Highly selective, absorbent, free-standing, paper-like membranes made of ammonium vanadium oxide (NH(4)V(4)O(14)) nanobelts have been engineered by taking advantage of the nanoscaled self-assembly of architectures that display a mesh structure with an average periodic pore size of about 5 to 10 nm. The NH(4)V(4)O(14) nanobelts are synthesized by using a simple hydrothermal process, and exhibit the same orientation and assemble into bundles, each about 40 to 80 nm in width, 3 to 5 nm in thickness, and up to several millimeters in length. Importantly, the as-obtained NH(4)V(4)O(14) nanobelt membranes can highly selectively absorb a variety of organic solvents, covering both polar and non-polar solvents, for example, the absorbent capacity of glycol is 28 times as high as the initial weight of the membrane, and it can even separate organic solvents with similar polarities and absorb solid contaminants in organic solvents. These highly selective, absorbent membrane materials can be an ideal candidate for the separation and removal of pollution in industrial and environmental applications.