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Studies on the conversion of cellulose into biofuels and chemicals have been one of the most intensive pursuits worldwide [1], [2], [3], [4].Among various cellulose conversion processes, hydrolysis of cellulose to glucose is virtually an essential step in most practical cellulosic chemical or biofuel production [5].However, cellulose is a highly crystalline polymer of d . Part B Polym. Kaur, B., Gur, I. S. & Bhatnagar, H. L. Thermal degradation studies of cellulose phosphates and cellulose thiophosphates. Prod. Opin. Iranmahboob et al. Concentrated Acid Hydrolysis - an overview | ScienceDirect Topics Based on widely published work carried out since the 90's at the University of Sherbrooke, lignocellulosic biomass is first separated into four fractions, namely hemicelluloses, cellulose, lignin, and extractives (if desired) (Lavoie et al., 2011). Open Access articles citing this article. Ethanol production from wood via concentrated acid hydrolysis, chromatographic separation, and fermentation. Frka-Petesic, B., Sugiyama, J., Kimura, S., Chanzy, H. & Maret, G. Negative diamagnetic anisotropy and birefringence of cellulose nanocrystals. Fortunati, E. et al. Increased enzyme binding to substrate is not necessary for more - PNAS Continuous metal-organic framework biomineralization on cellulose nanocrystals: extrusion of functional composite filaments. Chem. UMaine https://umaine.edu/pdc/nanocellulose/ (2020). Ind. Rnby, B. G. The colloidal properties of cellulose micelles. & Hu, T. Q. Structure-process-yield interrelations in nanocrystalline cellulose extraction. Correlating cellulose nanocrystal particle size and surface area. Rev. The solution was then diluted to 4 wt% sulfuric acid by adding 84 mL of water, before being placed in an autoclave at 121C for 1 h. After 20 min of cooling and neutralization to pH 56, the mixture was filtered (0.2 m) and the glucose concentration was measured by high performance liquid chromatography (HPLC) (ASTM International, 2007). 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. Scand. Chem. Surface chemistry, morphological analysis and properties of cellulose nanocrystals with gradiented sulfation degrees. 7, 62876294 (2019). The glucose yield vs. H+/OH molar ratio, obtained with both the 20 and 40 wt% NaOH solutions, was found to have the same pattern. Clausen, E. C., and Gaddy, J. L. (1993). 131, 40525 (2014). A novel approach for the preparation of nanocrystalline cellulose by using phosphotungstic acid. Bionanocomposites based on poly(-caprolactone)-grafted cellulose nanocrystals by ring-opening polymerization. Carbohydr. Solutions of 20 wt% NaOH and 40 wt% NaOH were compared by subjecting the cellulose to a 2 h pre-treatment at 30C and 72 wt% H2SO4 for a mass ratio of H2SO4/dry cellulose of 12, followed by a post-hydrolysis at 121C for 10 min. & Danumah, C. Analysis of cellulose nanocrystal rod lengths by dynamic light scattering and electron microscopy. 157, 114121 (2017). Marett, J., Aning, A. Cellulose nanocrystals from pineapple leaf, a new approach for the reuse of this agro-waste. Res. Mater. The hydrolysis is conducted at 100 C for 30-120 min and the corresponding yield of sugar is 78-82%. & Vrhegyi, G. A round-robin study of cellulose pyrolysis kinetics by thermogravimetry. Bioresour. Effect of source on the properties and behavior of cellulose nanocrystal suspensions. (1970). 88, 772779 (2012). Cellulose nanocrystal-based materials: From liquid crystal self-assembly and glass formation to multifunctional thin films. Prod. Polym. 33, 6366 (2011). Environ. Biotechnol. Chromatographic recovery of Monosaccharides for the production of bioethanol from wood. US Patent 20100151159A1 (2009). Carbohydr. Biomacromolecules 4, 10131017 (2003). Biophys. Int. ASTM International (2007). Phil. 87, 689696. Results Chemical composition analysis performed on samples obtained after different pretreatment conditions showed that up to 96% and 85% of hemicellulose and lignin fractions, respectively, were removed by this two-step method when sodium hydroxide concentrations of 1% (m/v) or higher were used. Acid hydrolysis of cellulose is a classic way to break down cellulose into glucose and can be done using either dilute acid or concentrated acid. The efficiency of the transformation was examined by gravimetry, atomic force microscopy and transmission electron microscopy. J. Ind. Hosseinidoust, Z., Alam, M. N., Sim, G., Tufenkji, N. & Van De Ven, T. G. M. Cellulose nanocrystals with tunable surface charge for nanomedicine. Mater. Vanderfleet, O.M., Cranston, E.D. Cellulose comprisesbetween 35 and 50% of the total dry mass and consists of long chains of-anhydroglucose units linked by 1,4-glucoside bonds. & Berry, R. Iridescent solid nanocrystalline cellulose films incorporating patterns and method for their production. A 1, 39383944 (2013). Carbohydr. A. S. Subcritical water: a method for green production of cellulose nanocrystals. Heterogeneous aspects of acid hydrolysis of a-cellulose. Given the fibrous texture of the straw (non-edible part of the plant), the latter was mechanically cut to approximately 3 cm-long pieces in order to facilitate the downstream treatment. Cellulose 25, 293304 (2018). 121, 202209 (2013). Polym. Yue, Y. et al. Comparison of the properties of cellulose nanocrystals and cellulose nanofibrils isolated from bacteria, tunicate, and wood processed using acid, enzymatic, mechanical, and oxidative methods. & Zhang, L. One-pot preparation of hydrophobic cellulose nanocrystals in an ionic liquid. Mukherjee, S. M. & Woods, H. J. X-ray and electron microscope studies of the degradation of cellulose by sulphuric acid. In the most efficient case, a glucose yield reaching 100% could be achieved and this involved a swelling pre-treatment performed at 30C for 2 h, 72 wt% H2SO4 and using a mass ratio of H2SO4/dry cellulose of 36; followed by partial neutralization with 20 wt% NaOH, and an H+/OH molar ratio of 2.32.5; and post-hydrolysis at 121C for 10 min. Shafiei-Sabet, S., Hamad, W. Y. 7, 990996 (2018). Hydrolyse Thermochimique de la Cellulose et Rcupration des Acides/Bases Utiliss Dans un Contexte de Production D'thanol Cellulosique. Research and Markets https://www.researchandmarkets.com/reports/4827614/the-global-market-for-nanocellulose?utm_code=bcb85m&utm_medium=BW (2019). & Foster, E. J. (2002). The first treatment solubilizes the hemicelluloses fraction whereas the second treatment, carried out using an alkaline catalyst, allowed the solubilization of lignin (Lavoie et al., 2011). Periodate oxidation followed by NaBH4 reduction converts microfibrillated cellulose into sterically stabilized neutral cellulose nanocrystal suspensions. A., Coppick, S., Howsmon, J. Res. Angew. & Dufresne, A. Thus, an aqueous solution of sulfuric acid at 72 wt% has some similarities with an ionic liquid since it is a liquid composed exclusively of anions and cations. Biomacromolecules 11, 36523659 (2010). E1758 01 Standard Test Method for Determination of Carbohydrates in Biomass by High Performance Liquid Chromatography. Lavoie, J.-M. (2016). Prod. volume6,pages 124144 (2021)Cite this article. Technol. 101, 15701580. Cellulose 19, 11731187 (2012). Molnes, S. N., Paso, K. G., Strand, S. & Syverud, K. The effects of pH, time and temperature on the stability and viscosity of cellulose nanocrystal (CNC) dispersions: implications for use in enhanced oil recovery. from Lignocellulosic Biomass, View all J. Nanomed. 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. Van De Ven, T. G. M. & Sheikhi, A. Hairy cellulose nanocrystalloids: a novel class of nanocellulose. Influence of operating parameters on the glucose yield have been investigated. 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. 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. Despite this observation, the glucose yield under the most efficient conditions was higher with sodium hydroxide than with aqueous ammonia. Vasconcelos, N. F. et al. Nanoscale 7, 1664716657 (2015). 76, 607615 (2009). doi: 10.1016/S0960-8524(01)00212-7, Taherdazeh, M. J., and Karimi, K. (2007). Sci. & Ek, M. Esterification and hydrolysis of cellulose using oxalic acid dihydrate in a solvent-free reaction suitable for preparation of surface-functionalised cellulose nanocrystals with high yield. Hence, reducing the amount of enzyme needed or increasing the enzyme productivity in the process is a promising approach. From there on, the oligosaccharides, obtained as a result of the ionic liquefaction, are converted into monomeric sugars by a post-hydrolysis step using dilute acid. Received: 16 January 2018; Accepted: 29 March 2018; Published: 24 April 2018. 93, 112 (2016). The Erlenmeyer flask was cooled to 20C and its contents vacuum-filtered using a 1.5 m porosity glass microfiber filter (VWR brand) for medium retention particles using a Buchner funnel. Cellulose 13, 171180 (2006). Front. Beck-Candanedo, S., Roman, M. & Gray, D. Effect of conditions on the properties behavior of wood cellulose nanocrystals suspensions. Anim. Prod. The research focused on the effects of integrating nanocellulose in the solidification of metal ions into metal oxide particles or metallic electrodeposits. Sci. With these same post-hydrolysis conditions but using 29 wt% NH3(aq) for partial neutralization, the corresponding conditions giving highest glucose yields were as follows: pre-treatment at 30C with 72 wt% H2SO4 for 2 h, mass ratio of H2SO4/dry cellulose of 36, and an H+/NH3 molar ratio of 1.61.8. BlueFire Renewables (2010). Solid and dotted lines are a guide to the eye. 19, 55645567 (2017). CNCs can be used to improve the. Mater. ACS Sustain. Beck, S., Bouchard, J. The authors are also thankful to MITACS for JK-WC's and XD's salaries and to BioFulNet Canada for funding part of this work. Polym. Araki, J., Wada, M. & Kuga, S. Steric stabilization of a cellulose microcrystal suspension by poly(ethylene glycol) grafting. Google Scholar. Main parameters of the hydrolysis process and range of values investigated. Standards Council of Canada. & Rojas, O. J. Cellulose nanocrystals: chemistry, self-assembly, and applications. Cellulose 10, 299306 (2003). Angew. Habibi, Y., Chanzy, H. & Vignon, M. R. TEMPO-mediated surface oxidation of cellulose whiskers. Transition metal salt assisted dilute acid hydrolysis for - Springer Sbe, G., Ham-Pichavant, F., Ibarboure, E., Koffi, A. L. C. & Tingaut, P. Supramolecular structure characterization of cellulose II nanowhiskers produced by acid hydrolysis of cellulose I substrates. Rusli, R., Shanmuganathan, K., Rowan, S. J., Weder, C. & Eichhorn, S. J. Polym. Optimization of the process of chemical hydrolysis of cellulose to Polym. Implementing 2nd generation liquid biofuels in a fossil fuel-dominated market: making the right choices. The hydrolysate obtained from this step was analyzed to determine its glucose and 5-hydroxymethyl furfural (5-HMF, a glucose degradation product) concentration (see section Determination of Glucose and 5-HMF Concentrations) and to calculate the glucose yield from cellulose hydrolysis. Biomacromolecules 14, 12231230 (2013). As shown in Figure 3, with a mass ratio of acid/dry cellulose of 12 and a mass percentage of acid of 62 wt%, the glucose yield was 24% and increased to 85% when the mass percentage of acid reached 72 wt%. Energy 71, 7780. Tang, J., Sisler, J., Grishkewich, N. & Tam, K. C. Functionalization of cellulose nanocrystals for advanced applications. The mixture from this second steam treatment was filtered and the solid fraction obtained was used as cellulose feed in this research work. Polym. Silvrio, H. A., Flauzino Neto, W. P., Dantas, N. O. Nanotechnol. Nanoscale 6, 77647779 (2014). Crop. Wijaya, C. J. et al. Sci. Cudjoe, E. et al. Faraday Soc. Chem. Brinkmann, A. et al. (2008). Arkenol, A. & Torget, R. W. in Applied Biochemistry and Biotechnology (eds Davison, B. H., Lee, J. W., Finkelstein, M. & McMillan, J. D.) 505514 (Humana Press, 2003). The effect of NaOH concentration on glucose yield was investigated and the results are given in Figure 7. Flowability, binding and release property of "self-lubricating & Kargarzadeh, H. Extraction of cellulose nanocrystals from mengkuang leaves (Pandanus tectorius). 191, 205215 (2018). ACS Sustain. Chem. Their pre-treatment step was done at a mass ratio of H2SO4/dry wood chips of 2.5 and 80 wt% H2SO4, and distilled boiling water was added to the so-formed paste to achieve 26 wt% H2SO4. Vanderfleet, O. M. et al. React. The University of Maine. & Ni, Y. Preparation and characterization of thermally stable cellulose nanocrystals via a sustainable approach of FeCl3-catalyzed formic acid hydrolysis. Langmuir 31, 55965602 (2015). Crop. Macromol. Effect of H+/OH ratio on glucose yield with NaOH concentration of 20 wt% () and 40 wt% () with a pre-treatment at 30C, 72 wt% H2SO4 for 2 h, mass ratio of H2SO4/dry cellulose of 12, and post-hydrolysis for 10 min at 121C. Cellulose enzymatic hydrolysis is generally preferred and shows distinct advantages over acid-catalyzed hydrolysis methods (higher hydrolysis yields, mild process conditions, few hazardous and waste disposal problems, low cost utilities which require nonexpensive corrosion-resistant reactors) ( Zhang and Lynd, 2004, Pan et al., 2005, Li and Zhao. Available online at: http://bfreinc.com/2015/02/the-export-import-bank-of-china-renews-letter-of-intent-to-bluefire-renewables-for-fulton-project-due-diligence-continues-to-reach-a-financial-closing (accessed September 22, 2017). US Patent 8030039B1 (2011). The use, distribution or reproduction in other forums is permitted, provided the original author(s) and the copyright owner are credited and that the original publication in this journal is cited, in accordance with accepted academic practice. Cryst. Preparation and characterization of functionalized cellulose nanocrystals. Cellulose 23, 35553567 (2016). Sirvi, J. Polym. Polym. React. 3, 28392846 (2015). An overview of second generation biofuel technologies. These steps are depicted in Figure 2. & Yang, R. Tailored and integrated production of carboxylated cellulose nanocrystals (CNC) with nanofibrils (CNF) through maleic acid hydrolysis. Polym. Cellulose 23, 23892407 (2016). Tan, X. Y., Abd Hamid, S. B. Variations of this method have the potential of being economically attractive if a minimum acid/cellulose ratio is used for the ionic liquefaction step and a high glucose yield is obtained after post-hydrolysis. 107, 505514. & Pasquini, D. 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ACS Appl. Polym. Eng. . Henrique, M. A., Silvrio, H. A., Flauzino Neto, W. P. & Pasquini, D. Valorization of an agro-industrial waste, mango seed, by the extraction and characterization of its cellulose nanocrystals. Dong, S., Bortner, M. J. Microcrystalline-cellulose hydrolysis with concentrated sulphuric acid. WO2006007691 A1. Cellulose 21, 33473359 (2014). 7 Articles, This article is part of the Research Topic, http://www.arkenol.com/Arkenol%20Inc/tech01.html, http://bfreinc.com/2015/02/the-export-import-bank-of-china-renews-letter-of-intent-to-bluefire-renewables-for-fulton-project-due-diligence-continues-to-reach-a-financial-closing, Creative Commons Attribution License (CC BY). Cellulose 22, 17431752 (2015). doi: 10.1016/j.biortech.2013.03.104, PubMed Abstract | CrossRef Full Text | Google Scholar, Pulidindi, I. N., Kimchi, B. Eng. Copyright 2018 Kong-Win Chang, Duret, Berberi, Zahedi-Niaki and Lavoie. Chem. Battista, O. Google Scholar. This difference in terms of water added together with the base also explains the observations reported in section Influence of Acid/Base Molar Ratio, namely glucose yield under most efficient conditions being higher with 20 wt% NaOH than with 29 wt% NH3. Sugiyama, J., Vuong, R. & Chanzy, H. Electron diffraction study on the two crystalline phases occurring in native cellulose from an algal cell wall. Schematic diagram of the two-step hydrolysis process used to convert triticale cellulose to second generation sugars. Polym. Moreover, 5-HMF was detected in the hydrolysates but its concentration was below the lower limit of quantification of the HPLC. Kovacs, T. et al. Sodium periodate oxidation of cellulose nanocrystal and its application as a paper wet strength additive. Critical discussion of light scattering and microscopy techniques for CNC particle sizing. Curr. The other authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest. contracts here. Crop. 87, 564573 (2012). Dong, X. M., Revol, J.-F. & Gray, D. G. Effect of microcrystallite preparation conditions on the formation of colloid crystals of cellulose. Additional requirements include recovering and recycling the used ions, and conditioning the final glucose solution for subsequent fermentation using established microbial systems. Langmuir 25, 497502 (2009). Bacterial cellulose nanocrystals produced under different hydrolysis conditions: Properties and morphological features. Lemke, C. H., Dong, R. Y., Michal, C. A. The measured mass difference with respect to the initial mass of humid cellulose was calculated as being the percentage humidity of the cellulose. 76, 9499 (2009). Carbohydr. Control. Firstly, the cellulose was isolated as highly crystalline ca. Polym. 8, 71827191 (2020). 42, 480488 (2013). CNCs can be used to improve the performance of a large range of materials such as emulsions and foams, biomedical devices, electronics and sensors, high-viscosity fluids and polymer composites. Rev. Moreover, this hydrolysis process is attractive from an industrial point of view since it can use cellulose as obtained from the fractionation method (6065% humid), involves smaller volumes, and produces hydrolysates with a higher glucose concentration. Collectively, these results demonstrate that mechanical pretreatment followed by enzymatic hydrolysis under specific conditions is a suitable method to produce nanocellulose with a high yield and tunable properties such as purity, rod-like or spherical forms, high thermal stability, and high crystallinity. The individual effect of seven key parameters on the glucose yield of a two-step cellulose hydrolysis process with partial neutralization was studied in this work and the obtained results enabled identifying the conditions giving the highest glucose yield. 109, 38043810 (2008). & Renneckar, S. Nanocellulose life cycle assessment. These parameters and their range of values are given in Table 1. In addition, the potential of the proposed enzyme-mediated hydrolysis process to produce nanocelluloses with different morphologies at high yields was evaluated by investigating the effects of different enzyme types (endoglucanases, xylanases, and cellulases), composition ratio, and loadings on the yield and properties of cellulose . J. & Capron, I. 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. The global market for nanocellulose. Leung, A. C. W. et al. 53, 98429860 (2018). J. Extraction and characterization of nanocellulose structures from raw cotton linter. Polym. Figure 3. 29, 1701469 (2017). Hamelinck, C. N., Hooijdonk, G., and van Faaij, A. P. (2005). & Dorgan, J. R. Single-step method for the isolation and surface functionalization of cellulosic nanowhiskers. J. Mol. Cellulose is a linear polymer of D-anhydroglucopyranose monomers connected by -1,4-glycosidic bonds (Zhang et al., 2012) and its degree of polymerization varies typically between 2,000 to 27,000 glucan units, depending on the type of plant (Taherdazeh and Karimi, 2007). Cellulose 24, 44794491 (2017). Aggregation behavior of aqueous cellulose nanocrystals: the effect of inorganic salts. Chem. Part 2: technical and practical aspects. Flauzino Neto, W. P. et al. Thus, to get a high yield of glucose during post-hydrolysis, it is important to take into account not only the mass percentage of acid but also the quantity of water added during the partial neutralization step since the latter was shown to have a strong effect on the efficiency of post-hydrolysis. Although their process used less acid for the pre-treatment, it required dried feedstock and a much longer post-hydrolysis time than the process used in the present work. Zhou, Y., Saito, T., Bergstrm, L. & Isogai, A. Acid-free preparation of cellulose nanocrystals by TEMPO oxidation and subsequent cavitation. From vapour to gas: optimising cellulose degradation with gaseous HCl. Brnsted acidic ionic liquids for cellulose hydrolysis in an aqueous 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.
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