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Fe3O4@C nanoparticles were prepared by an in situ, solid-phase reaction, without any precursor, using FeSO4, FeS2, and PVP K30 as raw materials. The nanoparticles were utilized to decolorize high concentrations methylene blue (MB). The results indicated that the maximum adsorption capacity of the Fe3O4@C nanoparticles was 18.52 mg/g, and that the adsorption process was exothermic. Additionally, by employing H2O2 as the initiator of a Fenton-like reaction, the removal efficiency of 100 mg/L MB reached ~99% with Fe3O4@C nanoparticles, while that of MB was only ~34% using pure Fe3O4 nanoparticles. The mechanism of H2O2 activated on the Fe3O4@C nanoparticles and the possible degradation pathways of MB are discussed. The Fe3O4@C nanoparticles retained high catalytic activity after five usage cycles. This work describes a facile method for producing Fe3O4@C nanoparticles with excellent catalytic reactivity, and therefore, represents a promising approach for the industrial production of Fe3O4@C nanoparticles for the treatment of high concentrations of dyes in wastewater.

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Fe3O4@C nanoparticles were successfully synthesized by an in situ solid-phase method using FeSO4, FeS2, and PVP K30 as the starting materials under the nitrogen atmosphere. In addition, the mechanism of the synthetic of Fe3O4@C nanoparticles was studied through in situ characterizations. The results showed that the pyrolysis of PVP K30 participated in the solid-phase reaction and resulted in the formation of carbon shells and a reduction in particle size. The structure of the Fe3O4@C nanoparticles was core–shell with the average particle size of ∼30 nm and the thickness of the carbon shell of ∼2 nm. Besides, the Raman spectrum revealed that the carbon shell mostly existed in the form of amorphous carbon. The surface area and the pore volume of the Fe3O4@C nanoparticles were estimated to be 37.74 m2 g−1 and 0.227 cm3 g−1. Magnetization hysteresis curve exhibited the values of coercivity and remanence and saturation magnetization are found to be approximately 0.16 kOe, 12.8 emu g−1, and 77 emu g−1, respectively.