用V^(5+)氧化邻硝基甲苯制备邻硝基苯甲醛

Electro-oxidation of o-Nitrotoluene to o-Nitrobenzaldehyde by V ^(5+)

以V5+ 为氧化剂 ,在硫酸溶液中氧化邻硝基甲苯为邻硝基苯甲醛 ,然后电解再生V5+ 。实验表明 ,在硫酸浓度为 10mol/L、V5+ 与邻硝基甲苯的摩尔比为 1∶11、反应温度为 80℃、反应时间为 6h、加入相转移催化剂十六烷基三甲基溴化铵 (1 3% )的条件下 ,硝基苯甲醛的收率为 4 4 6 %。反应后的水溶液相经分离后 ,在6 0℃、阳极电流密度 1 0× 10 -3 A/cm2 条件下 ,于石墨阳极上可电解再生V5+ 。

o-Nitrobenzaldehyde was prepared by oxidation of o-nitrotoluene by ammonium metavanadate in sulfuric acid solution. The maximum yield of o-nitrobenzaldehyde was 44.6% under the conditions:H 2SO 4 10 mol/L, mole ratio of ammonium metavanadate to o-nitrotuluene 1∶11, reaction temperature 80 ℃, reaction time 6 h, in the presence of cetyltrimethylammonium bromide:1.3%(mass fraction). The used aqueous solution could be separated and oxidized on graphite electrode for regeneration of V 5+ ion at 60 ℃ and anodic current density 1.0×10 -3 A/cm 2.