In this study, we propose a virtual reality biphasic separator methodology in an immersive industrial environment. It allows the training of students or engineers in process and automatic control. On the other hand, the operating performance of a biphasic separator requires advanced automatic control strategies because this industrial process has multivariable and nonlinear characteristics. In this context, the virtual biphasic separator allows the testing of several control techniques. The methodology, involving the immersive virtualization of the biphasic separator, includes three stages. First, a multivariable mathematical model of the industrial process is obtained. The second stage corresponds to virtualization, in which the 3D modelling of the industrial process is undertaken. Then, the process dynamic is captured by the plant model implemented, in the software Unity. In the third stage, the control strategies are designed. The interaction between the virtual biphasic separator and the control system is implemented using shared variables. Three control strategies are implemented and compared to validate the applicability: a classic control algorithm, namely, the proportional integral derivative (PID) control method, as well as two advanced controllers—a numerical controller and model predictive control (MPC). The results demonstrate the virtual separator’s usability regarding the operating performance of the virtual biphasic separator, considering the control techniques implemented.