A triboelectrostatic separation system for removing unburned carbon from coal fly ash is designed and evaluated. Fly ash from a coal-fired power plant is used as an accepted additive in concrete where it adds strength, sulfate resistance and reduced cost, provided acceptable levels of unburned carbon are maintained. Unfortunately, unburned carbon in coal fly ash absorbs some of other additives and reduces the concrete strength. This paper describes to investigate dry triboelectrostatic process to separate unburned carbon from coal fly ash and utilize it into economically valuable products. The laboratory-scale triboelectrostatic separation system consists of a particle feeding system, a tribocharger, a separation chamber, and collection systems. Particles of unburned carbon and fly ash can be imparted positive and negative surface charges, respectively, with a copper tribocharger due to differences in the work function values of the particles and the tribocharger, and can be separated by passing them through an external electric field. Results showed that fly ash recovery was strongly dependent on the electric field strength and the particle size. 70wt% of fly ash containing 6.5wt% of carbon contents could be recovered at carbon contents below 3%. The triboelectrostatic separation system showed a potential to be an effective method for removing unburned carbon from coal fly ash.