Preparation of porous zirconia microspheres as chromatographic packing materials by compound processes of hydrothermal and PICA

• 1、Department of Chemistry, Institute of Science, Tianjin University

Abstract：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—3μm, 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 5μm zirconia microspheres. Porous zirconia microspheres sintered at 700 ºC 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.

Keywords： zirconia chromatographic packing materials hydrothermal synthesis microspheres