六方中孔硅分子筛的合成与表征  

Synthesis and characterization of hexagonal mesoporous silica molecular sieve

作　　者：陈君华[1,2] 王飞[1] 丁志杰[2] 陈忠平[2] 张平[2] 吴俊[2] 伏再辉[3] 

机构地区：[1]南京林业大学化学工程学院,江苏南京210037 [2]安徽科技学院化学系,安徽凤阳233100 [3]湖南师范大学化学化工学院,湖南长沙410081

出　　处：《南京林业大学学报（自然科学版）》2008年第6期13-18,共6页Journal of Nanjing Forestry University：Natural Sciences Edition

基　　金：国家自然科学基金资助项目(29773013);安徽省高校自然科学基金资助项目(2001Kj059);安徽科技学院重点学科基金(YZD2004-21)

摘　　要：以十二胺(DDA)为模板剂,采用溶胶凝胶法室温下合成了六方中孔硅分子筛原粉(HMS-DDA),分析了焙烧法与有机溶剂抽提法,特别是溶剂、抽提时间等因素对合成六方中孔硅分子筛(HMS)中孔结构的影响,利用XRD、FT-IR、HRTEM、XPS及TG-DTA等分析手段对其进行了表征。结果表明:焙烧温度、抽提溶剂及抽提时间对HMS-DDA的脱模及HMS材料的晶格重组、结构有序度及骨架稳定性有显著影响,其中以丙酮为溶剂抽提样品9 h,材料具有良好的中孔有序度和最稳定的中孔结构。同时证实了在HMS-DDA合成过程中,荷电为零的无机硅物种(I°)与中性伯胺分子(S°)之间依靠非静电力协同完成S°I°分子自组装。Using dodecyl amine （DDA） as template agent, hexagonal mesoporous silica molecular sieve containing DDA （HMS-DDA） was successfully synthesized by sol-gel method at room temperature. Then the effects of calcination and solvent-extraction, especially the solvents and extraction time on the structure of HMS in the course of extracting or calcining DDA from HMS-DDA were investigated. Characterization of the mesoporous silica materials was carried out by means of FT - IR, XRD, HRTEM, XPS and TG - DTA. The experimental results showed that the calcination temperature, extraction time and solvents had great effects on the crystal lattice recombination, mesoporous degree and framework stability of HMS. The HMS material had higher mesoporous ordered degree and the most stable mesoporous structure when HMS - DDA was extracted with acetone for 9 hours. In addition, the S° I° molecule self-assembly mechanism of HMS - DDA was confirmed.

关 键 词：六方中孔硅 合成 抽提 表征 

分 类 号：O643.3[理学—物理化学]