The upgrade of sustainable resource waste into a valuable and beneficial material is an urgent task. The current paper outlines the development of an economical, sustainable, and prolonged adsorbent derived from Sargassum siliquastrum biomass and its use for potent 2,4-dichlorophenoxyacetic acid (2,4-D) removal. A simple carbonization approach was applied to obtain the highly functionalized carbon structure, which was subsequently transformed into a novel magnetic nanoadsorbent. The magnetic nanoadsorbent was characterized using Fourier transform infrared spectrometer (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), Brunauer Emmett Teller (BET)-specific surface area, and vibrating sample magnetometer (VSM). The characterization results confirm the successful formation of a high specific surface area and a uniform distribution of Fe3O4/NiS NPs grafted activated carbon. The adsorption kinetics was more accurately described via the pseudo-second order model; nevertheless, the isothermal data showed that the Langmuir model was most suitable. The monolayer adsorption capacity for 2,4-D was 208.26 ± 15.75 mg/g at 328 K. The favourability and spontaneity of the adsorption process were demonstrated by thermodynamic studies. The adsorbent displayed exceptional selectivity for 2,4-D and high stability in multi-cycle use. Electrostatic attraction, π-π stacking, and hydrogen bonding were all believed to have an impact on the sorbent’s robust 2,4-D adsorption. Analyses of real tap and Nile River water samples showed little effect of the sample matrix on 2,4-D adsorption. This study presents an innovative approach for developing highly efficient adsorbent from natural biomass and offers an affordable way to recycle algal waste into beneficial materials.
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