Semiconductor hybrids based photocatalytic reaction is one of the prominent methods to treat wastewater, containing the organic pollutants. In the present work, we report the development of ZnS QDs-LDH hybrid structure for the photocatalytic treatment of methylene blue (MB) dye. The as-synthesized ZnS QDs-LDH hybrid structure was characterized by XRD, FESEM, HRTEM, EDX, XPS, and FTIR to analyze the formation, morphology and chemical structure. The UV-Vis DRS was used to investigate the optical absorption characteristics of the ZnS QDs-LDH hybrid. The photocatalytic performance of the asprepared samples was investigated against the methylene blue dye molecule under UV-Vis light irradiation. The scavenging experiments were carried out in order to probe the radical formation by using EDTA, benzoquinone, and 2-proponal. The cycling experiments were performed to check the stability of the ZnS QDs-LDH hybrid photocatalyst after repeated photodegradation experiments.