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研究了采用溶胶-凝胶技术制备的4～6μm粒径氧化锆微球的晶体结构、比表面积、孔容、孔径分布及表面酸碱性,测得氧化锆以单斜相和四方相2种相存在.微球的比表面积为21m~2/g;总孔容为0.128cm~3/L;平均孔直径为8.6nm.氧化锆的表面存在酸碱两性.分别以异丙醇/环己烷、二氧甲烷/环己烷及三氯甲烷/环己烷为流动相研究了苯酚衍生物、芳香烃衍生物及苯胶等碱性化合物的保留行为.氧化锆对苯酚衍生物的保留较强且色谱峰拖尾较严重,中性化合物有一定程度的保留,碱性化合物能达到较好分离且色谱峰对称.
The crystal structure, specific surface area, pore volume, pore size distribution and surface acidity and basicity of 4 ~ 6μm particle size zirconia microspheres prepared by sol-gel technique were studied. Two kinds of zirconia microspheres with monoclinic phase and tetragonal phase The specific surface area of the microspheres was 21 m 2 / g, the total pore volume was 0.128 cm 3 / L and the average pore diameter was 8.6 nm. Alkane, dioxane / cyclohexane and trichloromethane / cyclohexane as mobile phase to study the retention behavior of the basic compounds such as phenol derivatives, aromatic hydrocarbon derivatives and benzene gum, etc. The retention of phenol derivatives by zirconia Strong and more severe peak tailing, neutral compounds have a certain degree of retention, alkaline compounds can achieve better separation and chromatographic peak symmetry.