Emerging pollutants are causing global health and environmental challenges, necessitating the advancement of methodologies for their efficient removal. In this study, we present the efficacy of superhydrophobic FeNi3/Al2O3 Janus particles in the removal of oils and microplastics from water, combined with the degradation of azo dyes, leveraging their surface properties. Field Emission Scanning Electron Microscopy (FESEM) and Energy Dispersive X-ray Spectroscopy (EDS) revealed the morphology and elemental composition of these particles, which were further complemented by X-ray diffraction (XRD) for phase identification. After surface functionalization of the FeNi3/Al2O3 Janus particles with lauric acid, they exhibited superhydrophobicity (152 ± 1°) and superoleophilicity (0°). High-resolution X-ray photoelectron spectroscopy (HR-XPS) showed that the alumina face was modified with lauric acid, while the intermetallic face remained as FeNi3. Significantly, the alumina face demonstrated 99 % efficiency in separating oils and microplastics, while the FeNi3 face facilitated the complete degradation (100 %) of methyl red within three minutes, as shown by ultraviolet-visible spectrophotometry. These results highlight the multifunctional properties of superhydrophobic FeNi3/Al2O3 Janus particles in removing and degrading various pollutants.