钒钼杂多酸盐相转移催化环戊烯氧化制备戊二醛
收稿日期: 2022-09-21
修回日期: 2022-10-14
网络出版日期: 2022-12-14
基金资助
国家自然科学基金(21878166); 山东省自然科学基金(ZR2020MB131)
Phase Transfer Catalytic Oxidation of Cyclopentene to Glutaraldehyde by Vanadium Molybdenum Heteropolyacid Salts
Received date: 2022-09-21
Revised date: 2022-10-14
Online published: 2022-12-14
Supported by
National Natural Science Foundation of China(21878166); Natural Science Foundation of Shandong Province(ZR2020MB131)
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[C4H9N2C3H3(CH3)]5VMo7O26, 并对溶剂种类、H2O2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(H2O2)∶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.
张旭征 , 于凤丽 , 袁冰 , 解从霞 , 于世涛 . 钒钼杂多酸盐相转移催化环戊烯氧化制备戊二醛[J]. 有机化学, 2023 , 43(4) : 1444 -1451 . DOI: 10.6023/cjoc202209027
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 [C4H9N2C3H3(CH3)]5VMo7O26 was screened out. The conditions of solvent type, H2O2 dosage, catalyst dosage, reaction temperature and time were optimized. Under the optimized reaction conditions [V(ethyl acetate)∶V(water)=4∶1, n(Cat.)∶n(H2O2)∶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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