Modular Polyoxometalate‐Layered Double Hydroxide Composites as Efficient Oxidative Catalysts

The exploitation of intercalation techniques in the field of two‐dimensional layered materials offers unique opportunities for controlling chemical reactions in confined spaces and developing nanocomposites with desired functionality. In this study, the exploitation of the novel and facile “one‐pot” anion‐exchange method for the functionalization of layered double hydroxides (LDHs) is demonstrated. As a proof‐of‐concept, we demonstrate the intercalation of a series of polyoxometalate (POM) clusters, Na₃PW₁₂O₄₀]?15 H₂O (Na₃PW₁₂), K₆P₂W₁₈O₆₂]?14 H₂O (K₆P₂W₁₈), and Na₉LaW₁₀O₃₆?32 H₂O (Na₉LaW₁₀) into tris(hydroxymethyl)aminomethane (Tris)‐modified layered double hydroxides (LDHs) under ambient conditions without the necessity of degassing CO₂. Investigation of the resultant intercalated materials of Tris‐LDHs–PW₁₂ ( 1 ), Tris‐LDH–P₂W₁₈ ( 2 ), and Tris‐LDH–LaW₁₀ ( 3 ) for the degradation of methylene blue (MB), rhodamine B (RB) and crystal violet (CV) has been carried out, where Tris‐LDH–PW₁₂ reveals the best performance in the presence of H₂O₂. Additionally, degradation of a mixture of RB, MB and CV by Tris‐LDH–PW₁₂ follows the order of CV>MB>RB, which is directly related to the designed accessible area of the interlayer space. Also, the composite can be readily recycled and reused at least ten cycles without measurable decrease of activity.