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The role of salt on cellulose dissolution in ethylene diamine/salt solvent systems

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Abstract

Ethylene diamine (EDA)/salt solvent systems can dissolve cellulose without any pretreatment. A comparison of the electrical conductivity of different salts in EDA was made at 25 °C, and conductivity decreased in the order of KSCN>KI>NaSCN at the same molar concentration. Among the salts tested, potassium thiocyanate (KSCN) was capable of dissolving both high molecular weight (DP>1000) and low molecular weight (DP = 210) cellulose, and this was confirmed by polarized light microscopy. 39K and 14N NMR experiments were conducted at 70 °C as a function of cellobiose concentration with EDA/KSCN as the solvent. The results showed that the K+ ion interacts with cellobiose more than the SCN− ion does. Recovered cellulose was studied by infrared spectroscopy (FTIR) and wide angle X-ray diffraction (WAXD). Changes in the FTIR absorption bands at 1,430 and 1,317 cm−1 were associated with a change in the conformation of the C-6CH2OH group. The changes in positions and/or intensities of absorption bands at 2,900, 1,163, and 8,97cm−1 were related to the breaking of hydrogen bonds in cellulose. X-ray diffraction studies revealed that cellulose, recovered by precipitating cellulose solutions with water, underwent a polymorphic transformation from cellulose I to cellulose II.

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Acknowledgements

The authors gratefully acknowledge the NTC (National Textile Center) for funding this project, Dr. Ivan Keresztes, NMR Instruments Laboratory, Department of Chemistry and Chemical Biology, for technical support regarding the NMR measurements, and Prof. David B. Zax, Department of Chemistry and Chemical Biology, and Prof. David B. Wilson, Department of Molecular Biology and Genetics, Cornell University, for reviewing this paper.

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  1. Department of Fiber Science and Apparel Design, Cornell University, College of Human Ecology, 299 MVR Hall, Ithaca, NY, 14853-4401, USA

    Min Xiao & Margaret W. Frey

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  1. Min Xiao
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  2. Margaret W. Frey
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Correspondence to Margaret W. Frey.

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Xiao, M., Frey, M.W. The role of salt on cellulose dissolution in ethylene diamine/salt solvent systems. Cellulose 14, 225–234 (2007). https://doi.org/10.1007/s10570-007-9110-7

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  • DOI: https://doi.org/10.1007/s10570-007-9110-7

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