表面引发聚合反应制备色谱固定相  

PREPARATION OF STATIONARY PHASE FOR HPLC THROUGH SURFACE INITIATED POLYMERIZATION

作　　者：刘淑娟[1] 周峰[1] 蒋生祥[1] 刘维民[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：《高分子材料科学与工程》2003年第6期65-68,共4页Polymer Materials Science & Engineering

摘　　要：巯丙基硅烷在硅胶表面组装形成潜在的自由基链转移点,向表面的自由基链转移及表面引发聚合反应可在硅胶表面形成化学键合的聚合物膜,反应过程用红外光谱(FT-IR)、X射线光电子能谱(XPS)、拉曼光谱(Raman)及热重分析(TGA)进行表征。随着巯丙基硅烷修饰硅胶用量的增加,溶液中形成的自由聚合物的分子量及聚合物在硅胶表面的接枝量减小,单体的接枝量随着聚合时间的逐渐增大,直至平衡值。用此方法得到的聚甲基丙烯酸甲酯修饰的硅胶呈现良好的反相色谱性能,对几种含氧芳烃衍生物的保留时间按下列顺序增加:对羟基苯甲酸<α-萘乙酸<β-苯乙醇<苯酚<对羟基苯甲酸甲酯<苯甲酸甲酯<苯甲酸乙酯<苯甲酸丁酯。In this paper, it is demonstrated that radical chain transfer reaction could be used as an intermediate reaction to fabricate ultra-thin polymer film on silica surface. Both thiol-terminated self-assembled monolayer and polymer over-layer were characterized by FT-IR, XPS, TGA and element analysis. The molecular weight of free polymer formed in bulk solution and also the grafting amount of polymer decreased with increasing the content of thiol terminated silica in polymerization solution. The grafting amount of monomer increased with polymerization time until a maximum value of more than 5 monomers per nm^2 was obtained. The chromatographic property of the thus prepared polymer modified silica was evaluated. It acted as a reverse chromatographic stationary phase that exhibited excellent separation capacity for a series of oxygen-containing aromatic compounds.

关 键 词：表面引发聚合 制备 色谱固定相 表面链转移反应 分子自组装 聚甲基丙烯酸甲酯 

分 类 号：TQ325.7[化学工程—合成树脂塑料工业]