The development of heterogeneous Co-based catalysts with an effective combination mode of Co/Fe and supporter, a facile synthetic method, and a low treatment costs is an important environment challenge for azo dyes degradation by peroxymonosulfate (PMS) activation. In this study, NaA zeolite supported Co x Fe y with various molar ratio of Fe/Si and Co/Fe was synthesized by a facile hydrothermal process, and used to activate PMS for Acid Orange 7 (AO7) degradation. NaA zeolite supported Co 2 Fe 1 with the Fe/Si molar ratio of 1:10 showed superior catalytic performance compared with other NaA zeolite supported Co x Fe y . In a system containing 0.6 g/L catalysts, 4 mM PMS, pH 5 and T = 30℃, 95.8% AO7 and 79.1% COD conversion could be achieved at 20 and 60 min, respectively, and the rst order kinetic rate constant reached 0.14795 min − 1 . Moreover, NaA zeolite supported Co 2 Fe 1 /PMS system exhibited excellent catalytic effect in a wide pH range of 3-9. Temperature had an obvious effect on AO7 degradation, and the activation energy was 31.36 kJ/mol. HCO 3 − demonstrated an obvious depression on AO7 degradation, while Cl − , SO 4 2− and H 2 PO 4 − had a relatively poor impact. Quenching experiments showed that both sulfate radicals (SO 4 •-) and hydroxyl radicals (•OH) were generated in the PMS reaction system, and the (SO 4 •-) was the dominant active radical. During 3 cycles experiments, an acceptable AO7 conversion ratio (91.8%) within 30 min was arrived, suggesting the good stability of NaA zeolite supported Co 2 Fe 1 .