In this paper, the effect of urea-hydrogen peroxide (UHP) solution on desulphurization and demineralization of coal with high sulphur and high ash by using HNO3 and microwave pretreatment was investigated. The oxidation process is strongly dependent on irradiation power and time for microwave pretreatment, UHP concentration, leaching time and temperature of the UHP solution. X-ray diffraction and Fourier transform infrared technique have been performed for the raw and treated coals. Compared with the UHP alone, successive treatments with HNO3 and microwave pretreatment resulted in the significant removal of total sulphur and mineral matter from the coal. The proposed experimental method has the meaning of practical guide to the desulphurization and deashing of coal by microwave.