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Under microwave irradiation, the ternary CuMgAl-HTLcs precursors were synthesized and MoO42- was loaded on the surface of these HTLcs. The results of XRD, FT-IR and SEM analysis indicated that the Mo anion was successfully loaded on the surface of the CuMgAl-HTLcs precursors. The activity of CuMgAl-31 for phenol hydroxylation was the highest, the conversion of phenol was 42.88% and ratio of catechol to hydroquinone was 2:1. CuMgAl-Mo-HTLcs advantageously increased the selectivity of hydroquinone with the ratio of hydroquinone to catechol reaching to 6:1 and about 4% conversion decreasing. Proposed the reaction mechanism of phenol hydroxylation by MoO42- supported HTLcs.