A novel three-dimensional network nickel foam/PbO2 combination electrode (PbO2-NF) with high electrochemical degradation efficiency to norfloxacin was successfully fabricated through the electrodeposition of PbO2 on the substrate of nickel foam. The characterization of an PbO2-NF electrode, including surface morphology, elemental components, electrochemical performance, and stability was performed. In electrochemical oxidation tests, the removal efficiency of norfloxacin (initial concentration for 50 mg/L) on PbO2-NF reached 88.64% within 60 min of electrolysis, whereas that of pure nickel foam was only 30%. In the presence of PbO2-NF, the optimum current density, solution pH, electrode spacing for norfloxacin degradation were 30 mA/cm2, 11, and 3 cm, respectively. The electric energy consumption for 80% norfloxacin was approximately 5 Wh/L. Therefore, these results provide a new anode to improve the removal of norfloxacin in the wastewater with high efficiency and low energy consumption.