Wastewater is characterized by multipollutant, and the presence of competitive adsorption could affect removal efficiency. Hence, the decontamination of water by adsorption in a multicomponent system allows an understanding of the practically and adsorbent efficiency. In this study, we present an analysis of the adsorption phenomena in a binary solution comprising compounds from distinct families, a dye, and an antibiotic, utilizing activated carbon obtained through a sustainable procedure. Locally available agricultural biowaste, specifically macadamia nutshell (MNS), served as a sustainable precursor to produce hierarchical porous activated carbon. The activation conditions were fine-tuned using the Box–Behnken experimental design. The resultant activated carbon was employed to remove a binary solution (BS) comprising the cationic dye, methylene blue (MB) and an ionic molecule amoxicillin (AMX) under specified conditions, including a pH range of 2 to 12, an initial concentration of BS ranging from 50 to 800 mg/L, and an adsorbent dosage within the range of 0.1 g to 0.3 g in a single adsorption system. The results revealed that higher temperatures adversely impacted the carbon yield, with a pronounced interaction effect observed between temperature and time. The activation temperature and K2CO3:precursor molar ratio predominantly influenced the textural and morphological properties of the activated carbon. Under optimal conditions (900 °C, 1 h, and a K2CO3:precursor ratio of 2:1), remarkably high-surface area (1225 m2/g), pore volume (0.801 cm3/g), and a nanopore size of 0.406 nm were achieved. In binary adsorption studies, R2-MNS demonstrated a maximum adsorption capacity of 578.925 mg/g. A pH above 4.5 produced an antagonistic effect on the removal of AMX due to competitive adsorption. Evaluation of three isotherm models demonstrated that the Khan isotherm best describes the affinity of BS to R2-MNS. The pseudo-second-order kinetic model best describes the data, indicating a chemisorption mechanism. The interparticle diffusion test revealed that the adsorbent exhibited very fast adsorption behaviour at the initial stage.
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