The mesoporous N, S-codoped TiO2(B) nanobelts are synthesized via hydrothermal synthesis and post-treatment, and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), N-2 adsorption-desorption measurements (BET), X-ray photoelectron spectra (XPS), and UV-vis diffuse reflectance spectra (DRS). The results show that the prepared samples are mesoporous structured and exhibit stronger absorption in the visible light region with red shift in the absorption edge. The photocatalytic activity of N, S-codoped mesoporous TiO2(B) nanobelts is evaluated by the photocatalytic photodegradation of potassium ethyl xanthate (KEX) under visible light irradiation. It is found that the photocatalytic activity of the prepared samples increases with increasing the molar ratio of thiourea to Ti (R). At R = 3, the photocatalytic activity of the N, S-codoped TiO2(B) sample TBLTS-3 reaches a maximum value. With further increasing R, the photocatalytic activity of the sample decreases. The high photocatalytic activity of N, S-codoped TiO2(B) nanobelts can be attributed to the balance between strong absorption in visible light region and low recombination rate of electron/hole pairs. (C) 2010 Elsevier B.V. All rights reserved.