Valorization and characterization of agricultural and forest biomass residues through colloidal lignin particle production

Abstract

The valorization of secondary biomass streams is an important step toward more resource-efficient biorefinery concepts and reduced dependence on fossil-based materials. In this study, agricultural and forest residues, namely Atlas cedar cones, mixed conifer cones, hazelnut shells, walnut shells, coffee silverskin, and cocoa shells, were investigated as feedstocks for producing colloidal lignin particles. Lignin-rich extracts were obtained by Organosolv pretreatment using 60 wt% aqueous ethanol, followed by particle formation through solvent shifting and purification by ultrafiltration. A particular novelty of this work is that highly different feedstocks were processed under identical Organosolv and solvent-shifting conditions, enabling a direct comparison of their suitability for colloidal lignin particle production within one consistent process route. The feedstocks differed markedly in extractive content and chemical profile, as shown by sequential Soxhlet extraction and qualitative GC-MS screening. Despite these differences in extract composition, solvent shifting yielded colloidal lignin particles with largely similar properties. Dynamic light scattering showed hydrodynamic diameters of 65–88 nm immediately after precipitation for all samples except cocoa shell, which formed strong agglomerates. The ultrafiltration step further introduced an industry-relevant downstream purification stage by removing most water-soluble low-molecular-weight compounds before product evaluation. After purification and redispersion, particle sizes ranged from 121 to 389 nm, indicating partial aggregation but overall successful recovery of stable colloidal dispersions. All purified particle suspensions exhibited comparable antioxidant activity in the FRAP (ferric reducing antioxidant power) assay, ranging from 12.3 to 18.4 mg lignin per mg ascorbic acid equivalents. These results demonstrate that even chemically diverse biomass side streams can be converted into purified colloidal lignin suspensions with similar colloidal behavior and functional performance. The findings highlight the potential of low-value agricultural and forest residues as promising raw materials for lignin-based antioxidant and material applications.