Abstract: In this work an optimization of the solvent-free acetylation of cellulose with acetic anhydride under microwave heating with iodine as a catalyst was performed. The optimized parameters included the microwave irradiation power from 300 W to 800 W, the reaction time between 5 to 40 min, the reaction temperature from 80 to 130 °C, and the amount of iodine from 1 to 15 mol%. The extent of the acetylation was measured by yield and the degree of substitution (DS), which was determined by a back-titration method. Acetylated cellulose was characterized by FT-IR, CP/MAS 13C-NMR, WRXD, and thermogravimetric analysis. The results showed that within the range of catalyst amounts studied, the DS increased as the amount of iodine used increased, however, it was barely affected by microwave output. It was also found that the reaction time and temperature had an active influence on the extent of acetylation, however, this did not mean that at the higher temperature a better acetylation of cellulose would be obtained. The optimal reaction time and temperature found in this work were 30 min and 130 °C.
Keywords: cellulose; acetylation; microwave irradiation; iodine; solvent-free
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Li, J.; Zhang, L.-P.; Peng, F.; Bian, J.; Yuan, T.-Q.; Xu, F.; Sun, R.-C. Microwave-Assisted Solvent-Free Acetylation of Cellulose with Acetic Anhydride in the Presence of Iodine as a Catalyst. Molecules 2009, 14, 3551-3566.
Li J, Zhang L-P, Peng F, Bian J, Yuan T-Q, Xu F, Sun R-C. Microwave-Assisted Solvent-Free Acetylation of Cellulose with Acetic Anhydride in the Presence of Iodine as a Catalyst. Molecules. 2009; 14(9):3551-3566.
Li, Jing; Zhang, Li-Ping; Peng, Feng; Bian, Jing; Yuan, Tong-Qi; Xu, Feng; Sun, Run-Cang. 2009. "Microwave-Assisted Solvent-Free Acetylation of Cellulose with Acetic Anhydride in the Presence of Iodine as a Catalyst." Molecules 14, no. 9: 3551-3566.