二氧化钛负载磷钨钼杂多酸催化合成缩醛(酮)  

Catalytic Synthesis of Acetals and Ketals with H_3PW_6Mo_6O(40)/TiO_2

作　　者：杨水金[1] 童文龙[1] 

机构地区：[1]湖北师范学院 生化分析技术湖北省重点实验室,湖北黄石435002

出　　处：《稀有金属材料与工程》2007年第A03期316-319,共4页Rare Metal Materials and Engineering

基　　金：国家自然科学基金项目(20471044);湖北省自然科学基金项目(2005ABA053)资助

摘　　要：首次采用回流法制备了二氧化钛负载磷钨钼杂多酸催化剂H_3PW_6Mo_6O_(40)/TiO_2,该催化剂的适宜制备条件为:原料质量比m(TiO_2):m(H_3PW_6Mo_6O_(40))=1:2.0,水的用量30 mL,回流反应时间2.0h,活化温度150℃。以H_3PW_6Mo6O_(40)/ TiO_2为催化剂,对以环己酮、丁酮、正丁醛、苯甲醛与二元醇(乙二醇、1,2-丙二醇)为原料合成的8种缩醛(酮)反应条件进行对比,较系统研究了醛(酮)与二元醇摩尔比、催化剂用量、反应时间对收率的影响。结果表明,在n(醛(酮:n(乙二醇(1,2-丙:二醇))=1.0:1.4、催化剂用量占反应物料总质量的0.8%、反应时间1.0 h的条件下,8种缩醛(酮)的收率在53.0%～86.9%之间。A new environmental friendly catalyst, H3PW6Mo6040/TiO2 was prepared. The optimum conditions have been found, that is, mass ratio of m（TiO2）： m（H3PW6Mo6O40） 1/2.0, volume of water 30 mL, the reflux reaction time 2 h, and activated temperature 150 ℃. H3PW6Mo6O40/TiO2 was used as catalyst in catalytic synthesis of acetals and ketals, namely cyclohexanone ethylene ketal, cyclohexanone 1,2-propanediol ketal, butanone ethylene ketal, butanone 1,2-propanediol ketal, 2-phenyl-1,3-dioxolane, 4-methyl- 2-phenyl-1,3-dioxolane, 2-propyl-1,3-dioxolane, 4-methyl-2-propyl-1,3-dioxolane. Effects of n（aldehyde（ketone ））：n（glycol）, catalyst dosage and reaction time on yield were investigated, Optimal conditions were： n（aldehyde（ketone））：n（glycol）=1.0：1.4; mass fraction of catalyst to reactants, 0.8%; reaction time, 1.0 h and cyclohexane as water-stripped reagent, 10 mL. Under these conditions, yield of cyclohexanone ethylene ketal, cyclohexanone 1,2-propanediol ketal, butanone ethylene ketal, butanone 1,2-propanediol ketal, 2-phenyl-1, 3-dioxolane, 4-methyl-2-phenyl-1, 3-dioxolane, 2-propyl-1,3-dioxolane and 4-methyl-2-propyl-1, 3-dioxolane were 81.3%, 86.9%, 53.0%, 66.9%, 72,3%, 79.0%, 66.8%, 76.9% respectively.

关 键 词：磷钨钼酸 二氧化钛 缩醛 缩酮 催化 

分 类 号：O623.51[理学—有机化学]