The use of solar photocatalytic degradation of pollutants is one of the most promising technologies to solve water pollution problems and achieve solar energy conversion. By changing the amount of g-C3N4 added, g-C3N4/Co3O4 catalysts with different g-C3N4 mass fractions are prepared based on the calcination method with cobalt nitrate hexahydrate (Co(NO3)2-6H2O) and urea (NH4CNO) as raw materials. The samples are analyzed and characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and ultraviolet visible absorption spectroscopy (UV-vis DRS). To speculate on the active species of the catalyst, capture agent experiments are conducted on it. The results indicate that the synergistic effect between g-C3N4 and Co3O4 can improve the transfer and separation efficiency of charge carriers at the interface between the two phases. Under visible light, the degradation effect of 10% g-C3N4/Co3O4 is the best, with a degradation rate of 66.50%, which is higher than the degradation effect of single Co3O4 (degradation rate of 35.90%). The active species of the catalyst are mainly superoxide radicals(·O2-) and holes(h+). After compounding with g-C3N4, the drawbacks of Co3O4 electron hole pair, such as too fast recombination and a deficient energy level structure, are improved, providing ideas for the degradation of organic pollutants in the future.