Anodes having NiCo.sub.2 O.sub.4 catalyst used in the electrohydrodimerization of acrylonitrile to adiponitrile result in anode voltage requirements of less than about 2000 millivolts at 100 milliamperes per square centimeter of anode area. Typically, oxygen evolving anodes comprised of lead or carbon steel are utilized in the hydrodimerization of acrylonitrile to adiponitrile resulting in high voltage requirements. Anodes containing NiCo.sub.2 O.sub.4 catalyst require substantially reduced voltages and perform well in the conventional electrochemical adiponitrile production environment.