Abstract: Construction of heterojunction materials with efficient charge transfer pathways is the key to photocatalytic degradation of composite pollutants in water. CdS QDs@MOX(Al) heterojunction photocatalyst was prepared by dispersion of CdS quantum dots (CdS QDs) in metal-organic gel MOX(Al) using the gel-confinement-method. The compositional structure and interfacial charge transfer efficiency of the samples were characterized and analyzed by XRD, TEM, XPS, N₂ adsorption-desorption, UV-Vis DRS, transient photocurrent (TPC) response and electrochemical impedance spectroscopy (EIS), and the catalytic activity and mechanism for the synergistic degradation of norfloxacin (NF) and reduction Cr(VI) under visible light were investigated. The results show that 1.0-CdS QDs@MOX(Al) exhibite excellent photocatalytic activity for the NF/Cr(VI) complex pollutant system, the degradation process conforms to the pseudo-first-order kinetic model, and the apparent rate constants k are 6.1 (8.5) and 5.3 (3.5) times higher than those of pure MOX(Al) and CdS, respectively. Compared with the single pollutant system, the photocatalytic efficiency of CdS QDs@MOX(Al) for the NF/Cr(VI) complex pollutant system is significantly improved. The combination of active species capture experiments confirm that h⁺ and •O₂⁻ are the main active species. The enhanced photocatalytic activity is mainly attributed to the Type-II heterostructure formed between MOX(Al) and CdS QDs, which accelerates the effective separation and transfer of photogenerated charges at the interface of the heterostructure.