Abstract:HCl/Cl2 system to dissolve pretreated spent vinyl acetate catalyst was studied. Gold was reduced from hydrochloric acid solution bearing gold and palladium by sponge palladium powder. Reduced sponge gold powder was boiled with dilute nitric acid to remove excess palladium powder. Reduction mother liquor was used to recover palladium by sodium sulfide replacement. The purity of final gold and palladium product is 99.95% above with recovery rate of 99.8% above.