Activated carbon aerogels (ACAs) with excellent microporosity (e.g., 0.44 cm(3)/g) and mesoporosity (e.g., 1.72 cm(3)/g) were prepared by CO2 activation. Their structures were investigated with transmission electron microscopy and N-2 adsorption-desorption analysis. Subsequently, their adsorption properties toward organic vapors were studied with static and dynamic adsorption experiments. The micropores of the ACAs had stronger adsorption ability than those of normal porous carbons. Furthermore, the condensation of organic vapors in the mesopores of ACAs greatly enhanced their equilibrium adsorption at high relative pressures. As a result, the adsorption capacities of organic vapors on the typical ACAs prepared were about 2-3 times greater than those on normal porous carbons. In addition, they also possessed excellent adsorption dynamics and outstanding desorption and regeneration properties. (c) 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 2263-2267, 2006