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Synthesis and characterization of a novel charring agent and its application in intumescent flame retardant polypropylene system

机译:新型炭化剂的合成,表征及其在膨胀型阻燃聚丙烯体系中的应用

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摘要

A novel halogen-free charring agent bi(4-methoxy-1-phospha-2, 6, 7-trioxabicyclo [2.2.2]-octane-1-sulfide) phenylphosphate (BSPPO) was synthesized from phenylphosphonic dichloride (PPDC), and 4-hydroxymethyl-1- phospha-2, 6, 7-trioxabicyclo[2.2.2]-octane-1-sulfide (SPEPA) which was synthesized from pentaerythritol and thiophosphoryl chloride in this article. The structure of BSPPO and SPEPA was characterized by Fourier transform infrared (FTIR), ~1H-NMR, ~(13)C-NMR, and ~(31)P-NMR. Combined with ammonium polyphosphate (APP) and melamine pyrophosphate (MPP), the flame retardance and dripping resistance of BSPPO added in polypropylene (PP) were investigated. The fire performance of the flame retardant PP system was investigated by limiting oxygen index (LOI), vertical burning test (UL-94), and cone calorimeter. The thermal stabilities of the composites were studied by thermogravimetric analysis (TGA). The flame retardance mechanism was investigated by FTIR and scanning electronic micrograph (SEM). The mechanical properties and water solubility were also investigated. The residue of BSPPO is 40.6% at 600°C, which indicates BSPPO has excellent charring ability. The char residue of the polypropylene intumescent flame retardant (PP-IFR) system is 22% at 600°C, which suggests that the flame retardation synergy of APP, BSPPO, and MPP is good. With the optimum formulation, the LOI of the IFR-PP system is 32.0, and the UL-94 is V-0 rating. The heat release rate (HRR), total heat release (THR), smoke production rate (SPR), total smoke production (TSP), and mass loss rate (MLR) of IFR-PP with the optimum formulation decrease significantly comparing to pure PP from cone calorimeter analysis. The FTIR and SEM results indicate that the char properties and the char yield have direct effect on the flame retardance and antidripping behaviors.
机译:新型的无卤炭化剂双(4-甲氧基-1-磷-2,6,7-三氧杂双环[2.2.2]-辛烷-1-硫醚)苯基磷酸酯(BSPPO)由苯基膦酸二氯化物(PPDC)合成,并本文由季戊四醇和硫代磷酰氯合成了4-羟基甲基-1-磷酸2-,6、7-三氧杂双环[2.2.2]-辛烷-1-硫化物(SPEPA)。 BSPPO和SPEPA的结构通过傅立叶变换红外(FTIR),〜1H-NMR,〜(13)C-NMR和〜(31)P-NMR表征。结合多磷酸铵(APP)和三聚氰胺焦磷酸盐(MPP),研究了聚丙烯(PP)中添加的BSPPO的阻燃性和抗滴落性。通过极限氧指数(LOI),垂直燃烧试验(UL-94)和锥形量热仪研究了阻燃PP系统的防火性能。通过热重分析(TGA)研究了复合材料的热稳定性。通过FTIR和扫描电子显微镜(SEM)研究了阻燃机理。还研究了机械性能和水溶性。 BSPPO在600°C时的残留率为40.6%,这表明BSPPO具有出色的炭化能力。聚丙烯膨胀型阻燃剂(PP-IFR)系统的炭渣在600°C下为22%,这表明APP,BSPPO和MPP的阻燃协同作用良好。采用最佳配方,IFR-PP系统的LOI为32.0,UL-94为V-0等级。与纯PP相比,具有最佳配方的IFR-PP的放热率(HRR),总放热(THR),烟雾产生率(SPR),总烟雾产生(TSP)和质量损失率(MLR)显着降低来自锥形量热仪分析。 FTIR和SEM结果表明,炭的性质和炭的收率对阻燃性和抗滴落行为具有直接影响。

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