The free radical precipitation copolymerization of the polar monomer glycidyl methacrylate (GMA) and the nonpolar monomer 1‐octene (Oct) in supercritical carbon dioxide (sc‐CO2) is reported under different conditions of pressure and temperature. According to 1H NMR studies, in the obtained statistical copolymers (GMA‐stat‐Oct) the molar fraction of the olefin (FOct) increases when the pressure and temperature of the reaction increased from the reference values T = 125 °C and P = 34 bar. In particular, when the initial molar fraction of Oct (fOct) is 0.83, the molar fraction of this monomer in the final copolymer reaches a maximum value of 0.22 at 124 bar and T = 155 °C. On the other hand, for fOct = 0.89, it is obtained that FOct = 0.25 at 124 bar and T = 155 °C. Copolymers obtained are characterized by NMR, scanning electron microscopy, and size exclusion chromatography techniques. Finally, two copolymers were selected to demonstrate the feasibility of modifying the GMA moiety in order to introduce OH polar groups giving rise to Oct‐stat‐glycerol methacrylate copolymers.
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