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New routes for biomass valorization have been developing by the scientific community. The aim of this work was developing a novel OrganoCat-based protocol and deeply understand the structure of the obtained lignins. Microwave-assisted OrganoCat-based process was performed using a biphasic system (ethyl acetate and oxalic acid or HCl) at mild conditions. OrganoCat-based lignins (OCLs) were characterized by compositional analysis, FTIR, 1 H, 13 C, 1 H 13 C HSQC, 31 P NMR, TGA and GPC. The solubility of OCLs in different organic solvents and their antioxidant capacity against DPPH were investigated. The spectroscopic analyses showed that OCLs have high residual extractives and the lignin motifs were preserved. OCLs have presented lower thermal stability than MWL, but showed great antioxidant activities and high solubility in a wide range of organic solvents. A novel biorefinery protocol yielded coconut shell lignins with peculiar structural and compositional features and several technological applications through an eco-friendly, sustainable and relatively low-cost biphasic pulping process., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)