Abstract
The aim of this study was to determine the effects of hydrothermal treatment of microfibrillated cellulose (MFC) on its gel stability, water retention and rheological behavior. MFC gel was prepared by fibrillating endoglucanase pre-treated, never-dried dissolving pulp. The MFC gel samples were then exposed in a static chamber for different times at different temperatures. At temperatures of 120–150 °C, the viscosity profile of the gels was not significantly changed and a characteristic series of 3 successive regimes in the course of increasing shear rate, showing different behavior was revealed. The amount of water released by the samples under pressure, on the other hand, was notably increased after hydrothermal treatment. After further exposure to prolonged treatment times (24 h) and higher temperature (180 °C), a significant decrease in viscosity and shear modulus was observed. Analysis of filtrates revealed the formation of cello-oligosaccharides, glucose and HMF and a decrease in surface tension indicating peeling and molecular degradation of the sample matrice. The microfibralled cellulose sample decomposition and gel network structure breakdown on a molecular level is discussed.
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References
Agoda-Tandjawa G, Durand S, Berot S, Blassel C, Gaillard C, Garnier C, Doublier JL (2010) Rheological characterization of microfibrillated cellulose suspensions after freezing. Carbohydr Polym 80(3):677–686. https://doi.org/10.1016/j.carbpol.2009.11.045
Álvarez E, Vázquez G, Sánchez-Vilas M, Sanjurjo B, Navaza JM (1997) Surface tension of organic acids + water binary mixtures from 20 °C to 50 °C. J Chem Eng Data 42(5):957–960. https://doi.org/10.1021/je970025m
Atalla RH, Ellis JD, Schroeder LR (1984) Some effects of elevated temperatures on the structure of cellulose and its transformation. J Wood Chem Technol 4(4):465–482. https://doi.org/10.1080/02773818408070662
Borrega M, Sixta H (2013) Purification of cellulosic pulp by hot water extraction. Cellulose 20(6):2803–2812. https://doi.org/10.1007/s10570-013-0086-1
Davidson GF (1943) The rate of change in the properties of cotton cellulose under the prolonged action of acids. J Text Inst Trans 34(10):87–96. https://doi.org/10.1080/19447024308659271
Eyholzer C, Bordeanu N, Lopez-Suevos F, Rentsch D, Zimmermann T, Oksman K (2010) Preparation and characterization of water-redispersible nanofibrillated cellulose in powder form. Cellulose 17(1):19–30. https://doi.org/10.1007/s10570-009-9372-3
Fall AB, Lindström SB, Sundman O, Ödberg L, Wågberg L (2011) Colloidal stability of aqueous nanofibrillated cellulose dispersions. Langmuir 27(18):11332–11338. https://doi.org/10.1021/la201947x
Gehlen MH (2010) Kinetics of autocatalytic acid hydrolysis of cellulose with crystalline and amorphous fractions. Cellulose 17(2):245–252. https://doi.org/10.1007/s10570-009-9385-y
Grignon J, Scallan AM (1980) Effect of pH and neutral salts upon the swelling of cellulose gels. J Appl Polym Sci 25(12):2829–2843. https://doi.org/10.1002/app.1980.070251215
Håkansson H, Ahlgren P (2005) Acid hydrolysis of some industrial pulps: effect of hydrolysis conditions and raw material. Cellulose 12(2):177–183. https://doi.org/10.1007/s10570-004-1038-6
Heggset EB, Chinga-Carrasco G, Syverud K (2017) Temperature stability of nanocellulose dispersions. Carbohydr Polym 157:114–121. https://doi.org/10.1016/j.carbpol.2016.09.077
Helmerius J, Vinblad von Walter J, Rova U, Berglund KA, Hodge DB (2010) Impact of hemicellulose pre-extraction for bioconversion on birch kraft pulp properties. Bioresour Technol 101:5996–6005. https://doi.org/10.1016/j.biortech.2010.03.029
Hiltunen S, Sirén H, Heiskanen I, Backfolk K (2016) Capillary electrophoretic profiling of wood-based oligosaccharides. Cellulose 23(5):3331–3340. https://doi.org/10.1007/s10570-016-1011-1
Iotti M, Gregersen ØW, Moe S, Lenes M (2011) Rheological studies of microfibrillar cellulose water dispersions. J Polym Environ 19(1):137–145. https://doi.org/10.1007/s10924-010-0248-2
Johnson RK, Zink-Sharp A, Renneckar SH, Glasser WG (2009) A new bio-based nanocomposite: fibrillated tempo-oxidized celluloses in hydroxypropylcellulose matrix. Cellulose 16(2):227–238. https://doi.org/10.1007/s10570-008-9269-6
Karppinen A, Saarinen T, Salmela J, Laukkanen A, Nuopponen M, Seppälä J (2012) Flocculation of microfibrillated cellulose in shear flow. Cellulose 19(6):1807–1819. https://doi.org/10.1007/s10570-012-9766-5
Lahtinen P, Liukkonen S, Pere J, Sneck A, Kangas H (2014) A comparative study of fibrillated fibers from different mechanical and chemical pulps. BioResources 9:2115–2127
Lowys MP, Desbrières J, Rinaudo M (2001) Rheological characterization of cellulosic microfibril suspensions. Role of polymeric additives. Food Hydrocolloids 15(1):25–32. https://doi.org/10.1016/S0268-005X(00)00046-1
Maloney TC (2015) Network swelling of TEMPO-oxidized nanocellulose. Holzforschung 69(2):207–213
Naderi A, Lindström T (2016) A comparative study of the rheological properties of three different nanofibrillated cellulose systems. Nordic Pulp Paper Res J 31(3):354–363
Naderi A, Lindström T, Erlandsson J, Sundström J, Flodberg G (2016) A comparative study of the properties of three nano-fibrillated cellulose systems that have been produced at about the same energy consumption levels in the mechanical delamination step. Nordic Pulp Paper Res J 31(3):364–371
Nguyen H, Nikolakis V, Vlachos DG (2016) Mechanistic insights into Lewis acid metal salt-catalyzed glucose chemistry in aqueous solution. ACS Catal 6(3):1497–1504. https://doi.org/10.1021/acscatal.5b02698
Notley SM (2008) Effect of introduced charge in cellulose gels on surface interactions and the adsorption of highly charged cationic polyelectrolytes. Phys Chem Chem Phys 10:1819–1825. https://doi.org/10.1039/B718543J
Oefner PJ, Lanziner AH, Bonn G, Bobleter O (1992) Quantitative studies on furfural and organic acid formation during hydrothermal, acidic and alkaline degradation of d-xylose. Monatshefte für Chemie Chem Mon 123(6):547–556. https://doi.org/10.1007/BF00816848
Olszewska A, Eronen P, Johansson LS, Malho JM, Ankerfors M, Lindström T, Ruokolainen J, Laine J, Österberg M (2011) The behaviour of cationic nanofibrillar cellulose in aqueous media. Cellulose 18(5):1213–1226. https://doi.org/10.1007/s10570-011-9577-0
Örså F, Holmbom B, Thornton J (1997) Dissolution and dispersion of spruce wood components into hot water. Wood Sci Technol 31(4):279–290. https://doi.org/10.1007/BF00702615
Pääkkö M, Ankerfors M, Kosonen H, Nykänen A, Ahola S, Österberg M, Ruokolainen J, Laine J, Larsson PT, Ikkala O, Lindström T (2007) Enzymatic hydrolysis combined with mechanical shearing and high-pressure homogenization for nanoscale cellulose fibrils and strong gels. Biomacromolecules 8(6):1934–1941. https://doi.org/10.1021/bm061215p
Pääkkönen T, Dimic-Misic K, Orelma H, Pönni R, Vuorinen T, Maloney T (2016) Effect of xylan in hardwood pulp on the reaction rate of TEMPO-mediated oxidation and the rheology of the final nanofibrillated cellulose gel. Cellulose 23(1):277–293. https://doi.org/10.1007/s10570-015-0824-7
Palme A, Theliander H, Brelid H (2016) Acid hydrolysis of cellulosic fibres: comparison of bleached kraft pulp, dissolving pulps and cotton textile cellulose. Carbohydr Polym 136:1281–1287. https://doi.org/10.1016/j.carbpol.2015.10.015
Peng L, Lin L, Zhang J, Zhuang J, Zhang B, Gong Y (2010) Catalytic conversion of cellulose to levulinic acid by metal chlorides. Molecules 15(8):5258–5272. https://doi.org/10.3390/molecules15085258
Potvin J, Sorlien E, Hegner J, DeBoef B, Lucht BL (2011) Effect of NaCl on the conversion of cellulose to glucose and levulinic acid via solid supported acid catalysis. Tetrahedron Lett 52(44):5891–5893. https://doi.org/10.1016/j.tetlet.2011.09.013
Quiévy N, Jacquet N, Sclavons M, Deroanne C, Paquot M, Devaux J (2010) Influence of homogenization and drying on the thermal stability of microfibrillated cellulose. Polym Degrad Stab 95(3):306–314. https://doi.org/10.1016/j.polymdegradstab.2009.11.020
Rovio S, Simolin H, Koljonen K, Sirén H (2008) Determination of monosaccharide composition in plant fiber materials by capillary zone electrophoresis. J Chromatogr A 1185(1):139–144. https://doi.org/10.1016/j.chroma.2008.01.031
Sattler C, Labbé N, Harper D, Elder T, Rials T (2008) Effects of hot water extraction on physical and chemical characteristics of oriented strand board (OSB) wood flakes. Clean Soil Air Water 36(8):674–681. https://doi.org/10.1002/clen.200800051
Shafiei-Sabet S, Martinez M, Olson J (2016) Shear rheology of micro-fibrillar cellulose aqueous suspensions. Cellulose 23(5):2943–2953. https://doi.org/10.1007/s10570-016-1040-9
Shatkin JA, Wegner TH, Bilek E, Cowie J (2014) Market projections of cellulose nanomaterial-enabled products—part 1: applications. Tappi J 13(5):9–16
Silveira RL, Stoyanov SR, Kovalenko A, Skaf MS (2016) Cellulose aggregation under hydrothermal pretreatment conditions. Biomacromolecules 17(8):2582–2590. https://doi.org/10.1021/acs.biomac.6b00603
Song T, Pranovich A, Holmbom B (2012) Hot-water extraction of ground spruce wood of different particle size. BioResources 7(3):4214–4225
Taheri H, Samyn P (2016) Effect of homogenization (microfluidization) process parameters in mechanical production of micro- and nanofibrillated cellulose on its rheological and morphological properties. Cellulose 23(2):1221–1238. https://doi.org/10.1007/s10570-016-0866-5
Tanaka R, Saito T, Hondo H, Isogai A (2015) Influence of flexibility and dimensions of nanocelluloses on the flow properties of their aqueous dispersions. Biomacromolecules 16(7):2127–2131. https://doi.org/10.1021/acs.biomac.5b00539
Tenhunen TM, Peresin MS, Penttilä PA, Pere J, Serimaa R, Tammelin T (2014) Significance of xylan on the stability and water interactions of cellulosic nanofibrils. React Funct Polym 85:157–166
Tingaut P, Zimmermann T, Lopez-Suevos F (2010) Synthesis and characterization of bionanocomposites with tunable properties from poly(lactic acid) and acetylated microfibrillated cellulose. Biomacromolecules 11(2):454–464. https://doi.org/10.1021/bm901186u
Vesterinen AH, Myllytie P, Laine J, Seppälä J (2010) The effect of water-soluble polymers on rheology of microfibrillar cellulose suspension and dynamic mechanical properties of paper sheet. J Appl Polym Sci 116(5):2990–2997. https://doi.org/10.1002/app.31832
Willför S, Sjöholm R, Laine C, Roslund M, Hemming J, Holmbom B (2003) Characterisation of water-soluble galactoglucomannans from norway spruce wood and thermomechanical pulp. Carbohydr Polym 52(2):175–187. https://doi.org/10.1016/S0144-8617(02)00288-6
Acknowledgments
Johanna Lyytikäinen (M.Sc) is thanked for measuring the surface tension of the filtrates. Anthony Bristow (Dr.) is thanked for linguistic revision of the manuscript. Stora Enso Oyj is thanked for financial support.
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Hiltunen, S., Heiskanen, I. & Backfolk, K. Effect of hydrothermal treatment of microfibrillated cellulose on rheological properties and formation of hydrolysis products. Cellulose 25, 4653–4662 (2018). https://doi.org/10.1007/s10570-018-1884-2
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DOI: https://doi.org/10.1007/s10570-018-1884-2