TiO2/SiO2 aerogels with different molar ratio of SiO2/TiO2 were prepared via non-supercritical method using tetrabutyl titanate and silica sols as raw materials. The samples were characterized by TEM, SEM, BET, IR, XRD and so on. The results indicate that the BET surface area of TiO2/SiO2 aerogels calcined at 550 degrees C which consisted of anatase structure of TiO2 with narrow distribution pores of 5-25 nm is as high as 357.89 m(2 center dot)g(-1). For the photocatalytic degradation of pyridine, the catalytic activities of TiO2/SiO2 aerogels are much higher than that of TiO2 powder. The photocatalytic activity of TiO2/SiO2 aerogels calcined at 800 degrees C is the optimum. The higher the content Of SiO2, the higher the photocatalytic activity of TiO2/SiO2 aerogels. The cost for preparation of the aerogels is greatly reduced by using non-supercritical drying method, and the aerogels are hopefully applied in the treatment of industrial waste water such as coking effluent treatment.