Ultrathin and hydrophilic MXene membranes can efficiently separate nanosized oil/water emulsions, which paves a new avenue for 2D material applications. Safety concerns about oily wastewater emerging from the petroleum-drilling industry, industrial sewage or spillage from tankers, or pipeline accidents have attracted longstanding worldwide attention. The sieving property of the innately hydrophilic MXene sheets can be adjusted using the corresponding interlayer space, which offers perfect materials for 2D membranes for oily wastewater treatments. This chapter addresses functionalized organic and inorganic materials for oil/water separation. Low-dimensional materials such as graphene and MXene are important materials in this wastewater treatment field. Organic-coated membranes are also discussed for comparison to elucidate the structural advantages of low-dimensional materials. Membrane surface engineering is the main focus of this chapter. Copolyamide 6,10 electrospun mats were used to filter single-layered or multilayered Ti 3 C 2 T x solutions to obtain MXene-coated polymer mats for water/vegetable oil emulsion treatment.