Optimization of cellouronic acid synthesis by TEMPO-mediated oxidation of cellulose III from sugar beet pulp

Microfibrillated cellulose from purified sugar beet pulp was converted into cellulose III by immersion in liquid ammonia. When freed from ammonia, this product was oxidized in water at pH-10 using NaBr, NaOCl and 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO) under various conditions and concentrations. The resulting water-soluble cellouronic acid-i.e. cellulose oxidized at the C6 position- was analyzed by high performance size exclusion chromatography (HPSEC) together with C-13 NMR spectroscopy. The oxidation parameters, namely reaction time, temperature, NaBr and TEMPO concentrations were varied to determine the optimum reaction conditions. A low TEMPO concentration, a rather fast reaction time and the conducting of the oxidation at 0 degrees C were critical to obtain pure cellouronic acid in high yield, high purity and high DP.