固体超强酸SO_4^(2-)/TiO_2-ZrO_2催化β-月桂烯与马来酸酐的Diels-Alder反应研究  

Study on Diels-Alder Reaction between β-Myrcene and Maleic Anhydride Catalyzed by SO_4^(2-)/TiO_2-ZrO_2 Solid Superacid

作　　者：罗金岳[1] 安鑫南[1] 雷福厚 

机构地区：[1]南京林业大学化学工程学院,江苏南京210037 [2]广西民族大学化学与生态工程学院,广西南宁530006

出　　处：《林产化学与工业》2007年第6期90-94,共5页Chemistry and Industry of Forest Products

基　　金：江苏省自然科学基金资助项目(BK2007218);广西高校人才小高地科研基金资助项目(无编号)

摘　　要：研究了SO42-/TiO2-ZrO2型固体超强酸催化剂的制备及其催化β-月桂烯与马来酸酐的Diels-Alder反应,通过GC、GC-MS和红外分析,确定其主产物为4-(4-甲基-3-戊烯基)-4-环己烯-1,2-酸酐。结果表明,该催化剂对β-月桂烯与马来酸酐的Diels-Alder反应有较高的催化活性和较好的选择性。考察了其催化性能的影响因素。结果表明,适宜的催化剂制备条件是:n(钛)∶n(锆)为1∶1,焙烧温度450℃。Diels-Alder反应优化的工艺条件:n(β-月桂烯)∶n(马来酸酐)为1∶1、反应时间4 h、反应温度60℃、催化剂用量1%。该条件下β-月桂烯转化率96.5%,产物选择性94.0%,产物得率90.7%。同时考察了催化剂放置时间对异构产物的影响和催化剂重复使用情况。Diels-Alder reaction between β-myrcene and maleic anhydride catalyzed by SO4^2-/TiO2-ZrO2 solid superacid was investigated. By using GC, GC-MS and IR, main product in this reaction is confirmed to be 4-（4-methyl-3-pentenyl）-4-cyclohexene-1,2-dicarboxylie anhydride. The result shows that this catalyst has high catalytic activity and good selectivity to the DielsAlder reaction between β-myrcene and maleic anhydride. The effects of catalyst to its catalytic activity are investigated. The result also shows that the optimum conditions for the preparation of SO4^2-/TiO2-ZrO2 catalysts are as follows： n（Ti） ： n（Zr） 1 ： 1, calcination temperature at 450 ℃. Under these conditions, the optimum conditions for the Diels-Alder reaction are as follows： n（β- myrcene） ： n（maleic anhydride） 1 ： 1, reaction time 4 h, reaction temperature 60 ℃, and the ratio of solid superacids to β- myrcene mass part 1% , the β-myrcene conversion is 96.5 %, and the 4-（4-methyl-3-pentenyl） -4-cyclohexene-1 ,2-dicarboxylic anhydride selectivity is 94.0 %, or yield is 90.7 %. Furthermore, the effect of storage time of the catalysts on the reaction and the experiments on regeneration of catalysts are carried out.

关 键 词：Diels—Alder反应 β-月桂烯 马来酸酐 SO4^2-/TiO2-ZrO2催化剂 

分 类 号：TQ426[化学工程] O643.36[理学—物理化学]