具硫基官能基之中孔洞材料 SBA-1 的合成與鑑定;Synthesis and Characterization of Cubic Mesoporous Silicas SBA-1 with Thiol Functionality

Please use this identifier to cite or link to this item: http://ir.lib.ncu.edu.tw/handle/987654321/6205

Title:	具硫基官能基之中孔洞材料 SBA-1 的合成與鑑定;Synthesis and Characterization of Cubic Mesoporous Silicas SBA-1 with Thiol Functionality
Authors:	沈姿誼;Tzu-Yi Shen
Contributors:	化學研究所
Date:	2006-07-05
Issue Date:	2009-09-22 10:15:36 (UTC+8)
Publisher:	國立中央大學圖書館
Abstract:	中文摘要在本篇研究是以MPTMS ((3-Mercaptopropyl)trimethoxysilane) 與TEOS (Tetraethtyl orthosilicate) 為共同矽源，使用 C16TEABr (cetyltriethylammonium bromide) 作為模板試劑，在反應溫度為273 K下直接合成具有硫基官能基的中孔洞材料SBA-1，之後經由HCl / EtOH溶劑做萃取處理，移除模板後，得到的中孔洞材料仍然具有SBA-1的結構存在。研究發現硫基官能基化的中孔洞材料SBA-1，其MPTMS含量可達20%，對於中孔洞立方結構不會造成相轉變或是結構破壞，而其表面積、孔洞體積以及孔洞直徑均會隨MPTMS含量的增加而有遞減的趨勢。藉由改變不同的酸量、不同的水熱時間、不同的攪拌時間以及不同矽源，探討對於合成具有硫醇官能基的SBA-1的影響。在改變不同的酸量的方面，可以觀察到不同的結果，在XRD 的結果中，可發現隨著酸量的增加，可加入在SBA-1中的MPTMS 之含量也隨之增加，而在29Si MAS NMR也觀察到隨著酸量的增加，有助於中孔洞材料SBA-1結構的穩定。在水洗測試也可得知，加入官能基可以有效的改善SBA-1結構不能水洗及不能溶劑萃取的缺點。 Abstract One-step synthesis of well-ordered cubic mesoporous silicas SBA-1 containing simultaneously tetraethoxysilane (TEOS) and 3-mercapto- propyltrimethoxysilane (MPTMS) and has been synthesized by cetyltriethylammonium bromide (CTEABr) under strongly acidic conditions. In order to get optimized the thiol-functionalized mesoporous silicas SBA-1 which has been studied by in a wide range of synthesis conditions. All kinds of results of formating the parameter, including the relative reagent concentration (TEOS/MPTMS ratio), HCl concentration, synthesis temperature, and hydrothermal time. The materials obtained were characterized by a variety of techniques including powder X-ray diffraction (XRD), nitrogen sorption measurements, 13C and 29Si magic angle spinning (MAS), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA). The lower TEOS/MPTMS ratios resulted in materials with higher functional group loadings. The direct synthesis of thiol- functionalized SBA-1 materials, the concentration of MPTMS that can co-condense with TEOS will be up to 20% without observing a significant loss in the structure order and uncontrollable phase transformation of the cubic SBA-1 mesostructure. The HCl concentration of change was found that can determine the stability of thiol-functionalized SBA-1 towards the solvent extraction treatment. The difference in the morphology between pure SBA-1 and thiol- functionalized SBA-1 becase of the incorporated MPTMS can slow down the condensation rate of TEOS.
Appears in Collections:	[Graduate Institute of Chemistry] Electronic Thesis & Dissertation

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