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以苯基膦酰二氯及(1-氧基磷杂-4-羟甲基-2,6,7-三氧杂双环[2.2.2]辛烷(PEPA)为主要原料,在氨气存在的条件下反应合成了双笼环状有机膦酸酯高效阻燃剂,即双(2,6,7-三氧杂-1-磷杂双环[2.2.2]辛烷-1-氧代-4-羟甲基)苯基膦酸酯(BCPPO)。探讨了反应温度、时间、物质的量比对产率的影响,得到最佳合成工艺条件为n(苯基膦酰二氯)∶n(PEPA)=1∶2.5,80℃反应4h,产率88.6%。通过傅里叶转换红外线光谱(FT IR)、核磁共振氢谱(1 H NMR)和热重-差热分析(TG-DTA)等方法验证了产物的结构及性能。研究表明,在聚对苯二甲酸丁二醇酯(PBT)中加入质量分数为20%BCPPO时,其极限氧指数为29%。
Using phenylphosphonic dichloride and (1-oxylphosphino-4-hydroxymethyl-2,6,7-trioxabicyclo [2.2.2] octane (PEPA) as main raw materials in the presence of ammonia (2,6,7-trioxa-1-phosphabicyclo [2.2.2] octane-1-oxo- 4-hydroxymethyl) phenylphosphonate (BCPPO). The effects of reaction temperature, time and mass ratio on the yield were discussed. The optimal synthesis conditions were n (phenylphosphonic dichloride): n (PEPA) = 1: 2.5 at 80 ℃ for 4h, the yield was 88.6% .Four FT-IR, 1 H NMR and TG-DTA ) And other methods to verify the structure and properties of the product.Research shows that the limit oxygen index is 29% when the mass fraction of BCPPO is 20% in polybutylene terephthalate (PBT).