Zhang Cui, Zhou Wei, Liu Shuangxi
Institute of New Catalytic Materials Science, College of Chemistry, Nankai University, Tianjin 300071, People's Republic of China.
J Phys Chem B. 2005 Dec 29;109(51):24319-25. doi: 10.1021/jp0515885.
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.
分别通过接枝法、传统模板溶胶 - 凝胶技术和原始分步模板溶胶 - 凝胶技术成功合成了四种有机官能化的（分别由苯基、3 - 氨丙基、3 - 氯丙基和N - 氨乙基氨丙基官能化）介孔硅酸盐MCM - 41（以下简称R - MCM - 41）。通过粉末X射线衍射（XRD）、29Si和13C MAS NMR光谱、等温氮吸附 - 脱附分析、包括原位漂移技术的傅里叶变换红外光谱（FT - IR）以及热重分析（TGA）对制备的无机 - 有机杂化材料进行了详细表征。通过一系列研究和比较，本文引入的有利的分步模板溶胶 - 凝胶技术被证明是一种卓越的方法，它兼具当前接枝法和传统水热共缩合合成的优异性能，从而在MCM - 41载体上实现热力学稳定固定以及相对较高含量的有机官能团。这种新颖的合成策略还显著缩短了具有规则特定结构的有机官能化MCM - 41的结晶时间。
