Synthesis and characterization of organofunctionalized MCM-41 by the original stepped templated sol-gel technology.
Synthesis and characterization of organofunctionalized MCM-41 by the original stepped templated sol-gel technology.
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DOI：
10.1021/jp0515885
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发表时间：
2005-12
期刊：
影响因子：
--
通讯作者：
Cui Zhang;Wei Zhou;Shuangxi Liu
中科院分区：
文献类型：
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作者：
Cui Zhang;Wei Zhou;Shuangxi Liu
采用接枝法、传统的模板溶胶-凝胶技术和原有的阶梯式模板溶胶-凝胶技术，成功地合成了四种有机功能化的介孔硅酸盐MCM-41(以下简称R-MCM-41)。采用粉末X射线衍射仪、29Si和13C MAS核磁共振仪、氮气等温吸附-脱附分析、原位漂移红外光谱和热重分析等手段对所制备的无机-有机杂化材料进行了详细的表征。通过一系列的研究和比较，证明了本文所介绍的具有优势的阶梯模板化溶胶-凝胶技术是一种引人注目的方法，它结合了目前的接枝法和传统的水热共缩合合成方法的优良性能，从而在热力学上得到了牢固的固定，并在MCM-41载体上获得了较大的有机官能团含量。新的合成策略也明显缩短了具有规则特殊结构的有机功能化MCM-41的结晶时间。
Four types of organofunctionalized (by phenyl, 3-aminopropyl, 3-chloropropyl, and N-aminoethylaminopropyl, respectively) mesoporous silicates MCM-41 (hereafter R-MCM-41) have been successfully synthesized via the grafting method, the conventional templated sol-gel technology, and the original stepped templated sol-gel technology. The prepared inorganic-organic hybrid materials were characterized in detail by powder X-ray diffraction (XRD), 29Si and 13C MAS NMR spectrometry, isothermal nitrogen adsorption-desorption analysis, FT-IR spectrometry including in situ drift technique, and thermogravimetric analysis (TGA). Through a series of investigations and comparisons, the advantageous stepped templated sol-gel technology introduced in this paper is demonstrated to be a remarkable approach that gathers the superior properties of the current grafting method and the conventional hydrothermal co-condensation synthesis, yielding as a consequence both thermodynamically firm fixation and relatively large content of organic functional species on the MCM-41 support. The novel synthetic strategy also evidently shortens the crystallization time for the organofunctionalized MCM-41 with regular specific structure.