间接电还原制备4-氯-3,5-二氨基苯甲腈  

Preparation of 4-Chloro-3,5-diaminobenzonitrile by Indirect Electroreduction Method

作　　者：高乾善[1] 颜国刚[1] 吕瑞敏[1] 高光杰 胡建强 

机构地区：[1]山东省分析测试中心,山东济南250014 [2]山东博士伦福瑞达制药有限公司,山东济南250101

出　　处：《山东化工》2009年第2期4-7,共4页Shandong Chemical Industry

摘　　要：采用间接电化学还原路线,在离子膜电解槽中,以铜板作阴极电极,石墨作阳极电极,电流密度50mA/cm2,将Sn4+还原为Sn2+,然后用该电解液还原4-氯-3,5-二硝基苯甲腈为4-氯-3,5-二氨基苯甲腈。实验结果表明,盐酸浓度为4mol/mL,反应温度20℃,Sn2+与4-氯-3,5-二硝基苯甲腈的物质的量之比为6.6/1有最佳的反应效果。母液循环试验5次,平均产率88.1%,平均电解效率74.2%。4 -Chloro- 3,5 -diaminobenzonitrile was prepared by indirect electrochemistry reduction. At first, Sn^4＋ was reduced to Sn^2＋ in ionic membrane electrolytic cell using the copper plate as negative electrode and the graphite as anode electrode, and the current density was 50mA/cm^2, then, 4 - ehloro - 3,5 - dinitrobenzonitrile was reduced to the product by the electrolyte. The optimum react conditions were given in this paper. The concentration of HCl was 4.0 mol/L, and the react temperature was 20℃, and the molar ratio of Sn^2＋ and 4 - chloro - 3,5 - dinitrobenzonitrile was 6.6/1. The recycle use of the mediator was also studied and the average yield of product was 88.1%. and the average current efficiency was 74.2%.

关 键 词：4-氯-3 5-二硝基苯甲腈 4-氯-3 5-二氨基苯甲腈 间接电还原 制备 

分 类 号：TQ246.3[化学工程—有机化工]