A new nano composite matertal of EDTACoMgAl layered double hydroxides (EDTACoMgAlLDHs) was synthesized in the ways of coprecipitation. Then, Xray 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 EDTACoMgAlLDHs 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.