In this study, the preparation of layered double hydroxide-metal oxide (ZnAl-ZnO, MgAl-ZnO, and NiAl-ZnO) was successful. The characterization of the catalyst used XRD, FTIR, and SEM analysis. The catalyst shows high oxidative desulfurization of dibenzothiophene. The percentage conversion of dibenzothiophene on ZnAl-ZnO, MgAl-ZnO, and NiAl-ZnO was 99. 38%, 99. 34%, and 99. 90%, respectively. The acidities of ZnAl-ZnO, MgAl-ZnO, and NiAl-ZnO were 0. 798, 2. 469, and 0. 184 mmol/g, respectively. The catalysts are heterogeneous systems, and the advantage is that they can be used for reusability. After 3 cycles of catalytic reactions at 323 K for 30 min, reusability proves that the percentage conversion of dibenzothiophene on ZnAl-ZnO, MgAl-ZnO, and NiAl-ZnO had a stable structure.