Production and Evaluation of Redispersible Oven-Dried Cellulose Nanofibers

Document Type : Complete scientific research article

Authors

1 MSc, Student, Dept., of Wood Composites, Faculty of Wood and Paper Engineering, Gorgan University of Agricultural Sciences and Natural Resources

2 Gorgan University of Agricultural Sciences and Natural Resources

3 Faculty of wood and paper engineering-University of agricultural and natural resources Siences- GORGAN

10.22069/jwfst.2026.24652.2157

Abstract

Abstract

Background and objectives: Cellulose nanofibers (CNF) possess remarkable properties, including high mechanical strength, a vast specific surface area, and inherent characteristics of being bio-based, biocompatible, and biodegradable. These attributes position CNF as a material with significant potential for widespread application across diverse industries. These sectors span from construction, automotive, and electronics to air, water, and gas filtration, paper and packaging, textiles, sporting goods, medicine and biomedical engineering, the food industry, paints and coatings, aerospace, and beyond. However, existing production methods for this valuable nanomaterial have traditionally been wet-based. This results in the initial nanomaterial being produced and supplied with a very high water content, often as much as 98%. The conventional supply of CNF as a low-concentration aqueous suspension or gel presents considerable logistical challenges. These include significantly high transportation and storage costs, as well as the inherent risk of microbial degradation during storage. Consequently, drying emerges as an ideal solution to overcome these practical hurdles. Nevertheless, conventional and typical thermal drying processes often lead to an irreversible phenomenon known as hornification. This process involves the formation of permanent hydrogen bonds between the cellulose nanofibers, resulting in a loss of their redispersibility in water. To address and overcome this critical limitation, this research was undertaken with the specific aim of developing a dry, redispersible form of nanocellulose through the strategic addition of carboxymethyl cellulose (CMC).

Materials and Methods: The materials used in this research included cellulose nanofiber gel supplied by NanoNovin Polymer (knowledge-based company, Iran) and carboxymethyl cellulose (CMC) obtained from Dr. Mojalli Co. The CNF suspension or gel was mixed with varying amounts of CMC (1%, 2%, 3%, 5%, 10%, and 15%), and the mixtures were dried in a conventional oven at 70 °C. The redispersibility of the dried CNF powders in water and the physicochemical properties of the reconstituted gels were evaluated and compared with those of the never-dried CNF (control sample) through rheological measurements, FTIR spectroscopy, XRD analysis, FE-SEM imaging, and tensile testing.

Results: The results demonstrated that the presence of CMC effectively prevented irreversible hornification and enabled complete redispersion of CNFs in water. The sample containing 2% CMC (CNF2%) was identified as the optimal formulation, as its viscosity and tensile strength showed no statistically significant difference from the control sample, while FE-SEM images confirmed a uniform distribution with minimal fiber aggregation. FTIR and XRD analyses further indicated no undesirable chemical modifications or degradation of cellulose crystallinity. This research presents a practical, cost-effective, and scalable approach for producing dry cellulose nanofibers, offering a promising route to mitigate logistical challenges and facilitate the industrial utilization of this valuable nanomaterial.



Keywords: Cellulose nanofibers (CNF); Carboxymethyl cellulose (CMC); Thermal drying; Redispersion

Keywords

Main Subjects

References

1.Yousefi, H., Mashkour, M., & Yousefi, R. (2015). Direct solvent nanowelding of cellulose fibers to make all-cellulose nanocomposite. Cellulose. 22, 1189-1200.
2.Kaffashsaie, E., Yousefi, H., Nishino, T., Matsumoto, T., Mashkour, M., Madhoushi, M., & Kawaguchi, H. (2021). Direct conversion of raw wood to TEMPO-oxidized cellulose nanofibers. Carbohydrate Polymers. 262, 117938.
3.Jamali, A., Yousefi, H., Mashkour, M., & Khazaeian, A. (2024). Fabrication and evaluation of Respiratory Filter adsorbent media properties using Wood-driven Cellulose Nanofibers. Journal of Wood and Forest Science and Technology.  31(1), 121-142. [In Persian]
4.Jamali, A., Yousefi, H., Mashkour, M., Severtson, S. J., Dufresne, A., & Kumar, P. (2024). Scalable pilot production of highly efficient 5-ply respiratory masks enhanced by bacterial cellulose nanofibers. International Journal of Biological Macromolecules. p. 135354.
5.Amiri Moghaddam, Y., Yousefi, H., Tabarsa, T., Mashkour, M., Kaffashsaei, E., & Jamali, A. (2025). Green multi-density fibreboards bound with mechanically processed wood nanofibers derived from industrial residues.
Wood Material Science & Engineering. Pp: 1-11.
6.Jamali, A., Yousefi, H., Mashkour, M., Severtson, S. J., Dufresne, A., & Kumar, P. (2025). Fog Spraying Deposition of Wood Cellulose Nanofibers Containing Tert‐Butanol on Tissue Paper for Air Filtration. CLEAN–Soil, Air, Water.  53(12), e70059.
7.Sungsinchai, S., Niamnuy, C., Wattanapan, P., Charoenchaitrakool, M., & Devahastin, S. (2022). Spray drying of non-chemically prepared nanofibrillated cellulose: Improving water redispersibility of the dried product. International Journal of Biological Macromolecules.  207, 434-442.
8.Butchosa, N., & Zhou, Q. (2014).
Water redispersible cellulose nanofibrils adsorbed with carboxymethyl cellulose. Cellulose. 21:, 4349-4358.
9.Liimatainen, H., Haavisto, S., Haapala, A., & Niinimäki, J. (2009). Influence of adsorbed and dissolved carboxymethyl cellulose on fiber suspansion dispersing, dewaterability, and fines retention. BioResources. 4(1).
10.Lowys, M. P., Desbrieres, J., & Rinaudo, M. (2001). Rheological characterization of cellulosic microfibril suspensions. Role of polymeric additives. Food Hydrocolloids.
15(1), 25-32.
11.Hu, L., Xu, W., Gustafsson, J., Koppolu, R., Wang, Q., Rosqvist, E., Sundberg, A., Peltonen, J., Willför, S., & Toivakka, M. (2022). Water-soluble polysaccharides promoting production of redispersible nanocellulose. Carbohydrate Polymers.  297, 119976.
12.Huntington, B., Pitcher, M. L., & Sheikhi, A. (2022). Nanoengineering the redispersibility of cellulose nanocrystals. Biomacromolecules. 24(1), 43-56.
13.Nordenström, M., Kaldéus, T., Erlandsson, J., Pettersson, T., Malmstrom, E., & Wågberg, L. (2021). Redispersion strategies for dried cellulose nanofibrils. ACS Sustainable Chemistry & Engineering. 9(33), 11003-11010.
14.Priya, G., Narendrakumar, U., & Manjubala, I. (2019). Thermal behavior of carboxymethyl cellulose in the presence of polycarboxylic acid crosslinkers. Journal of Thermal Analysis and Calorimetry. 138, 89-95.
15.Nongnual, T., Butprom, N., Boonsang, S., & Kaewpirom, S. (2024). Citric acid crosslinked carboxymethyl cellulose edible films: A case study on preserving freshness in bananas. International Journal of Biological Macromolecules.  267, 131135.
16.Albornoz-Palma, G., Ching, D., Valerio, O., Mendonça, R. T., & Pereira, M. (2020). Effect of lignin and hemicellulose on the properties of lignocellulose nanofibril suspensions. Cellulose. 27(18), 10631-10647.
17.Sorvari, A., Saarinen, T., Haavisto, S., Salmela, J., Vuoriluoto, M., & Seppälä, J. (2014). Modifying the flocculation of microfibrillated cellulose suspensions by soluble polysaccharides under conditions unfavorable to adsorption. Carbohydrate polymers. 106, 283-292.
18.Giovanini de Lima, R., Nascimento,
D. M. e. d., Portugal, R. V., & Bernardes, J. S. (2025). Improving Redispersibility of Nanocellulose via Interaction with Arginine. ACS Sustainable Chemistry & Engineering.
19.Segal, L., Creely, J. J., Martin Jr, A., & Conrad, C. (1959). An empirical method for estimating the degree of crystallinity of native cellulose using the X-ray diffractometer. Textile research journal.  29(10):, 786-794.
20.Fackler, K., Stevanic, J. S., Ters, T., Hinterstoisser, B., Schwanninger, M., & Salmén, L. (2011). FT-IR imaging microscopy to localise and characterise simultaneous and selective white-rot decay within spruce wood cells.
21.Xu, F., Yu, J., Tesso, T., Dowell, F., & Wang, D. (2013). Qualitative and quantitative analysis of lignocellulosic biomass using infrared techniques: a mini-review. Applied energy. 104, 801-809.
22.Hospodarova, V., Singovszka, E., & Stevulova, N. (2018). Characterization of cellulosic fibers by FTIR spectroscopy for their further implementation to building materials. American journal of analytical chemistry. 9(6), 303-310.
23.Paladini, G., Venuti, V., Crupi, V., Majolino, D., Fiorati, A., & Punta, C. (2021). 2D correlation spectroscopy (2DCoS) analysis of temperature-dependent FTIR-ATR spectra in branched polyethyleneimine/TEMPO-oxidized cellulose nano-fiber xerogels. Polymers. 13(4), 528.
24.Hua, K., Rocha, I., Zhang, P., Gustafsson, S., Ning, Y., Strømme, M., Mihranyan, A., & Ferraz, N. (2016). Transition from bioinert to bioactive material by tailoring the biological cell response to carboxylated nanocellulose. Biomacromolecules. 17(3), 1224-1233.
25.Paladini, G., Venuti, V., Crupi, V., Majolino, D., Fiorati, A., & Punta, C. (2020). FTIR-ATR analysis of the H-bond network of water in branched polyethyleneimine/ TEMPO-oxidized cellulose nano-fiber xerogels. Cellulose.  27, 8605-8618.
26.Butchosa, N., & Zhou, Q. (2014).
Water redispersible cellulose nanofibrils adsorbed with carboxymethyl cellulose. Cellulose. 21(6), 4349-4358.
27.Naderi, A., Lindström, T., Sundström, J., & Flodberg, G. (2015). Can redispersible low-charged nanofibrillated cellulose be produced by the addition of carboxymethyl cellulose? Nordic Pulp & Paper Research Journal. 30(4), 568-577.
28.Xu, Y., Xu, Y., Chen, H., Gao, M., Yue, X., & Ni, Y. (2022). Redispersion of dried plant nanocellulose: A review. Carbohydrate Polymers. 294, 119830.
Journal of Wood and Forest Science and Technology
Volume 33, Issue 2
July 2026
Pages 143-161

Files

Share

How to cite

Statistics