磷酸根改性的二氧化钛固体酸催化合成草酸二异戊酯  

Synthesis of diisopentyl oxalate catalyzed by phosphate-promoted TiO_2 solid acid catalysts

作　　者：张晓丽[1] 任立国[1] 高文艺[1] 

机构地区：[1]辽宁石油化工大学化学与材料科学学院,辽宁抚顺113001

出　　处：《化学研究与应用》2011年第9期1195-1199,共5页Chemical Research and Application

摘　　要：通过沉淀、老化、过滤、洗涤、干燥、浸渍和焙烧等过程,从TiCl4和H3PO4制备了磷酸根助催化的二氧化钛固体酸催化剂,用Hammett指示剂法、正丁胺滴定法、XRD和N2-吸附进行了表征,研究了PO43-的质量分数和焙烧温度对酸性、结构和催化性能的影响。XRD结果表明PO43-抑制晶粒长大。Hammett指示剂法表明PO43-助催化的二氧化钛固体酸催化剂在400～550℃焙烧温度范围内焙烧可以形成固体超强酸。N2-吸附和正丁胺滴定结果表明PO43-的含量达到7.5%(质量分数)时,表面积、孔容和总酸量随着PO43-的质量分数增加而增大,尔后随着PO43-的质量分数增加而减小。磷酸根助催化的二氧化钛固体酸在草酸和异戊醇的酯化反应中具有良好的催化性能。The phosphate-promoted TiO2 solid acid catalysts was prepared from TiCl4 and H3PO4 by precipitation,aging,filtering,washing,impregnation and calcination processes.All the samples are characterized by Hammett indictor,n-butylamide titration,XRD and N2-adsorption methods.The effect of phosphate ion loading,calcination temperature on the acidic properties,textural properties and catalytic perfomance of phosphate-promoted TiO2 solid acid catalysts has been described.The XRD patterns show that phosphate decreases its crystallite size of TiO2.Hammett indictor method show that solid superacid was formed in the 400~550 ℃ temperature range.Surface area and porous volume as well as total acidity were found to increase with the increase in phosphate content up to 7.5% loading（mass fraction） and thereafter decreases.The phosphate-promoted TiO2 solid acid catalysts have good catalytic perfomance in the esterification of oxalic acid and isopentyl alcohol.

关 键 词：固体酸 酸性 表征 酯化 草酸二异戊酯 

分 类 号：O643.3[理学—物理化学]