The method of nickel-ferricyanide catalyst preparation is elaborated. The results of catalytic decomposition of trilon B on the prepared catalyst are presented. The developed method allows performing the efficient decomposition of trilon B (>99,9%) either in acid or in alkaline medium in temperature interval of 37-80°C. Technologically-fit dynamic conditions of the process, providing the intensity of a heterogeneous interaction, are selected and explored, and the nickel-ferricyanide catalyst resistance is achieved. The instrument flowchart of the developed method of catalytic decomposition is introduced for industrial application during the reprocessing of low- and medium-activity effluent, containing complexons.