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合成二维六方苯环桥联型杂化介孔材料的新方法
作者:翟尚儒1 董晓丽1 刘娜1 安庆大1 宋宇1 徐耀2 孙予罕2 
单位:1. 大连工业大学化工与材料学院 辽宁 大连 116034 2. 中国科学院山西煤炭化学研究所 太原 030001 
关键词:盐效应 有序介孔材料 有机-无机杂化材料 合成 
分类号:O648.1
出版年,卷(期):页码:2011,39(6):108-112
DOI:
摘要:
以苯基桥联硅氧烷[1,4-bis(trimethoxysilyl)benzene,BTSB]和三嵌段共聚物聚氧乙烯-聚氧丙烯-聚氧乙烯(EO20PO70EO20,P123)分别作为硅源和模板剂,在无酸体系中利用ZrOCl2-K2SO4的协同作用方便制得二维六方苯环桥联型杂化介孔材料(periodic mesoporous organosilicas,PMOs)。通过高分辨透射电镜、小角X射线散射、N2吸附-脱附等温线、固体13C 交叉极化和29Si核磁共振技术等分析手段系统表征PMOs的结构性能。分析结果表明:保持摩尔比n(K2SO4):n(Si) = 2,可在n(Zr):n(Si) = 0.01~0.10时制备高度规整的苯环桥联型杂化材料。基于ZrOCl2自身水解生成的弱酸性环境和K2SO4对P123胶束的作用特点,探讨无机盐组合在研究体系中的协同促进机制。
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Ordered benzene-bridged periodic mesoporous organosilicas (PMOs) with hexagonal frameworks were prepared with assistance of ZrOCl2-K2SO4 salt pairs using nonionic P123 (EO20PO70EO20) and 1,4-bis(trimethoxysilyl)benzene (BTSB) as a structure- directing agent and silica precursor, respectively. The product was thoroughly characterized by the small-angle X-ray scattering, high-resolution transmission electron microscopy and N2-adsorption/desorption isotherms, as well as solid state 13C cross polarization/29Si magic angle spinning nuclear magnetic resonance spectroscopy techniques. Analysis results show that, with mole ratio n(K2SO4):n(Si) = 2, high-quality benzene-bridged PMOs are easily prepared within a wide range of n(Zr):n(Si) = 0.01-0.10, thus clearly illustrating the cooperative effect of both salts in assembly of the hybrid mesostructure in the proposed synthesis system.
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基金项目:
国家自然科学基金(20901012)及辽宁省高校优秀人才支持计划(LR201005)资助项目
作者简介:
博士,副教授
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参考文献:
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