Titania nanoparticles were obtained by an ultrasonic assistant sol-gel method. The prepared titania nanoparticles were characterized by X-ray diffraction (XRD) and differential scanning calorimeter (DSC). The photocatalytic properties of the prepared titania were evaluated from the photodegradation of X-3B solution. The thermalanalysis results showed that the weight loss of prepared TiO2particles ends at about 500°C, and the appropriate condition of calcination was found to be 2 h at 500°C. The XRD results showed that anatase was the main phase of prepared TiO2nanoparticle, and the average crystallite size of the TiO2particles, calcined for 2 h at 500°C was calculated as 15.3 nm using the Scherrer equation. The results demonstrated that such nanoTiO2showed high photocatalytic activities for X-3B degradation, whether it is under UV irradiation or sunlight irradiation.