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Tobacco stem is an abundant and inexpensive renewable source to produce prebiotics by circular economy. In this study, hydrothermal pretreatments were evaluated on the release of xylooligosaccharides (XOS) and cello-oligosaccharides (COS) from the tobacco stem by a central composite rotational design associated with response surface methodology to evaluate the effects of temperature (161.72 to 218.3 °C) and solid load (SL) (2.93 to 17.07%). XOS were the main compounds released to the liquor. Desirability function was performed to maximize the production of XOS and minimize the effects of release of monosaccharides and degradation compounds. The result indicated yield of 96% w[XOS]/w[xylan] for 190 °C-2.93% SL. The highest value for COS and total oligomers content (COS + XOS) was 6.42 g/L and 17.7 g/L, respectively, for 190 °C-17.07% SL. The mass balance for the best yield XOS condition predicted 132 kg of XOS (X2-X6) from 1000 kg of tobacco stem., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier Ltd. All rights reserved.)

Enzymatic hydrolysis is a method to generate biofuel from biomass, and autohydrolysis is a popular method to pretreat biomass prior to enzymatic hydrolysis. The primary aim of the present study was to determine the role of lignin produced in the autohydrolysis process on the enzymatic hydrolysis of biomass. The HSQC and 31 P NMR analyses confirmed that β-O-4 of lignin was reduced, while β-5, β-β, and S/G-ratio of lignin were increased with intensifying the hydrolysis intensity.The increase in the hydrolysis intensity significantly enhanced the condensed and non-condensed phenolic OH group of lignin. Interestingly, the cellulase enzyme adsorbed more on lignin that had more phenolic content, and its association with lignin reduced its activity for hydrolyzing cellulose microcrystals. Strong negative correlations were observed between the enzymatic hydrolysis yield and the condensed S-OH (r 2  = 0.978) and G-OH (r 2  = 0.961) of lignin generated in the autohydrolysis process., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

The development of lignocellulosic biorefineries requires a first stage of pretreatment which enables the efficient valorization of all fractions present in this renewable material. In this sense, this review aims to show the main advantages of hydrothermal treatment as a first step of a biorefinery infrastructure using hardwood as raw material, as well as, main drawback to overcome. Hydrothermal treatment of hardwood highlights for its high selectivity for hemicelluloses solubilization as xylooligosaccharides (XOS). Nevertheless, the suitable conditions for XOS production are inadequate to achieve an elevate cellulose to glucose conversion. Hence, several strategies namely the combination of hydrothermal treatment with delignification process, in situ modification of lignin and the mixture with another renewable resources (concretely, seaweeds, and by-products generated in the food industry with high sugar content) were pinpointed as promising alternative to increase the final ethanol concentration coupled with XOS recovery in the hydrolysate., (Copyright © 2021 The Author(s). Published by Elsevier Ltd.. All rights reserved.)

Avocado industrial processing generates huge quantities of residues that are currently wasted without any valuable commercial application. This work deals with autohydrolysis of Avocado peel (AP) for the concomitant recovery of oligosaccharides and polyphenolics. Temperature of 150 °C allowed the highest recovery of oligosaccharides (14.3 g oligosaccharides/100 g AP) and high recovery of antioxidant phenolics (3.48 g gallic acid equivalents/100 g AP and 10.80 g Trolox equivalents/100 g AP measured with ABTS ●+ assay). The liquor obtained at this temperature was characterized by TGA and FTIR to study its thermal stability and functional groups. UHPLC-TOF MS analysis of an ethyl acetate extract of AP liquor enabled the tentative identification of 43 compounds, belonging to various metabolite families, including flavonoids, phenolic acids, organic acids, lignans and fatty acids. These findings demonstrated that autohydrolysis of AP is a suitable technology to obtain bioactive agents with potential uses in food and cosmetic industries., (Copyright © 2021 The Author(s). Published by Elsevier Ltd.. All rights reserved.)

Hydrothermal processes are an attractive clean technology and cost-effective engineering platform for biorefineries based in the conversion of biomass to biofuels and high-value bioproducts under the basis of sustainability and circular bioeconomy. The deep and detailed knowledge of the structural changes by the severity of biomasses hydrothermal fractionation is scientifically and technological needed in order to improve processes effectiveness, reactors designs, and industrial application of the multi-scale target compounds obtained by steam explosion and liquid hot water systems. The concept of the severity factor [log 10 (R o )] established>30 years ago, continues to be a useful index that can provide a simple descriptor of the relationship between the operational conditions for biomass fractionation in second generation of biorefineries. This review develops a deep explanation of the hydrothermal severity factor based in lignocellulosic biomass fractionation with emphasis in research advances, pretreatment operations and the applications of severity factor kinetic model., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

Microwave hydrothermal treatment (MHT), a novel advanced technology, was proposed for the fractionation of Paulownia wood (PW) at temperatures ranging 200-230 °C and residence times of 0-50 min, corresponding to severities of 2.93-4.70. This procedure allowed 80% of xylan recovery as xylooligosaccharides and an average of 95% cellulose recovery in the pretreated PW biomass, showing the selectivity of the treatment, that was also compared to conduction-convection heating autohydrolysis. Finally, a kinetic model was proposed for the prediction of PW fractionation using MHT, with the ultimate goal of being applied to a wide range of feedstocks and minimizing the number of parameters used. For that, two strategies were approached, allowing the reduction of 80 to 34 parameters, without significant influence in the kinetic fitting. To the best of our knowledge, this is the first kinetic modelization of MHT of PW, taking into account all the lignocellulosic fractions., (Copyright © 2021 The Author(s). Published by Elsevier Ltd.. All rights reserved.)

This work focuses on the effect of subcritical water pretreatment conditions on agave bagasse chemical composition, biomass fractionation, and enzymatic hydrolysis obtained from the different tequila production processes. The pretreatment was carried out in a batch pressurized reactor within an isothermal regime. The operational conditions for subcritical water pretreatment were (150-190 °C) and (10-50 min). The best operational conditions were selected, based on the increased cellulose content (>50%) in the pretreated solid phase. The conditions for 190 °C for 50 and 30 min of pretreated agave bagasse solids were chosen for enzymatic hydrolysis susceptibility (15 FPU/g of the substrate). The maximum conversion yield (cellulose to glucose) during enzymatic hydrolysis achieved was up to 61.62% (5.86 g/L) in industrial bagasse at 72 h and initial saccharification rate was 0.34 g/(L*h) at 12 h. This study indicates that the agave bagasse is a promising raw material in the development of second-generation biorefineries., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

Managing plastic waste remains an urgent environmental concern and switching to biodegradable plastics can reduce the dependence on depleting fossil fuels. This study emphasises the efficacy of macroalgae wastes, Eucheuma denticulatum residues (EDRs), as potential alternate feedstock to produce l-lactic acid (l-LA), the monomer of polylactic acid, through fermentation. An innovative environmental friendly strategy was explored in this study to develop a glucose platform from EDRs: pretreatment with microwave-assisted autohydrolysis (MAA) applied to enhance enzymatic hydrolysis of EDRs. The results indicate that MAA pretreatment significantly increased the digestibility of EDRs during the enzymatic hydrolysis process. The optimum pretreatment conditions were 120 °C and 50 min, resulting in 96.5% of enzymatic digestibility after 48 h. The high l-LA yield of 98.6% was obtained using pretreated EDRs and supplemented with yeast extract. The energy analysis implies that MAA pretreatment could further improve the overall energy efficiency of the process., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

In the quest to reduce global food loss and waste, fruit processing wastes, particularly citrus peel waste (CPW), have emerged as a promising and sustainable option for biorefinery without competing with human foods and animal feeds. CPW is largely produced and, as recent studies suggest, has the industrial potential of biological valorization into fuels and chemicals. In this review, the promising aspects of CPW as an alternative biomass were highlighted, focusing on its low lignin content. In addition, specific technical difficulties in fermenting CPW are described, highlighting that citrus peel is high in pectin that consist of non-fermentable sugars, mainly galacturonic acid. Last, recent advances in the metabolic engineering of yeast and other microbial strains that ferment CPW-derived sugars to produce value-added products, such as ethanol and mucic acid, are summarized. For industrially viable CPW-based biorefinery, more studies are needed to improve fermentation efficiency and to diversify product profiles., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

In this work, valorization of Paulownia wood (PW) was proposed following several process configurations for biofuels and value-added compounds production. Firstly, autohydrolysis and ethanol-organosolv strategies were assessed separately for the fractionation of PW to enhance the enzymatic digestibility of cellulose. A third strategy focused on a sequential process (autohydrolysis and organosolv) was explored. Two temperatures were selected for the first stage of the combined process. High concentration of oligosaccharides (26.29 g/L) and high concentration of degradation products (17.21 g/L) were obtained at 210 and 230 °C, respectively. The solids obtained from both pretreatments were subjected to organosolv delignification (200 °C, 3 h and 50% ethanol) achieving delignification of 58 and 30% for the autohydrolyzed biomass at 210 °C and 230 °C, respectively. The combined process resulted in susceptible biomass able to produce 64 g/L of ethanol. Therefore, the strategies explored in this work open the possibility to build a refinery around Paulownia wood., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

Alkali-extracted xylan from lignocellulosics is a promising feedstock for production of prebiotic xylooligosaccharides (XOS). An integrated process was established combining autohydrolysis, nanofiltration and xylanase hydrolysis. Results show that after autohydrolysis 48.37% of xylan was degraded into oligomers and dissolved into the autohydrolysate, of which 57.83% were XOS. By-products and xylose were removed by nanofiltration with discontinuous diafiltration, while high recovery yields of XOS (84.15%) and xylan (87.45%) were obtained. High yields of XOS were obtained by adding xylanase to the autohydrolysates; after enzymatic hydrolysis an XOS yield of 96-98% was obtained. The enzymatic hydrolysates showed positive prebiotic effects on B. adolescentis with an increase in cell concentration by 4.8-fold after fermentation for 24 h. The main products were short-chain fatty acids with carbon balanced during the whole fermentation process. This integrated strategy resulted in a final XOS conversion of 41.22% contrasted to the initial xylan in raw alkali-extracted xylan., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

Different pretreatments strategies have been developed over the years mainly to enhance enzymatic cellulose degradation. In the new biorefinery era, a more holistic view on pretreatment is required to secure optimal use of the whole biomass. Hydrothermal pretreatment technology is regarded as very promising for lignocellulose biomass fractionation biorefinery and to be implemented at the industrial scale for biorefineries of second generation and circular bioeconomy, since it does not require no chemical inputs other than liquid water or steam and heat. This review focuses on the fundamentals of hydrothermal pretreatment, structure changes of biomass during this pretreatment, multiproduct strategies in terms of biorefinery, reactor technology and engineering aspects from batch to continuous operation. The treatise includes a case study of hydrothermal biomass pretreatment at pilot plant scale and integrated process design., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Spent coffee grounds are a huge residual stream from instant coffee makers. The production of spent coffee oil and molecular weight fractionated hemicellulose hydrolysates via supercritical CO 2 and a hydrothermal treatment followed by concentration, separation, and purification through cascade ultrafiltration/diafiltration (30-10-5 kDa) was studied. Hemicelluloses extraction yield reached 3.49 g/100 g of dry defatted spent coffee after 40 min at 160 °C. The ultrafiltration system allowed concentrating up to 5-fold certain groups of hemicellulose, being most of them retained in the first membrane. Hemicellulose concentration and molecular weight of the feed exerted a great influence on the mass transfer through the membrane due to the formation of aggregates. However, purification through diafiltration allowed both to decrease by-products retentions from 45.6% to 8.7%, increasing the molecular weight of each fraction. Six hemicellulose products were obtained with purities between 83.7 and 97.8 wt% and weight-average molecular weights between 1641 and 49,733 Da., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Spent olive pomace from the two-phase extraction system of virgin olive oil and olive pomace oil, is a major agro-industrial residue. Present study aimed at the valorization of residual olive pomace and stones (seeds) by hydrothermal treatment and enzymatic hydrolysis of glucans. Both residues contain lignin (31.2% and 42.1%), glucans (13.8% and 15.3%) and xylans (18.9% and 20.3%). After hydrothermal pretreatment (130 °C, 30 min; severity factor log R 0  = 2.99), 65% and 75% of hemicelluloses (65% of xylan) were hydrolysed into xylo-oligosaccharides in pomace and stones, respectively. Cellulose and lignin were not substantially affected. Three commercial enzyme preparations, Saczyme Yield, Ultimase BWL 40 and Celluclast 1.5 L, were evaluated for saccharification of pomace or stones at three biomass loads (10, 20 and 30%, w/v). Saczyme and Ultimase were active with high solid loads (30%), reaching 80 and 90% of glucan conversion in pomace, and 40 and 55% in stones, respectively, after 5 h., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

The effects of exogenous ash (EA) from harvest wheat straw and its internal components on wheat straw autohydrolysis efficiency and subsequent enzymatic hydrolysis were investigated. Results showed that when EA and its insoluble mineral components were included in the autohydrolysis, the enzymatic efficiencies of pretreated residues were significantly reduced from 84.9% to 66.3% and 58.4%, respectively. This was found to be largely attributable to the buffering of free H + in the pretreatment medium which took place due to the ash. Specifically, the insoluble mineral fraction of said ash exerted strongest buffering capacity in EA. Furthermore, this decrease was found to linearly correlate with decreases to substrate enzymatic accessibility and hydrophobicity. These results demonstrate that the penalties of ash upon autohydrolysis are borne of specific fractions comprising the ash, making the case for ash removal processes or supplementation of processes with additives that will counter the negative effects of ash., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Chemi-mechanical pulping, a typical high-yield pulping method, combined with autohydrolysis pretreatment prior to pulping is an efficient and value-added utilization method for biomass in pulp and paper industry. This study investigated the surface lignin changes of poplar sapwood chips in autohydrolysis pretreatment and their effect on the subsequent alkali impregnation for chemi-mechanical pulping. The results showed that the surface lignin content went up with the increase of autohydrolysis intensity, and that the existence of the surface lignin had nearly no impact on the subsequent alkali impregnation in making chemi-mechanical pulps (CMPs) compared to the volume porosity, which was validated by using the stepwise regression analysis. It can be further concluded that autohydrolysis can facilitate the subsequent alkali impregnation of the autohydrolyzed sapwood chips in making CMP, which would be of significance for the combination of biomass refinery and pulp and paper industry., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Following an integrated approach, Eucalyptus nitens wood samples were subjected to consecutive stages of aqueous fractionation and organosolv delignification, in order to separate hemicelluloses (mainly converted into soluble products from the aqueous stage) from lignin (largely converted into soluble fragments in the organosolv stage) and from cellulose (accumulated in the solid phase from pulping). The compositions of selected reaction media were studied by selected spectrophotometric, spectrometric, chromatographic, and nuclear magnetic resonance methods; and the solid phases from treatments were studied by diffractometry and scanning electron microscopy. The experimental information from the above tasks provides a deep insight on the yields, properties and potential applications of the target fractions in the scope of biorefineries., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

High ash content of waste wheat straw (WWS) is resistant to biorefinery autohydrolysis pretreatment due to its self-buffering effects. In this work, minor addition FeCl 3 and AlCl 3 were applied to overcome the self-buffering effects of WWS by cationic occupation of the negatively charged sites present on particulate ash's surface. The results showed that with the increasing concentrations (0-20 mM) of AlCl 3 and FeCl 3 , the enzymatic efficiencies of autohydrolyzed WWS were enhanced from 49.7% to 62.1% and 66.6%, respectively. Acid buffer and cation exchange capacity of pretreated WWS were decreased by adding metal chlorides and the reducing results were mainly attributed to cation exchange. Meanwhile, a maximum monosaccharide production (185.3 mg/g-WWS) was achieved with 62.0 mg/g-WWS xylooligosaccharide by using 20 mM FeCl 3 during WWS autohydrolysis. The results demonstrated that the implications of FeCl 3 and AlCl 3 in WWS autohydrolysis were an effective strategy to enhance autohydrolysis efficiency by overcoming self-buffering effects., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

The aim of this work was to study acetyl-assisted autohydrolysis of sugarcane bagasse for the production of xylo-oligosaccharides without additional chemicals. A xylo-oligosaccharide yield of 50.35% was obtained in 10 min through sugarcane bagasse autohydrolysis at 200 °C; this yield was 49.64% after acetyl-assisted autohydrolysis of a 65:35 mixture of sugarcane bagasse/white birch at 160 °C for 100 min. The yield of xylo-oligosaccharides was close to that obtained at 180 °C/40 min and 200 °C/10 min through the autohydrolysis of sugarcane bagasse. Compared to sugarcane bagasse alone, the xylo-oligosaccharide (degree of polymerization 2-5) yield from the acetyl-assisted autohydrolysis at 200 °C for 10 min was 52.99%. In addition, the yield of glucose from the solid residue following autohydrolysis pretreatment was 96.87% after 72 h of enzymatic hydrolysis. These results demonstrate that acetyl-assisted autohydrolysis is a promising method for the production of xylo-oligosaccharides., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

The production of tequila in Mexico generates a large amount of agave bagasse per year. However, this biomass can be considered as a potential source for biofuel production. In this study, it is described how the hydrothermal pretreatment was scaled in a bench scale, considering the severity index as a strategy. The best condition was at 180 °C in isothermal regime for 20 min with 65.87% of cellulose content and high concentration of xylooligosaccharides (15.31 g/L). This condition was scaled up (using severity factor: [logR 0 ] = 4.11), in order to obtain a rich pretreated solid in cellulose to perform the enzymatic hydrolysis, obtaining saccharification yields of 98.5 and 99.5% at high-solids loading (10 and 15%, respectively). The pre-saccharification and fermentation strategy was used in the bioethanol production at 10 and 15% of total pretreated solids, obtaining 38.39 and 55.02 g/L of ethanol concentration, corresponding to 90.84% and 87.56% of ethanol yield, respectively., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

This work investigated the changes in the physical structure of autohydrolyzed poplar sapwood chips and the effect on the subsequent alkali liquor diffusion properties for chemi-mechanical pulping (CMP). An alkali impregnation process was conducted by using the autohydrolyzed poplar sapwood with different levels of autohydrolysis intensity. The results showed that the volume porosity, water constraint capacity, and saturated water absorption of the autohydrolyzed poplar sapwood chips increased. Also, the effective capillary cross-sectional area (ECCSA) in the radial direction and the diffusion coefficients of NaOH solution in both the radial and axial directions all increased. Autohydrolysis pretreatment enhanced the alkali liquor diffusion properties in poplar sapwood chips, and the diffusion coefficient was increased more greatly in the radial direction than that in the axial direction., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

This work presents an integrated and multi-step approach for the recovery and/or application of the lignocellulosic fractions from corncob in the production of high value added compounds as xylo-oligosaccharides, enzymes, fermentable sugars, and lignin in terms of biorefinery concept. For that, liquid hot water followed by enzymatic hydrolysis were used. Liquid hot water was performed using different residence times (10-50min) and holding temperature (180-200°C), corresponding to severities (log(R 0 )) of 3.36-4.64. The most severe conditions showed higher xylo-oligosaccharides extraction (maximum of 93%) into the hydrolysates and higher recovery of cellulose on pretreated solids (maximum of 65%). Subsequently, hydrolysates and solids were used in the production of xylanases and cellulases, respectively, as well as, pretreated solids were also subjected to enzymatic hydrolysis for the recovery of lignin and fermentable sugars from cellulose. Maximum glucose yield (100%) was achieved for solids pretreated at log(R 0 ) of 4.42 and 5% solid loading., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

The aim of this work was to compare the two most common hydrothermal pre-treatments for wood - mild steam explosion and hot water extraction - both with the prospect of enabling extraction of hemicelluloses and facilitating further processing. Although both involve autohydrolysis of the lignocellulosic tissue, they are performed under different conditions: the most prominent difference is the rapid, disintegrating, discharge employed in the steam explosion opening up the structure. In this comparative study, the emphasis was placed on local composition of the pre-treated wood chips (of industrially relevant size). The results show that short hot water extraction treatments lead to significant variations in the local composition within the wood chips, while steam explosion accomplishes a comparably more even removal of hemicelluloses due to the advective mass transport during the explosion step., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

A biologically-based lignocellulosic biorefinery process for obtaining carbohydrates from raw biomass was investigated across six diverse biomasses (three hardwoods & three nonwoods) for the purpose of decoding lignin's influence on sugar production. Acknowledging that lignin could positively alter the economics of an entire process if valorized appropriately, we sought to correlate the chemical properties of lignin within the process to the traditional metrics associated with carbohydrate production-cellulolytic digestibility and total sugar recovery. Based on raw carbohydrate, enzymatic recovery ranged from 40 to 64% w/w and total recovery ranged from 70 to 87% w/w. Using nitrobenzene oxidation to quantify non-condensed lignin structures, it was found that raw hardwoods bearing increasing non-condensed S/V ratios (2.5-5.1) render increasing total carbohydrate recovery from hardwood biomasses. This finding indicates that the chemical structure of hardwood lignin influences the investigated biorefinery process' ability to generate carbohydrates from a given raw hardwood feedstock., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

The aim of this work was to evaluate the efficiency of an ionic liquid (IL) 1-butyl-3-methylimidazolium acetate ([C 4 mim][OAc]) pretreatment (110°C for 30min) in comparison to high severity autohydrolysis pretreatment in terms of delignification, cellulose crystallinity and enzymatic digestibility. The increase in severity of autohydrolysis pretreatment had positive effect on glucan digestibility, but was limited by the crystallinity of cellulose. [C 4 mim][OAc] pretreated sugarcane bagasse exhibited a substantial decrease in lignin content, reduced cellulose crystallinity, and enhanced glucan and xylan digestibility. Glucan and xylan digestibility was determined as 97.4% and 98.6% from [C 4 mim][OAc] pretreated bagasse, and 62.1% and 57.5% from the bagasse autohydrolyzed at 205°C for 6min, respectively. The results indicated the improved digestibility and hydrolysis rates after [C 4 mim][OAc] pretreatment when compared against a comparable autohydrolyzed biomass., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

This work is aimed at investigating the influence of changes in the content of hemicelluloses of the autohydrolyzed poplar sapwood on the subsequent alkali impregnation for chemi-mechanical pulping (CMP). An alkali impregnation process was conducted using the autohydrolyzed poplar sapwood with different content of hemicelluloses as raw materials. The results showed that both the amount of NaOH consumption and swelling degree of poplar sapwood increased with the removal of hemicelluloses, thus enhancing the alkali impregnation effectiveness. The hemicelluloses removal can also shorten the alkali impregnation time for the autohydrolyzed poplar sapwood to achieve the similar impregnation effectiveness of unautohydrolyzed poplar sapwood. All of these can be attributed to the fact that the hemicelluloses removal would result in the exposure of more free hydroxyl groups on the cellulose and an increase in the porosity of the fiber cell walls., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

The aim of this work was the evaluation of lime pretreatment combined or not with previous step of autohydrolysis for oat straw valorization. Under selected conditions of lime pretreatment, 96% of glucan and 77% of xylan were recovered and 42% of delignification was achieved. Xylose fermentation to ethanol by metabolic engineered Saccharomyces cerevisiae (MEC1133) strain improved the ethanol production by 22% achieving 41g/L. Alternatively, first step of autohydrolysis (S0=4.22) allowed a high oligosaccharides recovery (68%) and subsequent lime pretreatment attained a 57% of delignification and 99% of glucan to glucose conversion. Oat straw processed by autohydrolysis and lime pretreatment reached the maximal ethanol concentration (50g/L). Both strategies led to oat straw valorization into bioethanol, oligosaccharides and lignin indicating that these pretreatments are adequate as a first stage within an oat straw biorefinery., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Autohydrolysis with different severity factors was performed on poplar wood chips prior to pulping, and the wettability, absorbility and the following impregnation of NaOH solution for the poplar wood chips were then investigated. The results showed that after autohydrolysis pretreatment the porosity, shrinkage and fiber saturation point (FSP) of the poplar wood chips were increased, while the surface contact angle decreased as the severity factor was increased. The autohydrolyzed chips absorbed more NaOH in impregnation that resulted in a low NaOH concentration in the bulk impregnation liquor (i.e., the impregnation liquor outside wood chips), while the concentration in the entrapped liquor (i.e., the impregnation liquor inside wood chips) was increased. Autohydrolysis substantially improved the effectiveness of alkali impregnation., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Agricultural feedstocks (brewers' spent grain - BSG, corncob - CC, corn husk - CH, wheat straw - WS and Luffa sponge - LS) were pretreated by liquid hot water (LHW) in order to increase cellulose recovery and enzymatic saccharification. LHW-pretreatment resulted in hemicellulose solubilization, and solids enriched in cellulose. Chemical analysis showed different susceptibilities of the feedstocks to LHW-pretreatment and enzymatic hydrolysis. Pretreated feedstocks presented higher crystallinity (determined through X-ray diffraction) and thermal stability (determined through thermogravimetric analysis) than untreated feedstocks. SEM images confirmed the effect of LHW-pretreatment on structural changes. Moreover, enzymatic hydrolysis and cellulose conversion to glucose (CCG) were improved for pretreated feedstocks, with exception of LS. CCG (in relation to glucose potential on solids) followed the order: BSG>CH>WS>CC>LS. LHW-pretreatment showed to be a good technology to pretreat multi feedstocks and for improving the enzymatic hydrolysis of recalcitrant agricultural feedstocks to sugars, which can be further converted to ethanol-fuel and other value-added chemicals., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Samples of Eucalyptus urograndis and Eucalyptus grandis sawdust were autohydrolyzed in aqueous conditions to reach temperatures in the range 110-190°C and reaction times of 0-150min in a minireactor. In each minireactor were used a liquor:wood ratio (10:1 L:kg dry wood), in order to assess the effects of the autohydrolysis severity and the crystalline properties of cellulose. The content of extractives, lignin, holocellulose, cellulose, hemicelluloses and crystallinity index obtained from the solid fraction after autohydrolysis of sawdust were determined. This study demonstrated that the hemicelluloses were extensively removed at 170 and 190°C, whereas cellulose was partly degraded to Eucalyptus urograndis and Eucalyptus grandis sawdust. The lignin content decreased, while the extractives content increased. It was defined that during autohydrolysis, had a slight decreased on crystalline structure of cellulose of Eucalyptus urogandis and Eucalyptus grandis., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

A comparative analysis of the response of agave bagasse (AGB) to pretreatment by ammonia fiber expansion (AFEX™), autohydrolysis (AH) and ionic liquid (IL) was performed using 2D nuclear magnetic resonance (NMR) spectroscopy, wet chemistry, enzymatic saccharification and mass balances. It has been found that AFEX pretreatment preserved all carbohydrates in the biomass, whereas AH removed 62.4% of xylan and IL extracted 25% of lignin into wash streams. Syringyl and guaiacyl lignin ratio of untreated AGB was 4.3, whereas for the pretreated biomass the ratios were 4.2, 5.0 and 4.7 for AFEX, AH and IL, respectively. Using NMR spectra, the intensity of β-aryl ether units in aliphatic, anomeric, and aromatic regions decreased in all three pretreated samples when compared to untreated biomass. Yields of glucose plus xylose in the major hydrolysate stream were 42.5, 39.7 and 26.9kg per 100kg of untreated AGB for AFEX, IL and AH, respectively., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Vine shoots were subjected to non-isothermal aqueous processing. A range of severities (S0) from 3.20 to 4.65 was assayed and their effects in terms of solubilization, composition, molar mass distribution, structural characterization and thermal stability of the liquors were studied using HPLC, HPSEC, TGA and FTIR. The spent solids were characterized by HPLC and FTIR. When autohydrolysis was carried out at S0=4.01, the substrate solubilization achieved a 38.7% of the raw material and 83.1% of the initial xylan was converted into xylooligosaccharides (XOS). The amount of TOS (total oligosaccharides) in the hydrolysates was 28.4g/L while the other non volatile compounds (ONVC) were 0.08g/g NVC. The spent solid from the treatment at S0=4.01 was composed about 90% of cellulose and lignin. Therefore, it can be concluded that autohydrolysis is a suitable pretreatment of vine shoots such as a first stage of a biomass refinery., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Autohydrolysis pretreatment with different severity factors was performed on poplar chips prior to chemi-thermomechanical pulping (CTMP) in order to investigate the change in pH value and its effect on the autohydrolysis pretreatment. The results showed that the dissolution amount of acetic acid increased with raising the severity factor of the pretreatment and declining the size of poplar chips, respectively. Besides, a logarithmic relationship between the amount of acetic acid released in the autohydrolysis liquor (AHL) and pH value of the AHL was observed. The amounts of glucose and xylose (including those in the form of monomers, oligomers, and polysaccharides) as well as furfural and hydroxymethylfurfural (HMF) also depended on the pH value of the AHL to some extent., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

In the present work, the hydrothermal valorization of an abundant agricultural residue has been studied in order to look for high added value applications by means of hydrothermal pretreatment followed by fed-batch simultaneous saccharification and fermentation, to obtain oligomers and sugars from autohydrolysis liquors and bioethanol from the solid phase. Non-isothermal autohydrolysis was applied to barley straw, leading to a solid phase with about a 90% of glucan and lignin and a liquid phase with up to 168 g kg(-1) raw material valuable hemicellulose-derived compounds. The solid phase showed a high enzymatic susceptibility (up to 95%). It was employed in the optimization study of the fed-batch simultaneous saccharification and fermentation, carried out at high solids loading, led up to 52 g ethanol/L (6.5% v/v)., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

Eucommia ulmoides Oliver (EU) wood was successively treated by autohydrolysis and organosolv pretreatment integrated process. Autohydrolysis pretreatment facilitated xylooligosaccharides production, subsequent organosolv pretreatment to obtain high-purity lignin and digestible cellulose-rich residue. Results showed that the lignin fractions obtained exhibited smaller molecular weights, narrow polydispersity, more phenolic OH groups and higher syringyl/guaiacyl ratios (S/G) than the milled wood lignin. NMR characterization of the lignin revealed that the β-O-4 linkages significantly cleaved and the structure of stilbene formed, but its resinol (β-β) was resistant to be degraded by organosolv delignification. Moreover, the glucose yield of the integrated residue achieved a maximum value of 89.3% after enzyme hydrolysis, separately about 1.0, 1.3, 3.8 times as compared to that of the ethanol organosolv residue, the hydrothermally treated residue and the EU wood, respectively, which indicated that the integrated process was a promising approach to value-added utilization of the EU wood., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

This work proposes the biorefining of eucalyptus residues (ER), wheat straw (WS) and olive tree pruning (OP) combining hydrothermal pretreatment (autohydrolysis) with acid post-hydrolysis of the liquid fraction and enzymatic hydrolysis of the solid fraction towards maximal recovery of monosaccharides from those lignocellulose materials. Autohydrolysis of ER, WS and OP was performed under non-isothermal conditions (195-230°C) and the non-cellulosic saccharides were recovered in the liquid fraction while cellulose and lignin remained in the solid fraction. The acid post-hydrolysis of the soluble oligosaccharides was studied by optimizing sulfuric acid concentration (1-4%w/w) and reaction time (10-60 min), employing a factorial (2(2)) experimental design. The solids resulting from pretreatment were submitted to enzymatic hydrolysis by applying commercial cellulolytic enzymes Celluclast® 1.5L and Novozyme® 188 (0.225 and 0.025 g/g solid, respectively). This strategy provides high total monosaccharide recovery or high glucose recovery from lignocellulosic materials, depending on the autohydrolysis conditions applied., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

The autohydrolysis process has been considered a simple, low-cost and environmental friendly technology for generation of sugars from biomass. In order to improve accessibility of enzymes during enzymatic hydrolysis as well as to allow the recovery of hemicellulose in the filtrate, the sugarcane bagasse was pretreated using autohydrolysis followed by a mechanical refining process. The autohydrolysis was carried out in three different conditions. Autohydrolysis at 190°C for 10min provided the highest overall sugar (19.2/100g raw bagasse) in prehydrolyzate. The enzymatic hydrolysis step was performed for all the post-treated solids with and without refining at enzyme loadings of 5 and 10FPU/g for 96h. A total of 84.4% of sugar can be recovered from sugarcane bagasse at 180°C for 20min with 5 FPU/g enzyme charge. The economic analysis for the proposed method showed that the bioethanol production can have a financial return larger than 12%., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

Wheat straw was subjected to three different processes prior to saccharification, namely alkaline pulping, natural pulping and autohydrolysis, in order to study their effect on the rate of enzymatic hydrolysis. Parameters like medium concentration, temperature and time have been varied in order to optimize each method. Milling the raw material to a length of 4mm beforehand showed the best cost-value-ratio compared to other grinding methods studied. Before saccharification the pulp can be stored in dried form, leading to a high yield of glucose. Furthermore the relation of pulp properties (i.e. intrinsic viscosity, Klason-lignin and hemicelluloses content, crystallinity, morphology) to cellulose hydrolysis is discussed., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

This study investigated the autohydrolysis pre-treatment prior to chemi-thermomechanical pulping (CTMP) process including the effects of autohydrolysis pretreatment with a lower severity on characteristics of the autohydrolysis liquor and hydrolyzed chips. The intensity of autohydrolysis, characterized by the severity factor, increased from 1.76 to 3.54, the hydrolyzed chips yield decreased from 99.0% to 86.7% and the xylose extraction yield increased from 0.8% to 44.0%. The content of holocellulose, pentosan and acid soluble lignin remained in the hydrolyzed chips decreased dramatically with increasing the treatment severity. After the autohydrolysis pretreatment, the resultant poplar chemi-thermomechanical pulp with a severity factor of 2.37 could obtain a 15.3 Nm/g tensile index, 58.6% ISO brightness and a 2.39 cm(3)/g bulk., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

Steam explosion and steam pre-treatment have proved capable of enhancing enzymatic saccharification of lignocellulosic materials. However, until now, these methods had not been compared under the same operational conditions and using the same raw material. Both pre-treatments lead to increased yields in the saccharification of Eucalyptus globulus; but results have been better with steam pre-treatments, despite the more accessible surface of exploded samples. The reason for this finding could be enzymatic inhibition: steam explosion causes a more extensive extraction of hemicelluloses and releases a greater amount of degradation products which can inhibit enzymatic action. Enzymatic inhibition is also dependent on the amount and chemical structure of lignin, which was also a contributing factor to the lower enzymatic yields obtained with the most severe pre-treatment. Thus, the highest yields (46.7% glucose and 73.4% xylose yields) were obtained after two cycle of steam treatment, of 5 and 3 min, at 183°C., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

The optima conditions of production and purification of xylooligosaccharides (XOS) from Miscanthus x giganteus (MxG) were investigated. Using autohydrolysis, XOS were produced at 160, 180 and 200°C at 60, 20 and 5min, respectively. XOS yield up to 13.5% (w/w) of initial biomass and 69.2% (w/w) of xylan were achieved. Results from HPAEC-PAD analysis revealed that X1-X9 sugar oligomers were produced. Higher temperature and longer reaction time resulted in lower product molecular weight. The three optimum conditions had similar degrees of polymerization XOS. Using 10% activated carbon (w/v) with ethanol/water elution recovered 47.9% (w/w) of XOS from pretreated liquid phase. The XOS could be fractionated by degree of polymerization according to ethanol concentration in the ethanol/water elution. Most of the XOS were washed out in 30% and 50% ethanol/water (v/v) fractions. Recoveries of 91.8% xylobiose, 86.9% xylotriose, 66.3% xylotetrose, 56.2% xylopentose and 48.9% xylohexaose were observed in XOS., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

Growing interest in alternative and renewable energy sources has brought increasing attention to the integration of a pulp mill into a forest biorefinery, where other products could be produced in addition to pulp. To achieve this goal, hemicelluloses were extracted, either by steam explosion or by steam treatment, from Eucalyptus globulus wood prior to pulping. The effects of both pre-treatments in the subsequent kraft pulping and paper strength were evaluated. Results showed a similar degree of hemicelluloses extraction with both options (32-67% of pentosans), which increased with the severity of the conditions applied. Although both pre-treatments increased delignification during pulping, steam explosion was significantly better: 12.9 kappa number vs 22.6 for similar steam unexploded pulps and 40.7 for control pulp. Finally, similar reductions in paper strength were found regardless of the type of treatment and conditions assayed, which is attributed to the increase of curled and kinked fibers., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

Oil palm empty fruit bunches (OPEFB) fibre, a by-product generated from non-woody, tropical perennial oil palm crop was evaluated for xylooligosaccharides (XOS) production. Samples of OPEFB fibre were subjected to non-isothermal autohydrolysis treatment using a temperature range from 150 to 220 °C. The highest XOS concentration, 17.6g/L which relayed from solubilisation of 63 g/100 g xylan was achieved at 210 °C and there was a minimum amount of xylose and furfural being produced. The chromatographic purification which was undertaken to purify the oligosaccharide-rich liquor resulted in a product with 74-78% purity, of which 83-85% was XOS with degree of polymerisation (DP) between 5 and 40., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

Wheat straw was pretreated using an autohydrolysis process with different temperatures (160-200 °C) and times (10-20 min) in order to allow the recovery of hemicellulose in the filtrate and help open up the structure of the biomass for improved accessibility of enzymes during enzymatic hydrolysis. Autohydrolysis at 190 °C for 10 min provided the highest overall sugar (12.2/100g raw wheat straw) in the autohydrolysis filtrate and recovered 62.3% of solid residue. Before enzymatic hydrolysis, the pulps obtained from each pretreatment condition were subjected to a refining post-treatment to improve enzyme accessibility. Enzymatic hydrolysis was performed for all the pretreated solids with and without refining post-treatment at the enzyme loadings of 4 and 10 FPU/g oven dry substrate for 96 h. A total of 30.4 g sugars can be recovered from 100g wheat straw at 180 °C for 20 min with 4 FPU/g enzyme charge., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

Bamboo (Phyllostachys pubescens) was successfully fractionated using a three-step integrated process: (1) autohydrolysis pretreatment facilitating xylooligosaccharide (XOS) production (2) organosolv delignification with organic acids to obtain high-purity lignin, and (3) extended delignification with alkaline hydrogen peroxide (AHP) to produce purified pulp. The integrated process was comprehensively evaluated by component analysis, SEM, XRD, and CP-MAS NMR techniques. Emphatically, the fundamental chemistry of the lignin fragments obtained from the integrated process was thoroughly investigated by gel permeation chromatography and solution-state NMR techniques (quantitative (13)C, 2D-HSQC, and (31)P-NMR spectroscopies). It is believed that the integrated process facilitate the production of XOS, high-purity lignin, and purified pulp. Moreover, the enhanced understanding of structural features and chemical reactivity of lignin polymers will maximize their utilizations in a future biorefinery industry., (Copyright © 2013 Elsevier Ltd. All rights reserved.)