An investigation on lead dioxide electrodeposition from methanesulfonate electrolytes additionally containing Ni 2+ is reported. It is shown that the lead dioxide electrodes micromodified by nickel have different physicochemical properties vs. nonmodified PbO 2-anodes, that are formed during the deposition. The electrocatalytical reactivity of the electrodes involved in comparison to both the oxygen evolution, as well as to the electrooxidation of 2,4-dichlorophenoxyacetic (2,4-D) acid is investigated. The processes of electrochemical oxidation of 2,4-D on various materials occur qualitatively with the same mechanism and differ only in the reaction rate. It is shown that the Ni-PbO 2-anode possesses the highest electrocatalytic activity: the destruction rate of 2,4-D on it increases 1.5 times in comparison with the unmodified lead dioxide. The chemical oxygen demand (COD) of a 0.4 mM solution of 2,4-D, determined by the dichromate method, is 90.0 mg dm-3 which is 94 % of the theoretical value.