Magnetic separation is a promising strategy for removing nanoplastics (NPs) from water; however, it often requires complex processeses, such as synthesizing nano-Fe3O4 magnets and attaching them to specific carriers. This study presents an innovative and efficient strategy to in-situ synthesize and anchor nano-Fe3O4 onto polystyrene (PS) NPs through a two-step oxidation of ferrous ions, which significantly enhances NPs removal via magnetic separation. The two-step process involves initial alkalization of a ferrous aqueous solution under anoxic conditions, followed by oxidation in air. In the presence of PS spheres, nano-Fe3O4 forms in-situ on the PS surfaces, promoting sedimentation under a magnetic field. Results demonstrate that two-step ferrous oxidation achieves superior removal rates, with 99.32 % for 500 nm PS spheres (PS-500) and 93.16 % for 100 nm PS spheres (PS-100) using a low Fe2+ dosage of 0.1 mM. In contrast, the conventional one-step method, which simultaneously alkalizes and oxidizes ferrous sulfate in aerobic conditions, fails to form nano-Fe3O4 and results in low removal rates of only 56.49 % for PS-500 and 8.89 % for PS-100, respectively. Furthermore, the turbidity and residual Fe can be reduced to below 1 NTU and 0.1 mg/L by using two-step process, respectively, meeting drinking water safety and hygiene standards. This approach not only simplifies the magnetic nanomaterial preparation process but also substantially improves the NP removal efficiency, offering a promising solution for enhanced water treatment technologies and safer drinking water.
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