AbstractLeveraging date palm spikelets (DPS) as a precursor, this study developed a DPS-derived composite (ZnO@DPS-AC) for water treatment, focusing on methyl orange (MO) removal. The composite was synthesized through ZnCl2 activation and pyrolysis at 600 °C. Comprehensive characterization was conducted using TGA, FTIR, XRD, SEM/EDS, and pHPZC. Characterization revealed a highly carbonaceous material (> 74% carbon) with significant porosity and surface functional groups. ZnO@DPS-AC demonstrated rapid MO removal, achieving over 45% reduction within 10 min and up to 99% efficiency under optimized conditions. The Langmuir model-calculated maximum adsorption capacity reached 226.81 mg/g at 20 °C. Adsorption mechanisms involved hydrogen bonding, π-π interactions, and pore filling. The composite showed effectiveness in treating real wastewater and removing other pollutants. This study highlights the potential of agricultural waste valorization in developing efficient, sustainable adsorbents for water remediation, contributing to circular bioeconomy principles.