活性自由基聚合(Iniferter)法制备聚合物包覆硅胶固定相及其色谱性能评价  

Preparation of Polymer-encapsulated Silica by Using the Living Radical Polymerization (iniferter) Method and Chromatographic Performance Evaluation

作　　者：张海燕[1] 李保利[1] 张绪宏[1] 宿书芳[1] 张敏[1] 董襄朝[1] 

机构地区：[1]南开大学化学学院,天津300071

出　　处：《化学学报》2008年第19期2151-2156,共6页Acta Chimica Sinica

基　　金：国家自然科学基金(No.20575030)资助项目

摘　　要：应用活性自由基聚合法,在接枝iniferter的硅球表面键合甲基丙烯酸异辛酯-co-乙二醇二甲基丙烯酸酯聚合层,制备了聚合物包覆硅胶色谱固定相,并研究了合成条件对于聚合层及分离效果的影响.在一定聚合时间中,接枝聚合物质量与反应时间呈线性关系,并可以在得到聚合物包覆硅胶的基础上,利用包覆硅胶中的iniferter再次引发接枝聚合,体现了活性自由基聚合的特点.聚合物包覆硅胶对于烷基苯同系物、碱性化合物及羟基苯甲酸酯具有很好的色谱分离能力及柱效,同时,由于聚合层能够有效地覆盖硅球表面的硅羟基,减小了碱性化合物的拖尾.研究工作提供了新的聚合物包覆硅胶固定相的合成方法.The living radical polymerization （iniferter） method was used to prepare the polymer-encapsulated silica as a chromatographic stationary phase. The 2-ethylhexyl methacrylate and ethylene dimethacrylate were polymerized and grafted on the silica surface by the initiation of the iniferter bound on the silica. The influence of the synthetic conditions on the polymer layers and the chromatographic separation was studied. The linear relation between the polymerization time and the amount of the polymer grafted on the silica in certain reaction period was observed. Meanwhile, polymer-encapsulated silica could be re-initialized for the successive grafting reaction, which showed the character of the living radical polymerization. The polymer-encapsulated silica has shown good separation ability and column efficiency for the alkylbenzene, alkaline compounds and hydroxybenzoate. The alkaline compounds have small peak tailings on the polymer-encapsulated silica stationary phase, which indicated that silanol groups on the silica surface were effectively covered by the polymer layer. The work provided a new method for the synthesis of polymer-encapsulated silica.

关 键 词：聚合物包覆硅胶 活性自由基聚合 INIFERTER 色谱固定相 

分 类 号：O657.72[理学—分析化学]