Microwave-assisted synthesis of the lipase-catalyzed ring-opening copolymerization of ε-caprolactone and ω-pentadecanolactone: Thermal and FTIR characterization

Abstract

Microwave-assisted synthesis of the lipase-catalyzed ring opening polymerization of ε-caprolactone (ε-CL) and ω-pentadecanolactone (ω-PDL) monomers was studied. A series of P(CL-co-PDL), with different molar feed ratios, including (ε-CL/ω-PDL) 100/0, 75/25, 50/50, 25/75, and 0/100, were synthesized. The resulting polyesters were characterized by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). The microwave-assisted polymerization of the monomers reached high conversions (91–95%) within 60 min. FTIR spectra showed the typical absorption bands of these polyesters. A very intense band in the carbonyl region, which was shifted from 1,720 cm−1 for PCL to 1,732 cm−1 for PPDL homopolymer, as well as peaks owing to methylene groups in the 2,990–2,850 cm−1 range. DSC results revealed that all polyester samples were semi-crystalline. Interestingly, the copolymers exhibited only one melting peak (T m), and their T m values linearly increased from 57°C to 95°C as PPDL concentration was increased. Thermal stability of polyesters also depended on PDL content; an increase in PDL concentration increases polymer degradation temperature (T d).

Keywords

• microwave-assisted synthesis
• lipase-catalyzed ring-opening polymerization
• copolyesters
• ε-caprolactone
• ω-pentadecanolactone