In this paper, a titanium electrode was used in the electrochemical synthesis of 2,2'-dichlorohydrazobenzene (DHB) from o-chloronitrobenzene (o-CNB). The catalytic activity of four different catalysts PbO, Bi2O3, Sb2O3, and SnO2 on the titanium electrode was investigated. Both PbO and Bi2O3 demonstrated high catalytic activity. The chemical yield of DHB was 93.9% in 6 hours using PbO and 95.5% in 6.5 hours using Bi2O3, respectively. A new catalyst loading method on the titanium electrode was explored by cyclic voltammetry (CV). The CV method formed **aller and more uniform size PbO crystals at a scanning rate of10 mv/s and, ultimately, the yield of DHB reached 93% within a shorter reaction time. A possible reaction mechani** was presented and the origin of the by-product o-CA was found. (C) 2015 The Electrochemical Society. All rights reserved.