Discharging oil-contaminated wastewater into the environment without adequate treatment can have a negative impact on water resources, public water and wastewater treatment systems, and even human health. In this sense, it is essential to develop compact, easily automated, low-cost, and highly efficient unitary treatment processes in order to comply with legal requirements regarding effluent emission standards for water bodies. Therefore, the present study consisted of the development of two treatment processes aimed at the separation of oil emulsions stabilised by anionic surfactants: a sorption column using polyurethane/graphene foam composites as sorbent material and a continuous flow AC electroflotation reactor. Initially, composites with 0.5% and 1% w/w graphene (based on polyol mass) were developed using a dispersing agent (1-methyl-2-pyrrolidone). The foams were characterised in terms of morphology and mechanical and sorption properties. In the fixed bed column, the foams retained up to 77.15% of the emulsified oil and 52.36% of the anionic surfactants. In the continuous flow electroflotation reactor, emulsified oil removal efficiencies above 90% were achieved at all electrical currents tested, and up to 88.6% of anionic surfactants were removed at an electrical current of 150 A. Given the advantages and disadvantages of the two oily effluent treatment processes, their combined use in the same system proved promising.