Niu Mengna, Ma Hongyan, Hu Fei, Wang Shige, Liu Lu, Chang Haizhou, Huang Mingxian
Department of Chemistry, College of Science, University of Shanghai for Science and Technology, Shanghai 200093, China.
Se Pu. 2017 Jun 8;35(6):565-571. doi: 10.3724/SP.J.1123.2017.03018.
Large-pore silica microspheres were synthesized by utilizing weak cation exchange polymer beads as templates, -trimethoxysilylpropyl--trimethylammonium chloride (TMSPTMA) as a structure-directing agent, tetraethoxysilane (TEOS) as a silica precursor, and triethanolamine as a weak base catalyst. The hydrolysis and condensation of the silica precursors occurred inside the templating polymer beads yielded polymer/silica composite microspheres. After the organic polymer templates were removed in the calcination step, large-pore silica microspheres were produced. The effects of different reaction conditions on the morphology, structure and dispersibility of the formed silica microspheres were investigated. It has been shown that when the volume ratio of TMSPTMA, TEOS and triethanolamine was 1:2:2, silica microspheres with pore size range of 50-150 nm and particle size around 2 μm were obtained. The as-prepared silica microspheres were then bonded with chlorodimethyloctadecylsilane (C18), packed into a 50 mm×4.6 mm column, and evaluated for the separations of some common standard proteins and soybean isolation proteins. The results showed that the large-pore silica spheres from this work have potentials for protein separation in HPLC.
以弱阳离子交换聚合物微球为模板,-三甲基氯化铵三甲氧基硅丙酯(TMSPTMA)为结构导向剂,正硅酸乙酯(TEOS)为硅源前驱体,三乙醇胺为弱碱催化剂,合成了大孔二氧化硅微球。硅源前驱体在模板聚合物微球内部发生水解和缩合反应,生成聚合物/二氧化硅复合微球。在煅烧步骤中去除有机聚合物模板后,得到大孔二氧化硅微球。研究了不同反应条件对所形成二氧化硅微球的形貌、结构和分散性的影响。结果表明,当TMSPTMA、TEOS和三乙醇胺的体积比为1:2:2时,可获得孔径范围为50-150nm、粒径约为2μm的二氧化硅微球。然后将所制备的二氧化硅微球与氯代二甲基十八烷基硅烷(C18)键合,填充到50mm×4.6mm的色谱柱中,并对一些常见标准蛋白质和大豆分离蛋白进行分离评价。结果表明,本研究制备的大孔二氧化硅球在高效液相色谱中具有蛋白质分离潜力。