A range of superbase derived ionic liquids (SILs) was synthesised and characterised. Their ability to dissolve cellulose and the characteristics of the produced fibres were correlated to their specific structural and solvent properties. 17 ionic liquids (ILs) (including 9 novel) were analysed and six ILs were selected to produce fibres: 1-ethyl-3-methylimidazolium acetate [C2C1im][OAc], 1-ethyl-3-methylimidazolium diethyl phosphate [C2C1im][DEP] and the SILs 1-ethyl-1,8-diazabicyclo[5.4.0]undec-7-enium diethylphosphate [DBUEt][DEP], 1,8-diazabicyclo[5.4.0]undec-7-enium acetate [DBUH][OAc], 1,5-diazabicyclo[4.3.0]non-5-enium acetate [DBNH][OAc] and 1-ethyl-1,5-diazabicyclo[4.3.0]non-5-enium diethylphsophate [DBNEt][DEP]. The mechanical properties of these fibres were investigated. The obtained fibres were then carbonised to explore possible application as carbon fibre precursors. The fibres obtained using a mixture of 1,5-diazabicyclo[4.3.0]non-5-enium based SILs with acetate and hexanoate anions (9 : 1), [DBNH][OAc][Hex], showed a promising combination of strength, stiffness and strain at failure values for applications in textiles and fibre reinforcement in renewable composites. Using Raman spectroscopy it is demonstrated that these fibres exhibit a relatively high degree of structural order, with fewer defects than the other materials. On the other hand, analogous fibres based on imidazolium cation with acetate and hexanoate anions (9 : 1), [C2C1im][OAc][Hex] showed a decline in the quality of the produced fibres compared to the fibres produced from [C2C1im][OAc], [C2C1im][DEP] or [DBNH][OAc][Hex]
We report a method to extract lignin from willow, using triethyl ammonium hydrogen sulphate [Et3NH][HSO4. This method is used to manufacture fibers with a range of compositions.. This extraction achieved an 18% yield of lignin as characterized by ATR-IR and elemental analysis indicated a high carbon yield. 1-Ethyl-3-methylimidazolium acetate [C2C1im][OAc] was then used as a solvent to manufacture lignin-cellulose fiber blends. The Young's modulus of a 75:25 lignin:cellulose fiber was found to be 3.0 ±0.5 GPa which increased to 5.9 ±0.6 GPa for a 25:75 lignin:cellulose blend. From a characterization of the surface morphology using Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM) it was observed that a rich lignin content in the fiber blend increased the surface roughness. FT-IR analysis confirmed the presence of aromatic groups of lignin from the presence of peaks located at ~1505 cm -1 and ~1607 cm -1 . The presence of lignin improves the thermal stability of the fiber blends by allowing them degrade over a wider temperature range. This is potentially useful for the utilisation of renewable lignocellulosic biomass derived fibers as carbon fiber precursors. Although the mechanical properties of the regenerated fibers were diminished by the addition of lignin, the blends prepared produced a solution suitablefor a stable fiber spinning process.
The solubilities of the metal halides LiF, LiCl, LiBr, LiI, NaF, NaCl, NaBr, NaI, KF, KCl, KBr, KI, RbCl, CsCl, CsI, were measured at temperatures ranging from 298.15 to 378.15 K in the ionic liquid 1-butyl-3-methylimidazolium trifluoromethanesulfonate ([C 4 . This study compares the influence of metal cation and halide anion on the solubility of salts within this ionic liquid. The highest solubility found was for iodide salts and the lowest solubility, for the three fluoride salts. There is no outstanding difference in the solubility of salts with matching anions in comparison to halide salts. The experimental data were correlated employing several phase equilibria models, including ideal mixtures, van't Hoff, the λh (Buchowski) equation, the modified Apelblat equation, and the non-random two-liquid model (NRTL). It was found that the van't Hoff model gave the best correlation results. On the basis of the experimental data the thermodynamic dissolution parameters (ΔH, ΔS, and ΔG) were determined for the studied systems together with computed gas phase metathesis parameters. Dissolution depends on the energy difference between enthalpies of fusion and dissolution of the solute salt. This demonstrates that overcoming the lattice energy of the solid matrix is the key to the solubility of inorganic salts in ionic liquids.
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