In this work, kaolin/steel slag particle electrodes (KSPEs) were synthesized using a calcination method, and they were used to degrade norfloxacin (NOR) wastewater in three-dimensional (3D) reactor. Characterization methods used by KSPEs included SEM, XRF, XRD and BET. The effects of cell voltage, initial pH, KSPEs dosage and initial NOR concentration on NOR degradation were studied in the optimization experiment of operating parameters. The NOR degradation rate and COD removal rate can reach 96.02% and 93.45% under the optimal parameters within 30 min, and energy consumption is 0.99 kWh m−3. As a result, KSPEs shows excellent catalytic performance and cycling, and still has high electrocatalytic activity after 10 cycles. Finally, the degradation mechanism and degradation pathways of KSPEs to treat NOR are proposed.