Abstract
Cellulose nanocrystals were prepared from cotton fibers by a two-stage method involving ionic liquid swelling treatment followed by hydrolysis under mild acid conditions. Controlled swelling of cellulosic fibers was achieved in 1-butyl-3-methylimidazolium chloride ([BMIM]Cl) at 80 °C, while avoiding extensive dissolution of crystalline regions. Since the accessibility of the substrate was considerably enhanced, the hydrolysis occurred even under mild conditions, using up to 60 times less sulfuric acid than the traditional extraction methods based on concentrated sulfuric acid. The effects of process parameters on nanoparticle morphology, composition and stability were investigated. The individual rod-like nanocrystals, observed under field emission gun scanning electron microscopy, exhibited an average diameter of around 20 nm and a length ranging from 150 to 350 nm. According to X-ray photoelectron spectroscopy and thermogravimetric analysis, the surface of the so-extracted nanoparticles proved to be deprived of contaminating sulfate groups leading to significantly higher thermal stability with respect to cellulose nanocrystals extracted by traditional method in concentrated sulfuric acid.
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Acknowledgments
This research was supported by the European Union and Wallonia with the European Funds for Regional Development FEDER 2007-2013. The authors would also like to acknowledge Marie-Hélène Huguet, Youssef Habibi, Aline Roobroeck, Alice Belfiore, Yoann Paint and Olivier Talon for their technological contribution. MATERIA NOVA and CIRMAP thank the Belgian Federal Government Office Policy of Science (BELSPO) for its support in the frame of the PAI-6/27. J.-M. Raquez is “chercheur qualifié” by the F.R.S.-FNRS, Belgium.
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Lazko, J., Sénéchal, T., Landercy, N. et al. Well defined thermostable cellulose nanocrystals via two-step ionic liquid swelling-hydrolysis extraction. Cellulose 21, 4195–4207 (2014). https://doi.org/10.1007/s10570-014-0417-x
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DOI: https://doi.org/10.1007/s10570-014-0417-x