- 學位論文
修飾矽膠之擴散反射式紅外光表面光譜研究
Diffuse Reflectance Infrared Transform Spectroscopy(DRIFTS) Study of Modified Silica Gel Surface
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摘要
中文摘要 本研究以矽膠為基質，研製聚(2-甲基丙烯四級鏻鹽)的陰離子交換劑，以擴散反射紅外光譜DRIFTS (Diffuse Reflectance Infrared Fourier Transform Spectroscopy)鑑定矽膠表面特殊官能基振動吸收光譜，如：Si-O-Si、C=C、Si-C、-NH2，進而建立迅速且有高度再現性的定量分析法。 本研究探討改變矽膠粒徑大小對光譜的影響，發現粒徑越大，光譜精細結構(fine structure)不易見，而且無法獲致獨立吸收峰；小粒徑10mm矽膠做光譜分析為最佳，能獲得有效定性定量資訊。相較於穿透式紅外光譜，DRIFT光譜可明顯觀察矽膠表面性質。矽膠基質與KBr經由不同百分比例混合，光譜能獲得高定量線性結果。本研究法解析度設定以2cm-1獲得的光譜，最有利於定量分析。研究發現矽膠表面羥基與修飾劑反應時，於高濃度修飾劑下，修飾鍵結量與修飾劑成正比；定量修飾劑下亦隨反應溫度而成正比修飾反應。對反應時間作圖，發現初始時間，修飾反應速率明顯較快。矽烷耦合劑的聚合可與修飾矽膠的光譜進行比對，可判斷不同的官能基環境。在修飾矽膠表面做長鏈的聚合反應，光譜上觀察到明顯消失的吸收峰可做為聚合反應的證明。
並列摘要
Abstract In this study, DRIFT (Diffuse Reflectance Infrared Fourier Transform Spectroscopy) was applied on copolymerized silica-based ion-exchanger containing quaternary phosophonium salts. The rapid, high repeatable qualitative and quantitative analysis model was constructed to explain the surface spectra. For silica gel samples, finer particle size caused less severe spectral distortion and more effective analyzing results. Comparing with the conventional transmittance spectra, more accurate surface quantitative characters can be obtained by DRIFT method. By pretreating silica gel with different amount of KBr, the exact value for absorption yielded an excellent linear correlation between Kubelka-Munk function and the sample concentration. The high-resolution setting in DRIFTS was attributed to these serial spectra. Quantitative measuring the peak intensities, it was proportioned to the different reaction temperatures and various amount of coupling agents modified on silica gel. From the spectra of poly-coupling agents, peak absorption and shifts can be observed from force field effect. The kinetic results showed that the modified reactions were faster at initial time and assumed first order reaction.
參考文獻
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