Influence of method and conditions of spent Pd/AC catalyst regeneration on its catalytic activity was studied. It has been stated that supercritical fluid extraction (CO2) followed by heating in hydrogen atmosphere is an effective method of that catalyst regeneration. The results of FTIR and XPS investigations indicate that regeneration of a spent Pd/AC catalyst, irrespective of the reaction in which it has been used, should be based on the complete removal of by-products and cleaning the catalyst surface as well as on restoring the original form of the palladium. Proposed in this paper procedure i.e. SFE (CO2) and heating in H2 fulfils both above mentioned conditions.