Abstract: Copper is removed from spent solutions of complexing agents containing cuprous aluminum tetrahalide, such as CuAlCl.sub.4.toluene by (1) contacting said solutions with water so as to form a precipitate of cuprous halide, an aqueous phase and an organic phase; (2) oxidizing the cuprous halide to cupric halide thereby rendering it water soluble; (3) separating the organic phase and aqueous phase, (4) contacting the aqueous phase with an environmentally suitable metal higher than copper from the electromotive series, such as aluminum, thereby precipitating copper metal and (5) separating the precipitated copper metal from the aqueous salt-containing mixture.Alternatively, the spent complex solutions can be contacted with 1 molar to 6 molar aqueous solution of a non-oxidizing acid such as HCl thereby eliminating the necessity of the oxidizing step (2) since the cuprous halide is soluble in the acidified aqueous phase.