凝胶制备耐燃之聚甲基丙烯酸酯复合材料-国立高雄应用科技大学化学.DOC

中文摘要 本研究係以溶膠凝膠法(sol-gel process)製備耐燃之甲基丙烯酸酯(poly(methyl methacrylate)；PMMA)複合材料。實驗中，以丙烯酸類化合物取代溶膠凝膠法中之溶劑，作為反應型溶劑並作為分散劑以均勻分散溶膠凝膠溶液中之奈米無機顆粒，以完成無溶劑之溶膠凝膠反應。 在分散劑中，將甲基三甲基矽烷(Methyl trimethoxy silane；MTOS)及三甲基磷酸酯(Trimethyl phosphate；TMP)分別經水解(hydrolysis)、縮合(condensation)後，可各自製得無機奈米顆粒(氧化矽、氧化磷)之溶膠凝膠溶液。再將所製得之無機奈米顆粒添加進PMMA/MMA漿液中，經澆注及熱處理後可製得複合材料。 其間，利用奈米粒徑分析儀(particle size analyzer；PSA)分析溶膠凝膠溶液中粒徑與分佈與其經時變化情形、以電子顯微鏡(scanning electron microscopy；SEM)觀察無基奈米顆粒在PMMA基材中之粒徑大小與分佈情形、以紫外光譜儀(UV/Vis spectroscopy；UV/Vis)觀察各樣品在特定波長之穿透度、以熱重分析儀(thermogravimetric analyzer；TGA)及微差掃描熱分析儀(Modulated Differential Scanning Calorimetry；MDSC)來量測複合材料之熱穩定性與Tg點(玻璃轉化溫度)，最後再以極限氧指數 (limited oxygen index；LOI)測試儀進行各樣品之難燃性質測試。 實驗結果顯示：依本研究所提之無溶劑溶膠-凝膠法可製得高分散性之奈米顆粒分散液，而應用傳統的澆注方式與熱聚合法可製得PMMA/奈米顆粒複合材料。所製得之複合材料具有高透明性，且其LOI值均有所提升：SiOx-MAA系統之LOI值平均為27、SiOx-HEMA系統之LOI值平均為26、PxOy-MAA系統之LOI值平均為29，而PxOy-HEMA其平均值為28。相較於PMMA之LOI值18，各系統之LOI值均有顯著提升，可說明本研究所得之PMMA複合材料具有耐燃性。 英文摘要 The poly(methyl methacrylate) (PMMA) composites having flame-retardant and high transparency were prepared by a solvent-free sol-gel process. Acrylic compounds were selected as dispersion agents to homogeneously suspend the nano-particles, being as the non-volatile solvent to replace a volatile one regularly used for a sol-gel process. The inorganic nano-particles were respectively formed by using the methyl trimethoxy silane (MTOS) and trimethyl phosphate (TMP) as the precursors, which underwent hydrolysis and condensation in the dispersant at room temperature. Accordingly, the SiOx and PxOy nano-particles were obtained as dispersion, respectively. The PMMA composites were then prepared by a traditional casting and thermal polymerization process using polymer/monomer syrup mixed with the dispersion. The particle size and distribution of the nano-particles as-prepared and after time aging were measured by particle size analyzer (PSA) and scanning electron microscopy (SEM). Thermogravity analyzer (TGA) and modulated differential scanning calorimetry