Embedded nano-iron polysulfone membranes were prepared for dehydration of ethanol/water mixtures by pervaporation. It was found that the nano-iron particle can be prepared by in-situ thermal decomposition method in casting solution. The verification of the nano-particle dispersion in membrane was made by TEM measurement. It was found that the embedding nano-particle slightly increased the flux with the ordering polymer chains arrangement in membrane and also increased the separation factor. A remarkable enhancement in the separation factor of over 1000 can also be found in embedded membranes. But the flux of embedded membranes are lower (less than 350 g/m(2)-h) than the flux of non-embedded polysulfone membranes (500 g/m(2)-h). The increase in the separation factor of embedding membranes mainly contributed by the ordering/packing of polymer chains was caused by the surface effect of nano particle and limited the permeate diffusion behavior. On the other hand, it was found that the nano-particle embedding in the membrane showed a significant effect on the sorption behavior and presented a significant interaction between water and the embedded membrane. In this Study, the high performance dehydration membranes were successfully prepared with nano-particle embedding in polysulfone membranes.