The degradation of radioactive ion-exchange resin (IER) achieved by oxidizing it with hydrogen peroxide in an aqueous medium in the presence of iron (or copper) ion as catalyst was investigated. This method could be used to dissolve waste resins completely to form water and carbon dioxide in a short period of time while minimizing the production of organic sludge. The reaction kinetics of the solid resin and organic chemicals were obtained to describe the degradation system. The concentrations of metallic catalysts (CU2+ and Fe2+), different kinds of IERs and different concentrations of hydrogen peroxide were used to evaluate the optimum reaction conditions for degradation. The reaction paths Of CU2+ and Fe2+ were determined using SEM-EDS. It was found that acetic acid coexists with anionic IER in the oxidative-decomposing system, which leads to a high reaction rate and presents the foam from forming. The performance of a fed-batch process was evaluated for industrial applications.