摘要:
以三（2-羟乙基）异氰尿酸酯（THEIC）和苯氧基磷酰二氯（PDCP）为主要原料，合成了一种新型磷氮型阻燃剂（PNFR），借助FTIR、核磁共振光谱（1H-NMR、31P-NMR）对其结构与组成进行了表征。将PNFR与聚磷酸铵（APP）复配用于制备聚磷酸铵-新型磷氮型阻燃剂阻燃聚氨酯泡沫（APP-PNFR/PUF）复合材料，通过极限氧指数（LOI）、垂直燃烧测试、锥形量热和热失重分析对APP-PNFR/PUF复合材料的阻燃性能和热性能进行了研究。结果表明：成功获得了PNFR；此外，PNFR的TGA表明PNFR在N2气氛下的初始分解温度为249℃，800℃时的残炭量可达33.7%，其具有较高的热稳定性能。APP-PNFR的加入能有效改善PUF的阻燃性能，且当PNFR的添加量与组合聚醚的质量比为7.5%时，可获得综合性能较好的阻燃PUF材料，其中LOI从19%提高至24%，UL-94垂直燃烧等级达到V-0级，热释放速率峰值从110.6 kW/m2降低到94.5 kW/m2；同时，APP-PNFR/PUF3在N2气氛下的初始分解温度提高了6℃，最大分解速率降低了16.3%，800℃时的残炭量可达33.5%。PNFR的加入不会削弱PUF的物理力学性能。
Abstract:
A novel flame retardant containing phosphorus and nitrogen (PNFR) was synthesized by the reaction between 1, 3, 5-tris(2-hydroxyethyl)isocyanurate(THEIC) and phenyl dichlorophosphate(PDCP), and its structure and composition were characterized by FTIR, nuclear magnetic resonance spectroscopy (1H-NMR and 31P-NMR), respectively. PNFR was compounded with ammonium polyphosphate(APP) applied to prepare ammonium polyphosphate-novel flame retardant and polyurethane foam (APP-PNFR/PUF) composites, and the flame retardancy and thermal property of APP-PNFR/PUF composites were respectively investigated by limiting oxygen index (LOI), vertical burning testing, cone calorimeter testing and thermogravimetric analysis. The results show that the PNFR is successfully prepared. TGA of PNFR suggests that it has good thermal stability with initial degradation temperature 249℃, and the residue of PNFR is 33.7% at 800℃ under nitrogen atmosphere. The addition of APP-PNFR effectively enhances the flame retardany of polyurethane foam(PUF), and especially when the loading amount of PNFR is 7.5% based on the premixed polyether polyols' weight, the APP-PNFR/PUF has optimum comprehensive properties with LOI increasing from 19% to 24%, and UL-94 vertical burning grade reaching V-0 level. Meanwhile, the peak heat release rate of APP-PNFR/PUF3 decreases from 110.6 kW/m2 to 94.5 kW/m2. Additionally, the initial degradation temperature of APP-PNFR/PUF3 increases by 6℃, maximum decomposition rate decreases by 16.3%, and the residue is 33.5% at 800℃ under nitrogen atmosphere. The incorporation of PNFR does not impair the physical mechanical property of PUF.
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