磷钨钼杂多酸/MCM-48催化剂合成缩醛(酮)  

Synthesis of Acetals and Ketals over H_3PW_6Mo_6O_(40)/MCM-48 Catalyst

作　　者：杨水金[1] 尹国俊[1] 

机构地区：[1]湖北师范学院化学与环境工程系生化分析技术湖北省重点实验室,湖北黄石435002

出　　处：《石油化工》2007年第8期816-820,共5页Petrochemical Technology

基　　金：湖北省教育厅重点科研基金资助项目;湖北省自然科学基金资助项目(2005ABA053)

摘　　要：采用浸渍法制备了负载型H3PW6Mo6O40／MCM-48催化剂。采用X射线衍射、傅里叶变换红外光谱、核磁共振等方法对催化剂及缩醛（酮）进行了表征。表征结果显示，负载后的H3PW6Mo6O40仍保持着Keggin结构。用H3pw6Mo6O40／MCM-48催化剂对以环己酮、丁酮、苯甲醛、丁醛、乙二醇、1，2-丙二醇为原料合成8种缩醛（酮）的反应条件进行了研究。考察了醛（酮）与二元醇摩尔比、催化剂用量、反应时间对8种缩醛（酮）收率的影响。实验结果表明，在r／（醛（酮））：n（乙二醇（1，2-丙二醇））=1：1．5、催化剂用量占反应物料总质量的0．6％、反应时间0．5h的条件下，8种缩醛（酮）的收率为67．2％～86．2％。A new environmental friendly catalyst, H3PW6Mo6O40/MCM- 48, was prepared by impregnation and was characterized by means of XRD, F-FIR and ^1H NM1L The results showed that Keggin structure of H3PW6Mo6O40 in H3PW6Mo6O40/MCM-48 kept unchanged. Catalytic activities of H3PW6Mo6O40/MCM- 48 catalyst in syntheses of cyclohexanone ethylene ketal, cyclohexanone 1,2 - propanediol ketal, butanone ethylene ketal, butanal - 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 separately investigated. Under optimal reaction conditions, mole ratio of aldehyde or ketone to dihydroxy alcohol 1 ： 1.5, mass fraction of catalyst in total reactants 0. 6% and reaction time 0. 5 h, yields of synthesized acetals or ketals can be in the range of 67. 2% -86. 2%.

关 键 词：缩醛 缩酮 MCM-48分子筛 磷钨钼杂多酸催化剂 二元醇 

分 类 号：TQ426.91[化学工程]