Synthesis and Characterization of Sodium Alginate Spheres Functionalized with Dicarboxylic Acids for Copper Removal in Aqueous Media

New polymeric spheres of sodium alginate (AlgNa) containing dicarboxylic acids—maleic acid (MA) and oxalic acid (OA)—were developed for adsorption of copper metal from water. Water adsorption capacity, elementary composition, structural, morphological, vibrational, and thermal properties were characterized by scanning electron microscopy (SEM), intumescence degree (IG), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, and differential scanning calorimetry. SEM data revealed that functionalization with dicarboxylic acids affects the morphology and surface of the AlgNa matrix. Sample containing MA (0.35 ± 0.004 g) absorbs more water than the OA sphere (0.28 ± 0.007 g). XRD patterns showed that the AlgNa–MA and AlgNa samples exhibit an amorphous nature, whereas the AlgNa–OA sample has a partially crystalline phase. Adsorption experiments were conducted to analyze whether the synthesized spheres could be optimized to reach the best performance in copper adsorption. The adsorbents were most efficient at the highest dosage used (250 mg), corresponding to removal percentages of 84.54 ± 3.97% (AlgNa), 94.21 ± 3.04% (AlgNa–MA), and 84.22 ± 3.39% (AlgNa–OA). The energy-dispersive X-ray spectroscopy maps validated the incorporation of Cu²⁺ ions on the surface of the adsorbents. Kinetic and isotherm assays confirmed the highest efficiency of AlgNa–MA spheres.