无机材料学报

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混合表面活性剂法制备介孔SiO2微球及其Semi-batch法生长

邱健全, 赵翔, 金敏超, 蔡强, 李恒德   

  1. 清华大学材料科学与工程系先进材料教育部重点实验室, 北京 100084
  • 收稿日期:2005-07-04 修回日期:2005-08-29 出版日期:2006-05-20 网络出版日期:2006-05-20

Synthesis of Mesoporous Silica Spheres by Using Neutral-cationic Surfactant and Semi-batch Growth

QIU Jian-Quan, ZHAO Xiang, JIN Min-Chao, CAI Qiang, LI Heng-De   

  1. Department of Material Science and Engineering, Tsinghua University, Key Laboratory for Advanced Materials of Ministry of Education, Beijing 100084, China
  • Received:2005-07-04 Revised:2005-08-29 Published:2006-05-20 Online:2006-05-20

摘要: 以TEOS为原料, 以表面活性剂CTAB与十二胺的混合物为模板剂, 以C2H5OH、C3H7OH和H2O为共溶剂, 在弱碱性条件下制备出单分散SiO2介孔微球. 通过调变模板剂用量以及共溶剂的比例, 所得微球粒径在0.2~1.5μm范围内可调节. 并采用semi-batch(半间歇加料)方法进一步生长微球, 使其粒径增大到3μm. 此类微球具有3nm的平均孔径和较高的比表面积, 有望作为高效液相色谱(HPLC)的固定相而得到广泛应用. 在以上实验的基础上, 本文进一步讨论了SiO2 微球生长过程中的若干理论问题.

关键词: 介孔, SiO2微球, 表面活性剂, semi-batch

Abstract: A one-step synthesis of mono-dispersed mesoporous silica spheres by using the mixed surfactants CTAB and dodecylamine proceeded with the hydrolysis and condensation of tetraethylorthosilicate (TEOS) in a mixture of alcohol, isopropyl alcohol, water, and ammonia as a catalyst. The silica spheres have high specific
surface area and can be used as a good substrate in high performance liquid
chromatography (HPLC). The size of 0.2~1.5μm and morphology of the silica spheres can be controlled by varying the proportion of surfactant and co-solvent. The prepared silica spheres can be enlarged to the maximum diameter 3μm with a seeded growth method in a semi-batch reacting system. Based on the experiments above, several mechanisms were discussed on the growth
process of mesoporous silica spheres in the synthesis.

Key words: mesoporous, silica spheres, surfactant, semi-batch

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