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以三氯氧磷、三乙胺、丙烯酸羟丙酯(HPA)等为原料,通过多步法合成了一种磷酸酯反应型乳化剂。实验对原料配比、反应时间、反应温度等进行讨论,得到最佳工艺条件,并用红外光谱对产品进行结构表征。结果表明,合成甲基丙烯酰氧丙基磷酸酯中间体,选择n(三氯氧磷)∶n(三乙胺)∶n(HPA)=1.1∶1.3∶1,反应时间为1.5h,反应温度为25℃,第二步水解反应温度0~15℃,水解物料比为n(中间体产物)∶n(三乙胺)∶n(水)=1∶1.4∶1.2时,最终产物收率最高,可达98.80%。
A series of phosphoric ester reactive emulsifiers were synthesized by using phosphorus oxychloride, triethylamine and HPA as raw materials. Experiments on the ratio of raw materials, reaction time, reaction temperature were discussed, the best process conditions, and the use of infrared spectroscopy of the product structure characterization. The results showed that the synthesis of methacryloyloxypropyl phosphate intermediate, n (phosphorus oxychloride): n (triethylamine): n (HPA) = 1.1:1.3:1, the reaction time was 1.5h, the reaction The final product yield was 25 ° C, the second hydrolysis reaction temperature was 0-15 ° C, and the hydrolysis material ratio was n (intermediate product): n (triethylamine): n (water) = 1: 1.4: 1.2 The highest, up to 98.80%.