六(4-硝基苯氧基)环三磷腈的合成及其热稳定性研究

六(4-硝基苯氧基)环三磷腈(HNCTP)是一种环境友好型阻燃剂,因具有良好的耐热性和阻燃性而备受关注。以六氯环三磷腈(HCCP)、对硝基苯酚为原料合成了HNCTP,经傅里叶红外光谱(FT-IR)、核磁共振(NMR)、元素分析(EA)、热重-差示扫描量热分析(TGA-DSC)等分析手段对产物的结构和热稳定性进行了表征,并考察了反应溶剂、投料比例和反应时间3个因素对HNCTP收率的影响。结果表明,以丙酮为溶剂,n(对硝基苯酚)∶n(HCCP)=9∶1,56℃回流反应18h,HNCTP的收率为90.5%。热稳定性研究表明,HNCTP的热稳定性较好,在N2气氛下的初始分解温度为371.5℃,可作为添加型阻燃剂应用于聚合物基材中,而且适用于加工温度较高的体系。

Research on synthesis and thermal stability of hexa(4-nitrophenoxy)cyclotriphosphazene

Hexa(4-nitrophenoxy) cyclotriphosphazene (HNCTP) is an environmentally friendly flame retardant and it has attracted significant attention because of its excellent heat-resistance and flame-resistance. In the study, HNCTP was synthesized by the reaction of hexachlorocyclotriphosphazene (HCCP) with 4-nitrophenol, and characterized by means of Fourier transform infrared spectroscopy (FT-IR),nuclear magnetic resonance (NMR), elemental analysis (EA), thermogravimetric analysis and differential scanning calorimetry (TGA-DSC). The influences of solvent, raw material ratio and reaction time ( t ) on the yield of HNCTP were investigated. The results showed when n (4-nitrophenol)∶ n (HCCP)=9∶1, T =56 ℃, t = 18 h, acetone as solvent, the yield of HNCTP was the highest and amounted up to 90.5%.Thermal analysis results showed that the onset decomposition temperature of HNCTP was 371.5 ℃. Therefore, HNCTP is a flame retardant with perfect thermal stability, and it can be applied in high processing temperature system.