Nano-size CuFeO2 was prepared with chemical coprecipitation method and its nanoparticles were characterized by scanning electron microscopy/ energy disperse spectroscopy (SEM/EDS), X-ray diffraction (XRD), Fourier transform infrared (FT-IＲ) and BET analysis. The results show that the size of CuFeO2 synthesized is about 20 nm and its specific area is 258.3 m2/g. The adsorption of methylene blue (MB) is a pseudo second-rate kinetic process and reaches equilibrium in 40 min，in good agreement with the Langmuir adsorption model. CuFeO2 has good adsorption ability and its maximum adsorption capacity reaches 123.0 mg/g at room temperature and pH = 7. CuFeO2 can be used as adsorption material with high capacity for effective removal of methylene blue from waste water.