To eliminate organic pollutants, the Photo-Fenton reaction is an advanced approach. Graphite oxide was prepared through modified Hummers method in this study. By microwave assisted method, cobalt ferrite/reduced graphene oxide composites were synthesized. The chemical structure and properties of composites were characterized by Raman spectroscopy, then the prepared CoFe2O4/RGO composites were employed into experiment of degradation. The Raman spectroscopy demonstrated the peaks in low-frequency (200-700cm-1) were conformed to scattering modes of CoFe2O4, the Raman intensities ID/IG of composite increased obviously as the synthesis time on microwave increased may attributed to the forming the smaller sp2 domains during the reduction process. Moreover, different catalyst composites were introduced into photo degradation experiment under UV-light, the results showed the catalytic activity of CoFe2O4 was enhanced greatly by introduction of reduced graphene oxide. Meanwhile, the composite with microwave time 200 second found out to show the greatest degradation activity, which maintained 90% of performance ability for five times recycling test.