SO_4^(2-)/TiO_2负载磷钨酸型固体酸制备乙酸异龙脑酯

Synthesis of Isobornyl Acetate with Solid Acid Catalyst SO_4^(2-)/TiO_2 Supported by Phosphotungstic acid

TiCl_4水解同时加入磷钨酸,氨水沉淀后,采用硫酸铵混合后焙烧工艺制备了SO_4^(2-)/TiO_2负载磷钨酸型固体酸催化剂。用乙酸和莰烯进行反应合成乙酸异龙脑酯,对反应时间、催化剂用量、莰烯与乙酸物质的量比、反应温度进行了优化实验,采用气相色谱法进行产品检测。结果表明反应酸烯物质的量比为2:1、催化剂用量为酸烯总质量的3%、反应6h、反应温度80℃的条件下转化率最高,可达85.5%,经初步蒸馏后产品纯度可达95%以上。

TiCl_4 was hydrolysised simultaneously added in phosphotungstic acid,and precipitated by NH_3. The solid acid catalyst SO_4^(2-)/TiO_2 supported by Phosphotungstic acid was prepared by roasting and mixing ammonium sulfate with the sediment.Isobornyl Acetate was synthesized with acetic acid and camphene. The experiment was conducted to optimize the dosage of catalyst,the molar ratio of camphene and acetic acid,reaction time and reaction temperature. The product was tested by Gas Chromatography method. The results showed that the camphene has the highest conversion rate under such conditions the molar ratio of acetic acid and camphene 2: 1,catalyst dosage 3% to the total mass of camphene and acetic acid,6 h and 80℃. The highest conversion rate was 85. 5%. After initial distillation,the product purity could reach above 95%.