Abstract:A new nano composite matertal of EDTACoMgAl layered double hydroxides (EDTACoMgAlLDHs) was synthesized in the ways of coprecipitation. Then, Xray diffraction(XRD) and inductively coupled plasma(ICP) were used to characterize the properties of the material. The azo dye reactive black 5 was chosen as a target pollutant to study the effects of initial pH, concentration of target pollutant and temperature on adsorption. Finally, the properties of EDTACoMgAlLDHs as catalyst for Fenton reaction were discussed preliminarily. It is found that the maximum equilibrium adsorption was 330 mg?g-1 under the conditions of normal temperature and neutral pH. The catalytic oxidation and adsorption efficiency was complementary with increasing pollutant concentration. The total removal efficiency reaches up to 90% with the initial pollution concentration range of 120~360 mg?L-1.