An organosolv lignin, extracted in organic acid media, named Biolignin ™ , was acetylated with acetic anhydride in supercritical carbon dioxide (scC02). 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 31 P NMR and Differential Scanning Calorimetry (DSC). The reaction appeared ta be more efficient when a dried organosolv lignin was used (97% Dry Matter) and with a specific surface of 0.645 m 2 /g. The highest degree of substitution of acetylated samples was obtained after 1 h of reaction at a temperature of 100 '((180 bar) and in the presence of pyridine as a catalyst.