Using Tetrabutyl titanate (TBOT) as titanium source, the nanocrystal TiO2 was synthesized via hydrolysis deposition processing in cationic surfactant system at room temperature. The synthesized products were characterized by TEM and XRD. Photocatalytic degrade to NPE-10, phenol and DBS in solar irradiating were studied, respectively. The TiO2 powder showed excellent photocatalytic property. It was different to degrade three substances. NPE-10 was degraded nearly 70% in 2 hours, phenol was degraded nearly 95% in 8 hours, DBS was degraded nearly 82% in 8 hours.