Aluminum lithium hydroxide carbonate hydrate, also known as Al-Li double hydroxide or Al-Li hydrotalcite-like compound [Al2Li(OH)6]2CO3•nH2O, was prepared from basic aluminum sulfate. This compound was prepared by precipitation in homogeneous solution of an aluminum bisulfite solution. A sodium aluminate aqueous solution was prepared by dissolving basic aluminum sulfate in 1M sodium hydroxide. The Al-Li double hydroxide was obtained after addition of lithium carbonate satured solution to the sodium aluminate solution, at 60 °C. The synthesized powder was characterized by thermal analysis (TG, DTG and DTA), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). By this method crystalline Li-Al hydrotalcite like compound with composition near to Al4Li2(OH)12CO3 •3H2O was obtained.