Catalysts based on hydrotalcite-like precursors (Mg-Fe and Mg-Al-Fe) were synthesized by a co-precipitation method. The precursors and catalysts were characterised by XRD, TG, nitrogen physisorption, H2-TPR and Raman spectroscopy. The mixed oxides were applied in ethylbenzene dehydrogenation with CO2 and Mg-Al-Fe catalyst had better activity and stability. The improvement of Mg-Al-Fe in activities can be attributed to the better textural property and reduction property. There are two type of coke deposite on the catalysts and more coke deposit on Mg-Al-Fe catalyst.