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In this work, a novel nano-sized mixed-crystal TiO2 catalyst was obtained under microwave irradiation in hydrogen peroxide solution and its sonocatalytic activity was also investigated through degradation of congo red dye. It was found that the sonocatalytic degradation effect of congo red using nano-sized mixed-crystal TiO2 powder was much higher than that using pure nano-sized rutile phase TiO2 powder. At last, the congo red dyes in aqueous solution were degraded completely and became some simple inorganic ions such as NO, SO and so on. The experiments indicated that the degradation method using such treated nano-sized rutile TiO2 powder as sonocatalyst could be used to treat those non- or low-transparent wastewaters effectively. [ABSTRACT FROM AUTHOR]