对溴苯甲醛的间接电化学合成

Indirect Electrochemical Synthesis of p-Bromobenzaldehyde

以硫酸为介质,利用电解MnSO4生成Mn3+将对溴甲苯氧化为对溴苯甲醛;通过设计有机氧化正交实验L9(33),对电解氧化条件进行了优化.优化电解条件为:硫酸浓度6.5 mol/L、对溴甲苯与Mn3+摩尔比1∶4、电解时间6 h、合成时间3 h、温度65℃;相应的电流效率可达75.36%,对溴苯甲醛的产率可达75.47%.所采用的间接电化学合成工艺路线简单,使用后的媒质可以再生循环使用,符合绿色生产的要求.

p-Bromobenzaldehyde was electrochemical synthesized via indirect oxidation of p-bro motoluene by Mn^3＋ generated from electrolysis of MnSO4 in H2SO4. The electrolytic oxidation conditions were optimized based on orthogonal experiments of L9 （3^3）. The optimized electro lytic oxidation conditions were determined as concentration of sulphuric acid of 6.5 mol/L, mo lar ratio of p-bromotoluene to Mn^3＋ 1-4, electrolysis time of 6 h, synthetic time of 3 h, and temperature of 65℃. Under the optimized experiment conditions, the current efficieney and yield of p-bromobenzaldehyde could reach 75. 36% and 75.47%, respectively. The present indirect electrosynthesis process is simple in terms of operational path, and the used medium can be recycled without pollution, showing potential application for green production.