Abstract A novel graphitic carbon nitride g-C3N4-NiTi-layered double hydroxide heterojunction film photo-catalyst (g-C3N4-NiTi-LDH) was prepared by facile hydrothermal synthesis. The g-C3N4 and g-C3N4-NiTi-LDH film samples were characterized by AFM, SEM, EDX, PL, XRD and DRS analysis. DRS analysis indicated a significant red shift of absorption edge due to the interfacial coupling effect between g-C3N4 and NiTi-LDH. PL analysis showed an efficient inhibition of electron-hole recombination in the blended g-C3N4-NiTi-LDH. A fixed-bed photoreactor containing conjugated g-C3N4-NiTi-LDH film-coated glass was fabricated and employed to photocatalytic degradation of methyl orange (MO). As a result, the g-C3N4-NiTi-LDH film showed greater photocatalytic activity compared with pure samples of g-C3N4 and NiTi-LDH film samples. Maximum MO degradation efficiency (100%) was achieved using g-C3N4-NiTi-LDH films within 240 min.