Synthesis of 1,1,5-Trihydro-octafluoro Pentyl Glycidylether-A Monomer for Fluoro-carbonic Polyether An Investigation of Hydroxy-terminated Fluoro-carbonic Polyether for Special Polyurethane Prepolymer Ⅲ

Abstract

 In the synthesis of fluorocarbon polyether monomer 1,1,5-trihydrooctafluoropentyl In the process of producing glycidyl ether (FGE-2), gas-liquid chromatography was used to follow the condensation reaction of 1,1,5-trihydrooctafluoropentanol (FOH-2) and epichlorohydrin (ECH) in the presence of NaOH. Process, it was found that the reaction is a reversible reaction; when the reaction temperature is low (30℃), the reaction speed is too slow, and when the reaction temperature is too high (80℃), the equilibrium moves in the opposite direction. The more suitable reaction temperature is 50℃. When the moles of reactants When the ratio is: FOH-2/ECH/NaOH=1/3/1~1.2, in anhydrous medium, use the post-addition method of FOH-2, and the reaction will reach equilibrium in 4~5 hours; if the excess of NaOH is 5%~20%, The conversion rate reaches more than 90%, and the yield can reach 82%. Good results are also obtained by using ECH post-addition. The reactants are precision fractionated under reduced pressure, and after separation and recovery of ECH and FOH-2, they are collected under a vacuum of 266.6Pa bp 68 ℃ fraction, the FGE-2 product is obtained, with an epoxy value of 0.3440~0.3471mol/100g and a purity of more than 99%.