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3 ENERGY-EFFICIENT PROCESSES LICIL adducts like 2 dissociate to form N,N-dimethylformamide and dimethyl sul- fate). The pulping efficiency of the salts 8 and 9 is comparable to that of the ILs 2 and 4. Using the hydroxymethyleniminium salts 8 or 9 at a raised temperature (>100 °C) in combination with organic solvents like ethylene glycol, glycerol, 1,3-propandiole, methyl glycol or tetrahydrofurfuryl alcohol, enabled cata- lytic pulping of spruce wood within 2 hours for a mass ratio x (mwood : mIL : mco-solvent) = 15 : 2 : 108. High degrees of delignification were achieved using the co-solvents methyl glycol or tetrahydrofurfuryl alcohol. The fibre yields were between 45% and 54%; the lignin yields ranged from 21% to 25%. The cellulose content of the fibre fraction was about 82%; the lignin fraction contained approximately 84% lignin. The molar masses of the lignins were around 8500 D. Longer reaction times (8 h) change neither the yield nor the quality of the fibre or lignin fraction, though the molar masses of the lignins increases by about 10%. If instead of using the pulping systems involving 8 and methyl glycol or te- trahydrofurfuryl alcohol, pulping is carried out with mixtures of sulfuric acid and one of the co-solvents, both the fibre and lignin yields are reduced and the products have a strong yellow to brown discoloration. The cellulose fibres are also shorter and exhibit a very non-uniform fibre length distribution. The pulping systems involving the hydroxymethyleniminium salts and co-solvents could be used at least three times, as was demonstrated by a mixture of 8 (DMF/H2SO4) and methyl glycol (the total yield of extracted lig- nin was 18%), the fibre yield by the third extraction rose to 74%, as its lignin content increased. Initially, the pulping liquor was filtered or centrifuged to remove the cellu- lose. The lignin was then precipitated out of the filtrate by adding water and collected by filtration. The residual filtrate was then evaporated to dryness to recover the hemicellulose. Modifying the post-pulping workup procedure saved energy and made material recycling more effective. The new workup procedure involved neutralising the acidic filtrate once the cellulose had be- en removed and then distilling off the co-solvent. Addition of water to the residual solution caused precipitation of the lignin, which was then separa- ted by filtration. Subsequent evaporation to dryness yielded the hemicellu- lose. If the acid component was not neutralised, the molar mass of the lignin was twice as large (pulping with 2 in methyl glycol). This pulping method was also successful with spruce chippings. The effi- ciency of the pulping process is reflected in the fibre and lignin yields as well as in the shive fraction and is strongly dependent on the co-solvent used 238PDF Image | Chemical Processes and Use of CO2
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