Novel nanostructured composites of silica aerogel with Cu-BTC were synthesized using a slightly modified version of the conventional sol–gel method used to synthesize silica aerogels. The composite materials had monolithic structures with blue color consisting of well dispersed microporous domains of Cu-BTC in the mesoporous inorganic silica aerogel network. The Cu-BTC content in the composites ranged from 5 to 30 weight percent and the total surface area of the composites ranged from 1025 to 1138m²/g. The microporosity of the composites increased with the increasing amount of Cu-BTC indicating that the micropores of Cu-BTC were accessible and functional. XRD analysis indicated that Cu-BTC retained its crystal structure in the composite despite being immersed in a solution containing water, ethanol and tetraethylorthosilicate. Additionally, it was observed that increasing Cu-BTC content caused a decrease in the average desorption pore radius with a wider pore size distribution. Nitrogen adsorption isotherms for composites could be predicted using the experimentally obtained pure component isotherm for the silica aerogel, theoretically obtained isotherm for Cu-BTC and the weight fractions of the components within the composite material.