The invention is relates to the preparation and use of dual layer membrane containing nanocellulose material for separation of metal ions from aqueous solution. Unlike the cellulose powder product, the invented nanocellulose filled dual layer membrane can work at high pressure and high temperature for removing metal ions via adsorption process. Since the membrane is excellent in removing low concentrated metal ions, it can be applied by integrating with unit operations such as activated carbon adsorption column, wet-process precipitation and other filtrations to optimize the wastewater purification performance