A reagent KCN solution and an industrial wastewater containing CN- can be efficiently degraded photocatalytically in aqueous TiO2 Semiconductor dispersions. The disappearance of CN-, consumption of O2, formation of OCN- an intermediate and ultimate mineralization to CO2 and N2 were quantitatively determined. A large-scale photoreactor (5 1) was also manufactured, which is an excellent device for the photodecomposition of a large amount of cyanide.