A novel kind of photocatalyst,namely NiOx-loading Fe /K2La2Ti3O10,was prepared by means of sol-gelmethod and impregnation method,and the photocatalytic activity of the product for hydrogen generation from watersplitting was investigated. Then,the photocatalyst samples were characterized and analyzed by means of SEM,XRD,UV-vis DRS and XPS. The results show that the prepared catalysts with layered structure are sensitive to visiblelight,and that,after the loading of NiOx,the photocatalytic activity increases to 477.3 μmol /g ( calculated asthe hydrogen production after 6 hours of accumulation) ,the band-edge absorption value has a blue shift,the directforbidden gap widens and the redox ability of electron-hole pairs improves. Moreover,as for the photoca-talyticmechanism,lanthanum in the compound serves as the main electron donor,the loading of NiOx provides addedactive sites for reactant adsorbing,and the NiO groups on the surface produce captures of free electrons,thus promotingthe reduction of H+ on the catalyst surface.With this action,the reduced nickel in bulk produces capturesof photo-induced electrons and transfers them to the surface timely,thus decreasing the recombination ratio of electronsand holes.