Ti 2 O(PO 4) 2 •2H 2 O nanobelts were successfully synthesized by a simple, template and surfactant-free hydrothermal method,in which titanium sulfate(Ti(SO 4) 2) and concentrated phosphoric acid (H 3 PO 4) were used as titanium and phosphorus source, respectively. The synthesized materials were characterized by X-ray diffraction(XRD), Scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR). The nanobelts are ca. 60 nm in width as well as 20nm in thickness, and its length can reach several micrometers. The adsorption performance of the synthesized nanobelts was investigated. The results indicate that the Ti 2 O(PO 4) 2 •2H 2 O nanobelts have good adsorption ability to methylene blue (MB). The removal rate of MB could reach to 50 % within 10 min, the equilibrium adsorption time is about 70 min as well as the equilibrium capacity is about 150 mg/g at room temperature. It indicate that the Ti 2 O(PO 4) 2 •2H 2 O could be a promising candidates for waste water treatment. The possible adsorption mechanism was also suggested.