新型P－N－Si无卤阻燃剂的合成及其在棉纤维中的应用

以二氯磷酸苯酯(1)和γ-氨丙基三乙氧基硅烷(2)为原料，合成了一种新型的P－N－Si三元无卤阻燃剂--苯氧基-双-(三乙氧基硅丙基)磷酰胺(3),其结构经¹H NMR， ³¹P NMR和FT-IR表征。研究了溶剂，反应温度，反应时间，投料比r［n(2) : n(1)］和缚酸剂对3产率的影响。结果表明:在最佳合成条件［THF为溶剂，三乙胺为缚酸剂，1 8 mmol， r=2.4，于40 ℃反应6 h］下, 3的产率为88.2%。利用TGA测试了3的阻燃性能。结果表明：3的初始分解温度为150 ℃， 600 ℃残炭为14.6%。3在棉纤维(c)中的添加量为15%(质量百分数，即c-3¹⁵)时，600 ℃残炭为33.4%，高于c(7.6%)。

Synthesis of A Novel P-N-Si Halogen-free Flame Retardant and Its Application in Cotton Fiber

A novel ternary integrated P－N－Si halogen-free flame retardant, phenoxy-bis-(triethoxysilylpropyl)phosphamide(3), was synthesized by the reaction of phenylphosphonic dichloride(1) with (3-aminopropyl)triethoxysilane(2). The structure was characterized by ¹H NMR， ³¹P NMR and FT-IR. Effects of solvent, reaction temperature, reaction time, acid-blinding agent and molar ratio{r［n(2) n(1)］} on the yield of 3 were investigated. The results showed that the optimum reaction condition at 40 ℃ for 6 h were as followed: 1 was 8 mmol, r was 2.4, THF was solvent and trithylamine was acid-blinding agent. The yield of 3 was 88.2% under the optimum reaction conditions. The flame retardant property of 3 was characterized by TGA. The results indicated that the initial decomposition temperature of 3 was 150 ℃ and the char residue is about 14.6% at 600 ℃. Cotton fabrics(c) were treated with 3. The char residue of c-3¹⁵ (the mass portion of 3 was 15% in c) at 600 ℃ was 33.4%, which was better than c(7.6%).