The sonochemical degradation of toluene in the airproof aqueous solution was studied, and the mechanism and course of degradation was explored. It was found that the sonication time had great effect on the removal rate of toluene, and the degradation followed a pseudo-first-order kinetic law, and 90%-95% of toluene was removed only after being irradiated for 40 min, types of dissolved gas and pH also had some effects. After aqueous solution was analyzed pH and scanned UV-wavelength and identified components with SMPE-GC-MS, results confirmed that radical-oxidation controlled the sonochemical-oxidation of toluene, and main middle-products included benzaldehyde, bibenzyl, dibutyl phthalate, et al., final products were carbon dioxide and water.