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单分散高纯硅胶色谱柱填料的制备
引用本文:杨俊佼,张硕. 单分散高纯硅胶色谱柱填料的制备[J]. 高等学校化学学报, 2012, 33(4): 689-694. DOI: 10.3969/j.issn.0251-0790.2012.04.009
作者姓名:杨俊佼  张硕
作者单位:北京化工大学分析测试中心, 北京 100029
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  
收稿时间:2011-05-06

Preparation of Monodisperse and High-purity Silica Packing Materials
YANG Jun-Jiao , ZHANG Shuo. Preparation of Monodisperse and High-purity Silica Packing Materials[J]. Chemical Research In Chinese Universities, 2012, 33(4): 689-694. DOI: 10.3969/j.issn.0251-0790.2012.04.009
Authors:YANG Jun-Jiao    ZHANG Shuo
Affiliation:Analysis and Test Center of Beijing University of Chemical Technology, Beijing 100029, China
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.
Keywords:Silicon powder  Polymerization-induced colloid aggregation(PICA)  Silica packing material
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