Abstract: TiO₂ pillared graphene nanocomposites were synthesized by hydrothermal treatment in this paper, the TiO₂ nanoparticles and TiO₂ pillared graphene nanocomposites were prepared in different reaction times and reaction procedures, and the properties of catalytic degradation on methylene blue (MB) were studied. In the results, the optimum conditions for preparing composite materials are defined as the two-step hydrothermal method at the hydrothermal temperature of 180 ℃, the TiO₂ nanoparticles exhibits good crystal structure, and the nanocomposites show a higher photocatalytic efficiency in the process of MB degradation. This work can open up new ways to obtain the photoactive graphene-semiconductor nanocomposites.