The contamination of water sources with dyes like methylene blue poses significant environmental and health challenges.To overcome this problem, the development of materials capable of effectively removing dyes is essential.This research focuses on the synthesis, characterization as well as application of a CuO-based hydrogel nanocomposite (NAM@CuO NCs) as an adsorbent for methylene blue (MB) dye removal from wastewater.The NAM@CuO NCs have been prepared via the sol-gel method.Their properties were analyzed using methods like UV-visible (UV) spectroscopy, Fourier transform IR spectroscopy (FTIR), thermogravimetric anal. (TGA), X-ray diffraction (XRD), point of zero charge (PZC), XPS anal., gel permeation chromatog. (GPC), and SEM- energy dispersive studies (SEM-EDX).Adsorption experiments were performed in batch mode to estimate the nanocomposite′s effectiveness, considering variables like preliminary dye concentration, pH, contact time and adsorbent dosage.The NAM@CuO NCs exhibited excellent adsorption performance under optimal conditions, achieving an excellent removal efficiency of 93.99% for MB dye.The adsorption process conformed to the pseudo-second-order kinetic model and the equilibrium data aligned well with both the Langmuir and the Freundlich isotherm models, showing an adsorption capacity of 82.44 mg/g for MB dye.Regeneration experiments demonstrated the adsorbent′s reusability, with only a 9.6% efficiency reduction after five cycles.Addnl., the catalytic reduction of MB dye using NAM@CuO NCs reached 93.99% within 210 s in the presence of NaBH4 as a reduction agent, highlighting the rapid reduction of MB dye.This suggests that NAM@CuO NCs possess excellent catalytic activity under visible light exposure.With its high efficiency and potential for practical wastewater treatment applications, NAM@CuO NCs offer a sustainable and effective solution for the removal of methylene blue from contaminated water.