In this study, silica aerogel and silica aerogel-activated car-bon composites were synthesized using water glass precursor by ambient pressure drying method. Hydrophobicity of thesynthesized samples was obtained using surface modifica-tion reagent (TMCS) and replacement of hydrophilic OHgroups with hydrophobic CH3groups. Hydrophobic sil-ica aerogel with surface area (427.16 m2g−1), pore diameter(19.72 nm), and density (0.16 g cm−3) were obtained. Thesynthesized samples were nanometer and had pore size distribution between 2 and 50 nm with an average poresize of 8 and 16 nm for silica aerogel and silica aerogel-activated carbon composites respectively. In benzene static adsorption, silica aerogel and activated carbon had maximum equilibrium adsorption capacity (2.3 g g−1) and minimumequilibrium adsorption capacity (0.7 g g−1), respectively. Also,in ethyl benzene static adsorption, silica aerogel and sil-ica aerogel–2 wt% activated carbon composite had maximum equilibrium adsorption capacity (0.7 g g−1) and minimum equilibrium adsorption capacity (0.25 g g−1), respectively. Thehighest equilibrium adsorption capacity in benzene and ethylbenzene dynamic adsorption capacity was related to silica aerogel with 0.9545 g g−1and 0.219 g g−1, respectively. Regeneration of the adsorbents did not change adsorption capacity and the physical and structural properties of adsorbents and intensity of Si OSi Si and Si C peaks were equal in regenerated and new adsorbents.