A series of g-C3N4–Sb2S3/Sb4O5Cl2 (SCL-CX) composite photocatalysts were successfully prepared via a hydrothermal method. The as-prepared materials were characterized by TM3000, powder X-ray diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS) and UV–vis diffuse reflectance spectra (UV–vis DRS). The obtained photocatalyst showed higher photocatalytic activity than pure g-C3N4, Sb4O5Cl2 and Sb2S3/Sb4O5Cl2 (SCL). The optimum photocatalytic of the composite with the mass of 170mgg-C3N4 and a degradation efficiency up to 95% for methyl orange (MO) under visible light was achieved within 60min. The enhanced photocatalytic performance could be attributed to the stronger absorption in the visible region and the more efficient electron–hole separation.