Azo dyes discharged in the environment are persistent organic pollutants （POPs）, which are very difficult to remove. We developed a microwave-assisted Fenton-like process to degrade methyl orange （MO）, an azo dye, with hydrogen peroxide （H2O2） catalyzed by chromium compounds coexisting with MO in the solution. Comparison between the Cr（Ⅲ）-H2O2 and Cr（Ⅵ）-H2O2 systems shows＂ that Cr（Ⅵ） has a stronger and more stable catalytical activity than Cr（Ⅲ）, and Cr（Ⅲ） is more susceptible to a change in the acidity or alkalinity of the reaction system. With a Cr（Ⅵ） concentration of 10 mmol L^-1 or a Cr（Ⅲ） concentration of 12 mmol L^-1 in the solution under the microwave irradiation of a power larger than 300 W for 3 min, 10 mmol L^-1 H2O2 can degrade more than 95% of 1 000 mg L^-1 methyl orange; when the microwave power is increased to 700 W, the same amount of H2O2 can degrade all methyl orange in the solution with the same amount of Cr（Ⅵ ） catalyst. Ultraviolet-visible spectrography indicates the cleavage of the azo bond in methyl orange after treatment, suggesting the potential o of this Fenton-like process to degrade azo dye POPs. Reusing waste chromium compounds coexisting with dyestuff in wastewater to catalyze the degradation of azo dyes could be a cost-effective technique for azo dyes and chromate manufacturers and/or users to treat their wastewater and prevent POPs from endangering the environment. This is of particula importance to controlling the water quality of the Three Gorges Reservoir.
