Nanometer blocks of amide-functionalized Fe(Ⅲ)-based metal-organic frameworks, NH₂-MIL- 53(Fe), were prepared via ultrasonic method without any surfactants at room temperature and atmospheric pressure. The characterization for the as-prepared nano-structured MOFs was established by XRD, SEM, TEM, XPS and N₂ adsorption-desorption. The as-prepared sample with high specific surface area (179.9 m²·g^-1) showed excellent adsorption for methylene blue in the liquid phase. The as-prepared NH₂-MIL-53(Fe) adsorbent seems to be a promising material in practice for organic dye removal from aqueous solution.