Polymer/fluorocarbon surfactant membranes have been reported to display excellent oleophobic/hydrophilic behavior and outstanding oil/water separation properties. In this work, multiwalled carbon nanotubes (MWNTs) enhanced poly(styrene‐alt‐maleic anhydride)/fluorocarbon surfactant (PSMA/MWNTs/FS) membrane filters were prepared by dip‐coating PSMA/MWNTs/FS on stainless steel meshes for efficient oil/water separation. The microstructure, thermal properties, wettability, oil/water separation ability, and recyclability were investigated. The results revealed that the MWNTs are suitably dispersed in the membrane, further increasing the thermal stability, oil/water separation efficiency, and recyclability. The oil/water separation efficiency of the complex membrane filter containing MWNTs was 99% initially and 97% after 20 cycles. This work provides a simple, low‐cost, and environmentally friendly approach for efficient oil/water separation.