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    Please use this identifier to cite or link to this item: http://ir.lib.ncu.edu.tw/handle/987654321/6454

    Title: 具水熱穩定乙烷基官能基與磺酸官能基之中孔洞材料 SBA-1 的合成與鑑定;Synthesis and Characterization of Hydrothermally Mesoporous Stable Silicas SBA-1 Functionalized with Ethylane-bridge and Sulfonic Acid Groups
    Authors: 鄭光良;Guang-Liang Jheng
    Contributors: 化學研究所
    Keywords: 水熱穩定;乙烷;硫基;Hydrothermally;Sulfonic Acid;Ethylane-bridge
    Date: 2008-06-25
    Issue Date: 2009-09-22 10:19:48 (UTC+8)
    Publisher: 國立中央大學圖書館
    Abstract: 本篇研究主要為合成具高水熱穩定性之中孔洞分子篩,使用 BTEE (1,2-Bis(triethoxysilyl)ethane)及TEOS (Tetraethyl orthosilicate) 為共同矽源,以 C16TEABr (Cetyltriethylammonium bromide) 作為模板試劑,在酸性條件下直接合成含有乙烷有機官能基的 cubic (Pm3n) 中孔洞材料。經由粉末 X-ray 繞射、等溫氮氣吸脫附 (BET)、29Si 及 13C MAS-NMR、掃描電子顯微鏡 (SEM)、熱重分析儀 (TGA) 做鑑定。將模板移除後的樣品在沸水下迴流,藉此與純的 SBA-1 比較其水熱穩定性。然而,結果顯現出在混合矽源下合成其結構在經五天水煮後還保持部分的結構特性,相較於水煮一天結構就崩塌的純 SBA-1,此共同矽源明顯改善其水熱穩定性。 在另一部份則是使用TEOS與 MPTMS ((3-Mercaptopropyl)- trimethoxy silane) 為共同矽源,以 C16TEABr作為模板試劑,在酸性條件下以雙氧水當作氧化劑,利用直接合成將硫基官能基轉變成含有磺酸基有機官能基的中孔洞材料。然而,適量的雙氧水可促進其磺酸基的生成。藉由粉末 X-ray 繞射、等溫氮氣吸脫附 (BET)、29Si 及 13C MAS-NMR 鑑定之。 然而,重金屬的檢測及定量在區域的環境監控、污水管理,甚至生物演變在近年來雖然利用很多不同儀器的技術進行檢測,但在此將利用硫基對不同金屬的吸附性,以固態核磁共振儀鑑定之。除此之外,也發現也許可在不需要雙氧水的形況下,利用銅金屬將硫基轉換為磺酸基。 Hydrothermally stable periodic mesoporous organosilicas with cubic Pm3n frame structures were synthesized by using tetraethoxysilane (TEOS) and 1,2-bis(triethoxysilyl)ethane (BTEE) as silica source and cetyltriethylammonium bromide (CTEABr) as surfactant under acidic conditions.The synthesized materials were characterized by PXRD, SEM, N2 adsorption-desorption, 29Si MAS NMR, 13C CP MAS NMR and TG-DTA techniques. Hydrothermal stability of the synthesized material was evaluated by refluxing the sample under boiling water for various time periods and the results were compared with pure mesoporous silica material (Si-SBA-1). The results showed that the hybrid material is stable up to 5 days in boiling water with a slight decrease in structural properties, whereas Si-SBA-1 structure was collapsed after refluxing for one day. The improved hydrothermal stability of hybrid material is related to more hydrophobic environment induced inside the pore channels due to the presence of integrating ethane groups in the walls of the channels. On the synthesis of organosulfonic acid-functionalized mesoporous in a one-step approach of co-condensing inorganic–organic reagents in the presence of cetyltriethylammonium bromide (CTEABr) surfactant with in situ oxidation of the thiol groups to the sulfonic acid groups.It is a one-step condensation of tetramethoxysilane (TEOS) and 3-mercaptopropyltrimethoxysilane (MPTMS) in highly acidic medium. During the condensation process, the in situ oxidation of thiol (-SH) group to sulfonic acid (-SO3H) group was facilitated by hydrogen peroxide (30 wt % H2O2). Adsorption and structural properties of the aforementioned PMOs have been studied by nitrogen adsorption and X-ray diffraction, whereas their framework chemistry was quantitatively analyzed by solid-state 13C and 29Si MAS NMR. The detection and quantification of heavy metal ions are important in plethora of areas such as environmental monitoring, waste water management, developmental biology, and clinical toxicology. A number of techniques have been developed over the years for heavy metal ion analysis. Now, we used solid-state 13C CPMAS (cross polarization magic angle spinning) NMR spectroscopy as a characterization tools to obtain spectroscopic evidence for the heavy metal adsorption. By the way, the conversion of thiol-functionalized SBA-1 to disulfide-functionalized SBA-1 using Cu2+ without hydrogen peroxide was achieved.
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