The initial characteristics of Romanian fly ash from the CET II Holboca power plant show the feasibility of its application for the production of a new material with applicability in environmental decontamination. The material obtained was characterized using standard techniques: scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), instrumental neutron activation analysis (INAA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), the Brunauer–Emmett–Teller (BET) surface area, and thermogravimetric differential thermal analysis (TG-DTA). The adsorption capacity of the obtained material was evaluated in batch systems with different values of the initial Cu(II) ion concentration, pH, adsorbent dose, and contact time in order to optimize the adsorption process. According to the experimental data presented in this study, the adsorbent synthesized has a high adsorption capacity for copper ions (qmax = 27.32–58.48 mg/g). The alkali treatment of fly ash with NaOH improved the adsorption capacity of the obtained material compared to that of the untreated fly ash. Based on the kinetics results, the adsorption of copper ions onto synthesized material indicated the chemisorption mechanism. Notably, fly ash can be considered an important beginning in obtaining new materials with applicability to wastewater treatment.