This study proposes a unique way of preparation of biocoagulant from Moringa oleifera defatted seed press cake. The press cake used in this study is a waste material produced as a by-product during cold press oil making from Moring oleifera seeds. The prepared Moringa oleifera seed defatted press cake based biocoagulant was found more effective than presently used metallic and polymer-based coagulants and flocculants for removal of fine particles of colloidal size from the effluent generated in the process of coal beneficiation. The detailed characterization of Moringa oleifera defatted seed press cake and the prepared biocoagulant for Particle size, Field Emission Scanning Electron Microscopy, Energy Dispersive X-Ray analysis, Zeta Potential, Fourier-transform Infrared Spectroscopy, etc. was done. The biocoagulant has been found effective in 97.4% total suspended solids removal and 97.48% turbidity removal from coal beneficiation plant effluent. The biocoagulant has been found to work satisfactorily under high fluxes of turbidity and total suspended solids with high removal of fine particles. The age of biocoagulant had negligible effect on fine particle removal efficiency (97.4% for fresh to 95% for 3-week-old biocoagulant). Field Emission Scanning Electron Microscopy analysis reveals considerable increase in flocs size from 198 nm to a 20 μ size well-developed flocs. The biocoagulant has proved as an efficient substitute of the metallic and polymer-based coagulants for the efficient treatment of coal beneficiation plant effluent.