As a second step in our work of metal recovery from heavy oil fly ash, mutual separation of V/Fe was studied using a chelating resin, DIATON CR11 or a strong acid cation resin, DIAION SK1B. A prototype of a moving bed has been developed and applied for the separation of V/Fe. Sulfuric acid solution of V and Fe was one stream in the leaching process proposed by the authors. Metals should be separately removed from the solution so as to reuse the sulfuric acid solution. The resin CR11 selectively adsorbs Fe which is a major component in the stream, while SK1B removes a large qiantity of both metals. Vanadium can be recovered from the effluent with a bed of the resin SK1B. A moving bed applied with liquid pulse has been developed. Giving pulse to the liquid is effective to obtain a stable plug flow of resin in the bed and the resin flow rate is successfully controlled by amplitude and frequency of the pulse. Characteristics of V/Fe separation are studied under various operating conditions. Degrees of separation of V/Fe are enhanced by the operation applying a large bed height at a small resin flow rate.