Graphitic carbon nitride (g-C₃N₄) was prepared by a simple thermal polymerization method in this work. The effects of precursor type, thermal polymerization temperature, constant temperature time and atmosphere on the crystal structure, morphology, elemental composition, valence distribution, light absorption properties and photocatalytic activity of the prepared photocatalytic materials were investigated. Taking rhodamine B (RhB) as the target degradant, the blue light catalytic activity of the photocatalytic material was studied in detail. The experimental results showed that the final pyrolysis temperature and constant temperature time are positively related to the adsorption characteristics and photocatalytic ability of the prepared materials. In addition, the adsorption capacity and photocatalytic activity of the products obtained in Ar and H₂ atmospheres are better than those produced in CO and CH₄, which can be attributed to the combined effect of large specific surface area and structural defects of the materials. The sample's large specific surface area, wide band gap, and excellent photogenerated carrier separation and transfer capabilities make the adsorption performance and photocatalytic performance of the products obtained with ammonium thiocyanate and thiourea as precursors better than those prepared from melamine and dicyandiamide. g-C₃N₄ prepared by using ammonium thiocyanate as precursor at 550 °C for 5 h under a hydrogen atmosphere showed the best catalytic activity for the degradation of RhB under blue light. It was demonstrated that g-C₃N₄ prepared exhibited good stability and reusability after four repeat experiments. The active components that play major roles in the degradation of RhB described herein were holes and superoxide radicals, which was inferred by free radical trapping experiments. This work provides a theoretical basis for the idea of converting the mixed salts of desulfurization waste liquid containing ammonium thiocyanate into an excellent photocatalyst g-C₃N₄ with visible light response.