无外加酸体系中高温合成Al-SBA-15
Direct Synthesis of Al-SBA-15 at High Aging Temperature without Mineral Acid
作者单位E-mail
徐艳 常州大学石油化工学院, 常州 213164
中国科学院青岛生物能源与过程研究所, 青岛 266101 
 
邢立淑 常州大学石油化工学院, 常州 213164
中国科学院青岛生物能源与过程研究所, 青岛 266101 
 
李湘萍 中国科学院青岛生物能源与过程研究所, 青岛 266101  
石磊 山东轻工业学院, 山东省高校轻工精细化学品重点实验室, 济南 250353  
李学兵 中国科学院青岛生物能源与过程研究所, 青岛 266101  
林森 中国科学院青岛生物能源与过程研究所, 青岛 266101 linsen@qibebt.ac.cn 
李明时 常州大学石油化工学院, 常州 213164 mingshili@yahoo.com 
摘要: 在无外加酸的体系中,以三嵌段共聚物P123为模板剂,一步合成有序介孔材料Al-SBA-15。考查了高温和硅/铝源物种共水解对产物形貌和结构性质的影响。XRD,N2吸附脱附,IR,SEM,TEM等结果表明,在无外加酸的体系中,升高晶化温度至 423 K促使Al-SBA-15的短棒状颗粒分散、卷曲成环状。与较低晶化温度下得到的样品对比,孔径增大,比表面积明显降低。当晶化温度低于423 K,样品铝含量基本保持不变。研究还发现,硅源/铝源物种共水解时间超过20 h后,所得样品中铝含量明显降低。
关键词: Al-SBA-15  无外加酸合成  介孔材料  形貌  孔道结构
基金项目: 国家自然科学基金(20976076);中科院百人项目(Y11202220T);山东省高等学校科技计划项目(J12LA02)资助项目。
Abstract: Al-SBA-15 with a rod-like morphology and well-ordered mesostructure was hydrothermally synthesized through a one-step approach in an environmentally friendly medium by using triblock copolymer Pluronic P123 as a structure-directing agent. The influence of aging temperature and silica-alumina species co-hydrolysis on the morphologies and structural properties of the resultant materials were investigated by XRD, IR, SEM, TEM and nitrogen adsorption-desorption techniques at 77 K. Compared to silica-alumina co-hydrolysis, the aging temperature plays an important role in the formation of the ordered mesostructure. The mesopores are widened and the wall thickness becomes thinner when the aging temperature is increased. The particles have well-defined rod-like morphology with the uniform particle size from 2 to 4 μm and the diameter in the range of 400~600 nm. The Si/Al molar ratio of the final Al-SBA-15 samples will be obviously higher if the time for silica-alumina co-hydrolysis is longer than 20 h.
Keywords: Al-SBA-15  acid-free hydrothermal synthesis  mesoporous materials  morphology  pore structure
投稿时间:2012-10-08 修订日期:2013-03-26
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徐艳,邢立淑,李湘萍,石磊,李学兵,林森,李明时.无外加酸体系中高温合成Al-SBA-15[J].无机化学学报,2013,29(9):1849-1855.
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