In this work the effect on the adsorption of Cr (VI) by thermally treated Hydrotalcite-like Material (HTM) synthesized by the sol-gel method with a Mg/Al = 2 was studied. The characterization of the HTM before and after Cr (VI) removal, as well as the kinetic studies were carried out. When the HTM are thermally treated at 350ºC the hydrotalcite crystalline structure remains and the textural properties improve. The Cr (VI) adsorption capacity of HTM was 125 mg of Cr (VI) / g of HTM. This capacity augments at 132 mg of Cr (VI) / g of HTM after heating HTM at 300°C. The crystallinity as well the porosity of the HTM diminished after adsorption of Cr (VI), due to the obstruction of both the pores and the interlayer space. The adsorption of Cr (VI) occurred before 4 minutes contact time. It can be concluded that HTM exhibits a high Cr (VI) adsorption capacity in a short time.