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氧化锆微球因其化学稳定性优异、机械强度高以及热稳定性好,是很有前景的高效液相色谱填料材料。但如何制备出颗粒大小合适、粒径分布窄、比表面积大、孔径合适的氧化锆微球以满足使用要求是一个难点。以氯氧化锆为原料,以油乳液法制备氧化锆微球,并在反应体系中添加双氧水,研究了双氧水对锆离子水解沉积反应和最终产物性能的影响。结果发现H2O2能提高氯氧化锆的水解率和水解速度,增大最终微球产物的比表面积和孔容,同时减小平均孔径。
Zirconia microspheres are promising HPLC packing materials due to their excellent chemical stability, high mechanical strength and good thermal stability. However, how to prepare a zirconium oxide microsphere with suitable particle size, narrow particle size distribution, large specific surface area and suitable pore diameter to meet the requirements of use is a difficult problem. ZrO2 microspheres were prepared by the oil-emulsion method using zirconium oxychloride as the raw material, and hydrogen peroxide was added to the reaction system to study the effect of the hydrogen peroxide on the zirconium ion hydrolysation reaction and the final product performance. It was found that H2O2 can improve the hydrolysis rate and hydrolysis rate of zirconium oxychloride, increase the specific surface area and pore volume of the final microsphere product, and reduce the average pore size.