Composite materials CuO/g-C3N4 (CuOCN) were prepared using a solvothermal method to investigate their degradation effect on ciprofloxacin (CIP). The materials were characterized through X-ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), UV-visible diffuse reflectance spectrophotometry (DRS), and X-ray photoelectron spectroscopy (XPS). The toxicity of degradation products of CIP was assessed through antibacterial experiments, and the degradation mechanism of CIP was investigated using quenching agent capture and high-performance liquid chromatography-mass spectrometry (HPLC-MS). The results of XRD and FTIR indicate that the CuOCN composite has been successfully synthesized. The photocatalytic experiment shows that adding 15% (w/w) of Cu3(BTC)2(H2O)3 in melamine (CuOCN2) has a relatively good degradation effect on CIP and can be reused multiple times. The TEM results indicate that both CuO and g-C3N4 have a layered structure and are attached together. HRTEM analysis reveals that the two components in CuOCN2 are arranged in a layered structure, with CuO displaying two crystal planes. Energy Dispersive Spectrometer (EDS) analysis reveals that the proportion of CuO in the three composite materials is 7.86% (w/w), 15.93% (w/w), and 84.83% (w/w), respectively. DRS detection reveals that the greater the amount of CuO added, the broader the visible light absorption range of the composite material, and the narrower the bandgap width. The photocurrent and photoresistance indicate that CuOCN2 exhibits a good photoelectric effect. XPS analysis shows that the CuOCN2 composite material possesses both the chemical composition and structure of CuO and g-C3N4. During the catalytic degradation process of CIP, four active substances, h+, e−, ·O2 −, and ·OH, were produced, leading to a reduction in the toxicity of the degradation products. Through HPLC-MS analysis, it was found that CIP undergoes reactions such as defluorination, ring opening of piperazine, and quinolone during degradation, resulting in reduced toxicity. This study provides an experimental basis for the degradation of CIP by CuOCN2.