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To design more environmentally friendly, economical, and efficient demulsifiers for oily wastewater treatment, hydrophobic octadecylphosphonic acid (ODPA)-modified Fe3O4 nanoparticles (referred to as Fe3O4@ODPA) were prepared by condensation of hydroxyl groups between ODPA and Fe3O4 nanoparticles using the co-precipitation method. The prepared magnetite nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscope (SEM), Fourier transform infrared (FTIR) spectroscopy, and thermogravimetric/differential thermogravimetric (TG/DTG) analysis. The water contact angles (θW) of Fe3O4@ODPA nanoparticles were more than 120°, indicating hydrophobic nature, and the diameter of the obtained spherical-shaped magnetite nanoparticles was 12–15 nm. The ODPA coating amount (AO) (coating weight per gram Fe3O4) and specific surface area (SO) of Fe3O4@ODPA were 0.124–0.144 g·g−1 and 78.65–91.01 m2·g−1, respectively. To evaluate the demulsification ability, stability, and reusability, the magnetite nanoparticles were used to demulsify an n-hexane-in-water nanoemulsion. The effects of the magnetite nanoparticle dosage (CS), pH value of nanoemulsion, and NaCl or CaCl2 electrolytes on the demulsification efficiency (RO) were investigated. The RO of Fe3O4@ODPA samples was found to be higher than that of bare Fe3O4 samples (S0, ST, and SN) under all CS values. With the increase in CS, the RO of Fe3O4@ODPA samples initially increased and then approached equilibrium value at Cs = 80.0 g·L−1. A maximum RO of ~93% was achieved at CS = 100.0 g·L−1 for the Fe3O4@ODPA sample S2. The pH and two electrolytes had a minor effect on RO. The Fe3O4@ODPA nanoparticles maintained high RO even after being reused for demulsification 11 times. This indicates that the hydrophobic Fe3O4@ODPA samples can be used as an effective magnetite demulsifer for oil-in-water nanoemulsions. [ABSTRACT FROM AUTHOR]