改性二氧化硅固载磷钨酸催化合成环己酮甘油缩酮  

Phosphotungstic Acid Supported on Silylated Activated Silica for the Condensation of Cyclohexanone with Glycerol

作　　者：李贵贤[1] 王成君[1] 周洋[1] 李亚珍[1] 王洁[1] 王小瑞[1] 

机构地区：[1]兰州理工大学石油化工学院,甘肃兰州730050

出　　处：《精细化工》2012年第5期472-475,520,共5页Fine Chemicals

基　　金：国家自然科学基金(20961004)~~

摘　　要：以酸活化的活性二氧化硅为载体,采用化学键合的方法制备了3-氨丙基三乙氧基硅烷(APTES)化二氧化硅负载的Keggin型磷钨酸催化剂(HPW/APTES-SiO2),用红外光谱分析、X射线衍射、比表面积(BET)测定、热重-差热分析对催化剂进行了表征。将该催化剂用于合成环己酮甘油缩酮的反应,实验结果表明,2-羟甲基-1,4-二氧杂螺环[4,5]癸烷是主要产物,在优化反应条件下得到环己酮转化率为92.7%,主产物的选择性达97.8%,且催化剂便于从反应体系中分离,能重复使用4次。The catalyst（HPW/APTES-SiO2） of heteropoly acid supported on acid activated and silanizing silica（APTES-SiO2） by 3-aminopropyl-triethoxysilane（APTES） was prepared via chemical bonding.The properties of the catalyst was characterized by means of infrared spectroscopy,X-ray diffraction,Brunauer-Emmett-Teller（BET） specific area measurement and thermogravimetric analysis（TG-DTA）.The catalytic activity of the catalyst was determined by the condensation of cyclohexanone with glycerol.The highest conversion of cyclohexanone and the selectivity of 1,4-dioxa spiro decane-2-methanol reached 92.7% and 97.8%,respectively,by using HPW/APTES-SiO2 as the catalyst under the optimum reaction conditions.The recycling tests show that the catalyst can be easily separated from the reaction system and be reused four times.

关 键 词：活性二氧化硅 改性 磷钨酸 环己酮甘油缩酮 催化与分离提纯技术 

分 类 号：TQ426.91[化学工程]