The main objective of this study was to conduct an investigation on the performance of organophilic clay as adsorbent in the oil/water separation process. The originality of this work is its focus on Brazilian clay. The gray organophilic clay was prepared from gray clay and quaternary ammonium salts. The samples were characterized by X-Ray Diffraction, Differential Thermal and Thermogravimetric Analysis, Infrared Spectroscopy, Cation Exchange Capacity, Adsorption Capacity and the Foster Swelling test. The results indicated that the quaternary ammonium salts were intercalated between the layers of clay. A 22 factorial design was conducted with three central points in finite bath tests to determine the rate and capacity of oil removal by the organophilic clays. Values as high as 99.3 % of removal efficiency and 32.5 mg/g of removal capacity were reached in the assays, thus indicating that the use of organophilic clay has great potential in the oil/water separation process.