以钛酸丁酯为原料,利用聚合诱导胶体凝聚法(polymerization—induced colloid aggregation,PICA)合成了可供高效液相色谱(HPLC)使用的窄孔径和粒径分布的微米级中孔钛球。探索了以钛酸丁酯为原料制备胶体的方法和条件,考察了温度、溶液pH值、尿素和甲醛浓度对树脂微球成球的影响。同时对树脂微球的煅烧条件进行了考察。最终制备出适用于HPLC的平均粒径为3.5μm,平均孔径为18.9nm,比表面积为9.6m^2/g的二氧化钛填料。
By using tert-n-butyl titanate as the raw material, an improved process of polymerization-induced colloid aggregation was used to synthesize porous titanic microspheres with a very narrow particle size distribution(PSD) useful for HPLC column packing. The effects of temperature, solution pH and concentrations of urea and formaldehyde on aggregated microspheres and the sintering conditions were studied. The titania microspheres obtained have an average diameter of 3.5 μm, a surface area of 9.6 m^2· g^-1, an average pore volume of 0. 30 mL/g and an average pore diameter of 18.9 nm. The particles are rigid enough to withstand the high packing pressure for a HPLC column.