Abstract
The efficient isolation process and understanding of lignin properties are essential to determine key features and insights for more effective lignin valorization as a renewable feedstock for the production of bio-based chemicals including wood adhesives. This study successfully used dilute acid precipitation to recover lignin from black liquor (BL) through a single-step and ethanol-fractionated-step, with a lignin recovery of ~35% and ~16%, respectively. The physical characteristics of lignin, i.e., its morphological structure, were evaluated by scanning electron microscopy (SEM). The chemical properties of the isolated lignin were characterized using comprehensive analytical techniques such as chemical composition, solubility test, morphological structure, Fourier-transform infrared spectroscopy (FTIR), 1H and 13C Nuclear Magnetic Resonance (NMR), elucidation structure by pyrolysis-gas chromatography-mass spectroscopy (Py-GCMS), and gel permeation chromatography (GPC). The fingerprint analysis by FTIR detected the unique peaks corresponding to lignin, such as C=C and C-O in aromatic rings, but no significant differences in the fingerprint result between both lignin. The 1H and 13C NMR showed unique signals related to functional groups in lignin molecules such as methoxy, aromatic protons, aldehyde, and carboxylic acid. The lower insoluble acid content of lignin derived from fractionated-step (69.94%) than single-step (77.45%) correlated to lignin yield, total phenolic content, solubility, thermal stability, and molecular distribution. It contradicted the syringyl/guaiacyl (S/G) units' ratio where ethanol fractionation slightly increased syringyl unit content, increasing the S/G ratio. Hence, the fractionation step affected more rupture and pores on the lignin morphological surface than the ethanol-fractionated step. The interrelationships between these chemical and physicochemical as well as different isolation methods were investigated. The results obtained could enhance the wider industrial application of lignin in manufacturing wood-based composites with improved properties and lower environmental impact.