Microwave assisted lipase catalyzed solvent-free poly-ε-caprolactone synthesis

Microwave (MW) assisted enzymatic polymerizations is an area that is largely unexplored. In the current study, the effect of MW reaction parameters on poly-o-caprolactone (PCL) properties has been investigated using a statistical design. A {3,5} modified mixture experimental design was used to identify the parameter values that gave the desired properties of PCL. The three process parameters that were tested are temperature, MW intensity, and the reaction time. Experimental results showed that in the range of values tested, temperature had the highest positive influence on the properties of PCL, whereas high MW irradiation is not desirable. A cubic regression model was developed and optimal process parameters were obtained using this model. Conducting the polymerization reaction under optimal conditions (908C, 240 min, 50 W), PCL with M_n of 20,624 and polydispersity index of 1.2 were obtained. The regression model was validated by carrying out validation experiments and by 3D visualization.