Cellulose, especially wood-based cellulose, is increasingly important for making everyday materials such as man-made-regenerated textile fibers, produced via dissolution and subsequent precipitation. In this paper, the effect of cosolvents in ionic liquid-facilitated cellulose dissolution is discussed. Both microcrystalline cellulose and dissolving grade hardwood pulp were studied. Three different cosolvents in combination with ionic liquid were evaluated using turbidity measurements and viscosity. The ionic liquid precursor N-methylimidazole proved to be a promising cosolvent candidate and was thus selected for further studies together with the ionic liquid 1-ethyl-3-methylimidazolium acetate. Results show that dissolution rate can be increased by cosolvent addition, and the viscosity can be significantly reduced. The solutions were stable over time at room temperature and could be converted to regenerated textile fibers with good mechanical properties via airgap spinning and traditional wet spinning.Fibers spun from binary solvents exhibited significantly higher crystallinity than the fibers from neat ionic liquid.
This
article describes central features of the mass transport during
the coagulation in water of cellulose–1-ethyl-3-methylimidazoium
acetate ([C2mim][OAc]) solutions, namely, that the diffusivities are
mainly affected by the relative concentrations of water and [C2mim][OAc],
that the concentration of cellulose does not affect diffusivities
and coagulation rates, that the diffusivities of low-M
w compounds are similar to those in aqueous [C2mim][OAc]
solutions without macromolecules, that the polymer concentration is
diluted by the large influx of coagulant causing a positive net mass
gain, NMG, from diffusive fluxes, and that such NMG, although observed
only as a function in time, is also a function in space that has local
peaks significantly higher than the mean NMG value. The conclusion
from the first three findings was that the diffusion advances through
a liquid phase which possesses a continuous pore network and most
of the volume. The precipitated cellulose is concentrated into fibrils
whose inhibitive effect on the diffusion of small molecules through
the surrounding phase is marginal. This key understanding about mass
transport during coagulation also simplifies numerical modeling significantly.
Cotton production is reaching a global limit, leading to a growing demand for bio-based textile fibers produced by other means. Textile fibers based on regenerated cellulose from wood holds great potential, but in order to produce fibers, the components need to be dissolved in suitable solvents. Furthermore, the dissolution process of cellulose is not yet fully understood. In this study, we investigated the dissolution state of microcrystalline cellulose in aqueous NaOH by using primarily scattering methods. Contrary to previous findings, this study indicated that cellulose concentrations of up to 2 wt % are completely molecularly dissolved in 8 wt % NaOH. Scattering data furthermore revealed the presence of semi-flexible cylinders with stiff segments. In order to improve the dissolution capability of NaOH, the effects of different additives have been of interest. In this study, scattering data indicated that the addition of ZnO decreased the formation of aggregates, while the addition of PEG did not improve the dissolution properties significantly, although preliminary NMR data did suggest a weak attraction between PEG and cellulose. Overall, this study sheds further light on the dissolution of cellulose in NaOH and highlights the use of scattering methods to assess solvent quality.
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