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Abstract: CO2 separation from N2 over 3-aminopropyltrimethoxysilane-grafted mesoporous SAPO-34, which had been synthesized using an amphiphilic organosilane additive was investigated. The presence of mesopores with a mean pore diameter of ∼3.3nm was confirmed by the characteristic small angle X-ray diffraction peak at ca. 1.3°, transmission electron microscopy, and N2 adsorption isotherm. The CO2 adsorption isotherms of the SAPO-34 samples were obtained at 273, 298 and 303K, and the heat of adsorption was estimated using the Clausius–Clapeyron equation. The amine-functionalized mesoporous SAPO-34 showed a significantly improved CO2/N2 selectivity of 177 and a sharp breakthrough in the fixed bed adsorption. CO2 adsorption–desorption of the sample was stable and reproducible during five cyclic runs. [Copyright &y& Elsevier]