含磷氮原子有机硅聚合物的制备及性能研究

Preparation and properties of organosilicon polymers containing phosphorus and nitrogen atoms

以八甲基环四硅氧烷、氨基硅烷偶联剂等为原料,通过开环聚合反应制备了氨基硅油中间体(AS),再用AS与苯基膦酰二氯进行亲核取代反应合成含磷氮原子的有机硅聚合物(PSiNP)。用红外光谱(IR)、核磁共振氢谱(1HNMR)、热重分析对PSiNP进行结构和性能表征,研究了反应温度、反应时间、溶剂种类以及投料比n(NH2)∶n(PCl)对处理织物阻燃性和柔软性的影响。结果表明:合成PSiNP较佳条件为反应温度10℃,反应时间1 h,溶剂苯,n(NH2)∶n(PCl)=2.0∶1.0。未处理织物、AS处理织物、PSiNP处理织物的弯曲刚度分别为403、168、195 mN;燃烧时间分别为7.47、8.10、9.34 s;600℃残余量分别为5.9%、6.3%、7.5%。

Amino silicone oil (AS) was prepared by ring-opening polymerization using octamethylcyclo-tetrasiloxa ne, amino silane coupli ng age nt as raw materials. The orga no silic on polymer (PSiNP) containing phos phorus and nitrogen atoms was synthesized by nucleophilic substitution of AS and phenyIphosphonic dichloride. The structure and properties of PSiNP were characterized by infrared spectroscopy (IR), 1HNMR and thermogravimetric analysis. Effects of reaction temperature, reaction time, solvent type and feed ratio [n(NH2): n(PCI)] on the flame retardancy and softness of fabrics after finishing were studied. The results showed that the optimum conditions for synthesis of PSiNP were as follows: reaction temperature 10 ℃, reaction time 1 h, solvent ben zene, n(NH2)- n(PCI)=2.0: 1.0. The ben ding stiff ness of un treated fabrics, AS treated fabrics and PSiNP treated fabrics were 403, 168 and 195 mN, the burning time was 7.47, 8.10 and 9.34 s, and the residual at 600 ℃ was 5.9%, 6.3% and 7.5%, respectively.