摘要
氧化锆色谱填料相对于市场上普遍使用的硅胶填料,有着特殊的表面物理化学性能和分离选择性,特别适宜于碱性样品及蛋白质等生物大分子的分离。传统诱导聚合胶体凝聚工艺制备的氧化锆微球尺寸在2～3μm,导致色谱分离效率较低。制备直径在5～7μm,尺寸均一,孔径适宜的氧化锆微球,是氧化锆填料研究的关键。以氧氯化锆为原料,利用水热合成工艺制备稳定的二氧化锆纳米溶胶。控制酸性条件下脲醛树脂聚合反应条件,通过诱导聚合胶体凝聚工艺制备出尺寸均一、直径为5μm的氧化锆微球。(700℃,3h)煅烧的氧化锆微球其相组成以单斜氧化锆相为主,比表面积为10.5m2/g,孔径分布在5～26nm中孔范围内。作为正相色谱填料对碱性、中性化合物表现出良好的分离选择性。
The complex properties of zirconia＇s surface chemistry were suitable to separate alkaline compounds and biomolecules,which were superior to silica as stationary phase of HPLC. Zirconia microspheres prepared by traditional polymerization-induced colloid aggregation （PICA） process were only 2-3 μm,which affects its separation efficiency. In this work,the stabilized nanometer zirconia colloidal sols were synthesized using zirconyl chloride （ZrOCl2·8H2O） as raw material by hydrothermal process. Zirconia microspheres of about 5 μm with a narrow particle size distribution have been prepared by controlling polymerization of urea formaldehyde resin in the PICA process. The innovative combined process of hydrothermal and PICA was the key to get 5 μm zirconia microspheres. Porous zirconia microspheres sintered at 700 ℃ for 3 h were mainly monoclinic phase,with specific surface area of 10.5 m2/g and pores ranging from 5 to 26 nm in diameter. As chromatographic packing materials of normal phase chromatography,porous zirconia microspheres showed good separation properties for alkaline and neutral compounds.
基金
教育部留学回国人员科研启动基金资助项目(2009-1001)
国家自然科学基金资助项目(50972103)
关键词
氧化锆
色谱填料
水热合成
微球
zirconia
chromatographic packing materials
hydrothermal synthesis
microspheres
