高等学校化学学报

高等学校化学学报 ›› 2012, Vol. 33 ›› Issue (04): 689.doi: 10.3969/j.issn.0251-0790.2012.04.009

• 分析化学 • 上一篇    下一篇

单分散高纯硅胶色谱柱填料的制备

杨俊佼, 张硕   

  1. 北京化工大学分析测试中心, 北京 100029
  • 收稿日期:2011-05-06 出版日期:2012-04-10 发布日期:2012-04-10
  • 作者简介:杨俊佼, 男, 博士, 副研究员, 主要从事材料的制备、表征和有机分析研究. E-mail: yangjj@mail.buct.edu.cn

Preparation of Monodisperse and High-purity Silica Packing Materials

YANG Jun-Jiao, ZHANG Shuo   

  1. Analysis and Test Center of Beijing University of Chemical Technology, Beijing 100029, China
  • Received:2011-05-06 Online:2012-04-10 Published:2012-04-10

PDF (PC)

被引次数

15

摘要： 在氨水和氨气催化下使单晶硅粉水解, 合成了单分散、高纯的纳米二氧化硅水溶胶; 再利用聚合诱导胶体凝聚法(PICA)制备单分散脲醛二氧化硅复合微球, 经过高温煅烧后得到球形硅胶色谱柱填料. 通过电感耦合等离子-质谱(ICP-MS)、电子显微镜和BET比表面积测试等手段对球形硅胶的纯度、粒径分布及比表面积进行了表征, 并通过色谱分离对硅胶填料的性能进行了评价. 实验结果表明, 该方法合成的色谱柱填料具有纯度高、粒径分布均匀、机械强度高及分离能力强等优点.

关键词: 单晶硅粉, 聚合诱导胶体凝聚法, 硅胶柱填料

Abstract: Using silicon powder as silica source, monodisperse and high-purity nano-silica sol was synthesized under catalysis of aqueous ammonia and ammonia gas. The urea-formaldehyde polymer/SiO2 composite microspheres were prepared after polymerization-induced colloid aggregation(PICA) method in acidic media, and the spherical silica packing material was produced after calcining at high temperature. The purity of monodisperse nano-silica sol was tested by inductively coupled plasma mass spectrometry(ICP-MS), and the size and shape of the composite microspheres were characterized by scanning electron microscope(SEM). The performance of silica packing material was evaluated by non-chromatographic method(BET) and chromatographic method. The results show that the silica packing material has high purity, uniformity and high mechanical strength.

Key words: Silicon powder, Polymerization-induced colloid aggregation(PICA), Silica packing material

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