In this study, silica aerogel and silica aerogel activated carbon composites were synthesized using water glass precursor by ambient pressure drying method. Hydrophobicity of the synthesized samples was obtained using surface modification reagent (TMCS) and replacement of hydrophilic OHgroups with hydrophobic CH3 groups. Hydrophobic silica aerogel with surface area (427.16 m2g−1), pore diameter(19.72 nm), and density (0.16 g cm−3) were obtained. The synthesized 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.