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Using Dy2O3, C4H6CoO4·4H2O, C6H8O7·H2O and HNO3 as the main raw materials, DyCoO3 was successfully prepared by sol-gel method. The DyCoO3 were characterized by TG-DSC, XRD, SEM and FT-IR. Using azo dye methyl orange solution as simulated wastewater, the degradation activity of DyCoO3 under UV irradiation was studied by changing the synthesis temperature and illumination time. The results show that the pure DyCoO3 can be prepared from 750 °C to 1000 °C, DyCoO3 particles were relatively uniform with average grain size of 2–3 μm. The photocatalytic activity of DyCoO3 sample calcined at 800 °C was the best. When DyCoO3 photocatalytic degradation of 10 mg/L methyl orange for 60 min, the degradation rate was close to 100%. This shows that DyCoO3 is a new type of photocatalyst with high efficiency, which lays a foundation for the application of wastewater treatment. [ABSTRACT FROM AUTHOR]