ESTERIFICATION OF ACETIC ACID WITH GLYCEROL

The catalytic reaction was carried out at 105 °C and at atmospheric pressure in a round bottom flask reactor equipped with a magnetic stirrer. The sulfon­ic acid containing material was dried prior to use at 105 °C under vacuum (~1.33 Pa) for 18 h. The following concentrations ofthe reagents were used: 100 g acetic acid/L of glycerol and the catalyst concentration was 6.25 g/L of glycerol. First, the catalyst and glycerol are added together to the flask and are brought to reaction temperature. When the temperature is reached, the acetic acid is injected. Before analysis the samples are extracted with 1-heptanol and using o-xylene as an internal standard. The total yield of the esters was determined with gas chromatography. After one minute a sample of the reaction mixture is taken and analyzed with gas chromatography. This sample represents the starting point of the catalytic experiment. The recy­clability experiments were carried out under identical conditions as the cata­lytic tests. Therefore, the catalyst was separated from the liquid phase after 1 h and reused in a consecutive run without further treatment. The liquid phase was kept under reaction conditions and further followed as a function of time. Gas chromatography was performed with a Varian CP-3800 using a Cp-Sil 8CD column (Varian, Palo Alto, CA, USA) with a FID detector.