SO_4^(2-)/ZrO_2固体超强酸的制备及表征  

Preparation and Characterization of Solid Superacid SO_4^(2-)/ZrO_2

作　　者：莫晓兰[1] 张昭[1] 王优[1] 宁小杰[1] 

机构地区：[1]四川大学化工学院,四川成都610065

出　　处：《钛工业进展》2011年第2期14-18,共5页Titanium Industry Progress

基　　金：国家自然科学基金资助项目(50474071)

摘　　要：对传统沉淀-浸渍法制备SO42-/ZrO2(SZ)工艺进行了改进,探索用一步法制备SZ。分别以氯氧化锆(添加硫酸铵引入SO42-)和硫酸锆为锆源,以氨水为沉淀剂,经水解、水热、洗涤、干燥、焙烧制得高比表面积的SO42-/ZrO2。利用XRD、SEM、FT-IR、低温氮气吸附-脱附、Hamm ett指示剂法等进行结构及酸性的表征,研究了锆盐原料浓度、水解pH值、焙烧温度对SO42-/ZrO2性能影响。研究表明:水解pH值对SZ的比表面积影响最大;焙烧温度是制备SO42-/ZrO2固体超强酸的关键,当焙烧温度达到700℃时,负载SO42-的ZrO2才由无定形向单斜相和四方相转变,制得的SO42-/ZrO2显示出强酸性。In this paper,SO4 2-/ZrO2 was prepared by one step process based on an improving traditional precipitation-impregnation,respectively zirconium oxychloride（add ammonium sulfate） and zirconium sulfate as the zirconium source,ammonia as the precipitant.Through hydrolysis,hydrothermal treatment,washing,drying and calcining SO4 2-/ZrO2（SZ） with high specific surface area was obtained.The structure and acidity were characterized by XRD,SEM,FT-IR,low temperature N2 adsorption-desorption,Hammett indicator method,and the influence of zirconium salt concentration,hydrolysis pH,calcination temperature on the specific surface area of SZ was researched.The results show that hydrolysis pH is the greatest impact factor on the specific surface area of SZ,the formation of solid superacid depends on calcination temperature.When the calcination temperature reaches 700 ℃,amorphous ZrO2 is transformed to monoclinic and tetragonal phase,obtained SZ appears strong acidity simultaneously.

关 键 词：固体超强酸 SO42-/ZrO2 焙烧 比表面积 

分 类 号：O611.4[理学—无机化学]