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Abstract: Alkali-promoted hydrotalcite-based materials have showed CO2 sorption capacity up to 1.6 mmol⋅g−1 when CO2 separation is carried out at relatively high temperature (300–500 °C) and high partial pressure of steam and CO2, conditions that are prevalent in pre-combustion CO2 capture conditions. In addition to CO2 breakthrough experiments in situ XRD experiments have allowed identifying magnesium carbonate crystalline phase formation during CO2 sorption. The alkali promoted hydrotalcite-based material (Mg/Al ratio 2.9) has revealed that high CO2 capacities can potentially be achieved by using the extra storage capacity offered by the presence of excess magnesium oxide that can be converted into magnesium carbonate. The use of this extra capacity in Pressure Swing Adsorption process is further discussed. [Copyright &y& Elsevier]