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

Abstract

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.

Microwave-Assisted Biocatalytic Polymerizations

“…However only few reports exist on the applications of microwave assisted enzymatic reactions, focusing predominantly on organic small molecule transformations (7,35,(37)(38)(39). An understanding of this area is poor and often controversial (40). Researchers have reported enhancements in the initial rate of reaction (41,42), product yields (39,43) and enantioselectivity (38) when using microwave heating as compared to conventional heating.…”

“…The field of microwave assisted enzymatic polymerizations has been recently receiving attention for exploiting the synergistic benefits of lipase and microwave heating in the field of polymer chemistry (9,40,45,46). Kerep and Ritter investigated the influence of MW irradiation on lipase catalyzed ring opening polymerization of ε-caprolactone (46).…”

“…Recently other researchers in our laboratory investigated the effects of microwave process parameters (power, intensity, MW irradiation time and temperature) on lipase catalyzed polymerization of caprolactone (40). A 3-D plot predicting the Mn of the PCL was developed.…”

Biotic and Abiotic Synthesis of Renewable Aliphatic Polyesters from Short Building Blocks Obtained from Biotechnology

“…[261] As an example, the esterification of oleic acid by methanolc atalyzed by immobilizedC ALB in the bulk did not show any improvements under microwave irradiation. [266] Recently,t he transesterification of dimethyl succinate or di- Reviews methyl adipatewith 1,4-BDOinthe bulk or in diethyl ether catalyzed by N435 exhibited similar or lower molar massesw ith microwave irradiation than those with conventionalh eating. [263] Due to these mixed results, until now,o nly a limitedn umber of studies have been performed on polyester synthesis.…”

Green Polymer Synthesis: An Overview on Use of Microwave‐Irradiation

“…The polymerizations were carried out in a single-mode microwave oven using ethylene glycol (EG) as the initiator in the absence of any metallic compound catalyst. In a most recent study, MW assisted lipase catalyzed solventfree poly-e-caprolactone synthesis has been reported and the effect of reaction parameters on poly-e-caprolactone (PCL) properties has been investigated using a statistical design [169].…”