There is provided an improvement in a process for producing cobalt (III) hexammine sulphate which process comprises oxidatively pressure leaching nickel cobalt sulphides in an ammoniacal ammonium sulphate solution. The nickel and cobalt sulphides are oxidized to sulphates, and an ammoniacal leach liquor in which dissolved cobalt is predominantly in the (III) oxidation state is produced. The ammoniacal leach liquor is combined with ammonia to precipitate the triple salt of cobalt (III) hexammine sulphate, nickel (II) hexammine and ammonium sulphate which is further treated to produce a crystalline cobalt (III) hexammine sulphate and a nickel enriched leach liquor. The improvement involves the provision of a second oxidative pressure treatment effective to maximize the formation of the desired cobalt (III) hexammine ion, prior to the triple salt precipitation step.

 
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