The effect of by-products obtained during the low-temperature synthesis of Mg, Al- hydrotalcite on further thermal decomposition of hydrotalcite material was studied by X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy and infrared spectroscopy. By-products, which thermally decomposed below 450°C, led to the formation of α-Al2O3 and MgO; by-products which completely decomposed above 500°C resulted in the formation of MgAl2O4 and a sharp increase in MgO dispersity.