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Abstract A new type of photocatalytic La3+–Zn2+–Al3+–MoO4 2− layered double hydroxide (LDH) material (molar ratio, La/Zn/Al = 1:7:2) was prepared by a complexing agent-assisted homogeneous precipitation technique. The structure of the prepared LDH material was systematically studied. Under UV irradiation, the desulfurization efficiency of the LDH material was 87% in 2 h. For La3+–Zn2+–Al3+–MoO4 2− LDH material, the introduction of MoO4 2− increased the interlayer space for promoting the adsorption of benzothiophene (BT), and MoO4 2− might provide active sites for the oxidation of BT, resulting in the high desulfurization efficiency.