Characterization of kraft lignin prepared from mixed hardwoods by 2D HMQC and 31P NMR analyses

Abstract

This study was conducted to determine the lignin substructures, hydroxyl (phenolic + aliphatic) contents, and carboxyl contents in kraft lignin (KL) prepared from mixed hardwoods by using 2D Heteronuclear Multiple Quantum Coherence Nuclear Magnetic Resonance (HMQC NMR) and 31P NMR techniques. Based on 2D HMQC NMR analysis of KL, stilbene and vanillin substructures were present in the aromatic region, while trace amounts of β-O-4 and β-β moieties were detected in the oxygenated aliphatic region. The total hydroxyl content calculated from 31P NMR was 5.24 mmol/g KL. The aliphatic hydroxyl content was 1.04 mmol/g KL, and phenolic hydroxyl content was 4.20 mmol/g KL. Of the phenolic hydroxyl groups, the contribution of syringyl (S) and guaiacyl (G) was 1.02 and 0.97 mmol/g KL, respectively. The S/G molar ratio of KL calculated from 31P NMR was 1.05. The carboxyl content was 0.44 mmol/g KL.