表面自由基链转移反应制备聚合物修饰的色谱固定相  

Preparation of Polymer Modified Stationary Phases Through Surface Radical Chain Transfer Reaction

作　　者：刘淑娟[1] 敦惠娟[1] 周峰[1] 赵亮[1] 刘霞[1] 蒋生祥[1] 

机构地区：[1]中国科学院兰州化学物理研究所,甘肃兰州730000

出　　处：《色谱》2002年第5期432-435,共4页Chinese Journal of Chromatography

基　　金："973"项目子课题 (项目编号:G19990 2 2 50 0 )

摘　　要：利用巯丙基修饰硅胶的自由基链转移反应 ,在硅胶表面原位引发自由基聚合 ,制备了聚甲基丙烯酸甲酯修饰的反相高效液相色谱固定相。通过红外吸收光谱 (FTIR)、拉曼光谱、热失重 (TGA)和元素分析对该固定相进行了表征。该固定相对含氧芳香化合物。It is demonstrated that radical chain transfer to thiol terminated self assembled monolayer and surface initiated polymerization could be used for in situ grafting ultra thin polymer film on silica.The widely used silane coupling agent mercaptopropyltrimethoxysilane (MPS) was used to prepare the thiol terminated silica, and in the presence of which, chain transfer reaction and polymerization of methyl methacrylate (MMA) was carried out using azo di isobutylnitrile (AIBN) as the initiator. Both thiol terminated silica and polymer film modified silica were characterized by Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, thermogravimetric analysis (TGA) and elemental analysis. The results showed that the grafting amount of polymer on silica was higher than the traditional methods, which can effectively relieve the non specific adsorption of solute with uncovered hydroxyl groups on the surfaces of silica in subsequent chromatographic application. The obtained polymethylmethacrylate (PMMA) modified silica exhibited excellent separation capacity on the separation of the polar compounds and polycyclic aromatic hydrocarbons. This kind of surface initiated polymerization prospects for the preparation of polymer modified stationary phases.

关 键 词：制备 聚合物修饰 色谱固定相 表面引发聚合 自由基链转移反应 高效液相色谱 聚甲基丙烯酸甲酯 

分 类 号：O657.72[理学—分析化学]