甲基丙烯酰氯氧乙基二乙基磷酰胺的合成及乳化

Synthesis of Methacryloyl chloride ethyl diethyl phosphoric amide and Emulsification

摘要:

以三氯化磷、无水乙醇、四氯化碳、单乙醇胺、甲基丙烯酰氯为原料，合成出一种磷氮系纺织品阻燃剂——甲基丙烯酰氧乙基二乙基磷酰胺，其结构经过1HNMR ，13C NMR，31P NMR和IR表征。结果表明，17.2g氯磷酸二乙酯(0.1mol)和6.1g乙醇胺(0.1mol)、9.05g甲基丙烯酰氯（0.1mol）于0℃滴完，升至室温反应12h，三乙胺为缚酸剂，二氯甲烷为溶剂，产物在135℃/13.3Pa减压蒸馏的收率为69%。考察产物的乳化条件并测试了乳液的粒径及稳定性，表明在HLB为9时乳液的粒径最小，乳液的平均粒径为123.5nm，Zeta电位为+30.193mv。

Abstract:

A flame retardant containing nitrogen-phosphor for textile was synthesized from phosphorus trichloride, absolute ethylalcohol, carbon tetrachloride, monoethanol amine, methacryloyl chloride. The structure was characterized by 1H NMR，13C NMR, 31P NMR and IR. The result showed that 17.2g Diethyl chlorophosphate (0.1mol), 6.1g Ethanolamine(0.1mol) and 9.05g Methacryloyl chloride(0.1mol) reacted by dropping,then reacted 12h at room temperature， with Triethylamine as Acid-binding agent and Dichloromethane as solution, and the yield coefficient was 69% under the Vacuum distillation of 135℃/0.1mmHg. The diffient condition of emulsion was researched. After the grain diameter of latex emulsion and its stability were tested，it showed that the minimum diameter of emulsion forms in HLB9, and the average of diameter is 123.5nm, the Zeta is +30.193mv.