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It was proposed that pre-hydrolysing tule (Typha domingensis Pers) would make it possible to produce handsheets with strength-related properties similar to those of conventional commercial paper, in addition to valorizable hemicelluloses. The hypothesis was tested with a biorefining scheme involving autohydrolysis. Conditions were optimized to maximize the extraction of hemicelluloses while preserving glucan integrity. The autohydrolysis at a liquid to solid ratio of 13 at 141 °C for 45 min (optimized conditions) provided a commercially useful liquor containing primarily tule hemicelluloses. The autohydrolysis of tule before alkaline extraction made it possible to obtain a valuable liquid phase comprising between 23.3% and 71.6% of all hemicelluloses in the raw material. The gross heating value for the hydrolyzed tule was increased (1.6% to 7.9 %) with respect the raw material. The solid phase was subjected to soda-anthraquinone pulping. The yield, ethanol extractives, kappa number, viscosity, glucan, xylan, Klason lignin, soluble lignins, as well as the tensile index were evaluated. Tule was found to be amenable to industrial processing for the production of quality cellulose derivatives. Autohydrolysis provided valorizable liquor in addition to solid that yielded soda-anthraquinone pulp having properties similar to those obtained in its absence, but using milder operating conditions. [ABSTRACT FROM AUTHOR]

An innovative approach for preparing hemp fibers from hemp hurds for use in tissue and towel grades of paper is described. Hemp hurds are a low value by-product of industrial hemp processing that are generally used for animal bed litter. Tissue paper was fabricated from hemp hurd fibers by following three pulping processes: autohydrolysis (hydrothermal), sodium carbonate-based defibration, and high yield kraft pulping, and benchmarked against hardwood pulp. To meet industrial standards, hardwood and hemp pulp fibers were mixed at a dry mass ratio of 75:25, from which tissue paper sheets were prepared. Desirable tissue paper properties, such as water absorption, burst resistance, softness, and tensile strength (dry and wet), were measured and compared. Characterization of morphological and chemical properties of tissue handsheets was conducted with SEM and time-of-flight-secondary ion mass spectrometry (ToF-SIMS). The combined kraft pulped hardwood and autohydrolyzed hemp pulp fibers displayed improvements in tensile index, burst resistance, and softness of tissue handsheets compared to only kraft hardwood pulp handsheets without adversely impacting water absorption. Hardwood fibers showed a sparse distribution of surface lignin compared to hemp fibers using the same defibration. This technology can lead to a variety of eco-friendly tissue paper products that are not only highly energy efficient, but avoid harsh chemical processing. [ABSTRACT FROM AUTHOR]

Autohydrolysis and kraft pulping were sequentially applied to Eucalyptus urograndis wood to obtain added-value products from hydrolysis liquor. A biorefinery approach was used to bleach the resulting solid phase containing the cellulose pulp with an optimized O-D-(EP)-D bleaching sequence, where O denotes delignification with the sequence D bleaching with chlorine dioxide and EP alkaline extraction with soda and hydrogen peroxide. The pulp was then beaten to obtain paper sheets. The two-stage process yielded pulp with a small Kappa number relative to conventional delignification (4.9 to 13.7 vs 17.1). Using autohydrolysis temperatures of 160 °C to 170 °C during 0 min to 15 min made the process selective towards the extraction of hemicelluloses (xylan up to 43.9%). Additionally, the Kappa number and brightness obtained after bleaching with an O-DEP-D sequence were suitable for preparing dissolving grade pulp. The brightness of the pulp obtained was identical with that of the reference pulp (91.0%) and the Kappa number was smaller (0.2 to 0.6). Beating the pulp for 4500 PFI revolutions produced paper sheets with slightly better tensile strength and tear index than those for sheets from the reference pulp (viz., 90.3 N·m·g-1 and 9.9 mN·m²·g-1, respectively, versus 89.8 N·m·g-1 and 9.7 mN·m²·g-1, respectively). [ABSTRACT FROM AUTHOR]

Hydrolysate pretreatment (HP) uses hot water pre-hydrolysis liquor (HWPL) as partial or full pretreatment medium for biomass. Pentosan dissolution during Eucalyptus HP was studied under holding times between 0 min and 160 min, holding temperatures between 150 °C and 190 °C, a hot water pre-hydrolysate ratio (HWPR) from 20% to 100%, and a fixed liquid to wood ratio of 1:6. Both the pentosan removals in the hydrolysate pretreated solid (HPS) and the hydrolysate pretreatment liquor (HPL) pento-saccharides contents were determined and compared with those of hot water pre-hydrolysis (HWP). When compared to HWP, the HP enhanced pentosan removal from the solid phase, and enriched the saccharides or promoted the in-situ conversion of saccharides into other chemicals in the liquid phase. Pentosan removal in the HPS increased when holding time and temperature were increased. Increasing holding time first increased the pento-saccharide content in the HPL, and then decreased it after reaching the maximum. Elevating the holding temperature increased the pento-saccharide content in the HPL, except for arabino-oligosaccharide. Different HWPR had varying influences on pentosan removal in the HPS and on the saccharides concentration in the HPL. When controlled, HP positively influenced hemicellulose removal from biomass, and increased utilization value of the liquid phase obtained post pretreatment. [ABSTRACT FROM AUTHOR]

There is increasing demand for the production of biofuels from lignocellulosic biomass. Lignocellulosic biomass consists mainly of three polymeric components: cellulose, hemicelluloses, and lignin. The separation of these components requires an effective pretreatment process to ensure high quality glucose production, and is highly influenced by several factors, including moisture content, cellulose crystallinity, lignin content, and available surface area. Over time, numerous pretreatment methods have been utilized to change the lignocellulosic fiber structure and to enhance the enzymatic saccharification of cellulose to polysaccharides. This article reviews thermalbased pretreatment of lignocellulosic fiber used for glucose production. Based on the reviewed studies, autohydrolysis of lignocellusic biomass, followed by the "Instant pressure drop (DIC)," method can be regarded as an effective pretreatment process of lignocellusic biomass. [ABSTRACT FROM AUTHOR]

Untreated and hot-water-extracted (HWE) Norway spruce (Picea abies) sawdust was cooked using the sulfur-free oxygen-alkali (OA) method under the following conditions: temperature, 170 °C; liquor-to-wood ratio, 5:1 L/kg; and NaOH charge, 19% on the oven-dry sawdust. In comparison with earlier studies conducted with birch sawdust, the spruce cooking yield data, together with the amount of the pulp rejects (78% to 86% for reference pulps from the initial feedstock and 73% to 83% for pulps from the HWE feedstock), revealed that the pretreatment stage prior to spruce OA pulping caused different effects on pulping performance. The analyses of the three main compound groups (i.e., lignin, volatile acids, and hydroxy acids) in black liquor indicated that slightly higher contents (25.5 to 45.9 g/L) of dissolved lignin were detected in black liquors originating from the HWE sawdust than in the black liquors from the reference material (27.2 to 39.6 g/L). In contrast, considerably lower (~20% decrease) volatile acid contents and similar or slightly decreased hydroxy acids contents were detected in the black liquors from the HWE sawdust. [ABSTRACT FROM AUTHOR]

Aspen wood was subjected to autohydrolysis as a pre-treatment to characterize the structural changes occurring in lignin fractions during the pre-treatment process. Milled wood lignin (MWL) was isolated from both the native aspen wood and hydrolyzed wood chips, and its structural features were characterized by Fourier transform infrared (FT-IR), quantitative 13C, two-dimensional heteronuclear single quantum coherence (2D HSQC), and 31P nuclear magnetic resonance (NMR) spectroscopies, gel permeation chromatography/multi-angle laser light scattering (GPC-MALLS), and thermal analysis. The lignin remaining in the hydrolyzed wood chips revealed more phenolic OH groups, fewer aliphatic OH groups, higher syringyl/guaiacyl ratios (S/G), higher molecular weights, and narrower polydispersities than the native lignin of aspen wood. The inter-unit linkages of β-O-4 were noticeable cleaved, but the condensed structures in the lignin formed when undergoing autohydrolysis of high severity, resulting in elevated amounts of C-C linkages. Moreover, it was found that autohydrolysis promoted the removal of -OCH3 groups and increased the thermal stability of lignin fractions. [ABSTRACT FROM AUTHOR]

The chemical industry is being forced to evaluate new strategies for more effective utilization of renewable feedstocks to diminish the use of fossil resources. In this literature review, the integration of both acidic and alkaline pretreatment phases of hardwood and softwood chips with chemical pulping is discussed. Depending on the pretreatment conditions, high-volume sulfur-free fractions with varying chemical compositions can be produced. In case of acidic pretreatments, the major products include carbohydrates (mono-, oligo-, and polysaccharides), whereas under alkaline (i.e., aqueous NaOH) pretreatment conditions, the sulfur-free fractions of aliphatic carboxylic acids, lignin, and extractives are primarily obtained. All these fractions are potentially interesting groups of compounds and can be used in a number of applications. Finally, the effects of pretreatments on pulping are also considered. Although it is believed that there are important advantages to be gained by integrating this type of renewable raw material-based production, in particular, with kraft pulping, sulfur-free pulping methods such as soda-AQ and oxygen/alkali delignification processes are also briefly discussed. [ABSTRACT FROM AUTHOR]

Recovered papers are suitable biomass sources for conversion into sugars that can be used in bioethanol production. However, paper materials with a high lignin content have been found to be recalcitrant to enzymatic hydrolysis. To address this issue, several biomass pretreatment methods were employed to evaluate their efficiency on the conversion of newspaper with high lignin content to sugar. Autohydrolysis, a hot water treatment, was identified to adversely affect sugar conversion, presumably as a result of pore collapse under high-temperature pretreatment. Flexo ink, used in newspaper printing, had no effect on the enzymatic hydrolysis, with or without autohydrolysis. The ink was still detachable after autohydrolysis, as measured by hyperwashing. Compared to untreated newspaper, separate treatments of either mechanical refining or a non-ionic surfactant (sorbitan polyoxyethylene monooleate) improved the sugar conversion by 10% at enzyme dosages of 2 and 8 FPU/g substrate. The combination of both refining and surfactant resulted in the highest sugar conversions, i.e., 46.3%, 56.7%, and 64.1% at 2, 4, and 8 FPU/g enzyme dosages, respectively. Oxidative pretreatment (oxygen, 100 °C) marginally increased the sugar conversion, whereas alkaline and green liquor (NaCO3 and Na2S) pretreatments (at 160 °C) had either no effect or decreased the sugar conversion. Based on the results of the pretreatments, higher pretreatment temperatures of newsprint negatively impacted subsequent enzyme hydrolysis. [ABSTRACT FROM AUTHOR]

An integrated strategy was followed to valorise rice straw, one of the most relevant biomass feedstocks available worldwide, to selectively recover solubilised hemicelluloses and lignin. The pathway encompassed the use of autohydrolysis to hydrolyse the hemicelluloses and an ethanol-based organosolv process to solubilise lignin. Several autohydrolysis conditions were assayed with the best results obtained at 210 °C (log R0 4.15), which enabled high removal of hemicelluloses, yielding an oligosaccharide-rich hydrolysate and a treated biomass with low content of hemicelluloses and enriched in cellulose and lignin. The effects of ethanol concentration (5 to 75%), and reaction time (0 to 24 h) on lignin removal under mild temperature (30 °C) were studied. In optimal conditions (60.5% ethanol, 24h) the delignification yield reached 42%, whereas glucan solubilisation was below 17%. Lignin solubilisation yield was not influenced by the organosolv treatment duration while ethanol concentration favored the delignification up to 60.5% ethanol. The organosolv liquors contained economic interesting ligninderived compounds such as vanillin, ferulic, and coumaric acids. The chemical composition and enzymatic digestibility of the treated biomass from autohydrolysis and organosolv delignification were compared, with the latter presenting an almost 10% higher enzymatic digestibility than the former. [ABSTRACT FROM AUTHOR]

This study investigates the operating conditions used in the sodaanthraquinone pulping of Eucalyptus globulus wood after autohydrolysis pretreatment on the yield, kappa number, and brightness of the resulting unbleached pulp. Moreover, strength-related properties of the resulting handsheets was examined to identify the best pulping conditions and compare the outcome with that of a conventional soda-anthraquinone pulping process. The paper strength properties of the pulp were similar to or better than papers made from soda-AQ delignified pulps conducted in a single step. Also, a liquid fraction with a substantial content in hemicellulosic extracts was recovered in the simplified process. Autohydrolysis of the raw material facilitates carrying out soda-AQ pulping under milder conditions. In addition, autohydrolysis improves other properties relative to paper from raw cellulose pulp. Yield, kappa number, and brightness for pulp from solid residues of autohydrolysed eucalyptus wood were similar to those for pulp from untreated eucalyptus wood. [ABSTRACT FROM AUTHOR]

Autohydrolysis pre-treatments were performed for the production of hemicellulose-rich autohydrolysates from silver birch (Betula pendula) chips prior to chemical pulping. Pre-treatment conditions were varied with respect to time (from 30 to 120 min) and temperature (130 and 150 °C), covering a P-factor range from 10 to 238. Hydrolysates were analyzed in terms of carbohydrates, lignin, volatile organic acids, and furanoic compounds. The analytical data were subjected to various chemometric techniques to establish the relationships between dissolved organic components, hardwood and softwood used in the experiments, and applied pre-treatment conditions. Using this method, differences between the wood species could be clearly seen, and a relatively accurate model for the autohydrolysis of birch chips was developed. [ABSTRACT FROM AUTHOR]

Autohydrolysis of Eucalyptus globulus both with and without the addition of 5 g/L formic acid was explored for different liquid-to-solid (L/S) ratios at 150 ° C for 100 min. The L/S ratio has an impact on the dissolution of wood components during prehydrolysis. The extraction yield of wood components other than lignin decreased with increasing L/S ratio, while lignin removal increased with increasing L/S ratio, irrespective of acid reinforcement. The molecular weight (Mw) of dissolved hemicelluloses and lignin remained relatively constant. The average degree of polymerization of hemicelluloses isolated from the hot water extract was between 7 and 8 over a L/S ratio range from 3:1 to 50:1. The cellulose to glucose conversion yield of pretreated wood samples improved during prehydrolysis with 5 g/L formic acid. Although the conversion yield of autohydrolyzed wood meal stayed relatively constant, the conversion yield of dilute acid-pretreated wood samples increased with increasing L/S ratio. [ABSTRACT FROM AUTHOR]

Various chemometric techniques were used to establish the relationship between the autohydrolysis conditions prior to pulping and the chemical compositions of the soluble organic materials removed from Scots pine (Pinus sylvestris) wood chips. The aqueous chip pre-treatments (autohydrolysis) were administered at 130 °C and 150 °C for 30, 60, 90, and 120 min, and the hydrolysates obtained were characterized in terms of total carbohydrates (various mono-, oligo-, and polysaccharides together with uronic acid side groups), volatile acids (acetic and formic acids), lignin, and furans (furfural and 5-(hydroxymethyl)furfural). Based on the analytical data gathered, a relatively accurate model for pine chip autohydrolysis was developed. [ABSTRACT FROM AUTHOR]

Carbohydrate-containing hydrolysates (1.1 to 14.9% of wood dry matter) obtained from auto hydro lysis (at 130 to 150°C for 30 to 120 minutes) of birch (Betula pendula) chips prior to pulping were purified with respect to non-carbohydrate materials, without carbohydrate losses, either by ethyl acetate extraction or XAD-4 resin treatment. In the former case, about 50% of lignin and practically all the furanoic compounds (2-furaldehyde and 5-(hydroxymethyl)furfural) could be removed, whereas in the latter case, the corresponding amounts were about 30% and 50 to 90%, respectively. A partial recovery of various unsaturated impurities is of importance, because they may act as inhibitors when biochemically converting carbohydrates in hydrolysates into value-added products. [ABSTRACT FROM AUTHOR]

This study demonstrated the use of a pressurized mechanical refining system for the continuous steam explosion pretreatment of wheat straw. Wheat straw was first impregnated with either dilute acid (0.5% sulfuric acid) or water and then steam exploded in an Andritz pressurized refiner. The effect of a range of pretreatment conditions, including refining retention time and steam pressure/temperature on the resulting substrate composition and hydrolysability as well as overall sugars yield was investigated. For autohydrolysis, the optimum conditions, 198 °C/6 min gave an enzymatic hydrolysis yield of 93.3% and an overall glucose yield of 85.8%, while 198 °C/4 min gave an enzymatic hydrolysis yield of 88.7% and overall glucose yield of 88.4%. Longer retention time increased the enzymatic hydrolysability but reduced the overall glucose yield owing to the degradation reaction during pretreatment. For acid pretreatment, the most favourable condition for enzymatic hydrolysis and overall glucose yield coincided at 178 °C /6 min . [ABSTRACT FROM AUTHOR]

Xylo-oligosaccharides were obtained from Miscanthus x giganteus. The process was designed as a biorefinery scheme, which seeks the separation of the three main components: cellulose, hemicelluloses, and lignin. To extract the hemicelluloses, particularly xylans, in an efficient way, Miscanthus was subjected to autohydrolysis. The system was evaluated for the effects of temperature (160 to 200°C) and reaction time (15 to 60 min) on various parameters, reflecting the changes undergone during the process. The results showed that autohydrolysis is a suitable method for obtaining high yields of xylo-oligosaccharides, reaching values close to 65% of the dissolved xylans (based on the initial amount of potential xylose). Analysis of the process by using the severity factor (RO) allowed for the identification of a set of time-temperature values for which the fractionation was optimal. [ABSTRACT FROM AUTHOR]

Coastal Bermuda grass (CBG) is an agricultural residue with considerable potential as a feedstock for lignocellulosic-based ethanol. The treatment of biomass with water at high temperature, termed autohydrolysis, can be used to recover sugars in the filtrate and to improve enzyme digestibility of the pretreated solids. The effect of a twostage autohydrolysis process with respect to total sugar recovery relative to a one stage process was investigated. CBG was subjected to lab scale one-stage (150, 160, and 170°C) and two-stage (150/170°C and 160/170°C) isothermal autohydrolysis processes followed by enzyme hydrolysis on the residual solids with different loadings (5 to 30 FPU/g). Two-stage autohydrolysis (160/170°C) solubilized 94.2% of the hemicellulose based on the original CBG material but only 17.7% of the cellulose and 30.4% of the lignin. Increases in the severity factor (a combination of time and temperature) of autohydrolysis pretreatments decreased the recoverable carbohydrates and total solids. Two-stage autohydrolysis enhanced enzyme digestibility of the cellulose in pretreated solids relative to one-stage autohydrolysis, especially at higher values of FPU/g. The overall total theoretical sugar recovery achievable by the two stage process was 57.8% and for the one stage process only 51.6% with 30 FPU/g. This marginal increase would have to be considered relative to increased complexity of operations when deciding whether to implement one or two stage autohydrolysis. [ABSTRACT FROM AUTHOR]

Coastal Bermuda grass (CBG) has been shown to have potential as a biomass feedstock for sugar production. In this study, the effectiveness of ozone pretreatment for CBG to improve the sugar recovery via enzyme hydrolysis was investigated. Raw CBG and autohydrolysistreated CBG were pretreated with ozone at ozone consumption of 1.8 to 26.4 % (w/w) at room temperature. Lignin degradation and hemicellulose solubilization increased with increased ozone consumption. At 26.4% ozone consumption by weight on CBG the amount of lignin in the CBG was reduced by 34%. Autohydrolysis of CBG increased the reactivity of cellulose, hemicellulose, and lignin with ozone. The maximum total sugar recovery after enzymatic hydrolysis was 32% for a 14.0% consumption of ozone on raw CBG. For CBG samples pretreated with autohydrolysis followed by a 3.1% ozone consumption pretreatment the maximum total sugar recovery after enzyme hydrolysis was 40.1%. Autohydrolysis pretreatment followed by enzyme hydrolysis yielded a 36.4% sugar recovery, indicating that the application and benefits of ozone after autohydrolysis with the conditions studied herein are marginally better than autohydrolysis alone. [ABSTRACT FROM AUTHOR]

This paper presents the production of xylooligosaccharides from autohydrolysis liquors of wheat straw and sunflower stalk, as wells as the antioxidant activity of these autohydrolysis liquors. The autohydrolysis liquors (raw or refined by ultrafiltration) of both wastes were subjected to the action of two different endoxylanase to produce xylooligosaccharides with low degree of polymerization that are potentially useful as food additives. Trichoderma reseei xylanase led to the highest proportion of oligomers with degree of polymerization values in the range 1-3, while Aspergillus niger xylanase gave mainly oligomers with polymerization degree in the range 2-3. T reseei xylanase gave a higher increase in equivalent xylose concentration and produced more monosaccharide than A.niger xylanase. Membranes with a nominal MWCO 1 kDa did not reject antioxidant-related and other low molar mass compounds, and most of these compounds were recovered with monosaccharides in the permeate of the membrane. [ABSTRACT FROM AUTHOR]

Extraction of hemicelluloses from wood prior to pulping is being pursued to generate more value-added products, while still producing high quality pulp from the pre-extracted wood. For a better understanding of the factors limiting selective extraction, enzymatic hydrolysis in combination with size exclusion chromatography (SEC) was applied to milled wood and hydrothermally treated wood. Complete dissolution was achieved in a lithium chloride/dimethylacetamide solvent system after mild ballmilling of a Southern Hardwood Mixture (SHM), of SHM extracted using auto-hydrolysis, and of enzyme-treated SHM. SEC tests showed that severe degradation of wood polymers occurred after a milling time of 3 hours. The SEC data also confirmed the presence of lignin-carbohydrate complexes. Based on the results, it is suggested that linkages between lignin and polysaccharides may play an important role in limiting extraction of hemicelluloses. [ABSTRACT FROM AUTHOR]