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在两类离子液体([bmim]BF_4与[bmim]PF_6)及异丙醇或无溶剂等条件下考察了壬二酸合成中的溶剂效应,并采用过氧化氢氧化油酸经二步反应合成了壬二酸。结果表明,[bmim]PF_6是合成壬二酸的最好溶剂。第一步较佳反应条件为:反应温度60℃,n(油酸)∶n(过氧化氢)∶n(钨酸)∶n(溶剂)=1.0∶3.0∶0.04∶1.24,反应时间1 h;第二步较佳反应条件为:m(中间产物):m(过氧乙酸)=1∶4,反应温度90℃,反应时间3 h。壬二酸收率为39%,熔点104~105.3℃,纯度达98%。
Solvent effects in the synthesis of azelaic acid were investigated in two types of ionic liquids ([bmim] BF_4 and [bmim] PF_6) and isopropanol or in the absence of solvents and the oxidation of oleic acid with hydrogen peroxide was followed by a two-step reaction Azelaic acid. The results show that [bmim] PF_6 is the best solvent for the synthesis of azelaic acid. The first reaction conditions are as follows: the reaction temperature is 60 ℃, n (oleic acid): n (hydrogen peroxide): n (tungstic acid): n (solvent) = 1.0: 3.0: 0.04: ; The second step preferred reaction conditions: m (intermediate): m (peracetic acid) = 1: 4, the reaction temperature was 90 ℃, the reaction time 3 h. Azelaic acid yield of 39%, melting point 104 ~ 105.3 ℃, the purity of 98%.