Triboelectrostatic beneficiation, as a physical method, of fly ash cannot only meet the technical requirements of fly ash application but also recycle of an unburned carbon as a useful energy source. The aim of this study was to investigate the feasibility of improving efficiency of triboelectrostatic beneficiation of wet fly ash using microwave heating. The wet fly ash with different moisture contents had an average loss-on-ignition of 12.56%. The fly ash samples were heated in a microwave oven before the experiments. The experimental conditions were electric field voltage of 40 kV and air flux ranging from 12 to 30 m3/h. The influence of the microwave heating on the wet fly ash triboelectrostatic beneficiation was discussed under the conditions of different microwave intensity and irradiation time. The results indicated that the removal rate and recycle rate of the unburned carbon showed a significant increase performance as the wet fly ash was processed by the microwave heating which was attributed to changes of moisture contents and dielectric constants caused by the microwave heating. The feasibility had been verified according to the experimental study on fly ash with different moisture contents. It can be concluded that the microwave heating process was efficiently applied for the wet fly ash triboelectrostatic beneficiation.