Binary and ternary hydrotalcite-like (HT) materials containing copper, nickel, zinc, iron, magnesium and/or aluminum were synthesized by coprecipitation and characterized by elemental analysis, powder X-ray diffraction and N 2 adsorption–desorption at −196°C. Samples were calcined at 700°C for 4h, obtaining mixed oxides which were tested for sulfur oxides (SO x ) removal. Their performance was compared with a commercial SO x reducing additive by thermogravimetric SO x uptake. SO x adsorption was carried out by contacting the calcined solid with a mixture of 1% SO 2 in air at 650°C. The adsorbed species were reduced with H 2 at 550°C, 650°C and 700°C, in order to study their stability and the solid's regenerability. It was found that the isomorphic incorporation of a transition metal in the HT layers increased the mixed oxide's reduction ability. This was reflected on higher reduction rates and sulfate reduction amounts at 550°C. Furthermore, these materials showed greater adsorption–reduction properties than the commercial additive.