Abstract: To improve the catalytic performance of iron-based catalysts for dehydrogenation of ethylbenzene with CO₂, two samples, F4AZ10-imp and F4AZ10-pre, with the same contents of Fe, Al and Zr were prepared by the impregnation method and one-step precipitation method. The catalytic performance of these two samples for the dehydrogenation of ethylbenzene with CO₂ was tested at 550 ℃. Both the samples are characterized with XRD, NH₃-TPD, CO₂-TPD and H₂-TPR techniques and N₂ sorption experiment. It was shown that the preparation methods had a great effect on the catalytic performance. Compared to the impregnation method, the one-step precipitation method gave a more active catalyst because of a higher dispersion of active Fe₂O₃ on the catalyst surface and a stronger activation of CO₂.