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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、13CNMR、31PNMR和IR表征。结果表明,以三乙胺为缚酸剂,二氯甲烷为溶剂,将9.05 g甲基丙烯酰氯(0.1 mol)于0℃滴入装有17.2 g氯膦酸二乙酯(0.1 mol)和6.1 g乙醇胺(0.1 mol)的三颈瓶中,滴完,升至室温反应12 h,所得粗产物在135℃/13.3 Pa减压蒸馏,得到淡黄色黏稠液体,产率为69%。考察了产物的乳化条件并测试了其乳液的粒径及稳定性,表明在HLB=9时乳液的粒径最小,乳液的平均粒径为123.5 nm,Zeta电位为+30.193 mV。
To phosphorus trichloride, anhydrous ethanol, carbon tetrachloride, monoethanolamine, methacryloyl chloride as raw materials, synthetic a phosphorus nitrogen textile flame retardant - methacryloyloxyethyl diethyl phosphoramide Its structure was characterized by 1HNMR, 13CNMR, 31PNMR and IR. The results showed that 9.05 g methacrylic acid chloride (0.1 mol) was dropwise added to a flask containing 17.2 g diethylchlorophosphonate (0.1 mol) and 6.1 g ethanolamine (0.1 mol) in a three-necked flask. After the dropwise addition was completed, the mixture was allowed to rise to room temperature and reacted for 12 h. The crude product was distilled under reduced pressure at 135 ° C / 13.3 Pa to give a pale yellow viscous liquid with a yield of 69%. The emulsification conditions of the product were investigated and the particle size and stability of the emulsion were tested. The results showed that the particle size of latex was the smallest at HLB = 9. The average diameter of emulsion was 123.5 nm and the zeta potential was +30.193 mV.