The membrane separation process has been significantly highlighted for the treatment of water and effluents in a scenario of water resource scarcity. Effective treatments capable of reducing costs and waste are always necessary, with the planning of the experiments before their execution of interest. The purpose of this work was to evaluate, through experimental planning, the influence of the polyethersulfone (PES), polyvinylpyrrolidone (PVP), and clay variables on the membranes’ parameters (viscosity and contact angle), seeking the best compositions for the production of hollow fiber membranes. Membranes were produced according to the compositions proposed by the planning and were characterized by Viscosity, Contact Angle, X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), and flow measurements. Through XRD, it was shown that the characteristic peaks of the clay remained in the membranes with higher concentrations. SEM analysis showed the influence of clay on the membranes’ porosity as well as the relation between “fingers” formation and PVP. From the flow measurement test, the relation between the obtained flow and the polymer and clay contents was verified. These tests showed the significant influence of clay on the membranes’ performance. Thus, the use of experimental planning resulted in the development of membranes and their importance in the design of future studies, making it possible to predict and simulate experiments.