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Microwave-assisted rapid synthesis of a polyether from a plant oil derived monomer and its optimization by Box–Behnken design

Ahmadi, Reza, Ullah, Aman
RSC advances 2017 v.7 no.45 pp. 27946-27959
Fourier transform infrared spectroscopy, differential scanning calorimetry, epoxidation reactions, equations, experimental design, gel chromatography, melting point, microwave radiation, microwave treatment, molecular weight, nuclear magnetic resonance spectroscopy, olefin, polymerization, polymers, reflectance, regression analysis, solvents, temperature, thermogravimetry
In this study, a new strategy for making polyethers from α-olefin (1-decene) was developed using microwave irradiation and compared with a conventional method. The olefin was epoxidized and subjected to catalytic polymerization using both conventional and microwave synthesis techniques. The conventional epoxidation reaction of 1-decene took 1 hour while microwave-assisted epoxidation was completed in ∼5 minutes. A three-factor, three-level Box–Behnken response surface design was employed to investigate the effect of the process parameters such as time, temperature, and the solvent–monomer ratios on the yield of the ring-opening polymerization of 1,2-epoxydecane using MMAO-12/2,4-pentanedione. The obtained experimental data were fitted to a transferred second-order polynomial equation using multiple regression analysis with a high coefficient of determination (R²) value of 0.9881. Interestingly, the optimal predicted parameters based on all independent variables (reaction time 9.97 min, the temperature 99.69 °C, and solvent to monomer ratio 5.27 : 5) were determined by a maximum polyether yield of 82.51%, which was further confirmed by validation experiments. The synthesized polymers were characterized by using proton nuclear magnetic resonance spectroscopy (¹H-NMR), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA) and size exclusion chromatography (SEC). A high molecular weight polyether was synthesized with a melting temperature as high as 88.64 °C and a decomposition in the range of 325–418 °C. The rapid synthesis of a biopolyether with high molecular mass is extremely attractive both from an academic and industrial point of views.