Copper iron tungstate/carbon paper electrocatalytic composite electrode was prepared on carbon paper substrate by hydrothermal synthesis method and calcination method, and characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive spectroscopy (EDS). The electrochemical performance was tested by linear sweep voltammetry (LSV) and AC impedance spectroscopy (EIS). After that, diclofenac sodium was used as a pollutant in pharmaceutical wastewater, and the prepared electrode was used for electrocatalytic oxidation degradation test. The results showed that nano copper iron tungstate had been formed and successfully loaded on the carbon fiber surface of carbon paper. The oxygen evolution potential of copper iron tungstate/carbon paper composite electrode was higher than that of polydopamine modified carbon paper electrode. The radius of semicircular arc in EIS diagram was relatively small, indicating that the charge transfer resistance was small and the electrode reaction rate was relatively large. When the Cu: Fe ratio on the electrode surface was 1:1, the degradation rate of organic compounds was better than that of other electrode materials with Cu: Fe ratio. In the degradation experiment, it was found that when the current density was 50 mA/cm2, the initial concentration of diclofenac sodium was 2 mmol/L, the electrolyte concentration was 0.08 mol/L, and the pH value was 7, the degradation rate of diclofenac sodium and COD removal rate by the composite electrode were more than 90%. Therefore, the electrode has a good application prospect in the field of pharmaceutical wastewater treatment.