Zeolite NaA was successfully prepared from nickel laterite residue for the first time via a fusion–hydrothermal procedure. The structure and morphology of the as-synthesized zeolite NaA were characterized with a range of experimental techniques, such as X-ray diffraction, scanning electronic microscopy, and infrared spectroscopy. It was revealed that the structures of the produced zeolites were dependent on the molar ratios of the reactants and hydrothermal reaction conditions, so the synthesis conditions were optimized to obtain pure zeolite NaA. Adsorption of nitrogen and carbon dioxide on the prepared zeolite NaA was also measured and analyzed. The results showed that zeolite NaA could be prepared with reasonable purity, it had physicochemical properties comparable with zeolite NaA made from other methods, and it had excellent gas adsorption properties, thus demonstrating that zeolite NaA could be prepared from nickel laterite residue. Zeolite NaA was successfully prepared from nickel laterite residue for the first time via a fusion-hydrothermal procedure. The structure and morphology of the as-synthesized zeolite NaA were characterized with a range of experimental techniques, such as X-ray diffraction, scanning electronic microscopy , and infrared spectroscopy. It was revealed that the structures of the produced zeolites were dependent on the molar ratios of the reactants and hydrothermal reaction conditions, so the synthesis conditions were optimized to obtain pure zeolite NaA. Adsorption of nitrogen and carbon dioxide on the prepared zeolite NaA was also measured and analyzed. The results showed that zeolite NaA could be prepared with reasonable purity, it had physicochemical properties comparable with zeolite NaA made from other methods, and it had excellent gas adsorption properties, thus demonstrating that zeolite NaA could be prepared from nickel laterite residue.