It is composited two materials called Fe-MCM-41 and Cu-MCM-41 by the means of impregnation method and ammonia method ,which are based on the mesoporous materials (MCM-41) and used the Cu and Fe as modified materials. By static sequence batch experiment, the effects of pH value, adsorption time, dosage and initial concentration of U (Ⅵ) for two kinds of materials above on the adsorption of U (Ⅵ) were investigated. The results showed that when pH value was 5, the temperature was 30℃, the adsorption time set up about 180min, the dosage of Fe-MCM-41 and Cu-MCM-41 were 0.2 g/L all, initial concentration of U (Ⅵ) was 10mg/L, the maximum adsorption rate were 93% and 84.2% respectively. The Langmuir adsorption isotherm model and pseudo two order kinetics could fit the U (Ⅵ) adsorption process well. The Theoretical saturated adsorption capacity was 211.94mg/g and 185.94mg/g respectively. Through analysis methods of both EDS and FTIR, it was obvious that the adsorption layer was monolayer adsorption, especially chemical absorption. When 0.1mol/L HCl was acted as the analytical reagent, the adsorption rate was still up to 90% and more than 80% after cycling for 5 times, i.e., these materials both Fe-MCM-41 and Cu-MCM-41 could be reused.