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- 2017
六（γ-氨丙基硅烷三醇）环三磷腈的制备及其在膨胀阻燃聚丙烯中的应用
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Abstract:
以六氯环三磷腈、对羟基苯甲醛及γ-氨丙基硅烷三醇（KH553）为反应原料，合成了具有席夫碱结构的有机硅型成炭剂六（γ-氨丙基硅烷三醇）环三磷腈（HKHPCP）。以HKHPCP与聚磷酸铵（APP）的复配物为抗熔滴剂，以N-烷氧基受阻胺（NOR116）为阻燃协效剂，通过熔融共混技术制备了膨胀阻燃聚丙烯（PP）基复合材料（APP-HKHPCP-NOR116/PP）。利用FTIR、核磁共振（1H和31P NMR）对HKHPCP的化学结构进行了表征。采用热失重、极限氧指数、垂直燃烧、锥形量热、拉曼光谱和SEM研究了阻燃体系的热降解行为、阻燃性能及炭层的石墨化程度和致密性。HKHPCP的热失重结果表明，其在氧气氛围下的初始分解温度为300.2℃，1 000℃时残余率为34.8%。当添加总量为30wt%的阻燃剂时，APP-HKHPCP-NOR116/PP复合材料的极限氧指数（LOI）达到43%，且能通过UL-94 V-0级，其热释放速率（HRR）、总热释放速率（THR）及烟释放速率（SPR）、总烟释放量（TSP）相比于纯PP分别降低了75.0%、50.5%和88.0%、80.8%，表现出显著的隔热、抑烟性能。APP-HKHPCP-NOR116/PP复合材料燃烧后形成了高石墨化、致密的炭层。 A novel charring agent named as hexakis (γ-aminopropylsilanetriol) cyclotriphosphazene (HKHPCP) was synthesized by using hexachlorocyclotriphosphazene (HCCP), p-hydroxy benzaldehyde and γ-aminopropylsilanetriol (KH553). The intumescent flame retardant polypropylene (PP) matrix composites (APP-HKHPCP-NOR116/PP) was prepared using HKHPCP and ammonium polyphosphate (APP) as the anti-dripping agent and N-alkoxy hindered amine (NOR116) as the synergistic agent by the melt compounding method. The chemical structures of intermediate and HKHPCP were characterized by FTIR, 1H nuclear magnetic resonance (1H NMR) and 31P NMR. The effects of the flame retardant APP-HKHPCP-NOR116/PP on the thermal degradation, flame retardancy and char layer structure were investigated by thermogravimetric analysis (TGA), limiting oxygen index (LOI), vertical burning test (UL-94), cone calorimetric test, SEM and laser Raman spectroscopy, respectively. The TGA results show that the temperature of 5% mass loss of HKHPCP in oxygen is 300.2℃, and the residues at 1 000℃ of HKHPCP in oxygen is 34.8%. The results show that the LOI value of APP-HKHPCP-NOR116/PP is 43%, while the intumescent flame retardant loading is 30wt%. The APP-HKHPCP-NOR116/PP could reach a V-0 rating in the UL-94 tests. The cone calorimetry results indicate that heat release rate (HRR), total heat release (THR), smoke produce rate (SPR) and total smoke production (TSP) are reduced by 75.0%, 50.5%, 88.0% and 80.8%, respectively. In addition, the APP-HKHPCP-NOR116/PP can form a compact and more graphitic carbon char layer during combustion. 国家自然科学基金面上项目（51473024）
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