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The different mixing ratios of TiO2 nanoparticles were synthesized using sol–gel process by changing the temperature of calcinations. The crystal structures were characterized by X-ray diffraction (XRD). The photocatalytic action of TiO2 nanoparticles was investigated through the photooxidation of Rhodamine B in aqueous solution. The XRD results indicated that the rutile ratios of different calcination temperatures (500°C, 600°C, 700°C and 800°C, respectively) TiO2 nanoparticles were 0%, 20.87%, 92.41% and 100%, respectively. The TiO2 nanoparticles which calcinated at 600 °C had the highest photocatalytic action; under UV irradiation of 4 h, initial Rhodamine B concentration of 15 mg/L, TiO2 nanoparticles (calcinated at 600 °C) dosage of 1g/L, the degradation rate of Rhodamine B could achieve to 97.87%. The addition of rutile to anatase could particularly improve the photooxidation activity of TiO2 nanoparticles.