Free carbon is the main impurity in boron carbide and has many side effects on the quality of boron carbide. In this study, reverse flotation was used for the first time to remove free carbon in boron carbide. The response surface methodology was utilized to optimize the reverse flotation factors, and the samples were analyzed by X-ray diffraction, scanning electron microscope, laser particle size analyzer, and chemical analysis. The study results reveal that the main factors affecting the decarbonization ratio were slurry concentration, collector dosage, foaming agent dosage and pH value. Furthermore, the results also show that reverse flotation could be applied effectively to the removal of free carbon in boron carbide. Slurry concentration of 25.14%, collector dosage of 567.9 g/t, foaming agent dosage of 199.32 g/t and pH value of 8.4 were found to be the best conditions. Under the optimal conditions, the decarbonization ratio is 84.23%. Mass ratio of free carbon in boron carbide reduced from 2.98 to 0.47.