A series of La 2 O 3 -V 2 O 5 /MCM-41 catalysts with high specific surface area were prepared by means of incipient wetness impregnation for the dehydrogenation of ethylbenzene to styrene using CO 2 as oxidant. At 600°C, the conversion of ethylbenzene and selectivity to styrene over 10La15V/MCM-41 after an on-stream time of 4 h was about 86.5 and 91.0%, respectively. The properties of the catalysts before and after the reaction were characterized using techniques such as X-ray diffraction, specific surface area, Fourier transform infrared spectroscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, temperature-programmed desorption, and oxidation. The high catalytic activity and stability of 10La15V/MCM-41 during dehydrogenation of ethylbenzene is attributed to an optimized La/V atomic ratio. The accumulation of amorphous carbon species on the external surface of La 2 O 3 -V 2 O 5 /MCM-41 is the cause for catalyst deactivation.