Ni-Ce-Al layered double hydroxides (LDHs) with various Ni:Ce:Al molar ratios (3: 0.1:0.9, 3:0.2:0.8 and 3:0.5:0.5) were prepared by Co-precipitation. Ce can replace Al in a wide range of Ce/Al ratios to form Ni-Ce-Al-LDH with the unique layered structure of hydrotalcite. After the calcined at 600°C, LDHs samples were converted to mesoporous NiO-CeO2mixed oxides with a high surface area. The Ni-Ce-Al mixed oxide catalysts exhibit superior catalytic activity in oxidative dehydrogenation of propane and the excellent activities were attributed to mesoporous structure and the suppression of coke deposition.