Abstract. The large-pore mesoporous Bi-B-TiO2 nanoparticles with the different Bi/Ti rations were prepared by EISA(evaporation-induced self-assembly) method. The prepared catalysts were characterized by X-ray diffraction, transmission electron microscopy, N2 absorption-desorption, ultraviolet visible light spectroscopy and photoluminescence spectroscopy technologies. The results revealed that all the samples are large aperture mesoporous structures. The crystallite sizes were in the range7-11nm, as confirmed by the results obtained from TEM images. The photodecomposition experiments showed that the photodegradation activity of Bi-B-doped TiO2 was higher than that of undoped TiO2 in degradation of 2, 4–dichlorophenol under visible light irradiation.