<p>The aim of this study is the hydrothermally synthesize a highly superhydrophilic mesocellular foam (MCF), followed by surface functionalization with dithiooxamide (DTO) to enhance its surface characteristics. Synthesized superabsorbents to accurately evaluate their efficiency in the removal processes of pollutants such as methylene blue (MB), chromium (Cr) ions in two forms, trivalent (III) and hexavalent (VI) and cobalt (Co) ions in two forms bivalence (II) and trivalent (III) were used. To investigate various influencing parameters, a central composite design was used based on the principles of the response surface methodology, which allows comprehensive analysis of factors including the amount of DTO used (g), the pH level of solutions, and the concentration of pollutants (mg/L), the duration of the adsorption process (min) and the adsorbent mass (g) were provided. The optimal experimental conditions, with pH levels of 8.67 and 8.62, and using 0.10 and 0.14 g of MCF/DTO (0.04 g), pollutant concentrations of 18.5 and 19.09 mg/L, efficiencies of 99.99% and 94.80% were achieved for MB dye and Cr (III) metal ion at 10.54 and 15.10 min, respectively. It was also found that the equilibrium data related to the adsorption of MB dye is Anderson’s multi-layer model (V). In contrast, the equilibrium data of Cr (III) metal ion are in high agreement with Khan’s monolayer model, and the complexity and properties of the adsorption processes involved are highlighted. Furthermore, the results of this research showed that the adsorption behavior of MB dye is accurately described by the Elovich model, while the adsorption of Cr (III) metal ions is best represented by the intraparticle diffusion model. The analysis of the superabsorbent’s recovery and reuse reveals a significant decline in the removal efficiency of MB dye and Cr (III) metal ions by 44% and 52%, respectively, after 6 cycles.</p> Graphical Abstract <p></p>