Crystalline cyclodextrin-based metal-organic framework (CD-MOF) was synthesized by vapor diffusion of methanol into a KOH solution of -cyclodextrin (-CD). Its CO2 adsorption behaviors were evaluated both qualitatively and quantitatively. The adsorption behaviors of CD-MOF to separate and capture CO2 have been tested by using thermogravimetric analysis in the multiple adsorption-desorption process. The chemical sorption of CO2 was found to be caused by the formation of reversible carbonic acid. The adsorption amount of CO2 was tested in pure CO2 gas and 25vol CO2 in Ar gas. As a result, there is no difference of the adsorption amount against the CO2 concentration and the saturated adsorption amount was 24 mg-CO2/g-CD-MOF at 30oC. © 2016 The Authors.