Facile, one-pot synthesis of aromatic diamine-based phosphinated benzoxazines and their flame-retardant thermosets
作者:Ching Hsuan Lin、Hung Tse Lin、Jhao Wei Sie、Kuen Yuan Hwang、An Pang Tu
DOI:10.1002/pola.24247
日期:2010.10.15
Three aromatic diamine‐based, phosphinated benzoxazines (7–9) were prepared from three typical aromatic diamines—4,4′‐diamino diphenyl methane (1), 4,4′‐diamino diphenyl sulfone (2), and 4,4′‐diamino diphenyl ether (3) by a one‐pot procedure. To clarify the reaction mechanism, a two‐pot procedure was applied, in which the reaction intermediates (4–6) were isolated for characterization. The structures
由三种典型的芳族二胺(4,4'-二氨基二苯甲烷(1),4,4'-二氨基二苯砜(2)和4,4' )制备了三种基于芳族二胺的亚膦酸苯并恶嗪(7-9)。一锅法制得的二氨基二苯醚(3)。为了阐明反应机理,采用了两锅法,其中分离出反应中间体(4–6)进行表征。通过高分辨率质谱,IR以及1D和2D-NMR光谱确认了中间体和苯并恶嗪的结构。除自聚合外,(7-9)还与甲酚酚醛清漆环氧树脂(CNE)共聚。固化后,P(7–9)较脆,而(7-9)/ CNE的共聚物则较坚硬。动态力学分析表明(7-9)/ CNE共聚物的T g s分别为187、190和171°C。热力学分析表明(7-9)/ CNE共聚物的CTE分别为46、38和46 ppm。所有(7-9)/ CNE共聚物均属于UL-94 V-0级,显示出良好的阻燃性。©2010 Wiley Periodicals,Inc. J Polym Sci A部分:Polym