Dyes are a form of pollutant that has been dumped into water sources by a variety of industries, causing environmental and human health problems. As a result, the current research focuses on recycling 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. Adsorption studies were carried out to get the optimum condition for CR remediation process. Different parameters were employed such as, CR concentrations, adsorbent dose, effect of time and pH. Langmuir, Freundlich isotherms and kinetic studies evaluations were applied. Results declared that, the maximum adsorption capacities of AF-NCh and AF-NCh-Epichlorohydrin were 166.6 and 232.5 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.