将硅酸乙酯、过硫酸钾、盐酸、甲基丙烯酸钠共混,在一定条件下水解、聚合,经真空处理后,分散至石蜡油中,控制反应温度进行溶胶-凝胶化转变,合成了灌流硅胶微球材料。采用扫描电镜仪、比表面孔径测试仪、压汞仪等对其进行了表征,发现该微球材料具有多级孔结构,即纳米尺度的中孔和微米尺度的穿透孔。中孔能够提供大的比表面,而穿透孔有利于流动相通过,实现对流传质。该材料经十八烷基三乙氧基硅烷改性后,成功应用于苯同系物的高效快速分离。
The synthesis of a new liquid chromatographic packing of perforative silica gel microspheres was reported. The tetraethoxylsilane, potassium persulfate, hydrochloric acid and methacrylate sodium were mixed together at 60 ℃ for 4 h. Then the solution was connected to a vacuum pump for 4 h to get rid of by-product of ethanol. After that, it was magnetically dispersed into paraffin oil to undergo sol-gel transition. The as-synthesized silica gel was characterized by scanning electron microscopy, mercury porosimetry and nitrogen sorption measurements. The results shows that the silica gel demonstrates hierarchically porous structure of mesopores and perfusive macropores. The mesopores guarantee high surface area while the macropores, which traverse the microspheres, realize convective mass transfer. The successful application of the perforative silica gel in fast liquid chromatography was well demonstrated in the present work. Five benzene homologues can be baseline separated within 3 min.