Abstract: A novel Fe-H-732 was prepared by impregnation using a cationic resin as a support. The effect of the preparation conditions on the catalytic properties of Fe-H-732 has been studied based on single-factor experiments. The Fe-H-732 was used to activate persulfate (PS) to remove Metanil Yellow (MYG), and its catalytic capacity and degradation mechanism were investigated. The results show that Fe-H-732 has the highest MYG removal rate when the concentration of FeSO₄ solution is 0.05 mol·L^–1. The MYG removal rate of Fe-H-732/PS is 71.8% higher than that of FeSO₄, which indicated that Fe-H-732 exhibits excellent catalytic properties. MYG is eventually decomposed into CO₂, H₂O and inorganic salts, under the attack of sulfate (SO₄^·−) and hydroxyl radical (OH^·). The MYG removal rate of Fe-H-732 remained above 97.5% after five recycling runs, indicating the great stability of Fe-H-732. The results of this study can serve as a reference for the synthesis of high-efficiency and low-cost dye wastewater purification catalysts.