The magnetic Fe-MOFs derivatives obtained by high-temperature calcination under inert atmosphere have been studied and acted as high-efficiency catalysts in wastewater remediation. However, due to the shortcoming that the unstable structure of Fe-MOFs derivatives tends to collapse and agglomerate easily, it is necessary to find a support to improve its dispersibility and stability. In this work, an effective method was provided to fabricate biochar-loaded MIL-53(Fe) derivatives (BC@FexC) to activate peroxydisulfate (PDS) for norfloxacin (NOR) degradation. The efficiency of the BC@FexC/PDS system for NOR removal can reach to 91.2% within 15 min, and the reaction constant (k) was 52.15 times of BC/PDS and 22.19 times of FexC/PDS. Characterization results illustrated that the superior spatial pore structure and exposed active sites of BC@FexC allowed NOR to diffuse and interact with the catalyst efficiently. OH, SO4− and 1O2 were the main reactive oxygen species involved in NOR degradation. Moreover, the BC@FexC/PDS system exhibited excellent stability that almost unaffected by various environmental conditions (such as tap water, river water, and medical wastewater), which would provide a reference path for application in actual water treatment.