Abdalrhem Hossamaldin Ahmed Omer, Pan Yueyue, Gu Hongda, Ao Xiang, Ji Xiaohuan, Jiang Xiaoze, Sun Bin
State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, College of Materials Science and Engineering, Donghua University, Shanghai 201620, China.
Changshu Polyester Co., Ltd., Changshu 215535, China.
Polymers (Basel). 2023 Jan 28;15(3):662. doi: 10.3390/polym15030662.
To obtain industrialized poly(ethylene terephthalate) (PET) composites with highly efficient flame retardancy, a phosphorus-nitrogen (P-N) containing hyperbranched flame retardant additive was synthesized by 9,10-dihydro-9-oxa-10-phospho-phenanthrene-butyric acid (DDP) and tris(2-hydroxyethyl) isocyanurate (THEIC) through high temperature esterification known as hyperbranched DDP-THEIC (hbDT). The chemical structure of the synthesized hbDT was determined by FTIR, H NMR, C NMR, and GPC, etc. Subsequently, hbDT/PET composites were prepared by co-blending, and the effects of hbDT on the thermal stability, flame retardancy, combustion performance, and thermal degradation behavior of PET were explored to deeply analyze its flame retardant mechanism. The test results showed that hbDT was successfully synthesized, and that hbDT maintained thermal stability well with the required processing conditions of PET as retardant additives. The flame retardant efficiency of PET was clearly improved by the addition of hbDT via the synergistic flame-retardant effect of P and N elements. When the mass fraction of flame retardant was 5%, the LOI of the hbDT/PET composite increased to 30.2%, and the vertical combustion grade reached UL-94 V-0. Compared with pure PET, great decreased total heat release (decreased by 16.3%) and peak heat release rate (decreased by 54.9%) were exhibited. Finally, the flame retardant mechanism of hbDT/PET was supposed, and it was confirmed that retardant effect happened in both the gas phase and condensed phase. This study is expected to provide a new idea for the development of low toxic, environment-friendly and highly efficient flame retardant additive for polyesters in an industry scale.
为了获得具有高效阻燃性的工业化聚对苯二甲酸乙二酯（PET）复合材料，通过9,10 - 二氢 - 9 - 氧杂 - 10 - 磷杂菲 - 丁酸（DDP）和三（2 - 羟乙基）异氰脲酸酯（THEIC）经高温酯化反应合成了一种含磷 - 氮（P - N）的超支化阻燃添加剂，即超支化DDP - THEIC（hbDT）。通过傅里叶变换红外光谱（FTIR）、氢核磁共振（H NMR）、碳核磁共振（C NMR）和凝胶渗透色谱（GPC）等手段确定了合成的hbDT的化学结构。随后，通过共混制备了hbDT / PET复合材料，并探究了hbDT对PET的热稳定性、阻燃性、燃烧性能和热降解行为的影响，以深入分析其阻燃机理。测试结果表明，hbDT成功合成，并且作为阻燃添加剂，hbDT在PET所需的加工条件下具有良好的热稳定性。通过P和N元素的协同阻燃作用，添加hbDT明显提高了PET的阻燃效率。当阻燃剂的质量分数为5%时，hbDT / PET复合材料的极限氧指数（LOI）提高到30.2%，垂直燃烧等级达到UL - 94 V - 0。与纯PET相比，总热释放量大幅降低（降低了16.3%），热释放峰值速率大幅降低（降低了54.9%）。最后，推测了hbDT / PET的阻燃机理，并证实阻燃作用发生在气相和凝聚相。本研究有望为聚酯类低毒、环保且高效的工业规模阻燃添加剂的开发提供新思路。
