Abstract: Ferrocyanide ions ((Fe(CN)6), a stable pollutant in cyanide-containing wastewater from gold production. hinder effective wastewater treatment and compliant discharge. This study developed zinc oxide(Zn0)-loaded activated carbon materials to investigate their removal efficiency, ads sorption mechanisms, and pyrolytic regeneration for adsorption products of Fe(CN)6+-. Results show that optimal preparation conditions include a roasting temperature of 550 °C. roasting time of 2 h, and ZnO loading of 10 %. Complete adsorption can be achieved with the adsorbent. The adsorption mechanism involves the reaction of ZnO on the activated carbon surface with Fe(CN)6*-to form Zn2 Fe(CN)6. During pyrolysis regeneration of adsorption products, Znz Fe(CN)6 decomposes into Zn, Fe, C, and N2, while unreacted ZnO active sites are re-exposed, enabling adsorbent regeneration. Regenerated adsorbents exhibit optimal performance when the pyrolysis temperature is 350 °C and the pyrolysis duration is 2 h under argon atmosphere.