Globally, there is a rising demand for water purification. This demand is driven by numerous factors, including economic growth, increasing population, water shortage, and deterioration of water quality. The current work highlights the manufacturing of environmentally friendly and highly efficient sorbent based on chitosan nanoparticles after successive crosslinking (using glutaraldehyde) and modification through grafting of 4-aminoazobenzene-3,4′-disulfonic acid (AZDS) as a source of sulfonic groups. First, the produced sorbent was thoroughly specified using FTIR, TGA, SEM, SEM-EDX, pHpzc, BET (nitrogen sorption desorption isotherms), and elemental analyses (EA). The sorbent was tested for the sorption of Fe(III) before application to highly contaminated iron water well samples. Next, the sorption was improved as the sulfonation process was conducted under the selected experimental conditions within 25 and 20 min with a maximum capacity of 2.7 and 3.0 mmol Fe g−1 in visible light and under UV, respectively. Then, the uptake kinetics for both techniques were fitted by the pseudo-first-order rate equation (PFORE), in which the effect of the resistance to intraparticle diffusion has remained an unneglected factor, while the Langmuir equation has fitted the sorption isotherms. After that, the efficient desorption was achieved by using 0.2 M hydrochloric acid solution, and the desorption process was as fast as the sorption process; 15 min was sufficient for complete desorption. The sorbent shows high selectivity for heavy metal ions compared to the representative elements. Finally, the sorbent was used for the removal of heavy metal ions from a highly contaminated water well in the Bahariya Oasis and appeared to be highly efficient for heavy metal removal even in a diluted solution. Accordingly, it can be implemented in the task of water treatment.