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作 者:张旭征 于凤丽[2] 袁冰[2] 解从霞[2] 于世涛[1] Zhang Xuzheng;Yu Fengli;Yuan Bing;Xie Congxia;Yu Shitao(State Key Laboratory Base of Eco-chemical Engineering,College of Chemical Engineering,Qingdao University of Science and Technology,Qingdao 266042;College of Chemistry and Molecular Engineering,Qingdao University of Science and Technology,Qingdao 266042)
机构地区:[1]青岛科技大学化工学院生态化工国家重点实验室培育基地,青岛266042 [2]青岛科技大学化学分子与工程学院,青岛266042
出 处:《有机化学》2023年第4期1444-1451,共8页Chinese Journal of Organic Chemistry
基 金:国家自然科学基金(No.21878166);山东省自然科学基金(No.ZR2020MB131)资助项目。
摘 要:设计合成了一系列含高价态钼、钒等金属的杂多酸类相转移催化剂,用于催化环戊烯(CPE)氧化制备戊二醛的反应,筛选出催化活性最优的咪唑基钼钒酸盐催化剂[C_(4)H_(9)N_(2)C_(3)H_(3)(CH_(3))]_(5)VMo_(7)O_(26),并对溶剂种类、H_(2)O_(2)用量、催化剂用量、反应温度、时间等进行了条件优化.在优化的反应条件[V(乙酸乙酯)∶V(水)=4∶1,n(Cat.)∶n(H_(2)O_(2))∶n(CPE)=1∶170∶41.6,50℃,6 h]下,得到了88.7%的环戊烯转化率和62.1%的戊二醛选择性,并且催化剂在经过7次循环使用后仍能保持较高的催化活性.A series of heteropolyacid phase transfer catalysts containing high-valent molybdenum,vanadium and other metals were designed and synthesized to catalyze the oxidation of cyclopentene to glutaraldehyde,and the best imidazolyl molybdate-vanadate catalyst [C_(4)H_(9)N_(2)C_(3)H_(3)(CH_(3))]_(5)VMo_(7)O_(26) was screened out.The conditions of solvent type,H_(2)O_(2) dosage,catalyst dosage,reaction temperature and time were optimized.Under the optimized reaction conditions[V(ethyl acetate)∶V(water)=4∶1,n(Cat.)∶n(H_(2)O_(2))∶n(CPE)=1∶170∶41.6,50℃,6 h],88.7%cyclopentene conversion and 62.1% glutaraldehyde selectivity were obtained,and the catalyst still maintained high catalytic activity after 7 cycles of use.
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