Abstract: The advanced oxidation technology based on peroxymonosulfate (PMS) activation offers unique advantages in degrading emerging pollutants. In this experiment, iron disulfide (FeS₂) was encapsulated on nitrogen-doped carbon nanotubes (NCNT) to prepare FeS₂-modified nitrogen-doped carbon nanotubes (FeS₂@NCNT). Using norfloxacin (NOR) as the target pollutant, a study was conducted on the mechanism and performance of FeS₂@NCNT in electro-activating PMS for NOR degradation. The main research includes the following: characterization and electrochemical performance tests of the material revealed that FeS₂@NCNT exhibits excellent electrocatalytic activity and low impedance, with favorable charge storage capacity and electron transfer ability. In the FeS₂@NCNT/PMS system, the effect of various parameters on NOR removal efficiency was examined, and the optimal conditions were determined to be a current density of 15 mA/cm², pH of 6.0, and PMS concentration of 3 mmol/L. Under these conditions, NOR removal reached 93.0% within 60 minutes. Radical quenching experiments indicated that singlet oxygen (¹O₂) is the primary reactive species for NOR degradation, while superoxide radicals (O₂^•⁻), hydroxyl radicals (•OH), and sulfate radicals (SO₄^•-) also contribute to some extent. Additionally, the study explored the impact of coexisting anions on system performance and confirmed that FeS₂@NCNT maintained good catalytic activity after multiple cycles, highlighting the application potential of this composite material in water treatment.