The present work aimed to design a separation process for 2-phenylethanol (2-PEA) produced by whey fermentation and to evaluate its economic potential. The separation sequence consisted of a liquid–liquid extraction column followed by two distillation columns for 2-PEA purification and solvent recovery. In addition, the use of ethyl acetate as a solvent for the extraction process was analyzed. The results, aided by the Aspen Plus v.10 process simulator, showed that 2-PEA can be separated with a purity of 96% by weight. The operating cost of the process, estimated at USD 22.70 per kilogram, shows that the separation alternative developed in this work has a high economic potential. The use of ethyl acetate as a solvent was found to efficiently remove 2-PEA from the fermentation mixture. From a process safety analysis point of view, the use of a bioprocess safety index developed in this work identified the separation process sections that could require special attention as part of the safety engineering stage of the process implementation.