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Low-pressure steam explosion (LPSE) combined with alkaline peroxide (AP) pretreatment was first employed to separate hemicellulose from Lespedeza stalks. The monosaccharide composition and molecular weight distribution of the obtained hemicellulose fractions were characterized in this study. The results show that the hemicellulose extracted from Lespedeza stalks consisted of xylose, glucose, galactose, and mannose, which was a mixture of arabinoxylans and xyloglucans or β-glucans. The yield of hemicellulose fractions after AP pretreatment ranged from 11.2% (2.5% hydrogen peroxide (H2O2), w/v for 12 h) to 12.2% (3.3% H2O2, w/v for 72 h). The molecular weight of hemicellulose decreased from 2,458 g/mol to 1,984 g/mol after AP pretreatment, indicating its degradation reaction. The structure of hemicellulose was analyzed by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance, and heteronuclear single quantum coherence. The AP pretreatment partially cleaved the backbone and the ether linkage between lignin and hemicelluloses. Also, branched-chain α-Darabinofuranosyl in which β-D-xylose substituted at the C-3 position (monosubstituted) was removed, illustrating a partial debranching reaction. Therefore, the combination of low-pressure steam explosion and alkaline peroxide pretreatment (LPSE-AP) is an effective pretreatment method to separate hemicellulose from Lespedeza stalk. [ABSTRACT FROM AUTHOR]

A combination of steam explosion (SE) and alkaline peroxide (AP) used to pretreat bamboo was investigated. Steam explosion at 224 °C for 4 min was applied to bamboo, and the pretreated bamboo was delignified by alkaline peroxide. Enzymatic hydrolysis was compared in the pretreated samples. Steam pretreatment led to remarkable hemicellulose solubilization (63.2%). Lignin solubilization (93.1%) was achieved by alkaline peroxide treatment of steam-pretreated bamboo at 80 °C for 1 h in 0.88% (v/v) H2O2, whereas only 33.4% of lignin was solubilized when using raw bamboo. Pretreatment methods resulted in a low degree of polymerization and increased hydrolysis of cellulose. A maximum glucose yield of 90.5% was achieved with a combined steam explosion and alkaline peroxide pretreatment. The surface structure of treated bamboo and the adsorption of enzyme on the substrate were characterized by X-ray photoelectron spectroscopy. Delignification decreased enzyme adsorption and increased enzymatic conversion. SEM analyses indicated that SE-AP pretreatment disrupted lignin networks and exposed crystalline cellulose in bamboo more effectively than SE or AP pretreatment alone. [ABSTRACT FROM AUTHOR]

The major challenge for natural fiber composites is their inherent poor adhesion between fiber and the matrix, high moisture absorption, and UV degradation. Lignin and hemicelluloses are the major composites of natural fiber which are responsible for UV degradation and moisture absorption, respectively. In this study, the lignocelluloses (oil palm empty fruit bunch) were treated with alkaline peroxide to separate lignin and hemicelluloses. Composites were produced with treated and untreated fibers using up to 45% fiber with polypropylene matrix using twin-screw extruder followed by injection molding. To improve the interfacial bonding, maleic anhydride grafted polypropylene (MAPP) was used as a coupling agent in the formulation. Properties of composites were evaluated using tensile testing, flexural testing, impact testing, SEM, and FTIR. The tensile, flexural, and impact properties were found to be improved with alkaline peroxide-treated fiber composites compared to untreated fiber composites. Addition of coupling agent (MAPP) also found to provide improved properties of composites. [ABSTRACT FROM AUTHOR]

Abstract: A two-stage pretreatment method was proposed and tested for deconstruction of recalcitrant Miscanthus. During a 1st pretreatment at 50°C, 1.0–4.0% alkaline peroxide solutions were used to partially remove hemicellulose and lignin. The remaining solids were subjected to a 2nd pretreatment at 121°C with electrolyzed water. Using 15 filter paper units of cellulase per gram cellulose, a digestibility of 95% was achieved by the two-stage method, which was higher than 81% obtained from a 1% H2SO4 pretreatment (200°C, 8min). A mass balance for the two-stage process showed that 63% hemicellulose and 64% lignin were removed from the Miscanthus samples after the 1st pretreatment. The Scanning Electron Microscopy images and Fourier Transform Infrared Spectroscopy spectra revealed that after the 1st pretreatment, crystalline cellulose fibers were partially exposed and the linkages between residual lignin and hemicellulose disappeared. After the 2nd pretreatment, cellulose fibers were completely exposed even with cracks developed. [Copyright &y& Elsevier]

Treatment of dewaxed oil palm frond fiber; fast-growing poplar wood; maize stems; and barley, wheat, rice, and rye straws with 2.0% H2O2 at pH 11.6 for 16 hr at 45°C solubilized 85.7%, 49.5%, 78.2%, 79.7%, 87.1%, 92.7%, and 79.4% of the original hemicelluloses and 72.1%, 24.9%, 87.3%, 70.9%, 85.7%, 88.6%, and 89.8% of the original lignin, respectively. The results indicated that hydrogen peroxide at pH 11.6 had a significant effect on the release of hemicelluloses and delignification from oil palm frond fiber and cereal straws such as maize stems and barley, wheat, rice, and rye straws under the condition used. All the hemicellulosic preparations were much lighter in color and had relatively lower amounts of associated lignin than those obtained using traditional alkaline extraction in the absence of peroxide from the corresponding lignified materials. Xylose is the dominant sugar component in the hemicellulosic preparations isolated from oil palm frond fiber, fast-growing poplar wood, maize stems, and barley, wheat and rye straws, whereas the hemicelluloses obtained from rice straw are rich in glucose and xylose. The seven hemicellulosic samples were also studied by fourier transform infrared(FT-IR} and 1H- and 13C-nuclear magnetic resonance(NMR) spectroscopy, gel permeation chromatography(GPC), and thermal analysis. [ABSTRACT FROM AUTHOR]

Over 90% of the original hemicelluloses in the cell walls of bagasse were sequentially extracted with distilled water, 0.5 M NaOH, 0.5, 1.0, 1.5, 2.0 and 3.0% H2O2 at pH 11.5, and 2.0 M NaOH at 55 °C for 2 h. Meanwhile, the successive treatments also released 89.0% of the original lignin. Chemical composition, physico-chemical properties, and structures of the eight hemicelluloses were elucidated by a combination of sugar analysis, nitrobenzene oxidation of bound lignin, molecular determination, Fourier transform infrared, and 1H and 13C NMR spectroscopy and thermal analysis and the results are reported. The results showed that the sequential treatments were very effective on the fractionation of hemicelluloses from bagasse, and the extraction strength, such as alkali and H2O2 concentration, had a great influence on the chemical and structural features of the hemicelluloses, e.g. content of associated lignin and molecular weight. The hemicellulosic fraction, isolated with 0.5% H2O2 at pH 11.5 for 2 h under 55 °C, had a backbone of xylose residues with β-(1→4) linkages and were branched mainly through arabinofuranosyl and 4-O-methyl glucopyranosyl units. Ferulic and p-coumaric acids were found to be esterified to the hemicelluloses. [Copyright &y& Elsevier]

Two-stage treatments of Caligonum monogoliacum and Tamarix spp. with acidic organosolv and alkaline peroxide were performed. Pre-treatment with ethanol–H2O (60/40, v/v) under acid catalyst (0.2 N HCl) at 70 °C for 4 h released 18.7 and 17.8% hemicelluloses from dewaxed C. monogoliacum and Tamarix spp., respectively, Sequential treatment with 2% H2O2 at pH 11.5 for 16 h at 45 °C solubilized 26.2 and 26.5% hemicelluloses from pre-treated C. monogoliacum and Tamarix spp., respectively. Cellulose predominated in the insoluble residues, accounting for 36.7–37.8% of dry materials. It was found that the two alkaline peroxide soluble hemicellulosic preparations contained a much higher amount of xylose (74.1–77.3%) but lower in glucose (7.4–18.6%), galactose (3.0–8.3%), rhamnose (2.3–2.9%), mannose (0.8–2.7%), and arabinose (1.3–1.4%) than those of the two acidic organosolv soluble hemicellulosic fractions in which xylose (31.8–50.8%), glucose (21.4–30.3%), galactose (7.6–24.1%), and rhamnose (5.7–10.1%) were the major sugar components. The content of uronic acids was slightly higher in the two alkaline peroxide soluble hemicellulosic preparations (7.5–8.3%) than the two acidic organosolv soluble hemicellulosic fractions (5.0–6.5%). Furthermore, the studies showed that the two alkaline peroxide soluble hemicellulosic preparations were more linear and acidic, and had a large molecular mass (M¯w, 27,220–31,410 g mol−1) than the two acidic organosolv soluble hemicellulosic fractions (M¯w, 13,820–18,380 g mol−1). Lignin content and its composition associated in the four isolated hemicelluloses were determined by alkaline nitrobenzene oxidation and monitored with HPLC. No significant differences in lignin content (5.94–9.82%) and its composition were found. Further comparative study of the four hemicellulosic preparations and two cellulosic fractions was carried by both degraded methods such as acid hydrolysis and thermal analysis and non-degradation techniques such as FT-IR and 13C-NMR spectroscopy. [Copyright &y& Elsevier]

Eight hemicellulosic fractions were obtained by sequential treatment of dewaxed barley straw with 0.1 M NaOH at 45 °C for 3 h, 0.25, 0.5, 1.0, 1.5, 2.0, and 3.0% H2O2 at 45 °C for 3 h at pH 11.5, and 10% KOH–1% Na2B4O7·10H2O at 28 °C for 15 h under continuous agitation. The yields of the fractions were 8.0, 3.1, 3.3, 3.3, 2.2, 2.0, 2.0, and 9.9%, respectively, of the initial amount of barley straw, corresponding to the dissolution of 21.6, 8.4, 8.9, 8.9, 5.9, 5.4, 5.4, and 26.7% of the original hemicelluloses. Meanwhile, the successive treatment also solubilized 29.1, 15.8, 14.6, 10.8, 4.5, 3.2, 2.7, and 3.7% of the original lignin, respectively. This sequential extraction together resulted in dissolution of 91.1% of the original hemicelluloses and 84.8% of the original lignin. The 0.1 M NaOH-soluble hemicellulosic fraction contained mainly xylose, glucose, and arabinose, 44.2, 15.7, and 15.2%, respectively, while the 10% KOH–1% Na2B4O7·10H2O-soluble fraction predominated in xylose, 75.0%. The six alkaline peroxide-soluble fractions were composed of 50.3–54.4% xylose, 14.7–16.9% arabinose, 6.8–10.7% glucose, 6.8–8.5% glucuronic acid or 4-O-methyl-d-glucuronic acid, 0.4–1.5% mannose, and 0.3–1.2% rhamnose. All the hemicellulosic fractions contained substantial amounts of glucuronoarabinoxylans and noticeable quantities of β-glucans. In comparison, the six hemicellulosic fractions, isolated with alkaline peroxide, had much higher molecular weights (56,890–63,810 g mol−1) than those of the two hemicellulosic preparations (28,000–29,080 g mol−1), isolated with alkali in the absence of hydrogen peroxide. The thermal stability of the hemicelluloses increased with an increment of their molar mass. [Copyright &y& Elsevier]