The Fenton reaction is widely known as a promising method for treating organic pollutants. We investigated the photo‐assisted oxidative degradation of pollutants using various layered double hydroxides (LDHs) to develop heterogeneous Fenton catalyst capable of mineralizing organic pollutants. A LDH composed of Fe2+ and Al3+ (Fe2+Al3+‐LDH) under the irradiation of visible‐light (λ>420 nm) resulted in 2.5 times higher performance for the oxidative degradation (mineralization) of phenol as a model compound of organic pollutants compared with that without light irradiation. The ratio of Fe2+/Fe3+ on the surface of the Fe2+Al3+‐LDH after the reaction under the irradiation of visible‐light increased significantly compared with that without light irradiation. These indicated that the Fenton‐catalytic‐cycle was improved by reducing the Fe3+ generated after the Fenton reaction to the Fe2+ species by the photo‐assisted effects of the Fe2+Al3+‐LDH.
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