Optimization of the synthesis of 1-allyloxy-2-hydroxy-propyl-starch through statistical experimental design

The synthesis of 1-allyloxy-2-hydroxy-propyl starches was studied using a statistical experimental design approach. The etherification of two different granular maize starches with allyl glycidyl ether (AGE) in a heterogeneous alkaline suspension was investigated. The optimal reaction conditions were found via experimental design and the obtained response factor, e.g. the degree of substitution (DS) of the starch hydroxyl group, was statistically evaluated. The effects of six process factors on DS, namely the starch concentration, the reaction time, the temperature, and the amount of NaOH, Na2SO4 and AGE were investigated. The statistical analysis showed significant impact of the temperature, the amount of NaOH and the amount of AGE on the DS for both starches. Optimum conditions for the highest DS for waxy maize starch were: 0.0166% AGE (based on dry starch (ds)) and 1.0% NaOH (ds) at 34 °C in 4 h; on dent maize starch, these were 0.0099% AGE (ds) and 1.0% NaOH (ds) at 37 °C in 16 h.