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2006 , Vol. 21 >Issue 3: 558 - 564

DOI: https://doi.org/10.3724/SP.J.1077.2006.00558

研究论文

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
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  • 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

  网络出版日期: 2006-05-20

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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
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  • Department of Material Science and Engineering, Tsinghua University, Key Laboratory for Advanced Materials of Ministry of Education, Beijing 100084, China

Received date: 2005-07-04

  Revised date: 2005-08-29

  Online published: 2006-05-20

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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

本文引用格式

邱健全 , 赵翔 , 金敏超 , 蔡强 , 李恒德 . 混合表面活性剂法制备介孔SiO2微球及其Semi-batch法生长[J]. 无机材料学报, 2006 , 21(3) : 558 -564 . DOI: 10.3724/SP.J.1077.2006.00558

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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