A series of silica aerogels and composite materials based on Fe-silicalite-1 nanocrystals embedded into silica aerogel matrix in the form of monoliths and microspheres have been synthesized by drying with supercritical CO2. Using equivolume water/ethanol mixture as a medium for the aging of monoliths enabled to produce monoliths of silica aerogel and composite without cracks. The synthesis of the composite and silica aerogel microspheres by the emulsion/gelation technique has been designed. The different effects of the stirring rate during the emulsification on the particle size and texture of composites and silica aerogels has been observed. The synthesized samples were characterized by X-ray diffraction, scanning electron microscopy and nitrogen adsorption measurements.