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The direct dissolution of cellulose offers a pathway to production of regenerated textile fibers. However, fiber production in the Lyocell process requires a high recyclability of the solvent. Some compounds from the class of ionic liquids (IL) may have higher dissolving capacities together with a higher thermal stability than the conventional N‐methylmorpholin‐N‐oxide (NMMO), which makes them more valuable in an industrial process. A promising representative of such an advanced solvent for Lyocell process, 7‐Methyl‐1,5,7‐triazabicyclo[4.4.0]dec‐5‐ene acetate ([MTBDH][AcO]) was investigated in this study. A series of 21 consecutive cellulose dissolving and spinning trials via dry‐jet wet spinning was conducted with the same batch of solvent. In the spinning trials, the cellulose was regenerated into water consisting spinning bath. The solvent was recycled by removing the water from the spin bath via distillation in reduced pressure. Due these drastic changes in the water content of the IL during the whole process, the hydrolytic stability is an important aspect to assess the recyclability of the IL and viability of the whole process. The chemical composition of the IL was monitored by means of NMR spectroscopy. Although there was an increase of hydrolysis level of the solvent, cellulose could be dissolved constantly and spun to obtain staple fibers. The spinning behavior deteriorated slowly along the additional cycles, along with a measured increase in zero‐shear viscosity of the spinning dope. Nevertheless, the physical properties of the obtained fibers were barely influenced by the changes of the ionic liquid. [ABSTRACT FROM AUTHOR]

Cotton fibre dissolution has been investigated using ionic liquids having a functionalized imidazolium cation. Two ionic liquids, 3-butyric acid-1-methyl imidazolium chloride [HOOC4MIM][Cl] (IL-acid) and 3-N,N-diethyl-butyramide-1-methyl imidazolium chloride [(Et)2NOC4MIM][Cl] (IL-amide), were synthesized by passing both through the intermediate 1-(3-Ethoxycarbonyl-propyl)-1-methyl imidazolium bromide. Their chemical structures were then confirmed using NMR and FTIR. 5 wt% cotton fibers have been completely dissolved in both synthesized ionic liquids in 3 h at room temperature. The regenerated cellulose with water, as an anti-solvent, was characterized using XRD, FTIR, TGA, and degree of polymerization (DP) methods. The FTIR and XRD results showed that no other chemical reaction occurred by both synthesized ILs other than the breakage of hydrogen bonds during the dissolution and regeneration processes. In addition, the regenerated cellulose had a reduced crystallinity and a structural transition from cellulose I to cellulose II. TGA results confirmed the low crystallinity of regenerated cellulose by demonstrating its low thermal stability compared to cotton fibers. Furthermore, the DP of cotton fibers was reduced from 805 ± 15 to 737 ± 12 and 765 ± 10 after regeneration from IL-acid and IL-amide, respectively, confirming partial cellulose network degradation. The IL-acid has an oily appearance and a viscosity (44 ± 5 mPa.s at 25 °C), allowing it to dissolve 14.5 wt% cotton fibers at 25 °C, IL-amide can only dissolve 5 wt% in 5 h at 25 °C due to its viscous nature. These results imply that the produced ionic liquids can be considered as competitive solvents for dissolving cellulose. [ABSTRACT FROM AUTHOR]

Cellulose, as the most abundant sustainable resource on earth, can be chemically transformed into a variety of biodegradable materials, which have been proposed as the ideal substitutes for plastic products. The first challenge for the fabrication of cellulose-based functional materials is the successful dissolution of cellulose by solvents. However, most existing cellulose solvents have environmental, economic, and other drawbacks that limit their further industrial applications. Research on developing novel solvent systems with "greener" and "cheaper" properties is needed to meet the challenges. [ABSTRACT FROM AUTHOR]

We have found that the dissolution of cellulose in the binary mixed solvent tetrabutylammonium acetate/dimethyl sulfoxide follows a previously overlooked near-stoichiometric relationship such that one dissolved acetate ion is able to dissolve an amount of cellulose corresponding to about one glucose residue. The structure and dynamics of the resulting cellulose solutions were investigated using small-angle X-ray scattering (SAXS) and nuclear magnetic resonance techniques as well as molecular dynamics simulation. This yielded a detailed picture of the dissolution mechanism in which acetate ions form hydrogen bonds to cellulose and causes a diffuse solvation sheath of bulky tetrabutylammonium counterions to form. In turn, this leads to a steric repulsion that helps to keep the cellulose chains apart. Structural similarities to previously investigated cellulose solutions in aqueous tetrabutylammonium hydroxide were revealed by SAXS measurement. To what extent this corresponds to similarities in dissolution mechanism is discussed. [ABSTRACT FROM AUTHOR]