Abstract
Xylan sulfation using a Deep Eutectic Solvent (DES), formed by sulfamic acid and urea (1:2 molar ratio), was investigated with different reagent dosages (xylan/sulfamic acid molar ratio 1:10 and 1:5) and time (30 and 60 min). The effect of xylan/reagent ratio on the degree of substitution (DS) was higher than time, varying from 0.4 to 1.1. NMR spectra confirmed that the sulfate group was introduced into the C-2 and C-3 of the xylose moieties. Polyelectrolyte complex suspensions were prepared using the different sulfated xylan (SXyl) and chitosan (Ch) (mass ratio 55 SXyl/45 Ch) and deeply characterized. It was found that a precipitate was obtained for moderate conditions of sulfation; however for the others, stable suspensions were formed. Hydrogels with acceptable dry and wet mechanical properties (up to 45 MPa and 6 MPa of resistance, and 10% and 90% of elongation, respectively), and thermal properties were produced. Differences in crystallinity as well as in water uptake at 75% RH, depending on the SXyl used, were found. Promising results for potential use in drug delivery were the swelling capacity, which reached a maximum of 384% and was directly related to the degree of substitution of xylan, and the high water-resistant.
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Acknowledgments
This work was financed by: Agencia Nacional de Promoción de la Investigación, el Desarrollo Tecnológico y la Innovación- PICT 2019 (Nº 03246), Universidad Nacional del Litoral-CAI+D 2020 PI, Tipo II (Nº 50620190100135LI), Universidad de Buenos Aires-2018/2020 (Nº 20020170100255BA), and Consejo Nacional de Investigaciones Científicas y Técnicas-PIP (Nº 11220210100627CO) and PIP (Nº 11220200101158CO). The authors would like to thank Eng. Santiago J. Siccardi from Clorar Ingeniería SA for collaborating with the electrodialysis processes.
Funding
This work was financed by: Agencia Nacional de Promoción de la Investigación, el Desarrollo Tecnológico y la Innovación- PICT 2019 (No. 03246), Universidad Nacional del Litoral-CAI + D 2020 PI, Tipo II (No. 50620190100135LI), Universidad de Buenos Aires-2018/2020 (No. 20020170100255BA), and Consejo Nacional de Investigaciones Científicas y Técnicas-PIP (No. 11220210100627CO) and PIP (No. 11220200101158CO).
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All authors contributed to the study conception and design. Material preparation, data collection and analysis were performed by Yamil Nahún Solier, Frank Sznaider, Diego Alberto Navarro, Paulina Mocchiutti and María Cristina Inalbon. The first draft of the manuscript was written by Yamil Nahún Solier and all authors commented on previous versions of the manuscript. All authors read and approved the final manuscript.
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Solier, Y.N., Sznaider, F., Navarro, D.A. et al. Sulfation of poplar wood xylan using a deep eutectic solvent: effects of the degree of substitution on the properties of biobased hydrogels. Cellulose 31, 1189–1203 (2024). https://doi.org/10.1007/s10570-023-05651-5
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DOI: https://doi.org/10.1007/s10570-023-05651-5


