Multifaceted valorization of lignocellulose into advanced environmental functional materials is of considerable relevance for a carbon efficient circular economy. In this study, a tailored multi-scale engineering approach assisted by AlCl3·6H2O/glycerol deep eutectic solvents (DESs) fractionation was presented for the dual valorization of waste distillers' grains-derived lignocellulose. This approach allowed for the production of cellulose-derived pyrolyzed hydrochar microflowers (PHMs) and lignin-derived carbon dots (LCDs) for multiphase control of water pollutants. The PHMs exhibited a well-defined flower-like morphology with a large surface area (662 m2·g−1) and highly open porous structure. Rich active centers (Co-Nx, graphitic N, and Co0 species) make it a robust heterogeneous peroxymonosulfate (PMS) activator for the removal of antibiotics with great adaptability. Notably, the integration of PHMs membrane filtration with PMS activation achieved an impressive average 93.2% tetracycline removal over 30 cycles at a high permeate flux of 257.96 L·m−2·h−1, highlighting the membrane's suitability for industrial applications. Additionally, the excellent optical properties, photostability, and hydrophilicity of LCDs open the door for detecting Fe3+ from 10-150 μM, exhibiting a linear standard curve with a high correlation coefficient (R2 = 0.96). The proposed integrated technique platform enables the comprehensive upgrading of lignocellulosic biomass and provides advanced carbon materials for downstream wastewater restoration towards industrial relevant processes.

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