The three dimensions (3D) g-C3N4/TiO2 heterojunction photocatalyst has been synthesized and exhibits efficient pollutant degradation performances. The degradation efficiency of methylene blue (MB) and phenol is 4.0 and 4.5 times as high as bulk g-C3N4 in static system. In dynamic system, the pollutant can be continuously degraded without separation, and it is very stable for 90 h with a removal rate of 16.0%. The enhanced activity is mainly attributed to the 3D structure and heterojunction of g-C N-3(4)/TiO2. The 3D structure can not only effectively improve the adsorption-enrichment capability, but also supply multidimensional mass and electron transfer channels. Meanwhile, the heterojunction can promote the separation and migration of the photo-generated carriers. Therefore, the 3D g-C3N4/TiO2 heterojunction photocatalyst with separation free can facilitate the potential application in the treatment of water pollution.