新型磷-氮有机金属阻燃剂的合成及其热稳定性

Synthesis and Thermal Stability of A Novel P- N Organometallic Flame Retardant

以γ-氨丙基三乙氧基硅烷(1)和二苯基氯化膦(2)为原料,经取代反应制得N-(二苯基膦基)-1,1-二苯基-N-[3-(三乙氧基甲硅烷)丙基]膦氮配体(3);3与六水合氯化镍(4)反应合成了一种新型的磷-氮有机金属阻燃剂(5),其结构经1H NMR,31P NMR和FT-IR表征。研究了物料比[r=n(2)∶n(1)]、溶剂、反应时间和反应温度对3收率的影响。结果表明:在最佳反应条件[二氯甲烷为溶剂,1 19 mmol,r=2.3,于25℃反应14 h]下,3收率89.5%。TGA测试结果表明:5的初始分解温度为252℃,700℃残炭为31.9%。

N-( diphenylphosphino)-1,1-diphenyl-N-(3-( triethoxysilyl) propyl) phosphinamine(3) was prepared by substitution reaction of γ-aminopropyl triethoxysilane( 1) with chlorodiphenyl phosphine(2). A novel P- N organometallic flame retardant(5) was synthesized by the reaction of 3 with nickel chloride hexahydrate(4). The structures were characterized by1 H NMR,31 P NMR and FT-IR. Effects of molar ratio[r = n( 2) ∶ n( 1) ],solvent,reaction time and reaction temperature on the yield of 3were investigated. The optimum reaction conditions were as followed: dichloromethane was solvent,1was 19 mmol,r was 2. 3,reacted at 25 ℃ for 14 h. The yield of 3 was 89. 5% under the optimum conditions. TGA results showed that the initial decomposition temperature of 5 was 252 ℃ and the char yield was about 31. 9% at 700 ℃.