三聚氰胺-环三磷腈阻燃剂的制备及其应用  

Preparation and Application of Cyclotriphosphazene Modified with Etherized Hexamethylolmelamine

作　　者：吕梅香[1] 廖添 宋亭[1] 曾健[1] 曾和平[1] 

机构地区：[1]华南师范大学化学与环境学院,广州510006

出　　处：《华南师范大学学报（自然科学版）》2015年第2期78-83,共6页Journal of South China Normal University(Natural Science Edition)

基　　金：广东省自然科学基金项目(S2013020013091)

摘　　要：磷腈化合物是一类无卤、对环境友好且具有生物相容性的低毒性阻燃剂,但大部分磷腈衍生物是油溶性的,需要通过熔融共混、辊轧等方式才能制成阻燃纤维、塑料,操作工艺复杂,无法直接用于天然纤维,因此大大限制了其应用范围.该文以六羟甲基三聚氰胺和六氯环三磷腈为原料,通过亲核取代、醚化两步法合成了一种水溶性、醇溶性无卤磷腈阻燃剂.用红外光谱(FT-IR)、核磁共振谱(1H NMR、13C NMR、31P NMR)和电喷雾电离质谱(ESIMS)等进行了结构表征,证明其为无氯、P螺原子链接的目标化合物.将该阻燃剂用95%乙醇溶解,配成4种浓度梯度(5%、10%、15%、20%)的阻燃溶液,浸泡布料(医用纯棉纱布、化纤窗帘布)获得阻燃布,用热重分析仪(TGA)在氮气氛下对阻燃布料的热性能进行了分析,结果表明,该阻燃剂热稳定性较高,残碳率高达41.8%.阻燃布料点燃后最高残碳率达44.2%,极限氧指数(LOI)比未阻燃前提高了29.6%,对织物有较好的阻燃性能;仅含阻燃剂质量分数为3.0%的窗帘布点燃后不再有熔滴出现,有较好的抗熔滴效果.The phosphazene-based compounds are halogen-free and environmentally-friendly. Some of them are biocompatible and can be used as flame resistant materials. However,these compounds often lack water-soluble. Some reports attempted to produce a fire-retardant product by using melt blending or padding processes to combine the polymer with the textile. They can＇t be directly applied in natural fibers and are not desirable for some uses. In this paper,we synthesized the water / ethanol-soluble,nonhalogenated cyclotriphosphazene derivative flame retardant（ FR） with etherized hexamethylolmelamine and hexachloro-cyclotriphosphazene via a two-step nucleophilic substitution approach. It was characterized by infrared spectroscopy（ FT-IR）,nuclear magnetic resonance spectroscopy of1 H NMR,13 C NMR,31 P NMR and electrospray ionisation mass spectrometry（ ESI-MS）. It was proved that this new compound was a free chlorine and spirocyclic phosphazene-based target compound. The novel compound has good solubility in alcohol（ 95%） too. Cotton gauze and curtain cloth were soaked in four alcohol solutions of the flame retardant（ 5%,10%,15% and 20%） to obtain flame retardant gauze and flame retardant curtain cloth. Their thermal stabilities were tested under nitrogen using a thermogravimetric analyzer and were compared with both the raw material and the textile samples. The results demonstrated that the flame retardant textile had good thermal stability and the char yield up to 41. 8%. The flame retardant capability of the treated cotton gauze and curtain cloth was investigated by limiting oxygen index（ LOI） and flame test,the LOI value of treated samples increased 29. 6%than pure cotton gauze,a char yield of 44. 2% when burned in air. The curtain cloth of 3. 00% retardant had no molten dropping down in fire,which further improved the excellent flame resistance of the new flame retardant.

关 键 词：六羟甲基三聚氰胺 六氯环三磷腈 阻燃 熔滴 热性能 

分 类 号：TQ265.1[化学工程—有机化工]