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Instant controlled pressure drop (DIC) technology was utilized in the production of glucose from sago pith waste (SPW). In situ autohydrolysis was conducted in a DIC reactor to obtain the maximum glucose production. The influence of pressure, acid concentration, and treatment time on the glucose yield from SPW subjected to DIC-assisted in situ autohydrolysis was determined, and the experimental conditions were optimized using the response surface method. The results showed that the linear term of acid concentration and the quadratic terms of pressure and time had a significant effect on the glucose yield. The optimized experimental conditions for maximum glucose production (48.21%) from SPW subjected to DIC-assisted autohydrolysis were a pressure of 0.1 MPa, acid concentration of 0.1 M, and time of 4 min. The findings demonstrated that DIC technology has the potential to be utilized for the commercial production of glucose from SPW.

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 thermal-based 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.

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.

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.

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.

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.

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 ºC (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 ºC) 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 lignin-derived 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.

This study investigates the operating conditions used in the soda-anthraquinone 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.

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.

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 ºC 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.

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.

To assess the feasibility of implementing hemicellulose recovery stages in kraft mills, Eucalyptus globulus wood samples were subjected to aqueous treatments with hot, compressed water (autohydrolysis processing) to achieve partial dissolution of xylan. Autohydrolyzed solids were subjected to kraft pulping under selected conditions to yield a pulp of low kappa number, and to an optimized TCF bleaching sequence made up of three stages (alkaline oxygen delignification, chelating, and pressurized hydrogen peroxide), with minimized additions of pulping and bleaching chemicals. The final product had a relatively low kappa number (1.4), 641 mL/g ISO intrinsic viscosity, and 86.4% brightness.

Carbohydrate-containing hydrolysates (1.1 to 14.9% of wood dry matter) obtained from autohydrolysis (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.

The amount of residual lignin in birch wood after a hot water extraction in a batch reactor was investigated as a function of extraction temperature and time. A kinetic model fitting the experimental data was then developed to explain delignification of wood during a hot water treatment. Results showed that delignification kinetics involves simultaneous degradation and condensation reactions, with degradation of lignin being much faster than its condensation. Native lignin in wood was successfully modeled as the sum of two fractions with different degradation rates. The rates of degradation and condensation increased along with increasing extraction temperature. The proportion of acid-soluble lignin to acid-insoluble (Klason) lignin in the wood residue decreased with increasing extraction temperature and time, probably due to chemical and structural changes in the lignin during the hot water treatment. Condensed lignin was predominantly determined as Klason lignin. On the other hand, the amount of soluble lignin in the extraction liquor increased slightly with temperature, but remained mostly constant after any extraction time. An insoluble fraction in the liquor that originated from precipitated lignin fragments is believed to contain traces of degradation products from carbohydrates or other degradation compounds.

A trihybrid clone of Paulownia fortunei x tormentosa x elongata was used for pulp and paper production using the soda-anthraquinone (AQ) process, comparing the results with those from Paulownia fortunei. An autohydrolysis process had been previously carried out on this raw material. A composite central experimental design and a multiple regression were used for modeling and optimizing the process. A valuable liquid phase could be obtained from the autohydrolysis process of Paulownia, trying to minimize cellulose degradation for pulp and paper production. A compromise to maximize the glucan and minimize the xylan contents in the postautohydrolysis solid phase could be achieved at 187.5ºC and 15 minutes. A suitable cellulosic pulp with kappa number ranging from 12.2 to 69.2 and ISO brightness from 18.2 to 30.6% presented better results than those from other studies. Regarding handsheets physical properties (tensile index 37.3 N•m/g ) and viscosity (848 cm3/g), significant improvements could be obtained when compared with previous results of a similar process using Paulownia fortunei or Paulownia elongata.

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 two- stage 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.

This paper presents the production of xylooligosaccharides from auto-hydrolysis 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.

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 autohydrolysis-treated 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.

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 ball-milling 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.