固体酸Zr(SO_4)_2/TiO_2催化合成马来酸二丁酯

Catalytic Synthesis of Dibutyl Maleate from Solid Acid Catalyst Zr(SO_4)_2/TiO_2

制备了固体酸催化剂Zr(SO4)2蛐TiO2,并将其用于合成马来酸二丁酯,考察了Zr(SO4)2与TiO2的质量比、焙烧温度、焙烧时间等催化剂制备条件对催化活性的影响.采用FTIR与DTG对催化剂进行了表征分析.通过正交实验设计优化了固体酸Zr(SO4)2蛐TiO2催化合成马来酸二丁酯的工艺条件.实验结果表明,Zr(SO4)2蛐TiO2是合成马来酸二丁酯的良好催化剂,适宜的催化剂制备条件为:Zr(SO4)2与TiO2的质量比为60:40,焙烧温度为400℃,焙烧时间为2 h.适宜的催化合成反应条件为:酐醇物质的量比为1:2.5,催化剂用量1.25 g(每0.05 mol马来酸酐),带水剂苯5 mL,反应时间为3.0 h.在此条件下马来酸二丁酯的酯化率为99.2%.

Solid acid catalyst Zr（SO4）JTiO2 were prepared and applied to synthesis of dibutylmaleate. Effect, of mass ratio of Zr（SO4）2 and TiO2, calcination temperature, and calcination time on the catalytic activity were investigated. The catalyst were clharacterized by FTIR and DTG methods. Process for Catalytic Synthesis of dibutylmaleate were optimized by Orthogonal Experiment Design. The results showed that solid acid catalyst Zr（SO4）2/TiO2 exhibited high catalytic activity for the synthesis of dibutylmaleate, the appropriate conditions of catalysts preparation were as followed： m（Zr（SO4）2）：m（Ti02）=60：40, calcination temperature of catalyst 400 ℃, calcination time 2 h. Uwler suitable esterification conditions： mole ratio of maleic arthydride to n-butanol 1：2.5, catalyst dosage 1.25 g（based on 0.05 mol maleie anhydride）, water-carrying agent benzene 5 mL, and reaction time 3.0 h, the esterifieation rate is 99.2%.