Abstract
• NDMM-OH(aq) was used for the first time to dissolve cellulose. • MCC 3 wt% could be dissolved in 1-2M NDMM-OH(aq) with maximum dissolution of 7 wt%. • Two different pulps showed clear microscopy images with traces of fiber ballooning. • SEC and NMR showed high stability of cellulose solutions over refrigeratin. • DLS indicated molecular dissolution of majority of cellulose. N,N -dimethylmorpholinium hydroxide was synthesized and its ability to dissolve microcrystalline cellulose and pulp was assessed for the first time. Microscopy and UV–Vis measurements showed that dissolution occurred over a range of 1–2 M concentration of the solvent and a maximum solubility of 7 wt% microcrystalline cellulose could be achieved. The stability of cellulose solutions was evaluated by size exclusion chromatography, which did not detect degradation to any noticeable extent. This observation was further confirmed by 13 C NMR measurements. Finally, DLS studies confirmed that most of the cellulose was molecularly dissolved, with intrinsic viscosity values indicating cellulose chains expansion in this solvent.
Highlights
Growth in the world’s population and rapid changes in the climate highlight the urgency in shifting from fossil-based-materials towards the utilization of renewable resources, which would lead to a more sus tainable society
The challenge that remains is to minimize the limitations associ ated with existing solvents, which include instability of the dissolved state, low dissolution capacity, specific temperature requirements, chemical instability of the solvent, narrow concentration range required for dissolution and undesired reactions that cause a decrease in the degree of polymerization (DP) of cellulose [13]
N-dimethylmorpholinium hydroxide (NDMM-OH) was synthesized via a two-step procedure: (1) methyl ation of N-methylmorpholine to yield N,N-dimethylmorpholinium io dide (1H NMR and 13C NMR can be found in the supporting information) and (2) an ion exchange step to replace iodide with hydroxide ion (Fig. 1a)
Summary
Growth in the world’s population and rapid changes in the climate highlight the urgency in shifting from fossil-based-materials towards the utilization of renewable resources, which would lead to a more sus tainable society. Cellulose, which is the most abundant biopolymer on Earth, has far received considerable attention and both native fibres and man-made cellulose are widely processed for various applications. In such a context, the development of sustainable technologies that enable the reshaping of cellulose into textile fibres, films and membranes is of great importance [2,3], especially with respect to the fast increasing demand for textile materials. To be able to shape cellulose, processing through dissolution is a requisite, while a major existing challenge is cellulose insolubility in water and common organic solvents [4]. Further research is focused on understanding critical cellulose-solvent in teractions along with identifying new compounds/compound systems capable of providing dissolution power towards overcoming these limitations
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