A novel g-C3N4/NiTiO3 composite was fabricated by one-step calcination method using dicyandiamide, tetrabutyl titanate and nickel acetate as the precursors. The samples were characterized by scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, N2 adsorption/desorption isotherms, UV-vis diffuse reflection spectroscopy and photoluminescence spectroscopy. It was indicated that the hybrids owned a large surface area, mesoporous structure and improved visible light absorption. The optimal g-C3N4 content in the g-C3N4/NiTiO3 composite was 18.4 wt%, and the corresponding visible-light removal rate for nitrobenzene was 0.0132 min−1, about 1.6 times higher than that of pure NiTiO3. The enhanced photocatalytic activity may be attributed to the large surface area, stronger absorption in the visible region and efficient electron–hole separation.