摘要： The heavy metal copper ion from the industrial wastewater were recycled by sulfonated polystyrene, which were converted to Cu/Cu2O/CuO/SPS heterojunction photocatalyst through the hydrothermal synthesis process. The hydrothermal synthesis temperature was investigated on the surface morphology, crystal structure and photocatalytic performance of the as-prepared samples. The samples were characterized by scanning electron microscope (SEM), high resolution transmission electron microscope (HRTEM), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD) and UV–Vis diffuse reflectance spectra (UV–Vis DRS). The photocatalytic activities of the samples were investigated by the degradation of rhodamine B (RhB) under visible light irradiation. The results showed that Cu, Cu2O and CuO nanoparticles are uniformly distributed on the surface of sulfonated polystyrene microsphere. Meanwhile, the enhanced visible light absorption is originated from the surface plasmon resonance effect of Cu nanoparticles (CuNPs). The surface morphology and crystal structure of the sample were changed as the hydrothermal synthesis temperature rising. The sample by hydrothermal synthesis at 80 °C exhibited the preferable photocatalytic activity attributed the high dispersion of Cu, Cu2O and CuO nanoparticles and the formation of heterojunction between Cu2O and CuO.