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Esterification of organosolv lignin under supercritical conditions

Abstract : An organosolv lignin, extracted in organic acid media, named Biolignin™, was acetylated with acetic anhydride in supercritical carbon dioxide (scCO2). The effect of moisture and specific surface of lignin sample, temperature (50, 80, 100, 150 °C), reaction time and the use of a catalyst have been studied using analytical techniques such as FT-IR, quantitative 31P NMR and Differential Scanning Calorimetry (DSC). The reaction appeared to be more efficient when a dried organosolv lignin was used (97% Dry Matter) and with a specific surface of 0.645 m2/g. The highest degree of substitution of acetylated samples was obtained after 1 h of reaction at a temperature of 100 °C (180 bar) and in the presence of pyridine as a catalyst. When compared with conventionally acetylated lignin (using a solvent medium), it appeared that supercritical conditions allowed a higher yield of acetylation and a decrease of the glass transition temperature of the lignin.
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https://hal.archives-ouvertes.fr/hal-01886017
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Nadja Cachet, Séverine Camy, Bouchra Benjelloun-Mlayah, Jean-Stéphane Condoret, Michel Delmas. Esterification of organosolv lignin under supercritical conditions. Industrial Crops and Products, Elsevier, 2014, 58, pp.287-297. ⟨10.1016/j.indcrop.2014.03.039⟩. ⟨hal-01886017⟩

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