A novel CuCl@β zeolite with high CO capacity and high-selectivity for CO/N2 and CO/CO2 mixtures was developed. A series of CuCl@β zeolites were prepared by an auto single-layer dispersion method. The CuCl@βzeolites were characterized by N2 adsorption and XRD. The adsorption isotherms and dynamic breakthrough curves of CO on the adsorbents were measured separately by a static adsorption and fixed-bed experiments. The adsorption selectivities of CuCl@β zeolite for CO/N2 and CO/CO2 mixtures were estimated on the basis of ideal adsorbed solution theory (IAST). The results showed that (a) the loading of CuCl onto β zeolite significantly enhanced CO adsorption capacity of the resulting CuCl@β adsorbent and the CuCl loading was optimized to be 0.4. (b) it not only significantly enhanced CO uptake

but also weakened N2 and CO2 adsorption on the CuCl@β adsorbents. As a result

it significantly enhanced CO/N2 and CO/CO2 selectivities of the adsorbent further

which can be attributed to the mild Cu+-CO interaction by π-complexation bond. (c) the 0.4CuCl@β adsorbent achieved a superior adsorption selectivity up to 1600-5200 and 120-370 at low pressure range of 0-10 kPa for CO/N2 and CO/CO2 mixtures

much higher than parent β zeolite. The high CO adsorption capacity and selectivity of CuCl@β adsorbents made it a promising adsorbent for CO/N2 and CO/CO2 separation.