Biomass waste, generated globally in vast quantities, represents an underutilized yet highly valuable resource for advanced material production. This study highlights a novel valorization pathway for waste tangerine peels, sourced from Jeju Island, South Korea, by converting them into high-performance activated carbon (T-AC) with exceptional pore characteristics, specifically designed for volatile organic compound (VOC) removal. Utilizing a unique combination of hydrothermal carbonization (HTC) and dry carbonization (DC) processes, the structural properties of the biomass were optimized, significantly enhancing the fixed carbon content. Subsequent chemical activation with an alkaline agent yielded T-AC with an outstanding specific surface area (1530–3375 m2/g) and total pore volume (0.73–2.00 cm3/g), with a tailored pore distribution favoring the sub-mesopore range (2.0–4.0 nm). The T-AC demonstrated remarkable performance in removing methylene chloride (MC), a hazardous VOC, with methylene chloride activity (MA) increasing from 44.7% to 76.3% as the activation agent ratio increased, while methylene chloride working capacity (MWC) improved significantly from 17.1% to 55.9%. These results underscore the transformative potential of tangerine peel-derived AC as a sustainable solution for VOC remediation, combining environmental waste management with advanced adsorption technology. The findings not only advance the field of biomass utilization but also offer a scalable approach for tackling pressing environmental and industrial challenges.
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