Industrial manufacturing of regenerated cellulose fibers relies on an initial step with cellulose dissolution. For environmental and economic reasons, there are current research efforts directed towards developing aqueous media that can dissolve cellulose without excessive chemical degradation. The well-known insolubility of cellulose in pure water can be improved by strong acids or alkali, as well as various additives such as zinc chloride. Rational design of dissolution media requires an understanding of the basic intermolecular forces acting between cellulose, water, and the additives. Contemporary theories emphasize the amphiphilic properties of cellulose, thereby suggesting strategies from surface and colloid science to overcome the insolubility. Critical testing of the theories requires experimental methods that have the capability for molecular-level characterization of cellulose in the solid, solvent swollen, partially dissolved, and completely dissolved states. Here we describe a novel <sup>13</sup>C NMR-based approach appropriate for the hitherto rather neglected, but in our opinion critical, intermediate stages of dissolution. By combining features from solid-state and high-resolution liquids NMR, we are able to observe both solid and dissolved cellulose, as well as all organic additives, and even impurities and degradation products, in the native dissolution medium of typically very high viscosity, thereby giving information with sufficient detail to test the theories about the mechanisms for cellulose dissolution.

<sup>13</sup>C NMR method for characterization of partially dissolved cellulose in aqueous media

253rd National Meeting (2017)

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13C NMR method for characterization of partially dissolved cellulose in aqueous media

¹³C NMR method for characterization of partially dissolved cellulose in aqueous media