The D301R resin was screened to separate DSD acid from DSD acid wastewater. The effect of pH, temperature and time on adsorption behavior was investigated. Batch experiments indicated that the COD removal ratio of DSD acid wastewater was over 86%, and the COD of treated wastewater was under 100 mg/L at appropriate operating conditions. The results of column dynamic adsorption and regeneration showed that COD could be efficiently removed by the D301R resin from DSD acid wastewater, and the resin was easily regenerated by NaOH stripping.