Activation upcycling of plastic waste into high-value carbon materials for aquatic pollutant removal presents a promising avenue for addressing environmental challenges. Herein, a Fe-Ni alloy encapsulated in hierarchically ordered macro/meso-microporous carbon (FeNi@HOMC) was synthesized via activator-assisted pyrolysis of waste polystyrene and then employed for periodate (PI) activation. The Fe-Ni heterostructure not only facilitated the formation of porous carbon but also promoted PI activation, generating reactive oxygen species. Meanwhile, the carbon shell prevented metal core aggregation and enhanced electron mobility. FeNi@HOMC exhibited outstanding removal of diverse organic contaminants over a broad pH range (4.0-11.0), demonstrating strong resistance to the effects of anions and humic acids while maintaining long-term stability. Continuous-flow experiments and toxicity assessments confirmed complete pollutant mineralization and reduced biotoxicity within 120 h. Mechanistic investigations revealed a non-radical oxidation pathway driven by high-valent metal species and singlet oxygen (1O2), coupled with an electron-transfer mechanism. The exceptional catalytic performance of FeNi@HOMC-700 was attributed to its abundant Fe/Ni-Nx catalytic centers, nitrogen doping, high surface area, and superior conductivity. This work not only suggests a cost-effective and waste-derived solution for organic pollutant degradation but also provides insights into mitigating plastic-induced environmental hazards.
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