Wastewater from the olive oil mill (OMW) is an environmental hazard as it contains toxic and persistent compounds with significant organic load and high turbidity. The purpose of the present investigation is to assess the effectiveness of OMW treatment by flotation and coagulation procedure using Moringa oleifera. Physicochemical analysis of OMW showed high levels of the original chemical oxygen demand (COD) with a concentration of about 230.4 g/L, turbidity, and polyphenols with an initial concentration of around 5.4 g/L. After natural flotation, polyphenols, turbidity, and COD were reduced by 16.6%, 50%, and 31.2%, respectively. Turbidity, suspended solids, COD, polyphenols, and nitrates were all removed by natural flotation and coagulation by Moringa oleifera with percentages of about 83%, 74.5%, 57.6%, 65.6%, and 73.3%, respectively. Principal component correlation analysis between pollution removal parameters indicates that all variances are in the first component, with pH, nitrate, polyphenol, COD, and turbidity concentrations positively correlated. The proposed treatment process, which uses Moringa oleifera as a coagulant, can be applied in many industries due to its unique characteristics, including cheap cost and environmentally friendly approach.