Synthesis of sulfur containing polyphosphazene micro-nano sphere and its application in flame retarded epoxy resin
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摘要: 以六氯环三磷腈(HCCP)、4,4'-二羟基二苯硫醚(TDP)为原料合成了一种环交联型的聚磷腈(PTP)微纳米球,并将其加入到环氧树脂(EP)中制备成PTP微纳米球/EP(PTP/EP)复合材料,研究其阻燃性能。采用FTIR和SEM对PTP微纳米球进行表征;TG分析考察PTP/EP复合材料的热稳定性;极限氧指数(LOI)和锥型量热分析(CONE)对PTP/EP复合材料进行阻燃性能测试。研究结果表明,PTP微纳米球具有不溶不熔的特性,粒径在500 nm~3 μm之间,且拥有优异的热稳定性和成炭性,起始热分解温度高达453.2℃,800℃残炭为74.3%。PTP微球的加入显著提高了EP的阻燃性能。当PTP微纳米球添加量仅为5wt%时,PTP/EP的热释放速率峰值降低了55.43%;LOI值从纯EP的25.6%提高到了30.4%。PTP微球的加入还提高了EP的力学性能。PTP微纳米球因其不溶不熔的特点在EP中充当增强剂,在受热燃烧时充当高效的阻燃剂。本研究为功能性阻燃剂的研发提供了新思路。Abstract: The cyclic crosslinking poly(cyclotriphosphazene-co-4,4'-thiobisphenol) (PTP) micro-nano spheres were synthesized using hexachlorocyclotriphosphazene (HCCP) and 4,4'-thiobisphenol (TDP) as raw materials. The obtained PTP spheres were applied in flame retarded epoxy resin (EP) to prepare PTP/EP composites. The PTP spheres were characterized by FTIR and SEM. The thermal stability of PTP/EP composites was investigated by TG, and the flame retardancy was carried out by limiting oxygen index test (LOI) and cone calorimetry (CONE) tests. The results show that the PTP spheres are neither soluble in any organic solvents nor meltable at high temperature. The sphere size is about 500 nm-3 μm and possesses excellent thermal stability and charring ability. The initial decomposition temperature is as high as 453.2℃ and the char residue is 74.3% at 800℃. The addition of PTP spheres can significantly improve the flame retardancy of EP. The peak heat release rate (PHRR) of PTP/EP composite is reduced by 55.43% and the LOI value is increased from 25.6% to 30.4% when merely 5wt% of PTP added. The addition of PTP microspheres also enhanced the mechanical strength of EP. The mechanical strength of PTP/EP composites is also improved with the incorporation of PTP spheres. The PTP spheres can act as a reinforcing agent at room temperature due to the insolubility and infusibility, and also acts as the flame retardant under combustion. The study provides a new ideas and methods for functional flame retardants.
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Keywords:
- phosphazene /
- micro-nano spheres /
- flame retardant /
- epoxy resin /
- functionality /
- microstructure /
- composites
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