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[Display omitted] • Autohydrolysis enhanced the delignification of p -TsOH post-treatment of poplar. • Unexpectedly, the glucose yields of combined pretreated poplar decreased. • The intensified surface lignin coverage hindered the enzymatic hydrolysis. • Tween 80 enabled the excellent enzymatic hydrolysis of combined pretreated poplars. In this study, a combined pretreatment involving autohydrolysis and p -toluenesulfonic acid (p -TsOH) was performed on poplar to coproduce xylooligosaccharides (XOSs) and monosaccharides. The autohydrolysis (180 °C, 30 min) yielded 53.2 % XOS and enhanced the delignification efficiency in the subsequent p -TsOH treatment. Furthermore, considerably high glucan contents (64.1 %∼83.1 %) were achieved in the combined pretreated substrates. However, their enzymatic digestibilities were found to be extremely poor (9.6 %∼14.2 %), which were even lower than the single p -TsOH pretreated substrates (10.2 %∼35.8 %). The underlying reasons were revealed by systematically investigating the effects of the single and combined pretreatment strategies on substrate properties. Moreover, the Tween 80 addition successfully reversed the adverse effects of combined pretreatment on the enzymatic hydrolysis, achieving a high glucose yield of 99.3 % at an enzyme loading of 10 filter paper units/g (FPU/g) glucan. These results deepen the understanding of the synergy of combined pretreatment on biomass fractionation and enzymatic saccharification. [ABSTRACT FROM AUTHOR]

To elucidate the effects of lignin repolymerization on the combined pretreatment, the sequential acid and deep eutectic solvent (DES) pretreatment was implemented on Populus (poplar) in this study. Effects of acid pretreatment with or without phenolic additives (2-naphthol (2 N) and resorcinol (RS)) on the DES post-treatment efficiency were examined. The results showed that 2 N inhibited the lignin repolymerization in the first-step pretreatment, and slightly enhanced the lignin removal during DES post-treatment. However, RS intensified the lignin repolymerization, significantly decreasing the delignification of DES post-treatment from 73.6%∼79.4% to 39.0∼43.0%. Moreover, the poorer enzymatic hydrolysis was observed in the combined pretreated substrates as compared to the single DES pretreated ones, due to the higher surface lignin coverage. The addition of 2 N counteracted the adverse effects of acid pretreatment on the hydrolysis yields of combined pretreated substrates, and facilitated the yields from 25.8%∼36.0% to 26.2∼67.3%, while the RS addition further decreased the hydrolysis yields to 8.6∼9.6%. The mechanism for the changes on enzymatic digestibilities of the combined pretreated substrates was elucidated. [Display omitted] • 2-Naphthol inhibited lignin polymerization, while resorcinol intensified it. • Lignin repolymerization hindered the delignification of the DES post-treatment. • 2-Naphthol promoted the hydrolysis of pretreated poplar, but resorcinol impeded it. • 2-Naphthol addition benefited the lignin fractionation and valorization. [ABSTRACT FROM AUTHOR]

[Display omitted] • A novel combined H 2 SO 4 -ChCl/Gly pretreatment of reed stalks was developed. • Synergistic effect of H 2 SO 4 and ChCl/Gly eliminated xylan and lignin effectively. • H 2 SO 4 -ChCl/Gly-treated reed stalk was converted to glucose in a high yield of 91.1%. • High saccharification was due to enhanced accessibility and reduced lignin surface. In this study, an efficient combination of pretreatment solvents involving Choline chloride/Glycerol (ChCl/Gly) and H 2 SO 4 was firstly developed to assess the pretreatment performance and determine optimal pretreatment conditions. The results illustrated that the H 2 SO 4 -[ChCl/Gly] combination efficiently removed lignin (52.6%) and xylan (80.5%) from the pretreated reed stalk, and subsequent enzymatic hydrolysis yielded 91.1% of glucose. Furthermore, several characterizations were conducted to examine the structural and morphological changes of the reed stalk, revealing apparently enhanced accessibility (128.4 to 522.6 mg/g), reduced lignin surface area (357.9 to 229.5 m2/g), and substantial changes on biomass surface. Based on the aforementioned study, possible mechanisms for the H 2 SO 4 -[ChCl/Gly] pretreatment of reed stalks were proposed. The comprehensive understanding of combined H 2 SO 4 -[ChCl/Gly] pretreatment system for enhancing the saccharification of the reed stalk was interpreted in this work. Overall, this novel approach could be efficiently applied to pretreat and saccharify reed stalks, empowering the biomass refining industry. [ABSTRACT FROM AUTHOR]

An organosolv process using ethanol-water was optimized in order to recover high quality lignin from rice-straw previously pre-treated by autohydrolysis at 210 °C. The results showed a selective and appreciable removal of lignin under very mild conditions and the highest delignification yield occurred at 30 °C. The lignin extracts were characterised using capillary zone electrophoresis (CZE), size exclusion chromatography (SEC), Fourier transform infrared spectroscopy (FT-IR) and 31 P-NMR, and two-dimensional heteronuclear single quantum correlation NMR spectroscopy (2D-HSQC NMR), which enabled the identification of low molecular weight lignins with a syringyl/guaiacyl ratio of about 0.74 containing phenolic compounds with potential bioactive properties. In order to separate the target compounds, membrane technology has been used and an enriched extract containing value-added phenolic compounds such as tricin, vanillin, ferulic acid and p- coumaric acid was obtained. High membrane efficiency (around 80%) was obtained for target compounds. [ABSTRACT FROM AUTHOR]

To enhance the cellulose digestibility of energy grass hybrid Pennisetum ( P. americanum × P. purpureum , HP) with low energy-consumption and high efficiency, a novel combinatorial pretreatment of oxygen-aqueous alkaline ionic liquid (IL) 1-ethyl-3-methylimidazolium acetate ([Emim]Ac) media (OEA) was developed in this work. The combinatorial pretreatment was performed under the relatively low temperature (120 °C), short retention time (30 min), and 12 bar oxygen pressure. The combinatorial pretreatment of OEA was demonstrated effectively for pretreatment of hybrid Pennisetum , which evidenced by the removal of lignin, degradation of carbohydrate, and porosity property of the regenerated biomass. Subsequently, a higher glucose recovery (96.9%) at a low enzyme loading (20 FPU/g substrate) was obtained by the OEA pretreatment, and it was 9.1 times as much as the untreated samples. Overall, the novel OEA combinatorial pretreatment has the advantages of low thermal energy input and enzyme usage, and short retention time. [ABSTRACT FROM AUTHOR]

[Display omitted] • Additives in pretreatment notably raised fermentable sugars and bioethanol yields. • Mechanisms of reducing lignin repolymerization by additives were investigated. • −OH groups of additives suppressed lignin repolymerization by forming a new reaction. • More hydrophilic groups of lignin reduced non-specific binding into enzymes. • Enlarged biomass porosity and lower surface coverage reduced surface lignin barrier. Pretreatment is the key factor for producing fermentable sugars and biofuels from lignocellulosic biomass. However, during pretreatment lignin repolymerization occurs which reduces the efficiency of carbohydrates hydrolysis. In the present study, three additives (2-naphthol-7-sulfonate, 2-naphthol, and mannitol) were evaluated for boosting the effectiveness of combined pretreatment (liquid hot water + green liquor) of pine-wood biomass. The results revealed that supplied additives into combined pretreatment changed the physicochemical structure of lignin, therefore, alleviating the inhibitory effect of lignin repolymerization and notably raised sugars yield (glucose, xylose) ranging from 85% to 93%. XPS and FTIR analyses confirmed that −OH groups of additives led to lower formation of phenolic hydroxyl (PhOH) and higher hydrophilic groups of lignin, accounting for reduced non-specific binding of lignin into cellulase enzymes. Furthermore, additives increased surface lignin coverage, biomass porosity, and fiber swelling by 1.96–2.59, 1.66–1.86, and 1.13–1.29 folds respectively, comparing to corresponding sample without additives caused more liquified and extractable lignin, which notably reduced the surface lignin barrier. Hence, both factors including non-specific binding effect and surface lignin barrier, contributed to reducing lignin repolymerization, thereby increased cellulose accessibility for high production of fermentable sugars and bioethanol in softwood biomass. [ABSTRACT FROM AUTHOR]

• In-situ lignin modification improved enzymatic hydrolysis of acid-pretreated larch. • Lignin modification with 2-naphthol suppressed lignin repolymerization. • Lignin modification with PEGDE lowered the enzyme non-productive binding on lignins. • 2-Naphthol and PEGDE modification synergistically facilitated enzymatic hydrolysis. To overcome the recalcitrance of residual lignins in acid-pretreated larch (AL), a combined acid and alkali pretreatment with in-situ lignin modification was developed in this study. The results showed that introducing in-situ lignin modification with 2-naphthol to acid pretreatment (160 and 180 oC) improved the enzymatic digestibility of AL by 12.7-14.4%, through suppressing lignin repolymerization. The obviously higher improvement (57.8-88.3%) was achieved by applying alkali post-treatment (90 oC) with poly (ethylene glycol) diglycidyl ether (PEGDE) on AL, mainly due to the function of in-situ lignin modification with PEGDE for reducing enzyme non-productive binding on lignins. More importantly, the synergism of 2-naphthol and PEGDE modification facilitated the enzymatic hydrolysis of AL more significantly. Its beneficial mechanism was explored by investigating the effects of in-situ lignin modification on lignin properties, including extraction yields, functional groups, and enzyme affinity of lignins. Results will give insights into establishing an efficient pretreatment of softwood biomass. [ABSTRACT FROM AUTHOR]