Mg0.7Al0.3(OH)2(CO3)0.15.xH2O hydrotalcite was synthesized by co-precipitate method prior to the thermal decomposition in order to prepare the Mg(AlO)x supported molybdenum sulfide catalysts. Two MoS2/Mg(AlO)x samples were prepared by the wetness impregnation method. Both the Mg-AI hydrotalcite parent and MoS2/Mg-AI-O catalyst were characterized by XRD, SEM, TEM, EDX, and XPS. The characteristic results indicated a good dispersion of MoS2 on Mg(AlO)x periclase-like oxide matrix. The dispersion of MoS2/support is varied with the amount of MoS2 loading. A partial amount of S-2 moiety on the surface was spontaneously oxidized to sulfate ion after storing several weeks in air.