离子液体介入的均苯三甲酸氧钒催化氧化异丁香酚制香草醛  

Ionic Liquid-mediated Catalytic Oxidation of Isoeugenol to Vanillin via Oxovanadium 1,3,5-Benzenetricarboxylate

作　　者：黄红梅 肖毅[1,2] 杨晰雅 边文欢[1] 尹笃林 毛丽秋 

机构地区：[1]石化新材料与资源精细利用国家地方联合工程实验室 [2]化学生物学及中药分析教育部重点实验室,湖南师范大学化学化工学院,长沙410081

出　　处：《应用化学》2014年第8期952-957,共6页Chinese Journal of Applied Chemistry

基　　金：国家自然科学基金(20572021;20805014);湖南省教育厅科学研究基金(11C0809;12B077;12CY004)资助项目~~

摘　　要：合成了系列均苯三甲酸氧钒配合物催化剂,并进行了FT-IR、紫外-可见漫反射光谱(DR UV-Vis)及TG表征。系统考察了催化剂、不同种类的离子液体助剂、离子液体用量和反应时间等因素对异丁香酚氧化制备香草醛的影响。结果表明,n(VO2+)∶n(BTC(均苯三甲酸根))=1∶1时制备的催化剂VO(BTC)-1性能较佳。以VO(BTC)-1为催化剂、氯化1-十二烷基-3-甲基咪唑([C12mim]Cl)为助剂、丙酮为介质,当n(异丁香酚)∶n(H2O2)∶n([C12mim]Cl)=1∶2∶0.01时20℃反应24 h,异丁香酚可转化完全,香草醛收率达到87.2%。基于离子液体介入的催化剂光谱特征及反应结果,推测[C12mim]Cl/VO(BTC)-1与H2O2形成了高效的氧化反应体系从而有利于异丁香酚的温和转化。A series of oxovanadium 1,3, 5-benzenetricarboxylate complex catalysts was prepared and characterized by FT-IR, diffuse reflectance UV-Vis （DR UV-Vis ） and TG, respectively. The effects of catalyst, promoter such as ionic liquid, ionic liquid amount and reaction time on the oxidation of isoeugenol to vanillin were investigated systematically. VO （BTC）-1 with a molar ratio of VO^2＋ and BTC （1,3,5- benzenetricarboxylate） as 1 ： 1 exhibits better catalytic performance. Complete conversion of isoeugenol and 87. 2% yield of vanillin are achieved using VO（BTC）-1 as catalyst, 1-dodecyl-3-methylimidazolium chloride （ [ C12mim] Cl） as additive with the molar ratio of isoeugenol, H2O2 and [ C12mim] Cl as 1：2：0. 01 after 24 h reaction at 20 ℃ in acetone. The formation of a highly effective oxidation system from [ C12mim] C1/ VO（BTC）-1 and H2 02 is beneficial in the mild conversion of isoeugenol, as indicated by spectral characterization and the reaction results.

关 键 词：均苯三甲酸氧钒 香草醛 催化氧化 离子液体 异丁香酚 

分 类 号：O643.3[理学—物理化学] O625.4[理学—化学]