A porous aerogel sorbent was prepared by the carbonization of a biohydrogel consisting of cellulose and chitosan (CS/CE) biopolymers. The adsorbent was also modified with copper oxide nanoparticles to effectively remove formic acid from water in batch mode. Characterization techniques, including scanning electron microscopy, Fourier transform infrared, Brunauer−Emmett−Teller, and X-ray diffraction, were employed to study the prepared sorbents. The concentration of formic acid in the solution was exactly determined by using liquid chromatography. To achieve maximum removal efficiency, important process variables were optimized using a central composite design data-based algorithm. Under optimal conditions, i.e., the initial concentration of 167.98 mg/L, the amount of sorbent equal to 75.28 mg, the contact time of 10.41 min, and the sample volume of 22.56 mL, a maximum acid removal efficiency of 84% was obtained. The Langmuir isotherm model was appropriately fitted to the experimental data, which indicates the chemical interaction of the sorbent active sites with formic acid. An adsorption capacity of 116.28 mg/g was also attained. The adsorption followed a pseudo-second-order kinetic pattern. According to the thermodynamic criteria, the adsorption of formic acid on the copper oxide-modified aerogel was exothermic, entropy-reducing, and favorable at temperatures lower than 290 K. Based on the results, CS/CE hydrogels comprising CuO nanoparticles are promising precursors for synthesizing carbonized aerogel sorbents that are successful in removing formic acid from aqueous environments
