A process for preparing microspheres of TiO2/SiO2, aerogel includes such steps as dissolving TiOSO4 in deionized water, adding ammonia water to make pH=7-8, depositing, washing deposit, adding nitric acid, stirring to obtain TiO2 sol, mixing Si sol with nitric acid, adding alcohol to obtain SiO2 alcohol sol, mixing it with said TiO2 sol, adding formamide and epoxy propane, mixing to obtain TiO2/SiO2 sol, mixing heptane or hexane, Span-80, tween-85 and butanol or hexanol, stirring to obtain oil phase, adding TiO2/SiO2 sol, adding ammonia water to make pH=7-1, centrifugal separation of target microspheres, washing and drying.