羟基磷酸酯功能单体的合成研究

Synthesis and study on functional hydroxyl phosphate monomer

以曱基丙烯酸缩水甘油醋（GMA）与浓嶙酸为原料，制备了一种含羟基可交联聚合的磷酸酯功能单体。通过酸值测试跟踪反应进程，确定了GMA中的环氧基团发生开环酯化反应的最佳时间，分析了羟基磷酸酯（HPAM）合成反症机理，确定了最佳的合成工艺。将实验制得的5组HPAM与丙烯酸酯聚合，制备了羟基磷酸酯改性丙烯酸酯乳液，并研究了乳液和涂膜的性能。结果表明，HPAM功能单体的最佳合成工艺为：GMA和浓磷酸按摩尔比为2 ：1同步滴加到（0± 5） ℃的反应釜中进行开环酯化反应，然后升温至（65 ± 2）℃，保温3.5-4.0 h。将此工艺下制备的HPAM单体与丙烯酸酯共聚得到的羟基嶙酸酯改性丙埽酸醋乳液，具有较好的稳定性，乳液涂膜的附着力为1级，硬度H,冲击强度为50kg·cm。

A functional monomer of crosslinkable andpolymerizable hydroxyl phosphate （HPAM） was preparedfrom glycidyl methacrylate （GMA） and concentratedphosphoric acid. The reaction process was tracked by acidvalue test and the optimal time for ring-opening esterificationof epoxy group in GMA was determined. The synthesismechanism of hydroxyl phosphate was analyzed and theoptimal synthesis process was obtained. Five types ofhydroxyl phosphate modified acrylate emulsions wereprepared by polymerization of different HP AMs withacrylates. The performances of the emulsions and their filmswere studied. The optimal synthesis process of HPAMfunctional monomer is as follows： （1） adding dropwise GMAand concentrated H3P04with a molar ratio of 2：1 to a reactor at （0 ± 5） ℃ for ring-opening esterification reaction; （2）increasing temperature to （65 ± 2） ℃; and （3） maintaining thetemperature for 3.5-4.0 h. The HPAM modified acrylateemulsion obtained by the optimal polymerization process hasgood stability, and its coating features adhesion strength1grade, hardness H, and impact strength 50 kg·cm.