A process for recovery of zinc values contained in thermally activated iron containing copper and zinc sulfides in which said activated sulfides have been subjected to an acid leach in aqueous sulfuric acid to produce a solution of ferrous sulfate and a solids residue containing copper and zinc values. The solids residue containing copper and zinc values is reacted with an acidic copper sulfate solution to precipitate copper values as a simple copper sulfide with concurrent dissolution of iron and zinc values to form a solution of ferrous sulfate containing said dissolved zinc values and said solution of ferrous sulfate is separated from the simple copper sulfides and reacted with H.sub.2 S for precipitation of zinc values therefrom as zinc sulfide. Any nickel and cobalt values present in said activated sulfides is dissolved in said solution of ferrous sulfate and reacted with the H.sub.2 S at elevated temperature for selective precipitaton.