In this study, studies on the development of different metal-containing hydrotalcite-like materials have been carried out for the removal of Co-2 center dot 3Mg1Al, 3Mg1Fe and 3Mg1Mn hydrotalcite-like materials (molar ratio of M+2/M+3= 3), Mg-O and Al-O have been prepared by coprecipitation method. Synthesized materials were characterized by Xray diffraction (XRD), thermogravimetric-differential thermal (TGA-DTA), scanning electron microscopy (SEM),.. 2 adsorption-desorption, temperature-programmed CO2 desorption (CO2-TPD) and inductively coupled plasma optic emission spectroscopy (ICP-OES) analysis. Before calcination, XRD results showed that Mg-O material contains. Mg-5(CO3)(4)(OH)(2)center dot 4H(2)O-hydromagnesite and Al-O material contains mainly Al (OH)(3)-bayerite, gamma-AlOOH-boehmite and Al(OH)(3)-gibbsite structures. Hydrotalcite-like structures were obtained for the 3Mg1Al, 3Mg1Fe, and 3Mg1Mn materials. These results showed that hydrotalcite-like structures could be successfully obtained by using different metals. Mass losses in TGA-DTA analysis of Mg-O, 3Mg1Al, and Al-O materials were consistent with the theoretical values. After calcination, it was seen that mainly MgO-periclase structure was obtained for the hydrotalcite-like materials. Among the prepared hydrotalcite-like materials, 3Mg1Al was determined as having the highest surface area (133 m(2)/g) and the highest surface basicity CO2 sorption experiments were performed in a fixed bed reactor system using the feed mixture containing 4% CO2 in He with a GHSV of 3600 cm(3)/g.sa at 300 degrees C. 3Mg1Al sorbent was found as having the highest CO2 sorption capacity (0.17 CO2/sorbent) among the synthesized hydrotalcite-like materials. The initial reaction rate constant (k(0)) and the deactivation rate constant (k(d)) values were found by applying the non-linear regression of the deactivation model to the experimental data. The results showed that hydrotalcite-like materials were promising sorbents for CO2 sorption studies.