磷氮阻燃剂的合成及其在环氧树脂中的应用

Synthesis of Phosphorus-nitrogen Flame Retardant and Its Application in Epoxy Resin

摘要:

摘要：由亚磷酸，乙腈和苯膦酰二氯（PPDC）合成了一种添加型阻燃剂——苯膦酰二氨基双乙基四膦酸（PAEPA）。通过FTIR和ESI-MS对PAEPA的结构进行了表征。将PAEPA混入环氧树脂中制备阻燃环氧树脂，通过TGA，UL-94测试和LOI测试研究了用三乙烯四胺（TETA）固化的环氧树脂的阻燃性和热性能。结果表明，当w(P)=2.6% 时，环氧热固性材料表现出优异的阻燃性并通过UL94实验的V-0等级，LOI为29.8%。从热重曲线看出，800℃的残炭率为17.7%。SEM结果表明：EP/TETA体系中的PAEPA明显促进环氧树脂形成更致密、丰富的密封炭层，以提高燃烧过程中基体的阻燃性能。

Abstract:

Abstract：A novel flame-retardant additive, Phenylphosphonium diaminobisethyltetraphosphonic acid (PAEPA), was synthesized from phosphoric acid, acetonitrile and phenylphosphonic dichloride(PPDC). The structure of PAEPA was characterized by FTIR, and ESI-MS. PAEPA was blended into epoxy resin to prepare flame-retardant epoxy resins. The flame-retardant and thermal properties of epoxy resins cured with triethylenetetramine (TETA) were investigated by TGA, the UL-94 test, and LOI test. The results revealed that the epoxy thermosets exhibited excellent flame retardancy and passed the V-0 rating of the UL 94 test with an LOI of 29.8% when the phosphorus content was 2.6 %. From the thermogravimetric curve, the residual carbon at 800°C is 17.7%. SEM results showed that PAEPA in the EP/TETA system obviously accelerated the formation of a stronger, phosphorus-rich, sealing char layer to improve the flame-retardant properties of the matrix during combustion.