Recovery of palladium from an exhausted catalyst by chlorination: effect of carbon content and thermal treatment

The amount of Pd recovered from an exhausted olefin hydrogenation catalyst was found to depend on mixing technique, particle size, carbon percentage, chlorine flow, reaction time and temperature. Pd extraction was total when a sample in the 125-175 micrometre particle size range was chlorinated for 60 min at 723 K with 20 cm3 Cl2/min, for 60 min at 748 K with 30 cm3 Cl2/min and for 30 min at 773 K with 30 cm3 Cl2/min. No C addition was needed; the initial C content of the catalyst was sufficient for total recovery. Pd extraction was also affected by heat treatment in different atmospheres before chlorination. Treatment with O2, N2 and N2 with traces of O2 led to different degrees of oxidation of C and permitted the formation of oxidised Pd species. Thermal pretreatment in N2 with traces of O2 was most conducive to Pd extraction