In this paper, we report the synthesis of g-C3N4/CdS composites by using a simple, cost-effective, and eco-friendly process. The development of CdS nanoflakes on the surface of g-C3N4 nanosheet was carried out by in situ sol–gel method. The morphology and physical properties of g-C3N4/CdS composites were characterized and analyzed by SEM, XRD, TGA, FT-IR, UV-vis, XPS, and physical adsorption. The electrochemical properties of the composites were investigated by the open circuit potential method. The results showed that the recombination of photogenerated electron holes can be effectively inhibited by g-C3N4/CdS composites, and can transfer electron faster than pure g-C3N4. The most efficient photocatalytic degradation technology of methyl orange effluent was that the concentration of composites solution is 2g/L, PH is 7, the time was 90min and the temperature was at 35℃ with adding 30mL/L of H2O2. The findings indicate that CdS-based catalyst has great potential for the photocatalytic reduction of uranyl in actual environmental remediation.