Zeolite A and A + X mixtures were prepared from coal-fly ash procured from China by using an alkali fusion method. X-ray diffraction showed that both the materials were crystalline and reproducible. Scanning Microscopy revealed that pure zeolite A particles have cubic morphology while the mixture shows intergrowth of cubic and pyramidal crystals. The surface area for A + X mixture was around 330 m2/g which is higher than zeolite A, however, lower than typical X zeolite. CO2 and N2 adsorption isotherms were measured and the data was fitted by the Dual Site Langmuir equation. These zeolites were then tested for CO2 capture at different temperatures in a process with a nine step cycle. When compared with 13X zeolites at higher temperature (∼90 °C), both the zeolite A + X mixture and zeolite A prepared from fly ash showed better performance in CO2 capture from flue gas because they have higher selectivity of CO2 over N2.