Abstract: Photocatalytic degradation of toluene and xylene in the air was investigated using titanium dioxide (TiO2) loaded on activated carbon fibers(ACF). The TiO2 and ACF combination (TiO2-ACF) was prepared by sol-gel, followed by supercritical fluid CO2 dry process and calcination at 450 ℃ under the vacuum. And the aerogel properties of TiO2-ACF were obtained. SEM observation showed that the particles of TiO2 were uniform with an average size of about 15-20 nm, and TiO2 was deposited on almost each carbon fiber. After XRD analysis, anatase ratio was 77%; TiO2-ACF may effective eliminate or reduce toluene and xylene in the air, and photocatalytic degradation was 30% higher than ACF.