Using Ni3［Ge2O5］(OH)4 as the carrier and ammonium fluorotitanate as the raw material, the nano-TiO2/Ni3［Ge2O5］(OH)4 composite material was prepared by the hydrothermal-assisted liquid phase deposition method. The phase composition, structural characteristics and microscopic morphology were tested and analyzed through X-ray diffraction (XRD), Raman spectroscopy (RM), field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HTEM), ultraviolet-visible absorption spectroscopy (UV-Vis) and other characterization methods, and the effect of different loadings of titanium dioxide on the photodegradability of methylene blue of the nano-TiO2/Ni3［Ge2O5］(OH)4 composite material was explored. The results show that the experiment has realized the close combination and effective dispersion of nano-TiO2 and Ni3［Ge2O5］(OH)4. The TiO2 has an anatase structure with an average particle size of 20 nm. The composite material can effectively inhibit the recombination of photo-generated carriers, improve the adsorption performance of the material, and increase the photocatalytic efficiency of the material. When the molar ratio of TiO2 to Ni3［Ge2O5］(OH)4 in the composite material is 3.1∶1, the material has the highest photocatalytic efficiency for methylene blue, and the photodegradation rate of methylene blue in 90 min is 99.81%.