研究 133
4.5.3 PBCT25/SA-LDH奈米複合材料之分散性研究 135
4.5.4 PBCT25/OA-LDH奈米複合材料之熱穩定性 137
4.5.5 PBCT25/SA-LDH奈米複合材料之熱穩定性 139
4.5.6 PBCT25/OA-LDH奈米複合材料之機械性質 141
4.5.7 PBCT25/SA-LDH奈米複合材料之機械性質 143
4.5.8 PBCT25/OA-LDH奈米複合材料之微結構探討 145
4.5.9 PBCT25/SA-LDH奈米複合材料之微結構探討 148
4.5.10 PBCT25/m-LDH (OA-LDH、SA-LDH)奈米複合材料之生物降解性 151
4.6 細胞毒性測試(MTT) 156
第五章 結論 158
參考文獻 160

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