活性炭负载磷钨杂多酸催化合成缩醛(酮)  

Synthesis of acetals and ketals catalyzed by phosphotungstic acid supported on active carbon

作　　者：杨水金[1] 杜心贤[1] 吕宝兰[1] 

机构地区：[1]湖北师范学院化学与环境工程系,湖北黄石435002

出　　处：《北京化工大学学报（自然科学版）》2005年第1期81-84,共4页Journal of Beijing University of Chemical Technology(Natural Science Edition)

基　　金：湖北省优秀中青年科技创新团队基金(2004CX0711);湖北省教育厅重点科研基金(2004D007)

摘　　要：以活性炭负载磷钨杂多酸为催化剂 ,对以乙酰乙酸乙酯、环己酮、丁酮、苯甲醛和正丁醛与二元醇 (乙二醇 ,1 ,2 丙二醇 )为原料合成 1 0种缩醛 (酮 )的反应条件进行了研究 ,较系统地研究了醛 /酮与二元醇摩尔比、催化剂用量、反应时间诸因素对收率的影响。结果表明 ,在n(醛或酮 )∶n(乙二醇或 1 ,2 丙二醇 ) =1∶1 5 ,催化剂的用量占反应物料总质量的 1 0 %,反应时间为 1h条件下 ,1 0种缩醛 (酮 )的收率在 6 0 0 %～ 95Catalytic activities of the active carbon supported with phosphotungstic acid were reported for synthesizing 2 methyl 2 ethoxycarbonylmethyl 1,3 dioxolane,2,4 dimethyl 2 ethoxycarbonylmethyl 1,3 dioxolane, 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. It is demonstrated that the active carbon supported with phosphotungstic acid is an excellent catalyst. Various factors concerned in these reactions were investigated. The optimum conditions are found, that is, the molar ratio of aldehyde / ketone to glycol 1/1 5, the mass percent of the catalyst used to the reactants 1 0%, and the reaction time 1?h. Under these conditions, the yield of 2 methyl 2 ethoxycarbonylmethyl 1,3 dioxolane is 76 4%, and 2,4 dimethyl 2 ethoxycarbonylmethyl 1,3 dioxolane 75 8%, the yield of cyclohexanone ethylene ketal 70 8%, and cyclohexanone 1,2 propanediol ketal 83 3%, the yield of butanone ethylene ketal 60 0%, and butanone 1,2 propanediol ketal 84 6%, the yield of 2 phenyl 1,3 dioxolane 83 0%, and 4 methyl 2 phenyl 1,3 dioxolane 81 3%, the yield of 2 propyl 1,3 dioxolane 91 4%, and 4 methyl 2 propyl 1,3 dioxolane 95 4%.

关 键 词：磷钨酸 缩醛 缩酮 活性炭 催化 

分 类 号：TQ426.91[化学工程] TQ655