The current research aimed to use waste to treat waste; to recycling of acrylic fibers waste combined with nano-chitosan for use as an adsorbent to remove Congo red (CR) from wastewater. Acrylic fibers (AF) waste were mixed with nano-chitosan (NCh) with different ratios and converted into films by using phase inversion method to prepare two nanocomposites films coded, AF-NCh and AF-NCh-Epichlorohydrin. The nanocomposites films have been characterized using; Fourier transform infrared, scanning electron microscope, surface area, and thermal analysis. The results revealed successful incorporation of NCh into AF matrix with highly porous structure. Different parameters affecting adsorption efficiency such as, CR concentrations, adsorbent dose, effect of time and pH were employed. Adsorption isotherms and kinetic studies evaluations were applied to assess the adsorption mechanism and rate. Results declared that, the maximum adsorption capacities of AF-NCh and AF-NCh-Epichlorohydrin were 169 and 230 mg/g respectively. The adsorption isotherm and kinetic mechanism obey Langmuir and pseudo second order models. Regeneration of the synthesized composite films were studied for five cycles and showed relative stable reading with high efficiency. Graphical Abstract