Abstract

Miscanthus × giganteus bark was subjected to mild fractionation with peroxyformic acid by a two stage process. A factorial experimental design was used to study and quantify the effect of the variables (formic acid concentration (80–90%), hydrogen peroxide concentration (0.2–0.4%), temperature of the first stage (60–80 °C), and treatment time of the second stage (60–120 min)) on the main parameters of fractionation: pulp yield, remaining lignin and total polysaccharides in pulp. The dependence of lignin precipitation rate on hydrogen peroxide concentration in liquor was also studied. Hydrogen peroxide concentrations inferior to 0.5% seems to be suitable to recover high percentages of lignin. The isolated lignin was analysed by 2D-HSQC, 13C- and 31P NMR spectroscopy, FTIR spectroscopy, size-exclusion chromatography and chemical analysis. The most important chemical modifications taken place in the lignin during the fractionation were identified: β -O-4′ cleavage and hydrolysis of LC-bond structures. The C9-formula was also determined: C 9H 6.81O 2.90(OCH 3) 0.68(COOH) 0.07(OH Ph) 0.38(OH Al) 0.33.

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