Coal bottom ash is rich in metals and transition metals, and with microwave irradiation these metals can effectively degradate organic matter. Methylene blue degradation by coal bottom ash-microwave irradiation mainly through hydroxyl radicals to degrade organic matter, and metals and rare metals in bottom ash can be used as a catalyst for deep oxidation of organic matter, can reduce processing costs, and reduce environmental pollution. In the present paper the main parameters including the amount of coal bottom ash, H2O2 dosage and time of microwave irradiation were investigated. The UV-visible spectra of methylene blue were determined. The results show that: under coal bottom ash and H2O2 microwave condition the degeneration rate of methylene blue was almost 100%. The dosage of coal ash can accelerate the reaction process, speeding up the degradation of methylene blue. The increase of H2O2 may provide more ·OH and speed up the reaction process, but when up to a certain amount, the influence is weakened. The lengthening of microwave time may enhance the reaction temperature, and urge the methylene blue to degrade completely. For 0.125 g·L-1 of methylene blue, by adding 1.0 g coal bottom ash, 5 mL H2O2 and under mesotherm microwave temperature for 4 min, the methylene blue can be all degradated.