This research investigates the synthesis of a hybrid nanomaterial, denoted as Ni‐Zn−S@Cyclodextrine, through a cost‐effective and easy co‐precipitation method. The resulting nanomaterial has been thoroughly characterized and applied for the adsorptive removal of Crystal violet and Congo red dyes from their solutions. The study delves into the thermodynamics and kinetics of the sorption process, as well as helps to propose adsorption mechanism for both the dyes onto the Ni‐Zn−S@Cyclodextrine surface. A comprehensive analysis, encompassing techniques, such as XRD, FTIR, SEM‐EDX, TEM, TGA, Zeta potential, and XPS, have been conducted to explore the structural and morphological attributes of the prepared nanomaterial. Furthermore, key sorption parameters, including adsorbent's dosage, temperature, contact time, and solution pH, have been systematically optimized to achieve maximum efficiency. The TEM images of prepared nanomaterial indicated the particle size ranging between 60–80 nm. Moreover, it exhibited a strong affinity for both the dyes, with a maximum adsorption capacity of 138.20 mgg−1 for Congo red and 129.95 mgg−1 for Crystal violet dyes at 303 K. The thermodynamics of the adsorption process indicated an endothermic and spontaneous nature. Isotherm studies revealed that the data best aligned with the Freundlich isotherm, while the kinetics of the reaction adhered to a pseudo‐second order within the investigated temperature range. [ABSTRACT FROM AUTHOR]