一种含氟丙烯酸酯单体的合成与表征

Synthesis and Characterization of a Fluorinated Acrylate Monomer

首先以甲基丙烯酸与草酰氯室温反应3h得到甲基丙烯酰氯(Ⅰ);在三乙胺催化下,将Ⅰ与乙醇胺0℃反应5h,室温反应20h得到羟乙基甲基丙烯酰胺(Ⅱ)。全氟辛酸经酰氯化,再与Ⅱ于室温反应46h,成功制得含全氟基团的丙烯酸酯单体——全氟辛酸甲基丙烯酰胺基乙酯。探讨了各步反应的主要影响因素,并用FTIR、MS、13CNMR等对产物的化学结构进行了表征。

Firstly, the reaction of methacrylic acid with oxalyl chloride gave methacryloyl chloride （ Ⅰ） at room temperature. Under the catalysis of triethyl amine, Ⅰ was reacted with 2-aminoethanol for 5 h at 0℃ and 20 h at room temperature to yield N-（2-Hydroxyethyl）methacrylamide （ Ⅱ ）. The acylchloridization between the perfluorooctanoic acid and thionyl chloride gave perfluoroacyl chloride （ Ⅲ ）. Then, methylacryloylamidoethyl perfluorooctanoate was successfully obtained by the reaction of Ⅱ with Ⅲ for 46 h at room temperature. The chemical structure of product was confirmed by means of FTIR, ^13CNMR and mass spectroscopy methods. Various influencing factors on the reactions were also investigated and discussed.