In this work, aerogels were prepared using resorcinol-formaldehyde as a precursor in two synthetic routes, one basic and one acidic, to perform the adsorption of CO 2 at 0 • C and atmospheric pressure. Aerogels were Characterization by N 2 and CO 2 Physisorption, Raman Spectroscopy, Scanning Electron Microscopy, and Infrared Spectroscopy. In general, was found that aerogels have a polymeric, disordered, three-dimensional structure and have a microporous surface. Langmuir, Freundlich, Sips and Toth equilibrium models present a good data fit of CO 2 adsorption at relative pressure ranging between 1 × 10 −4 and 3 × 10 −2 . The diffusion intra-particle kinetic model explains the setps of this process; the Elovich model also showed a good fit, therefore, there are an energetic heterogeneity of the CO 2 superficial adsorption sites. The aerogel carbonized in basic medium at 1050 • C (ACB 1050) material was the best adsorbent of this pollutant, reaching an adsorption capacity of 6.43 mmol g −1 .Achieving economic and favorable separation of CO 2 from gas mixtures represents one of the main technological and environmental problems facing our society today [10]. The most studied post-combustion technology is chemical adsorption. Monoethanol amine (MEA) has been the chemical most used for this purpose. Alternative solvents, such as piperazine and ammonia, have also been proposed to achieve this objective [6]. The advantage of this method is the low partial pressure that is used because the CO 2 molecules are easily absorbed over liquids in flue gas streams [11]. The disadvantage is that the use of amine alkoxysilanes is very expensive [12], and the method requires high regeneration energy due to the large emission of combustion gases and the costs of repairing the process equipment [4]. Other common methods to achieve CO 2 sequestration include separation in membranes, cryogenic and biological methods, and physical adsorption [13].Capture and storage technology has been considered the best option to reduce carbon dioxide emissions from large sources, and particularly adsorption is considered a promising process to separate gas mixtures [14]. This process is inexpensive, requires less regeneration energy, is easy to handle, has fast kinetics, and has a high capacity of CO 2 adsorption and selectivity [4]. The adsorbents provide a high surface area, which is a fundamental parameter in this process. Among the different adsorbents, 13X zeolite has been investigated to adsorb CO 2 by oscillating the pressure [6]. It is generally recognized that CO 2 is physically adsorbed to activated carbon, mainly by condensation or liquefaction in pores with widths that are less than 1 nm [15]. The adsorption of this greenhouse gas in nanopore materials has also been investigated in zeolites exchanged with alkali metals, amino-modified and modified alkaline, mesoporous silicas, microporous polymers, carbons, and metalorganic structures [10]. It has also been established that the chemical properties of activated carbon play a relevant role in...