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通过水热法合成新型Dawson结构磷钨钼杂多酸催化剂,对催化剂进行FT-IR、TG-DTA表征,并用于催化30%H2O2氧化环己酮制备己二酸.通过正交实验确定了优化工艺条件,并探讨了反应机理.结果表明,当n(环己酮)∶n(过氧化氢)∶n(草酸)∶n(催化剂)=100∶400∶1.00∶0.15,反应温度100℃,反应时间5h,进行3次平行实验,己二酸平均收率为71.6%,纯度为99.7%.经蒸发浓缩,催化体系可重复使用5次,收率为50.3%.
A new Dawson phosphomolybdotungstomolybdic acid catalyst was synthesized by hydrothermal method. The catalysts were characterized by FT-IR and TG-DTA, and used to catalyze the oxidation of cyclohexanone with 30% H2O2 to prepare adipic acid. The optimum conditions The reaction conditions were discussed and the reaction mechanism was discussed.The results showed that when n (cyclohexanone): n (hydrogen peroxide): n (oxalic acid): n (catalyst) = 100: 400:1.00:0.15, reaction temperature 100 ℃, The reaction time was 5h, and three parallel experiments were carried out, the average yield of adipic acid was 71.6% and the purity was 99.7% .After evaporation and concentration, the catalytic system could be reused 5 times and the yield was 50.3%.