SO_4^(2-)/TiO_2-SnO_2固体超强酸无溶剂催化合成季戊四醇双缩苯乙酮  

Synthesize acetophenone pentaerythritol diketal catalyzed by SO_4^(2-)/TiO_2-SnO_2 solid superacid without solvent

作　　者：刘海舰[1] 郑晓凤[1] 

机构地区：[1]曲阜师范大学化学与化工学院,山东曲阜273165

出　　处：《化工中间体》2013年第9期48-53,共6页

摘　　要：在无溶剂条件下,以SO_(42)-/TiO_2-SnO_2固体超强酸为催化剂,合成了季戊四醇双缩苯乙酮,考察了催化剂的用量、反应物的摩尔比、反应时间和反应温度等对缩酮反应的影响。结果表明,催化剂的用量为反应物总质量的1.6%,季戊四醇和苯乙酮的摩尔比为1:2.2,反应温度为175℃,反应时间为4 h时,季戊四醇双缩苯乙酮的产率达98.6%。对产物进行了1HNMR、MS、单晶衍射表征。该方法具有合成工艺简单、温度可控、产率高、产物易于分离、不产生污染、催化剂可重复使用等优点,具有良好的工业应用前景。In this paper,acetophenone pentaerythritol diketal was synthesized under solvent-free condition,catalyzed by SO_4^(2-)/TiO_2-SnO_2 solid superacid.The influences of quantity of catalyst,ratio of reactants,reaction time and reaction temperature were investigated.As a result,the optimal conditions for this reaction was obtained as follows:the catalyst amount1.6%wt%of the whole reactants,molar ratio of pentaerythritol to acetophenone 1:2.2,reaction temperature 175℃ and reaction time 4 h.The yield of acetophenone pentaerythritol diketal was up to 98.6%.The compound was characterized by IR spectra.1 HNMR and single-crystal X-ray analyses.The method has good prospects for industrial applications based on the advantages such as the simple synthesis process,temperature-controlled,high yield,easy separation of the product,no pollution,reusable catalvst,etc.

关 键 词：季戊四醇 苯乙酮 季戊四醇双缩苯乙酮 固体超强酸 无溶剂条件 

分 类 号：TQ244.2[化学工程—有机化工]