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A new process for the separation of aluminium chloride from iron chlorides was studied from the standpoint of the recovery of aluminium from its ore and scraps. In this process, the aluminium chloride is transported from the aluminium-iron mixed chloride in the presence of sodium chloride. The separation experiments were conducted using double cells with two compartments. In the case of the AlCl3-FeCl3 system, FeCl3 tended to remain in the compartment in which the mixed chloride was placed, while A1C13 was transported to another compartment forming a NaAlCl4 stable complex. Transport efficiency and chloride purity were investigated under several conditions. The best separation was achieved when the molar ratio of NaCl to mixed chloride and the reaction time were 6 and 3 days, respectively. Transport efficiency of A1C13 increased with increasing temperature and became stable over 200°C. The chloride purity decreased corresponding to the increasing transport efficiency of FeCl3 over 200°C. A very high separation effect was observed when the sodium chloride was used compared to the separation result without sodium chloride. Separation of aluminium became more effective when the double cells were controlled at different temperatures. In the case of the AlClj-FeC^ system, very pure A1C13 (Fe:2 4 Died in 1989 ppm) and very high transport efficiency (99.95%) were obtained. The recovery of A1C13 by the reduction of AlCl3-FeCl3 mixture with aluminium and/or iron was shown to be effective.