载体用高比表面超细二氧锆的制备及结构表征

摘要

以氧氯化锆溶液为前驱体,一定量的PEG-600为分散剂,氨水为沉淀剂,通过化学沉淀法合成氢氧化锆沉淀.经后续洗涤、过滤、干燥和焙烧制得二氧化锆粉体材料.经过单因素实验确定沉淀法各工艺参数的影响范围,以单因素实验确定的主要因素设计正交实验,寻找制备高比表面超细二氧化锆的最佳工艺条件.通过正交实验结果分析可得:最佳工艺条件为氧氯化锆浓度为0.6 mol/L,氨水的pH为11.5,反应温度为55 ℃,焙烧温度为400℃.对正交实验最佳工艺条件下制得的二氧化锆进行了粒度检测和BET、SEM表征,结果发现:产品粒度微小均匀,平均粒径为1.3 μm,孔结构丰富,表面粗糙呈菜花状,比表面积可达214 m2/g,符合作载体的基本要求.%Zr(OH)4 was synthesized by chemical precipitation method with zirconium oxychloride solution as precursors,PEG-600 as dispersant,and ammonia as precipitant.The ZrO2 powder was prepared by subsequent washing,filtration,drying,and calcination.The influence range of the precipitation process parameters was determined by single factor experiment.The single factor experiment was used to determine the main factors to design the orthogonal experiment.The optimum conditions for preparation of ultrafine ZrO2 with high specific surface were obtained by orthogonal experiment.The results showed that the optimal conditions were as follows:the concentration of zirconium oxychloride was 0.6 mol/L,the pH of ammonia solution was 11.5,the reaction temperature was 55 ℃,and the calcination temperature was 400 ℃.The ZrO2 which was made under the optimum conditions of orthogonal experiment was characterized by BET,SEM,and particle size.The results showed that the average particle size was 1.3 μm,the pore structure was rich,the surface roughness was cauliflower,and the specific surface area was 214 m2/g,which accorded with the basic requirements of carrier.