Testing zinc chloride as a new catalyst for direct synthesis of cellulose di- and tri-acetate in a solvent free system under microwave irradiation

Abstract

This research demonstrates the effect of ZnCl2 as a catalyst on the esterification of commercial cotton cellulose using acetic anhydride in order to obtain di- and tri-cellulose acetates under microwave irradiation. It was discovered that microwave irradiation significantly increased the yield and reduced the reaction time. It was found that the maximum yield for cellulose triacetates was 95.83% under the reaction conditions that were as follows: 3min reaction time, 200mg of ZnCl2 catalyst and 20ml of Ac2O for 5g cellulose. However, the cellulose acetate obtained in this manner had the highest DS (2.87). The cellulose di-acetate was produced with the maximum yield of 89.97% and with the highest DS (2.69) using 25ml Ac2O, 200mg of ZnCl2 for 5g cellulose and in 3min reaction time. The effect of some factors such as the amount of used catalyst, the quantity of acetic acid anhydride and the reaction time of the esterification process have been investigated. The production of di- and tri-cellulose acetate and the degree of substitution were confirmed using Fourier-transform infrared (FTIR) and nuclear magnetic resonance (NMR). The thermal stability was investigated using thermo gravimetric analysis (TGA), differential thermal analysis (DTA) and differential scanning calorimetry (DSC). The molecular weight and the degree of polymerization were obtained using Gel Permeation Chromatography (GPC). The analysis confirmed the successful synthesis of di- and tri-cellulose acetate without degradation during the reaction; these results were found to be in contrast to some recent studies. The present study reveals that ZnCl2 is a new catalyst; it is effective as well as inexpensive and is a low toxicity catalyst for usage in cellulose esterification.

Keywords: Cellulose acetate; Esterification; Microwave; Zinc chloride.