Delignification of wood fibers using a eutectic carvacrol–methanesulfonic acid mixture analyses of the structure and fractional distribution of lignin, cellulose, and hemicellulose

Abstract

Delignification and fractional pretreatments are essential for valorization of wood biomass in various bioproducts. Herein, lignocellulose wood fibers were exposed to a eutectic mixture (EM) of carvacrol and methanesulfonic acid for different times. The resulting structural and chemical alterations in biomass were explored in terms of the fiber morphology and fractional chemical composition through fiber image analysis, field-emission scanning electron microscopy, high-performance liquid chromatography, and a novel approach based on fluorescence-lifetime imaging microscopy (FLIM). The autofluorescence of the lignocellulose fibers, which was primarily due to lignin with contributions from cellulose and hemicellulose, enabled application of FLIM in lignocellulose compositional analysis in micro-scale. FLIM analysis revealed that EM treatment efficiently removed lignin from the outer fiber layers. Furthermore, the effective EM treatment time was 3 h (with a residual lignin content of ~ 7 wt%), after which defects were observed on the fibers and the cellulose chains started breaking. This degradation was also indicated by a shift of the lifetime spectra toward the fluorescence lifetime of cellulose with increasing treatment time. Overall, our findings provide valuable insights to the response of lignocellulose fibers to EM treatment, contributing to the important goal of wood biomass application in bioproducts.