<p>An alternative two-step process has been disclosed for manufacturing low-density nano-AlF₃ from aluminum waste material to achieve sustainability resources preservation. The method involves utilizing spent die-cleaning solution waste as a raw-material, which is a by-product resulting from detaching the attached aluminum metal in the die cast during extrusion process. The first step involves the extraction of aluminum hydroxide (gibbsite) from spent-die cleaning solution through a carbonation process in the presence of specific carbon blocks. The second step involves the conversion of gibbsite to low-density non-gelatinous nano-AlF₃ using hydrofluoric acid and ammonia solution. The adding of different volumes of hydrofluoric acid and their effect on aluminum fluoride formation was investigated. The role of polyethylene glycol to form non-gelatinous aluminum fluoride was investigated. The two-step process has been successful in achieving a great demand for cheap sources of raw materials.</p>