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以十二烷基二甲基叔胺、1,3-丙烷磺内酯、磷钨酸/硅钨酸为起始原料经季铵化、酸化两步原子经济反应,合成了两种室温下为液相的多磺酸基官能化杂多酸离子液体S3ILs和S4ILs。目标离子液体的结构经红外光谱、核磁共振波谱得到确认。以S3ILs、S4ILs为均相催化剂,质量分数35%的H2O2为氧化剂,在无溶剂条件下实现了苯甲醇的选择性氧化,n(离子液体)∶n(醇)∶n(过氧化氢)=0.05∶30∶45,反应温度70℃,反应时间4 h时,S4ILs将苯甲醇氧化为对应的苯甲醛,产率81%~100%,S3ILs则将苯甲醇一步氧化为对应的苯甲酸,产率64%~94%。离子液体经旋蒸除水、乙醚洗涤、真空干燥即可循环使用,循环使用5次催化活性基本保持不变。
Using dodecyldimethyl tertiary amine, 1,3-propane sultone and phosphotungstic acid / silicotungstic acid as starting materials, the two-step atom economic reaction was quaternized and acidified. Two compounds were synthesized at room temperature Liquid Phase Sulfonic Functionalized Heteropolyacid Ionic Liquids S3ILs and S4ILs. The structure of the target ionic liquid was confirmed by infrared spectroscopy and nuclear magnetic resonance spectroscopy. Using S3ILs and S4ILs as homogeneous catalysts and 35% H2O2 as oxidant, the selective oxidation of benzyl alcohol was achieved under solvent-free conditions. N (ionic liquid): n (alcohol) 0.05: 45:45, the reaction temperature is 70 ℃, the reaction time is 4 h, S4ILs oxidizes benzyl alcohol to the corresponding benzaldehyde in the yield of 81% -100%. S3ILs oxidizes the benzyl alcohol to the corresponding benzoic acid in one step Rate of 64% to 94%. The ionic liquid was removed by rotary evaporation, washed with ether and dried under vacuum to be recycled. The catalytic activity remained unchanged after 5 cycles.