固体超强酸催化合成香草醛1,2-丙二醇缩醛  

Synthesis of Vanillin Propylene Glycol Acetal Catalyzed by Solid Superacid

作　　者：刘飞[1] 罗金岳[1] 

机构地区：[1]南京林业大学化学工程学院,江苏南京210037

出　　处：《精细化工》2010年第2期155-159,共5页Fine Chemicals

基　　金：江苏省自然科学基金资助项目(BK2007218);广西林产化学品开发与应用重点实验室开放基金课题(GXFC08-08)~~

摘　　要：研究了固体超强酸催化合成香草醛1,2-丙二醇缩醛的工艺。制备得到一系列固体超强酸,比较其对合成香草醛1,2-丙二醇缩醛的催化效果,其中SO42-/ZrO2最佳,固体超强酸催化效果均优于磷酸和柠檬酸。采用SO42-/ZrO2催化剂适宜的工艺条件为:香草醛用量为0.05mol,n(香草醛)∶n(1,2-丙二醇)=1∶2.4;带水剂为甲苯(20mL);催化剂用量为香草醛质量的0.25%;反应时间为1.0h。在该条件下,香草醛1,2-丙二醇缩醛收率为95.1%,经减压蒸馏后,总收率90.5%,相对质量分数为99.5%。利用红外、气质联用对产物结构进行了鉴定。将该催化剂焙烧后放置20d使用,收率仍可达91.1%。该工艺具有反应时间短,催化剂活性高、稳定,后处理简单等特点。The synthesis of vanillin propylene glycol acetal catalyzed by solid superacid was investigated. A series of solid superacids were prepared and used to synthesize vanillin propylene glycol acetal. Solid superacids excel phosphoric acid and citric acid, and SO2^4-/ZrO2 is the best Catalyst. The optimum conditions of using SO2^4-/ZrO2 are as follows：when vanillin is 0.05 mol,n（ vanillin）：n（ 1,2- propylene glycol） = 1 ： 2.4 ; the water-carrying agent is toluene （ 20 mL） ; the amount of catalyst is 0. 25% of the weight of vanillin; reaction time 1.0 h. Under these conditions, the yield of vanillin propylene glycol acetal is 95.1%. The total yield is 90. 5% and the relative mass fraction is 99.5% after vacuum distillation. The structure of the product was identified by IR and GC - MS. The yield can still achieve 91.1% when the catalyst was calcined 20 days later. The reaction time is short and the catalyst is efficient and stable. The post-processing is simple in this process.

关 键 词：固体超强酸 SO2^4-/ZrO2 香草醛1 2-丙二醇缩醛 香草醛 1 2-丙二醇 香料 

分 类 号：TQ655[化学工程—精细化工]