Cellulose (Avicel®) is converted to potentially useful products (formic acid, ethylene glycol, and lactic acid). Isosaccharinic acid is identified as the reaction intermediate. Homogeneous aqueous dispersions of cellulose were obtained with the aid of sonication (1 h.). The degradation of the cellulose dispersion was carried out in an alkaline (NaOH) medium under microwave (domestic) irradiation conditions. With 1, 4 and 10 wt. % cellulose dispersions, conversion values of 44, 58 and 54 wt. %, respectively, were observed upon 5 min. of microwave irradiation. The reaction products in each case have been analyzed by 1 H and 13 C NMR. products in the filtrate were analyzed using NMR ( 1 H, 13 C, DEPT) without further separation. In a large scale production process, based on the wide variation in the boiling point of ethylene glycol relative to formic acid and lactic acid, ethylene glycol could be separated using ordinary distillation whereas fractional distillation to be employed for the separation of formic acid and lactic acid from the product mixture as their boiling points are close. 1 H and 13 C NMR spectra of reaction products obtained from 1 wt. % cellulose (aqueous dispersion in alkaline medium) are shown in Figure 2. Two peaks at 61.1 and 168 ppm in the 13 C NMR spectrum were assigned to ethylene glycol and formic acid, respectively. The presence of formic acid, ethylene glycol and lactic acid, were confirmed by the observation of When the initial concentration of the cellulose (in the aqueous dispersion) is increased from 1 to 4 wt. %, a conversion of 58 wt. % is observed.
Isosaccharinic Acid Mediated Fine Chemicals Production from Cellulose
Journal of Fundamentals of Renewable Energy and Applications
Jo1 H and
13C NMR spectra of reaction products obtained from 4 wt. % cellulose (aqueous dispersion in alkaline medium) are shown in Figure 3. The peaks at 20.2, 61.3 and 168.3 ppm in the 13 C NMR spectrum were assigned to lactic acid, ethylene glycol and formic acid. The formation of the afore mentioned chemicals upon cellulose degradation is also confirmed by the presence of 1 H, doublet at 1.18 and 1.20 ppm (lactic acid), Table 1. For comparison, the 1 H and 13 C NMR spectra of authentic samples of formic acid, ethylene glycol and lactic acid are shown in Figure S1 and S2 respectively. Slight up field shift in the δ values of the reaction product formic acid (8.5 ppm, Figure 2 (a)) relative to the authentic sample (7.5 ppm, Figure S1) is attributed to the alkali under atmospheric pressure in the presence of air. The output of the domestic microwave reactor was 900 W. The microwave oven was modified so as to have provision for a distillation column passing through the MW oven (for enhanced safety of operation) as well as a stirring facility during the reaction [21]. The cellulose decomposition reaction was carried out in a batch mode in a round bottom flask with provision for a reflux condenser. Typically, each batch comprise of 10 mL of the aqueous dispersion of cellulose powder (1, 4 and 10 wt. ...