The volatilization kiln slag was produced by under over 1100℃ volatilizing a mixture composed of coke and the iron-vanadium and acid-leaching,which came from a zinc smelt system and from which a part of water was removed by drying.The content of carbon in the volatilization kiln slag reached 25.38%.The experimental study of recovering carbon from the volatilization kiln slag by floatation under the conditions of grind size being-0.074 mm 75%,using kerosene as collector and 2# oil frother was carried out,resulting in such better indexes as the grade of carbon concentrate of 80.90% and carbon recovery of 76.04%.