<p>We herein report successful syntheses of both nickel cobalt sulfide (NCS) and its composite with zeolite (NCS@Z) using a solvothermal method. Techniques such as EDX analysis, SEM, and molar ratio determination were used for product characterization. The incorporation of NCS significantly changed the surface roughness and active sites of the zeolite, improving the efficiency of methylene blue degradation and its reusability, especially under UV irradiation. In comparing the pseudo-first order rates, the highest degradation efficiency of methylene blue was achieved with NCS-2@Z, having a degradation extent of 91.07% under UV irradiation. This environmentally friendly approach offers a promising solution for the remediation of methylene blue contamination in various industries.</p>