Optimisation of Operatory Conditions for Synthesis of Sunflower Oil Biobased Polyols Using Design of Experiments and Spectroscopic Methods

摘要

The present work studies the synthesis of biopolyols based on epoxidized sunflower oil (ESFO) and obtained via alcoholysis reaction. The ring opening reaction ESFO (with an oxirane index: O.O% of 6.2%) was carried using an alcohol solution and boron trifluoride (as catalyst). The operatory conditions of synthesis were optimized using a design of experiment (DOE). Alcohol content, catalyst percent as well as temperature were varied according to a JMP software matrix. Reaction conversion was followed by determination of the decrease of epoxy ring using titration method as well as an increase of the hydroxide group. The synthesized polyols were characterized using Fourier transform infrared spectroscopy and proton nuclear magnetic resonance. The results showed that oxirane ring has totally disappeared (in some formulations) which means full conversion. The full factorial design is an efficient method for testing the effect of operatory conditions especially in limiting the number of synthesis experiments.