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Cellulose solubility in ionic liquids and regeneration in water and hydrogen peroxide solution: a comparative examination of morphology and physicochemical properties

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Abstract

The main objective of this work is to present a comprehensive analysis of the morphology, topography, and thermal behavior of modified cellulose as a function of solvation temperature, ionic liquid type, and regeneration agent. Avicel microcrystalline cellulose was dissolved at two temperatures (73 °C and 100 °C) in two competing imidazolium-based ionic liquids (1-ethyl-3-methylimidazolium acetate and 1-ethyl-3-methylimidazolium bromide). Aliquots of each solvent-polymer mixture were then washed and regenerated in competing baths (D.I. water and 25% hydrogen peroxide solution). A comparative analysis of the work is that the solvation temperature and ionic liquid counterion (AcO and Br) had direct relationships to polymer solubility and physicochemical properties of the cellulose samples. Also, treatment of hydrogen peroxide solution as a regenerative agent influenced crystal sizes within the samples. Partial dissolution of cellulose induced by 1-ethyl-3-methylimidazolium bromide influenced the production of unique morphological changes and thermal behaviors relative to microcrystalline cellulose and other cellulose preparations.

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Acknowledgments

A special thank you for the acquisition of x-ray data by Abneris Morales, Ph.D. student of The Center for Computational and Integrative Biology at Rutgers University–Camden and for technical support and training on the DEXS system by Dr. Paul Heiney, emeritus professor for the Department of Physics and Astronomy at the University of Pennsylvania and supervisor/coordinator for the DEXS facility. Salas-de la Cruz summer financial support was provided by NSF-CMMI (2037097) and NSF-DMR (2104376).

Funding

The authors are grateful for financial support from NSF-DMR-RUI 1809354 and NSF-CMMI 2037097, Rutgers-Camden Arts and Sciences Start-up Package, State of NJ ELF Grant and The Center for Computational and Integrative Biology TA Funds. The DEXS System is supported by NSF-MRSEC 17-20530, NSF-MRI 17-25969, ARO DURIP W911NF-17-1-02822, and the University of Pennsylvania.

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Conceptualization: SAL and DS-de laC; Methodology: DS-de laC and SAL; Formal analysis and investigation: SAL, EM, DSM, and SS; Writing—original draft preparation: SAL, EM, DSM, and SS; Writing—review and editing: SAL and DS-de laC; Funding acquisition: DS-de laC; Resources: DS-de laC; Supervision: DS-de laC and SAL.

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Correspondence to David Salas-de la Cruz.

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Love, S.A., Magaziner, E., Melissaratos, D.S. et al. Cellulose solubility in ionic liquids and regeneration in water and hydrogen peroxide solution: a comparative examination of morphology and physicochemical properties. Cellulose 30, 6149–6162 (2023). https://doi.org/10.1007/s10570-023-05258-w

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