The purpose of the study is to investigate the optimum conditions for the precipitation of sodium hexafluorosilicate (Na2SiF6) from waste hexafluorosilicic acid, an effluent from the phosphoric acid industry. Sodium chloride and sodium hydroxide were used as reactants to produce Na2SiF6. The effect of various parameters on the precipitation was investigated and includes; the molar ratio of the reactants, contact time, the temperature and the effect of seeding.The optimum reaction conditions were found to be as follows; excess sodium chloride or sodium hydroxide to hexafluorosilicic acid of 25%, contact time 40 minutes and a reaction temperature of 40°C.The reaction of hexafluorosilicic acid with an aqueous solution of sodium chloride at optimum conditions gave a maximum yield of 94.26% Na2SiF6 while the reaction of hexafluorosilicic acid with the aqueous solution of sodium hydroxide at optimum conditions gave a maximum yield of 97.3% Na2SiF6. The X-Ray diffraction (XRD) analysis reveals that the only crystals present in the precipitate are Na2SiF6. Also, Scanning Electron Microscope (SEM) analysis shows that the different morphology of these crystals depend on the precipitation conditions.