Abstract
Despite the many existing fibrillation processes for the production of cellulose nanofibrils (CNFs), their exact destructuration effects on fibers remain poorly understood. This work reports the use of disk refining, twin-screw extrusion (TSE), ultra-fine grinding and homogenization for CNF production, alone or in combinations. The same raw material (birch fibers) and pretreatment (enzymatic hydrolysis) were used for comparable process conditions, with a systematic measurement of the energy consumption and a calculation of the process theoretical shear rates. The modifications of cellulose fiber and nanofibril properties were assessed by morphological analysis, optical microscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD), nuclear magnetic resonance (NMR), tensile tests and multi-scale quality index analysis. The water retention value (WRV) and degree of polymerization (DP) were also measured. All processes resulted in 8–14 nm-wide CNFs as well as larger CNF bundles. Residual fiber fragments were observed after refining and TSE. The latter resulted in the most significant decrease of crystallinity index (CI), DP and mechanical properties, while CNFs produced by ultra-fine grinding and homogenization displayed the best mechanical and optical properties. These processes were then combined with a preliminary disk refining step, to assess the influence of the morphology of the initial fibers on their fibrillation efficiency. Such combinations had a negative effect for TSE and homogenization. Lower properties were obtained for these samples, compared to CNFs produced by the processes used individually. In contrast, the combination of disk refining and ultra-fine grinding was found to greatly enhance the resulting CNF properties, with a significant increase in optical transmittance. These results provide an insight on the destructuration effects of each process, and pave the way to further research on the physical phenomena at work.
Graphical abstract
The cellulose fibers destructuration effects of four mechanical fibrillation processes were evaluated in detail. The relevance or irrelevance of their combinations was assessed, the best results being obtained with processes with similar geometries.
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Acknowledgments
The authors gratefully thank the Association Nationale Recherche Technologie (ANRT) and Arjowiggins France SAS for financial and material support for the PhD thesis. LGP2 is part of the LabEx Tec 21 (Investissements d’Avenir—grant agreement #ANR-11-LABX-0030). LGP2 and CERMAV are part of Institut Carnot PolyNat (Investissements d’Avenir—grant agreement #ANR-16-CARN-0025-01). This research was made possible thanks to the facilities of the TekLiCell platform funded by Région Rhône-Alpes (ERDF: European regional development fund). The authors would like to thank Thierry Encinas (CMTC, Grenoble) for the XRD analysis, Valérie Meyer and François Cottin (CTP) for granting access to the homogenizer and homogenization handlings, the NanoBio-ICMG Platform (UAR 2607, Grenoble) for granting access to the electron microscopy and NMR facilities, Stéphanie Pradeau (CERMAV) for the NMR analyses, and Yoshiharu Nishiyama (CERMAV) for the gift of a xylan sample.
Funding
This work was supported by the Association Nationale Recherche Technologie (ANRT) and Arjowiggins France SAS. LGP2 is part of the LabEx Tec 21 (Investissements d’Avenir—grant agreement #ANR-11-LABX-0030). LGP2 and CERMAV are part of Institut Carnot PolyNat (Investissements d’Avenir—grant agreement #ANR-16-CARN-0025-01). This research was made possible thanks to the facilities of the TekLiCell platform funded by Région Rhône-Alpes (ERDF: European regional development fund).
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GB: conceptualization, investigation, methodology, writing—original draft. CG: investigation. DC: conceptualization, investigation, methodology, supervision. J-LP: investigation, methodology, resources. GD: conceptualization, supervision, funding acquisition. NB: writing—review and editing, supervision. JB: writing—review and editing, conceptualization, supervision, funding acquisition.
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Banvillet, G., Grange, C., Curtil, D. et al. Cellulose nanofibril production by the combined use of four mechanical fibrillation processes with different destructuration effects. Cellulose 30, 2123–2146 (2023). https://doi.org/10.1007/s10570-022-05016-4
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DOI: https://doi.org/10.1007/s10570-022-05016-4