Evaluation of molten inorganic salt hydrates as reaction medium for the derivatization of cellulose |
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Authors: | Steffen Fischer Katrin Thümmler Katy Pfeiffer Tim Liebert Thomas Heinze |
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Institution: | (1) Institut für Anorganische Chemie der TU Bergakademie Freiberg, Leipziger Strasse 29, D-09596 Freiberg, Germany |
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Abstract: | Molten inorganic salt hydrates are highly efficient solvents forcellulose. The carboxymethylation of the polymer dissolved in this new group ofcellulose solvents was investigated. The homogeneous carboxymethylation ofcellulose in molten LiClO43H2O using sodiummonochloroacetate in the presence of NaOH is possible. The formation of CMC wasconfirmed by FT- Raman spectroscopy. Structure analysis by means of HPLC afterchain degradation showed the formation of CMC with a DS of 2 after a shortreaction time of 4 h. The derivatives exhibit a statisticaldistribution of substituents along the polymer chain if prepared in moltenLiClO43H2O as solvent. A substituent distributioninthe order C-6 > C-2 C-3 for anhydroglucose units (AGU) was concludedfrom 1H-NMR measurements. The synthesis of CMC in the swellingmediumLiClxH2O (2 x 5) yields polymers with astatistical distribution of functional groups along the chain. The watercontentof the salt melts has a dramatic influence on the DSCMC. |
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Keywords: | Carboxymethyl cellulose 1H-NMR spectroscopy HPLC Molten salt hydrates Solvent |
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