Three well-formed film combinations of chitosan, in the beta form and cellulose acetate biopolymer, having different proportions, have been synthesized and characterized by X-ray diffraction and infrared spectroscopy. The film having a 1.0/0.50 proportion presented 6.87mmol of nitrogen atoms per gram of synthesized hybrid, with the highest affinity for adsorbing copper from aqueous solutions at 298±1K. The isotherm obtained in this adsorption showed a saturation plateau that corresponds to 1.92mmol of copper per gram of hybrid. The energetic effects caused by copper ion interaction were determined through calorimetric titration at the solid–liquid interface in aqueous solution and gave a net thermal effect that enabled the calculation of the exothermic enthalpic values and the equilibrium constant. The complete thermodynamic data showed that the system is favored by exothermic enthalpies, negative Gibbs free energies and positive entropies.