In order to overcome the photocatalytic degradation reaction with a need for light excitation, the exploration of a catalyst for the organic degradation reaction without light has become one of the core challenges in catalysis and pollution control. Here we report a novel Cu NiSe S nanosheet catalyst with a hexagonal structure by a feasible preparation method. The structure and composition of Cu NiSe S were well characterized by X‐ray diffractometry and electron microscopy, and X‐ray photoelectron spectrometry, respectively. The result indicated that the best Cu NiSe S‐2 of 25 mg displayed excellent activity even in the dark to complete the degradation of 100 mL of MB solution of 10 ppm within 5 min. This catalyst also showed relatively good stability and durability during the reusability tests. The reasons for the fast MB degradation in the dark were investigated and the reaction kinetic mechanism was proposed.