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Laurate (LA−)-intercalated nickel–chromium-layered double hydroxides (LDHs) were synthesized using the co-precipitation method and investigated as a potential photocatalyst for methylene orange (MO) degradation. For comparison, a series of LDHs with various molar ratios of Ni2+(or Mg2+)/Cr3+(or Fe3+)/LA−(or CO32−) were prepared. X−ray diffraction (XRD) and element analysis showed that Ni/Cr(2/1)−1.0 LA LDH had the most ordered crystal structure, and showed the same photocatalytic decolorization performance as Mg/Cr(2/1)−1.0LA LDH towards MO, which was significantly superior to Ni/Cr−CO3 LDH, Ni/Fe(2/1)−1.0LA LDH, and Ni/Cr−CO3 LDH with LA−, and Cr3+ with LA−. The photocatalytic removal rate of MO with the initial concentration of 100 mg/L by Ni/Cr(2/1)−1.0LA LDH (0.5 g/L) could be up to 80% with UV light irradiation for 3 h, which was almost twice higher than that of the sorption test. The photocatalytic reaction was in accordance with the pseudo-first-order kinetics, which implied that the catalytic process took place on the surface of the catalyst. All the results indicate the photodegradation of MO by Ni/Cr−LA LDHs was enhanced by the sorption of MO onto the intercalated LA− in the interlayer. The free radical capture experiments suggest that the main role of the photocatalytic mechanism of Ni/Cr−LA LDHs could be the •O2− with high oxidation activity produced by the electron-hole pairs of LDH, as excited by UV light. Additionally, the •O2− further reacted with the adjacent MO molecule pre-sorbed on the intercalated LA.

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