新型反应型P-N膨胀型阻燃剂的合成及其在棉织物中的应用

Synthesis of a novel reacting P-N intumescence flame retardant andits application in cotton fabrics

摘要:

以三聚氯氰、亚磷酸三乙酯和丙三醇为原料合成了一种新型结构的反应型P-N膨胀型阻燃剂三氧代(3-亚磷酸乙酯-5-氯-1-三嗪)丙三醇(TTCTG),并通过红外光谱(FTIR)、核磁共振氢谱和磷谱分析对其进行了结构表征,热重分析(TGA)表明TTCTG有优良的热稳定性能。以TTCTG为原料对棉纤维进行了阻燃改性,通过极限氧指数(LOI)和垂直燃烧实验测试表明当阻燃整理液中TTCTG的质量浓度为20%时,阻燃整理后棉织物(20%TTCTG-CF)的氧指数为27.3,阻燃等级可达国家标准B1级,TGA分析表明TTCTG在284℃便能促进棉织物快速分解成炭,700℃下的残炭率高达为35.7%,扫描电镜(SEM)分析发现20%TTCTG-CF燃烧后,其表面形成了致密的膨胀炭层,TTCTG阻燃整理后的棉纤维表现出了优异的阻燃性能。耐水性研究表明水洗20次后的20%TTCTG-CF的阻燃等级仍可达B1级,极限氧指数可达26.4,通过SEM和FTIR对水洗20次后20%TTCTG-CF进行结构分析,研究表明TTCTG与棉纤维通过共价键相连而融为一体,赋予棉纤维优良持久的阻燃性能。

Abstract:

A novel reacting P-N intumescence flame retardant, trioxo (3-triethylphosphite- 5-chlorine- 1-triazine) glycerin (TTCTG), has been synthesized and the molecular structure was characterized by FTIR, H NMR, and 31P NMR. The thermal degradation property of TTCTG was assessed by TGA, which revealed that it was good thermal stability on the high temperature condition. The flame retardancy of cotton fabrics with different TTCTG content was investigated by using TGA, vertical flammability test, LOI, and SEM,the results showed that when the content of TTCTG was 20%, the limiting oxygen index of 20%TTCTG-CF was up to 27.3%, the flame retardancy reached the class B1 of national standard of flame retardant fabrics．The TGA results indicated TTCTG could promote the rapid decomposition of cotton fabric into char at 284 ℃, SEM showed that the surface of 20%TTCTG-CF formed the dense expansive carbon layer after combustion. After washing for 20 times, the LOI of 20%TTCTG-CF was still as high as 26.4%, reaching class B1 of national standard of flame retardant fabrics. The structure of 20%TTCTG-CF after 20 washing times was analyzed by SEM and FTIR, and the results showed that TTCTG and cotton fiber were linked by covalent bond, which gave cotton fiber excellent and lasting flame retardancy.