锆钛铟超强酸的制备及催化酯化柠檬酸三乙酯  

Preparation of Zr-Ti-In solid superacid and its catalytic activities in esterification of citric acid

作　　者：陈丽凤[1] 杨大伟[1] 付颖寰[1] 郭宏[1] 

机构地区：[1]大连工业大学轻工与化学工程学院,辽宁大连116034

出　　处：《大连工业大学学报》2012年第3期191-194,共4页Journal of Dalian Polytechnic University

摘　　要：用共沉淀法,以铟(In)的质量分数、焙烧时间、焙烧温度为因素,通过L9(34)正交试验制备SO24-/TiO2-ZrO2-In2O3固体超强酸,以柠檬酸三乙酯合成考察了各因素对固体超强酸度的影响。结果表明,固体超强酸SO24-/TiO2-ZrO2-In2O3的最佳制备条件是In质量分数为1.5%,焙烧温度550℃,焙烧时间4h,其酯化率达97.8%。并用XRD、SEM、FTIR对固体超强酸进行了表征,加入In后,固体超强酸体积变大、膨松,可吸附更多的SO24-,使超强酸的酸性更强;固体超强酸中的TiO2由无定型结构转变为锐钛矿晶型结构,并随着焙烧温度的增加,TiO2的衍射峰逐渐变得尖锐。对酯化产物进行了红外光谱表征和折光率测定。Solid superacid SO2-4/TiO2-ZrO2-In2O3 was prepared by co-precipitation method.An orthogonal L9(34) test design was applied to select the optimum preparation parameters including content of In,calcining time and temperature.The influence of each parameter on solid superacid was investigated by esterification of triethyl citrate.The results show that the optimum condition to prepare solid superacid SO2-4/TiO2-ZrO2-In2O3 is In content 1.5%,calcining temperature 550 ℃ and calcining time 4 h,the yield of esterification is 97.8%.And the solid superacid was characterized by XRD,SEM and FTIR.The particle size of superacid growed and swelled after introducing of In,which results in higher adsorption of SO2-4and stronger acidity.Amorphous TiO2 in the superacid is turn to anatase and the diffraction peak become sharp with increasing of calcining temperature.The synthesized triethyl citrate is characterized with IR and refractive index.

关 键 词：固体超强酸 IN2O3 酯化 

分 类 号：O643.32[理学—物理化学]