Recently, more and more attention has been paid to the removal of nickel ions due to their negative effects on the environment and human health. In this research, fly ash obtained as a result of incineration of municipal sewage sludge with the use of circulating fluidized bed combustion (CFBC) technology was used to analyze the possibility of removing Ni(II) ions in adsorption processes. The properties of the material were determined using analytical methods, such as SEM-EDS, XRD, BET, BJH, thermogravimetry, zeta potential, SEM, and FT-IR. Several factors were analyzed, such as adsorbent dose, initial pH, initial concentration, and contact time. As a result of the conducted research, the maximum sorption efficiency was obtained at the level of 99.9%. The kinetics analysis and isotherms showed that the pseudo-second order equation model and the Freundlich isotherm model best suited this process. In conclusion, sewage sludge fly ash may be a suitable material for the effective removal of nickel from wastewater and the improvement of water quality. This research is in line with current trends in the concepts of circular economy and sustainable development.