Adsorption remains a promising separation process in the field of precombustion carbon dioxide capture [1].In this paper,CO2 separation from flue gases was performed using Mg-Zn-A1-Cl LDHs as the adsorbent.Mg-Zn-Al-CO3 layered double hydroxides (LDHs) with different molar ratios of Mg/Zn/A1 were synthesized by microwave assisted coprecipitation method at first.Decarbonation process using acetate-buffer/NaCl mixed solution was then followed to get Mg-Zn-Al-Cl LDHs [2].X-ray diffraction and thermogravimetric analysis (TGA) were used to investigate the structure and thermogrative properties for the samples.The CO2 adsorption capability (COAC) of the Mg-Zn-Al-Cl LDHs was determined by CO2 separation test firom flue gases.Decarbonation process using acetate-buffer/NaCl mixed solution was then followed to regenerate CO2 and Mg-Zn-Al-Cl LDHs.The amount of CO2 regenerated and the COAC of the regenerated Mg-Zn-Al-Cl LDHs were calculated after several cycles of CO2 adsorption testing.The results indicate the process of trapping and regeneration of CO2 can be efficient and of greatly potential in the industrial appfication.