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The reductive catalytic fractionation (RCF) of lignocellulosic biomass is an attractive method for the conversion of lignin toward valuable low-molecular weight aromatics. A limitation to the upscaling of such technology is represented by the use ofpressurized hydrogen gas. Here, the role of hydrogen gas within the RCF of wheat straw biomass is investigated. The use of H 2 is shown to enhance lignin depolymerization, by virtue of an improved hydrogenolysis and hydrogenation of lignin fragments, with a yield of phenolic monomers that increased from ca. 12 wt % of acid-insoluble lignin in the initial biomass under inert atmosphere to up to ca. 25 wt % under H 2 (in methanol, at 250 °C, with Ru/C). The adoption of methanol, ethanol or isopropanol as hydrogen-donor solvents was also investigated in the absence of H 2 . Ethanol was found to give the highest yield of monophenolic compounds (up to ≈20 wt %) owing to a better balance between solvolysis, hydrogenolysis, and hydrogenation of lignin. Nevertheless, a substantial loss of the carbohydrate fraction was observed. The use of a lower temperature (200 °C) in combination with H 3 PO 4 resulted in an improved recovery of cellulose in the pulp and in the solubilization of hemicellulose and lignin, with the formation of monosaccharides (≈14 wt % of polysaccharides in the initial biomass) and phenolic monomers (up to 18 wt %, in the absence of H 2 ). Overall, a tradeoff exists between the removal of H 2 from the process and the production of low-molecular weight phenolics during RCF., (© 2023 Wiley-VCH GmbH.)

Abiotic stress conditions, such as salinity, affect plant development and productivity and threaten the sustainability of agricultural production. Salt has been proven to accumulate in soil and water over time as a result of various anthropogenic activities and climatic changes. Species of the genus Salicornia thrive in the most saline environments and have a wide climatic tolerance. They can be found in a variety of subtropical, oceanic, and continental environments. This study aims to establish Salicornia europaea as a novel source of plant-based compounds that can grow in areas unsuitable for other crops. The morphological and compositional changes in the tissues of S. europaea in different consecutive developmental stages have not been investigated so far. Therefore, a comprehensive study of changes during the lifecycle of S. europaea was carried out, following changes in the plant's composition, including biomass yield, and soluble and insoluble compounds. For this, plants were cultivated in hydroponics for 15 weeks and harvested weekly to analyze biomass production, to determine soluble and insoluble compounds, protein content, and polyphenols. According to the results, glucan, xylan, and lignin increase with plant age, while water extractives decrease. Protein content is higher in young plants, while flavonoid content depends on the phenological stage, decreasing in the early flowering stage and then increasing as plants enter early senescence. Our results can aid in finding the optimal harvesting stage of S. europaea, depending on the component of interest.

The stone of Cornus mas L. remains the least known morphological part of this plant, whereas the fruit is appreciated for both consumption purposes and biological activity. The stone is considered to be a byproduct of fruit processing and very little is known about its phytochemical composition and biological properties. In this study, the complete qualitative determination of hydrolyzable tannins, their quantitative analysis, total polyphenolic content, and antioxidant properties of the stone of C. mas are presented for the first time. The 37 identified compounds included the following: various gallotannins ( 11 ), monomeric ellagitannins ( 7 ), dimeric ellagitannins ( 10 ), and trimeric ellagitannins ( 7 ). The presence of free gallic acid and ellagic acid was also reported. Our results demonstrate that C. mas stone is a source of various bioactive hydrolyzable tannins and shows high antioxidant activity which could allow potential utilization of this raw material for recovery of valuable pharmaceutical or nutraceutical substances. The principal novelty of our findings is that hydrolyzable tannins, unlike other polyphenols, have been earlier omitted in the evaluation of the biological activities of C. mas . Additionally, the potential recovery of these bioactive chemicals from the byproduct is in line with the ideas of green chemistry and sustainable production.

In this study Salicornia sinus-persica, a succulent halophyte was assessed for its potential to be used as a feedstock for bioethanol production. For such succulent, salty, green biomasses, direct fractionation and fermentation allow for water preservation in the process. Fresh biomass of S. sinus-persica was collected and split into two fractions by wet fractionation; liquid (juice) and solid (pulp). Sugar contents were found to be 1.0-1.5% for the juice fraction and 50% (w/w) for the fresh pulp. Direct fermentation of the juice using Saccharomyces cerevisiae showed no salt inhibition of the yeast and ethanol yields of ~70% were achieved. A pretreatment study was carried out for the pulp fraction applying mild hydrothermal pretreatment. Cellulose convertibility was found to be significantly higher for severity factors above 2.00, and the highest ethanol yield (76.91 ± 3.03%) was found at process severity of 3.06 (170 °C, 10 min).

The large water consumption (1.9-5.9 m(3) water per m(3) of biofuel) required by biomass processing plants has become an emerging concern, which is particularly critical in arid/semiarid regions. Seawater, as a widely available water source, could be an interesting option. This work was to study the technical feasibility of using seawater to replace freshwater in the pretreatment of date palm leaflets, a lignocellulosic biomass from arid regions, for bioethanol production. It was shown that leaflets pretreated with seawater exhibited lower cellulose crystallinity than those pretreated with freshwater. Pretreatment with seawater produced comparably digestible and fermentable solids to those obtained with freshwater. Moreover, no significant difference of inhibition to Saccharomyces cerevisiae was observed between liquids from pretreatment with seawater and freshwater. The results showed that seawater could be a promising alternative to freshwater for lignocellulose biorefineries in coastal and/or arid/semiarid areas., (© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Date palm residues are one of the most promising lignocellulosic biomass for bioethanol production in the Middle East. In this study, leaflets and rachis were subjected to hydrothermal pretreatment to overcome the recalcitrance of the biomass for enzymatic conversion. Evident morphological, structural, and chemical changes were observed by scanning electron microscopy, X-ray diffraction, and infrared spectroscopy after pretreatment. High glucan (>90% for both leaflets and rachis) and xylan (>75% for leaflets and >79% for rachis) recovery were achieved. Under the optimal condition of hydrothermal pretreatment (210°C/10 min) highly digestible (glucan convertibility, 100% to leaflets, 78% to rachis) and fermentable (ethanol yield, 96% to leaflets, 80% to rachis) solid fractions were obtained. Fermentability test of the liquid fractions proved that no considerable inhibitors to Saccharomyces cerevisiae were produced in hydrothermal pretreatment. Given the high sugar recovery, enzymatic digestibility, and ethanol yield, production of bioethanol by hydrothermal pretreatment could be a promising way of valorization of date palm residues in this region.

Salicornia bigelovii straw was characterized and evaluated as a potential lignocellulosic bioethanol feedstock. S. bigelovii used in the study was grown in the United Arab Emirates using saltwater (40ppt) for irrigation. Salt removal was performed prior to pretreatment to protect the processing equipment and avoid inhibition of enzymes and yeast. Composition of the washed biomass was comparable to traditional lignocellulosic biomasses with relatively high glucan and xylan content (26 and 22g/100gDM, respectively) but with lower lignin content (7g/100gDM). The washed feedstock was subjected to hydrothermal pretreatment, producing highly digestible (up to 92% glucan-to-glucose conversion) and fermentable (up to 100% glucose-to-ethanol conversion) fiber fractions. Liquid fractions obtained in the pretreatment did not show inhibition towards Saccharomyces cerevisiae. No significant differences among the enzymatic convertibility and microbial fermentability of the fibers as well as low xylose recoveries suggest that lower severity pretreatment conditions could be exploited for S. bigelovii., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

Prairie cordgrass (PCG) was pretreated by sequential extrusion and clean fractionation (CF) processing. Following CF, PCG was fractionated into cellulose, hemicellulose and lignin-rich fractions. Cellulose pulp was then enzymatically hydrolyzed, producing glucose. The main purpose of this study was to produce the highest glucose yield as possible. The effects of time, temperature, catalyst concentration and solvent mixture composition on the fractionation were tested. Different proportions of methyl isobutyl ketone (MIBK), ethanol and water with sulfuric acid as a catalyst were evaluated. Optimal conditions for sequential extrusion and clean fractionation (39 min, 129 °C, 0.69% catalyst, and 28% MIBK) resulted in higher glucose yield (92%), and more lignin (87%) and xylan (95%) removal than for clean fractionation alone. Pairwise comparison of raw PCG with extruded PCG clean fractionation revealed no difference in glucose yields, but xylan and AIL removal were higher in the case of clean fractionation of the pre-extruded PCG., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

The purpose of this study was to fractionate switchgrass (SG) to obtain hemicellulose-, lignin-rich fractions and highly digestible pulp, using a clean fractionation (CF) approach. The main objective was to produce highest glucose yield in the enzymatic hydrolysis of pulp. Effects of processing factors such as time (10-50 min), temperature (120-160 °C), catalyst concentration (0.21-0.93% w/w sulfuric acid) and organic solvent mixture composition (7-43% w/w methyl isobutyl ketone) were evaluated. Response surface methodology and central composite design were used for process optimization and statistical analyses. High lignin (75-93%) and xylan (83-100%) removal from biomass were obtained, leaving solid pulp rich in glucan (78-94%). High enzymatic hydrolysis glucose yields (more than 90%) were obtained for selected optimal conditions. Pulp can be used for ethanol production while separated xylan and lignin fractions can be used as a feedstock for value-added products which suggests the applicability of clean fractionation technology in a biorefinery concept., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

Switchgrass was used as a lignocellulosic feedstock for second generation ethanol production, after pretreatment using sulfuric acid-catalyzed modified clean fractionation based on NREL's (National Renewable Energy Laboratory) original procedure. Optimization of temperature, catalyst concentration and solvent composition was performed using Response Surface Methodology, and 59.03 ± 7.01% lignin recovery, 84.85 ± 1.34% glucose, and 44.11 ± 3.44% aqueous fraction xylose yields were obtained at 140.00 °C, 0.46% w/w catalyst concentration, 36.71% w/w ethyl acetate concentration, and 25.00% w/w ethanol concentration. The cellulose fraction did not inhibit the fermentation performance of Saccharomyces cerevisiae and resulted in an ethanol yield of 89.60 ± 2.1%., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

Lignin extracted from prairie cordgrass, switchgrass, and corn stover (using ethyl acetate-ethanol-water organosolv pretreatment) was analyzed and characterized using several methods. These methods included analysis of purity (by determination of Klason lignin, carbohydrate, and ash contents), solubility (with several organic solvents), phenolic group analysis (ultraviolet ionization difference spectra, and nitrobenzene oxidation), and general functional group analysis (by (1)H NMR). Results showed that all the examined lignin samples were relatively pure (contained over 50% Klason lignin, less than 5% carbohydrate contamination, and less than 3% ash), but switchgrass-derived lignin was observed to be the purest. All the lignins were found to contain high amounts of phenolic groups, while switchgrass-derived lignin was the most phenolic, according to the ionization difference spectra. Nitrobenzene oxidation revealed that all the lignin samples contained available guaiacyl units in high amounts., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

The main objective of this study was to fractionate prairie cordgrass (PCG) obtaining the highest cellulose digestibility. Following clean fractionation (CF) processing, the PCG lignocellulosic biomass was fractionated into three main building blocks: cellulose, hemicellulose and lignin. Effects of processing factors such as time, temperature, catalyst concentration and organic solvent mixture composition were evaluated. Organic solvent-aqueous mixture contained methyl isobutyl ketone (MIBK), ethanol and water in different proportions. Sulfuric acid was used as a catalyst. In order to evaluate the degree of pre-treatment, enzymatic saccharification was employed on the cellulose fraction obtained from the CF process. Response surface methodology was used for process optimization and statistical analysis. Optimal conditions (39 min, 154°C, 0.69% catalyst and 9% MIBK) resulted in 84% glucose yield and 87% acid insoluble lignin (AIL)., (Copyright © 2011 Elsevier Ltd. All rights reserved.)