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The glucose yield obtained without pre-treatment in concentrated sulfuric acid before post-hydrolysis was found to be 20% which can mainly be related to the amorphous fraction of cellulose. & Al-Deyab, S. S. Cellulose nanowhiskers extracted from TEMPO-oxidized jute fibers. ACS Sustain. 120, 12161224 (2018). Effect of fiber drying on properties of lignin containing cellulose nanocrystals and nanofibrils produced through maleic acid hydrolysis. BlueFire Renewables Inc., established in 2010 to deploy the Arkenol technology (BlueFire Renewables, 2010), was awarded funding from the US Department of Energy and a letter of intent from the Export Import Bank of China was renewed in February 2015 to provide up to 270 million US$ in debt financing for its intended commercial plant in Fulton, Mississippi. & Lin, N. in Advanced Functional Materials from Nanopolysaccharides (eds Lin, N., Tang, J., Dufresne, A. 29, 614 (2014). Edgar, C. D. & Gray, D. G. 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The biomass was planted on May 19, 2009 by CROM (Centre de recherche sur les grains) and CRSAD (Centre de recherche en sciences animales de Deschambault), and treated with the Buctril M herbicide on June 14, 2009. Biomacromolecules 14, 12231230 (2013). Polym. Biomacromolecules 8, 899904 (2007). Moreover, 5-HMF was detected in the hydrolysates but its concentration was below the lower limit of quantification of the HPLC. Du, H. et al. Crop. These include the 9598 wt% sulfuric acid used for pre-treatment and the bases (29 wt% aqueous ammonia and 20 wt% sodium hydroxide) used for partial neutralization. Afterwards, the biomass was impregnated with an 8 wt% sodium hydroxide solution and subjected to a second steam treatment at 180C for 2 min. Prod. Brinkmann, A. et al. Carbohydr. Int. US20040234441 A1. Tan, X. Y., Abd Hamid, S. B. In the meantime, to ensure continued support, we are displaying the site without styles The effect of NaOH concentration on glucose yield was investigated and the results are given in Figure 7. Periodic disorder along ramie cellulose microfibrils. However, adding water to dilute the sulfuric acid from 72 to 410 wt% results in a large volume of mixture, which implies higher handling costs. Habibi, Y., Chanzy, H. & Vignon, M. R. TEMPO-mediated surface oxidation of cellulose whiskers. This work was funded through Natural Sciences and Engineering Research Council of Canada (NSERC) Discovery Grant RGPIN-2017-05252 to E.D.C. Prod. Cellulose 25, 17431756 (2018). & Berry, R. Iridescent solid nanocrystalline cellulose films incorporating patterns and method for their production. Macromolecules 24, 41684175 (1991). Nanotechnologies characterization of cellulose nanocrystals ISO/TR 19716 (ISO, 2016). Eng. Revol, J.-F., Godbout, D. L. & Gray, D. G. Solidified liquid crystals of cellulose with optically variable properties. Acid-based hydrolysis processes for ethanol from lignocellulosic materials: a review. Chem. For example, cellulose hydrolyzed with 0.4 wt% acid at 215C for 3 min after pre-treatment (hemicelluloses hydrolysis) with 0.7 wt% sulfuric acid at 190C for 3 min gave a glucose yield of only 50% (Hamelinck et al., 2005). 107, 505514. 3, 649650 (1949). Although the influence of pre-treatment time on glucose yield was not investigated for mass ratio of sulfuric acid/dry cellulose of 12 and 24, the best pre-treatment time of 2 h was verified for the most desirable (lowest) ratio of 12 during the other trials determining the influence of concentration of base, post-hydrolysis time and temperature on the glucose yield. Cao, X., Dong, H. & Li, C. M. New nanocomposite materials reinforced with flax cellulose nanocrystals in waterborne polyurethane. Nickerson, R. F. & Habrle, J. (1996). For the partial neutralization step, sodium hydroxide was the preferred base for higher glucose yields after post-hydrolysis but aqueous ammonia also gave a very high glucose yield (around 95%). Biomacromolecules 13, 14861494 (2012). Carbohydr. Effect of surface charge on surface-initiated atom transfer radical polymerization from cellulose nanocrystals in aqueous media. New York, NY: Springer Science and Business Media. 23, 7491 (2019). US Patent 20190040158A1 (2019). Leguy, J. et al. Biophys. Teixeira, E. et al. Xiang, Q., Lee, Y. Y., Pettersson, P. O. Ind. Anim. Polym. Cellulose 22, 17531762 (2015). Periodate oxidation followed by NaBH4 reduction converts microfibrillated cellulose into sterically stabilized neutral cellulose nanocrystal suspensions. Handbook of Industrial Chemistry and Biotechnology. To some extent, these biofuels compete for land and water used for food and fiber production. Kaushik, M. & Moores, A. 87, 152165 (2019). Their ability to do so, however, is highly dependent on the way they are produced. JK-WC: generated the results by analyzing and interpreting the acquired data, and wrote, drafted and revised the article; XD: produced and checked the results and reviewed the article; VB: performed the experiments and acquired the data; HZ-N: supervised the work by providing an industrial orientation and offered technical guidelines; J-ML: managed and supervised the research, provided scientific and technical guidance, checked the results, and reviewed significantly and approved the article. 153, 143152 (2016). Revol, J.-F., Bradford, H., Giasson, J., Marchessault, R. H. & Gray, D. G. Helicoidal self-ordering of cellulose microfibrils in aqueous suspension. United States Patent and Trademark Office. Polymer 32, 15161526 (1991). Dissolution mechanism of cellulose in 72 wt% sulfuric acid (based on Feng and Chen, 2008). 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Mariano, M., Chirat, C., El Kissi, N. & Dufresne, A. Impact of cellulose nanocrystal aspect ratio on crystallization and reinforcement of poly(butylene adipate-co-terephthalate). Angew. Sirvi, J. A novel facile two-step method for producing glucose from cellulose. 6, 83178324 (2018). Kloser, E. & Gray, D. G. Surface grafting of cellulose nanocrystals with poly(ethylene oxide) in aqueous media. (2002). Correspondence to The standard procedure for the quantitative determination of carbohydrate in cellulose was carried out following the ASTM International method (E1758-01) where: 4.92 g of 72 wt% sulfuric acid was added to 0.3 g of cellulose for 1 h at 30C with agitation every 15 min. Lin, K.-H. et al. However, the interest toward increasing the production of biofuels is still very strong. The Export-Import Bank of China Renews Letter of Intent to BlueFire Renewables for Fulton Project Due Diligence Continues to Reach a Financial Closing. Frka-Petesic, B., Sugiyama, J., Kimura, S., Chanzy, H. & Maret, G. Negative diamagnetic anisotropy and birefringence of cellulose nanocrystals. Except for the hydrolysate produced after a pre-treatment of 2 h, in which 5-HMF was detected at a concentration below the lower limit of quantification of the HPLC, no 5-HMF peak was observed in the chromatograms obtained from the other pre-treatment times. 56, 175186 (2014). Despite this observation, the glucose yield under the most efficient conditions was higher with sodium hydroxide than with aqueous ammonia. Crystallinity of cellulose nanomaterials by powder X-ray diffraction, ISO/TC 229 PWI 23361 (in the press). Siqueira, G., Tapin-Lingua, S., Bras, J., da Silva Perez, D. & Dufresne, A. Morphological investigation of nanoparticles obtained from combined mechanical shearing, and enzymatic and acid hydrolysis of sisal fibers. Part B Polym. Bano, S. & Negi, Y. S. Studies on cellulose nanocrystals isolated from groundnut shells. 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X-ray and electron microscope studies of the degradation of cellulose by sulphuric acid. Bioresour. At a still higher mass ratio of sulfuric acid/dry cellulose of 36 and combined with a H2SO4 mass percentage of 72 wt%, a glucose yield of 98% was obtained, with a much smaller standard deviation among the triplicates than at lower mass ratios of sulfuric acid/dry cellulose. New insights into nano-crystalline cellulose structure and morphology based on solid-state NMR. J. Sugiyama, J., Vuong, R. & Chanzy, H. Electron diffraction study on the two crystalline phases occurring in native cellulose from an algal cell wall. & Kargarzadeh, H. Extraction of cellulose nanocrystals from mengkuang leaves (Pandanus tectorius). Chem. to improve the purity of cellulose, provided by the high sulfuric acid solution of 1.00 N for 120 min. Google Scholar. Cellulose 13, 171180 (2006). 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When using a higher mass ratio of sulfuric acid/dry cellulose of 24, the glucose yield rose from 34 to 94% when the mass percentage of acid was increased from 62 to 72 wt%. Polym. 6:117. doi: 10.3389/fchem.2018.00117. The research focused on the effects of integrating nanocellulose in the solidification of metal ions into metal oxide particles or metallic electrodeposits. Aggregation behavior of aqueous cellulose nanocrystals: the effect of inorganic salts. J. Santos, R. M. dos et al. 93, 8895 (2016). Csar, N. R., Pereira-da-Silva, M. A., Botaro, V. R. & de Menezes, A. J. Cellulose nanocrystals from natural fiber of the macrophyte Typha domingensis: extraction and characterization. https://doi.org/10.1002/ange.202002433 (2020). Crop. Polym. Chen, L. et al. A. International Organization for Standardization. Cellulose 22, 407420 (2015). Abstract. The preparation of cellulose nanocrystals (CNCs) from cellulose extracted from cotton gin motes (CGM) using an ionic liquid (1-butyl-3-methylimidazolium chloride, [BMIm]Cl) under dilute conditions is reported. Open Access articles citing this article. Water in cellulose: evidence and identification of immobile and mobile adsorbed phases by 2H MAS NMR. Effect of H+/NH3 (A) or H+/OH (B) molar ratio on glucose yield with mass ratio of H2SO4/dry cellulose ratio = 12(), 24(), 36() combined with a pre-treatment at 30C and 72 wt% H2SO4 for 2 h and a post-hydrolysis for 10 min at 121C. 11, 18081814 (2009). Implementing 2nd generation liquid biofuels in a fossil fuel-dominated market: making the right choices. Biomass Bioenergy 81, 584591 (2015). El Achaby, M., Kassab, Z., Aboulkas, A., Gaillard, C. & Barakat, A. Reuse of red algae waste for the production of cellulose nanocrystals and its application in polymer nanocomposites. A 1, 39383944 (2013). doi: 10.1016/j.cogsc.2016.09.009. It is found as stacks of linear chains with D-cellobiose repeating units and these chains are closely packed, with intramolecular hydrogen bonding within each single glucan chain and intermolecular hydrogen bonding between adjacent chains. Frka-Petesic, B., Guidetti, G., Kamita, G. & Vignolini, S. Controlling the photonic properties of cholesteric cellulose nanocrystal films with magnets. Recent advances in nanocellulose for biomedical applications. Biotechnol. 87, 564573 (2012). Each test was performed in triplicate and the mean humidity was calculated and used as reference for the mass balance of the hydrolysis tests. A study of the production of cellulose nanocrystals through subcritical water hydrolysis. Macromolecules 30, 63956397 (1997). Retsina, T., Pylkkanen, V. & van Heiningen, A. Key advances in the chemical modification of nanocelluloses. Prior to the first steam treatment, biomass was impregnated with water for 24 h at room temperature. Li, Q., McGinnis, S., Sydnor, C., Wong, A. As shown in Fig. Lopez-Exposito, P., Campano, C., van de Ven, T. G. M., Negro, C. & Blanco, A. Microalgae harvesting with the novel flocculant hairy cationic nanocrystalline cellulose. Johar, N., Ahmad, I. Res. 37, 9399 (2012). & Pasquini, D. Extraction and characterization of cellulose nanocrystals from agro-industrial residue - soy hulls. Cellulose on hydrolysis yields A. D F Fructose - D - F - Fructose B. D Glucose - D - Glucose C. D Glucose - D - Glucose D. D Fructose - D - Fructose class-12 biomolecules 1 Answer 0 votes answered Jun 22, 2019 by AmaanYadav (89.1k points) selected Jun 22, 2019 by EesvarSharma Best answer Correct Answer - C 175, 370376 (2017). & Zhang, Y. Reuse of waste cotton cloth for the extraction of cellulose nanocrystals. Characteristics and properties of carboxylated cellulose nanocrystals prepared from a novel one-step procedure. Mater. contracts here. Leo, R. M., Milo, P. C., Maia, J. M. L. L. & Luz, S. M. Environmental and technical feasibility of cellulose nanocrystal manufacturing from sugarcane bagasse. Ojala, J., Sirvi, J. Colloids Surf. New approach for single-step extraction of carboxylated cellulose nanocrystals for their use as adsorbents and flocculants. Nevertheless, in both cases, when an H+/NH3 molar ratio of 1.7 or an H+/OH molar ratio of 2.4 was used, the final mass percentage of sulfuric acid during the post-hydrolysis step was close to 19 wt% although the concentration of the base solutions used for partial neutralization was 29 wt% for ammonia and 20 wt% for sodium hydroxide. J. Nanopart. These conditions involve pre-treating cellulose at 30C using 72 wt% H2SO4 with a H2SO4/dry cellulose mass ratio of 36 over 2 h, followed by a partial neutralization using 20 wt% NaOH at an H+/OH molar ratio of 2.32.5 and a post-hydrolysis at 121C for 10 min. Carbohydr. Again in this situation, increasing the mass percentage of acid to more than 72 wt% did not improve the glucose yield. Under the conditions tested in this work, the most efficient H+/NH3 molar ratios were found to range between 1.6 and 1.8. Wahnon, D. (2008). Biomacromolecules 17, 30253032 (2016). 299, 532535 (1999). The hydrolysis of cellulose to high-yield glucose in water remains challenging owing to the limited acidity and substrate contact of sulfonated carbons. Green Chem. With regards to the other experiments, only the trials with conditions giving the highest glucose yield were carried out in triplicates to confirm the findings. & Liimatainen, H. Preparation of cellulose nanocrystals from lignin-rich reject material for oil emulsification in an aqueous environment. Segal, L., Creely, J. J., Martin, A. E. & Conrad, C. M. An empirical method for estimating the degree of crystallinity of native cellulose using the X-ray diffractometer. Cellulose 23, 12091219 (2016). Favier, V., Chanzy, H. & Cavaill, J. Y. Polymer nanocomposites reinforced by cellulose whiskers. & Capron, I. Cellulosic nanorods of various aspect ratios for oil in water Pickering emulsions. Man, Z. et al. 6, 321330 (2011). Cellulose 21, 25672577 (2014). The yield of reducing sugars (RS) by hydrolysis of synthetic cellulose exhibiting a 3140 DP, 80% DC, and highly depolymerization-resistant fibers was 27%. Eur. 1. BlueFire Renewables (2010). VB and HZ-N were employed by the company CRB Innovations Inc. Text. 1b, under the temperature at 80 and 90 C, low yield of water-soluble sugar was obtained, due to the insufficient hydrolysis of cellulose. As the most abundant natural polymer, cellulose has been consensually considered as a renewable resource to replace fossil for sustainable production of chemicals and fuels (Huang et al. Chen, L. et al. J. Nanopart. The cellulose used as feedstock was obtained from pronghorn spring triticale. Lett. The objectives of this work are to investigate the influence of key parameters of the two-step hydrolysis process with partial neutralization on the glucose yield, and to identify the conditions resulting in the highest glucose yield. 88, 392402 (2010). Cellulose nanomaterials test methods for characterization CAN/CSA-Z5100-17 (CSA Group, 2017). ACS Sustain. For Ctec2, yield was independent of DM below 15-18% DM, while yields decreased with increasing DM above . Beck, S., Bouchard, J. ( Klemm et al., 2011, Zhu et al., 2011). This observation could be explained by the fact that ammonia is a weak base and thus, more ammonia was needed to produce the required number of moles of hydroxide ions to get the same partial neutralization effect as with sodium hydroxide. Rev. Res. J. Appl. & Dawson-Andoh, B. E. Sono-chemical preparation of cellulose nanocrystals from lignocellulose derived materials. Polym. An overview of second generation biofuel technologies. Biomacromolecules 6, 10481054 (2005). Chem. Chem. The aim of this study was to characterize microcrystalline cellulose (MCC) isolated from Teff straw (TS) in a multi-step method that included alkaline treatment, alkaline hydrogen peroxide bleaching, and catalyzed dilute acid hydrolysis. A. Medronho, B., Romano, A., Miguel, M. G., Stigsson, L. & Lindman, B. Rationalizing cellulose (in)solubility: reviewing basic physicochemical aspects and role of hydrophobic interactions. US Patent 5629055A (1994). Eng. However, the curve obtained with the 20 wt% NaOH solution reached a higher maximum glucose yield at higher H+/OH molar ratios. https://doi.org/10.1038/s41578-020-00239-y, DOI: https://doi.org/10.1038/s41578-020-00239-y. 1. Increase of impregnation temperature to 100 and 110 C efficiently promoted water-soluble sugar yield. & Laborie, M. P. Ionic liquid-mediated technology to produce cellulose nanocrystals directly from wood. Main parameters of the hydrolysis process and range of values investigated. 2019; Mu et . New Pickering emulsions stabilized by bacterial cellulose nanocrystals. Ind. Prasad Reddy, J. I., and Palkovits, R. (2016). The extracted feedstock was then subjected to a first steam treatment carried out at 200C for 2 min. Carbohydr. & Putaux, J. L. Transmission electron microscopy of cellulose. The glucose yield was 30% when using an H+/NH3 molar ratio of 1 (low) and a mass ratio of sulfuric acid/dry cellulose of 12. Ind. 29, 3140 (2014). Macromolecules 48, 88448857 (2015). Method for vapor phase pulping with alcohol and sulfur dioxide. Beauchet, R., Berberi, V., Corcos, P. O., Guimont-Montpetit, G., Dion, Y., Eudes, F., et al. Eng. Prod. & Huang, H. Utilization of pineapple peel for production of nanocellulose and film application. US Patent 20170260298A1 (2017). The highest cellulose-to-glucose conversion was around 90% for a post-hydrolysis time of 90 min and temperature of 100C. and an NSERC Alexander Graham Bell Canada Graduate Scholarship to O.M.V. Kedzior, S. A., Zoppe, J. O., Berry, R. M. & Cranston, E. D. Recent advances and an industrial perspective of cellulose nanocrystal functionalization through polymer grafting. Biomacromolecules 12, 13631369 (2011). Fermentation of C6 carbohydrates from triticale straw hemicellulosic fraction as pretreatment for xylose purification. Cao, Y., Weiss, W. J., Youngblood, J., Moon, R. & Zavattieri, P. in Production and Applications of Cellulose Nanomaterial (eds Postek, M. T., Moon, R. J., Rudie, A. W. & Bilodeau, M. Ind. Ngo, T., Danumah, C. & Ahvazi, B. in Nanocellulose and Sustainability (ed. Angew. Cellulose 25, 293304 (2018). B 119, 162165 (2014). Langmuir 26, 1345013456 (2010). Polym. Small 7, 302305 (2011). Control. Figure 7. Int. Polym. Preparation, morphology and structure of cellulose nanocrystals from bamboo fibers. Sci. Zhou, Y., Saito, T., Bergstrm, L. & Isogai, A. Acid-free preparation of cellulose nanocrystals by TEMPO oxidation and subsequent cavitation. 4, 26322643 (2016). Sheltami, R. M., Abdullah, I., Ahmad, I., Dufresne, A. doi: 10.1016/j.polymdegradstab.2012.01.010, Keywords: cellulose hydrolysis, sulfuric acid, glucose, partial neutralization, triticale, Citation: Kong-Win Chang J, Duret X, Berberi V, Zahedi-Niaki H and Lavoie J-M (2018) Two-Step Thermochemical Cellulose Hydrolysis With Partial Neutralization for Glucose Production. Effect of post-hydrolysis time and H+/OH molar ratio of 1.7(), 2.0 (), 2.3(), on glucose yield with a pre-treatment of 2 h at 30C, 72 wt% H2SO4 and mass ratio of H2SO4/dry cellulose of 12, partial neutralization with 32.8 wt% NaOH solution, and post-hydrolysis at 121C. From vapour to gas: optimising cellulose degradation with gaseous HCl. 7, 990996 (2018). Wang, Q., Zhao, X. Retsina, T., Pylkkanen, V. & van Heiningen, A. Crop. Langmuir 25, 497502 (2009). First, it can be observed that the standard deviation among the triplicates at the most efficient conditions (giving highest glucose yields) is very small, such that the associated error bars are hardly distinguishable in Figure 8. US Patent 20100151159A1 (2009). Lu, Q. et al. Hirai, A., Inui, O., Horii, F. & Tsuji, M. Phase separation behavior in aqueous suspensions of bacterial cellulose nanocrystals prepared by sulfuric acid treatment. Extraction and characterization of nanocellulose structures from raw cotton linter. WO2006007691 A1. 4, 907915 (2014). ACS Sustain. & Zhou, Q. Hydrophobic cellulose nanocrystals modified with quaternary ammonium salts. Chem. This is why partial neutralization of the sulfuric acid by adding a base was considered as an efficient method to minimize the amount of water to be added for dilution. Sci. Beverly, MA: Scrivener Publishing LLC. Cellulose is a long-chain polysaccharide compound with a high crystallization area and is connected by d-glucose and -1,4 glycosidic bonds. is grateful for financial support and recognition through the Early Researcher awards from the Ontario Ministry of Research and Innovation, the Canada Research Chairs programme and the University of British Columbias Presidents Excellence Chair initiative. Sci. & Lai, C. W. Preparation of high crystallinity cellulose nanocrystals (CNCs) by ionic liquid solvolysis. Carbohydr. Andrews, M. P. & Morse, T. Method for producing functionalized nanocrystalline cellulose and functionalized nanocrystalline cellulose thereby produced.
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