Research studies for cellulose recovery from lignocellulosic materials are essential in order to propose sustainable alternatives to harness residual biomasses, solving problems caused by their abundance and inadequate use. In this study, olive-tree pruning biomass has been subjected to different pretreatments with different organosolvents (acetone, ethanol, and γ-valerolactone) with microwave radiation assistance. The effect of operating parameters has been studied, considering specific ranges of variables values according to each experimental design but, in any case, located in the ranges of 33–67% (chemical compound concentration), 130–170 °C (temperature), 5–30 min (reaction time), and 1/20–1/5 (solid/liquid ratio, s/L). Based on the R2 and R2adj values (mostly above 0.97), the experimental data were adequately adjusted to four selected response variables: post-solids cellulose and lignin content apart from removal percentages of both structural components. The optimization process resulted in post-treatment solids with meaningful cellulose yields (higher than 84.7%) and reduced lignin content (lower than 4.2%). The best results were obtained using 66.5% acetone (155 °C, 8.4 min and s/L = 1/19), involving greater material deconstruction, a high percentage of delignification (96.7%), not very significant cellulose loss (29.4%), and a post-treatment solid consisting almost exclusively of cellulose (≈99%).
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