FeCo@hydrochar nanocomposites as efficient peroxymonosulfate activator for organic pollutant degradation

Sulfate radical–based advanced oxidation processes (SR-AOPs) are renowned for their exceptional capacity to degrade refractory organic pollutants due to their wide applicability, cost-effectiveness, and swift mineralization and oxidation rates. The primary sources of radicals in AOPs are persulfate (PS) and peroxymonosulfate (PMS) ions, sparking significant interest in their mechanistic and catalytic aspects. To develop a novel nanocatalyst for SR-AOPs, particularly for PMS activation, we synthesized carbon-coated FeCo nanoparticles (NPs) using solvothermal methods based on the polyol approach. Various synthesis conditions were investigated, and the NPs were thoroughly characterized regarding their structure, morphology, magnetic properties, and catalytic efficiency. The FeCo phase was primarily obtained at [OH⁻] / [Metal] = 26 and [Fe] / [Co] = 2 ratios. Moreover, as the [Fe]/[Co] ratio increased, the degree of xylose carbonization to form a carbon coating (hydrochar) on the NPs also increased. The NPs exhibited a spherical morphology with agglomerates of varying sizes. Vibrating-sample magnetometer analysis (VSM) indicated that a higher proportion of iron resulted in NPs with higher saturation magnetization (up to 167.8 emu g⁻¹), attributed to a larger proportion of FeCo bcc phase in the nanocomposite. The best catalytic conditions for degrading 100 ppm Rhodamine B (RhB) included 0.05 g L⁻¹ of NPs, 2 mM PMS, pH 7.0, and a 20-min reaction at 25 °C. Notably, singlet oxygen was the predominant specie formed in the experiments in the SR-AOP, followed by sulfate and hydroxyl radicals. The catalyst could be reused for up to five cycles, retaining over 98% RhB degradation, albeit with increased metal leaching. Even in the first use, dissolved Fe and Co concentrations were 0.8 ± 0.3 and 4.0 ± 0.5 mg L⁻¹, respectively. The FeCo catalyst proved to be effective in dye degradation and offers the potential for further refinement to minimize Co²⁺ leaching.