应用离子交换膜法电解邻氯硝基苯合成2,2′-二氯氢化偶氮苯.讨论了电极活化条件、电流密度、电解液温度等因素对电解还原反应的影响.结果表明:在反应温度t=80℃,阴极、阳极电解液分别为10%和30%(by m ass)的NaOH溶液,电流密度4.2A/dm2条件下电解,电流效率最高,可达73%,收率为83%.
Using an ion exchange membrane as a separator,the 2,2′-Dichlorohydrazobenzene is synthesized by the electrolytic reduction of o-chloronetrobenzene.The effects of electrode activation condition,current density,electrolyte temperature on electrolytic reduction are discussed.It was found that the optimum reaction temperature is 80 ℃.When the electrolyte concentration was 30% NaOH at the anode and 10% NaOH at the cathode,current density is 4.2A/dm2,the current efficiency reached 73% and yield is 83%.
[1]Xu K X(徐克勋).Fine organic chemical technologyrawmaterial and intermediate[M].Beijing:ChemicalIndustry Press,1998.3-411.
[2]Song C M(宋车明),Li S D(李树德),Zhang F M(张凤明).Preparation of 1,2-diaminobenzene by catalytichydrogenation[J].Dyes Industry,1993,30(4):23-26,14.
[3]Wang Y L(王亚林),Mu W Y(木文宇),Qiu X Q(邱显权).New synthetic technology of 3,3′dichlorobenzi-dine hydrochloride[J].Journal of Chemical Technolo-gy,1998,12(4):22-27.
[4]Jiang L C(江琳才).Electrical syntheses[M].Beijing:High Education Press,1993.53-54.
[5]Zhai Z Y(翟振月),Wang L A(王领安).Study onelectrosyntheses technology of 2,2′-dichlorohydrazo-benzene[J].Chemical Technology of HeBei,2005,3:44-46.
[6]Ma C A(马淳安).Introduction of electro-organic syn-theses[M].Beijing:Science Press,2003.221-223.
[7]Wang Y D(王雅丹),Wang Q N(王其南),LI P J(李培金).Synthesis of dichlorobenzidine hydrochloride u-sing an ion exchange membrane[J].Journal of BeijingUniversity of Chemical Technology,2006,33(3):61-63.
[8]Hoormann D,Kubon C.Analysis and minimization ofcell voltage in electro-organic syntheses using the solidpolymer electrolyte technology[J].Journal of Electroa-nalytical Chemistry,2001,507:215-225.
