Maximizing the valorization potential of lignin through optimization of the Soda pulping conditions

Abstract

The valorization potential of lignin is strongly dependent on the yield that can be obtained during the pulping process as well as its chemical structure. Both of these are determined by factors such as the biomass type, the selected extraction strategy and the employed conditions. Within this study, Miscanthus x giganteus biomass was subjected to systematically varying Soda pulping conditions, i.e., temperature (100 °C – 180 °C), OH– concentration (0.158 mol/L – 1.000 mol/L) and time (60 min – 360 min). These pulping conditions can be combined into a single factor, reflecting the processing severity, which in this work varied from approximately 1 to 5. The resulting black liquor, precipitated lignin, lignin stock solution (i.e., lignin dissolved in the solvent used in the subsequent depolymerization step) and product pool after mild reductive catalytic depolymerization (200 °C, 10 bar H2 initial, 4 h) were thoroughly characterized using a plethora of analysis techniques. Increasing the severity factor of the pulping was found to result in an enhancement of the delignification degree from 25.3 ± 2.6 % to 95.4 ± 9.9 %. However, beyond a severity factor of 3, fragmentation of native ether linkages and condensation reactions start to cause unfavourable changes in the chemical structure of the lignin and depolymerization product pool. Furthermore, these reactions significantly reduce the total mass yield from biomass to depolymerization product pool. An Adaboost model with quadratic base estimator was trained against the experimental data, and subsequently used to optimize the pulping conditions, aiming at a maximum total mass yield with minimal fragmentation and, hence, condensation, of the lignin. The optimum was experimentally validated, which resulted in a lignin with high β-O-4 content (42.7 ± 2.8 linkages per 100 aromatic units) and a total mass yield of 30.9 ± 3.4 wt% and a pulp with a residual lignin content of 8.25 ± 0.94 wt%.