Nano-sized　TiO2　photocatalysts　were　prepared　by　drying　the　ethanol　gel　of　titanium　tetrabutoxide　through　natural　state,　supercritical　ethanol,　supercritical　carbon　dioxide　drying　methods　and　characterized　by　XRD,　FTIR　spectroscopy,　FT-Raman　spectroscopy　and　fluorescent　spectroscopy,　respectively.　We　regard　degradation　of　rhodamine　B　by　photocatalyst　as　a　model　reaction,　and　compare　photocatalytic　activities　of　samples　obtained.　The　experimental　results　show　that　different　drying　methods　have　strong　effect　on　crystal　structure,　energy　band　structure,　optical　adsorption　property,　surface　quality　and　photocatalytic　activity,　TiO2　photocatalyst　prepared　by　supercritical　carbon　dioxide　drying　method　has　superior　photocatalytic　activity.