The iron oxychloride/pillared montmorillonite (FeOCl/MMT) catalyst was prepared by wet impregnation method and solid melting method. Various characterization techniques were used to analyze the microscopic morphology and structure of a series of catalysts. Moreover, the catalysts were used to treat magenta simulated dye wastewater through catalytic wet peroxide oxidation (CWPO) degradation. The magenta removal rate and chemical oxygen demand (COD) removal rate of the magenta simulated dye wastewater were used to evaluate the catalytic performance of the catalyst, and the optimal catalyst preparation conditions were selected. The results showed that the solid melting method was more favorable to the preparation of the catalyst, and the COD removal rate of wastewater can reach 70.8% when the FeOCl load was 3%. Moreover, 96.2% of the magenta in the solution has been removed. The COD removal rate of the magenta wastewater decreased by only 12.4% after the catalyst was repeatedly used six times, indicating that the catalyst has good activity and stability. The Fermi equation can simulate the reaction process of the catalyst treating magenta wastewater at high temperature.