Synthesis of a Phosphorus-Based Epoxy Reactive Flame Retardant Analog to Diglycidyl Ether of Bisphenol A (DGEBA) and its Behavior as a Matrix in a Carbon Fiber Composite
Synthesis of a Phosphorus-Based Epoxy Reactive Flame Retardant Analog to Diglycidyl Ether of Bisphenol A (DGEBA) and its Behavior as a Matrix in a Carbon Fiber Composite
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DOI：
10.1016/j.polymdegradstab.2022.110144
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发表时间：
2022-09
影响因子：
5.9
通讯作者：
Mustafa Mukhtar;D. Klosterman;V. Benin;A. Morgan
中科院分区：
文献类型：
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作者：
Mustafa Mukhtar;D. Klosterman;V. Benin;A. Morgan
本文介绍了一种磷基阻燃剂的合成，它是双酚a二甘油酯醚（DGEBA）的化学类似物，并将其作为基体掺入碳纤维层压板中。碳纤维复合材料，如果用于大规模运输车辆（飞机、火车）的结构应用，将需要在某些方面改进防火性能，以便在这些应用中安全使用。第一阶段的工作涉及开发两种不同的合成路线来生产阻燃单体，称为磷- dgeba或简称为P-DGEBA。第二步是通过各种实验混合配方和与脂肪胺固化剂的固化条件来确定化合物聚合行为的可行性。采用差示扫描量热法（DSC）评价了P-DGEBA与脂肪胺固化剂混合时的固化行为，并采用动态力学分析（DMA）观察了碳纤维复合材料的玻璃化转变温度（Tg）。热重分析（TGA）研究了P-DGEBA/DGEBA共混物的热稳定性和热降解行为。最后一步包括复合材料的制造和他们的可燃性测试使用锥形量热计。P-DGEBA的DMA测试测得的热重比基于DGEBA的碳纤维复合材料高10°C， DSC研究发现，P-DGEBA / DGEBA共混物与胺固化剂有很好的聚合。TGA、MCC和锥量热仪的数据得出了不同的结果，TGA和MCC表明P-DGEBA具有更强的凝聚相/焦相阻燃活性，而锥量热仪显示P-DGEBA具有更强的气相阻燃活性。总的来说，P-DGEBA作为环氧+碳纤维复合材料的反应性FR表现出一定的前景，但还需要更多的研究。
This paper describes the synthesis of a phosphorus-based flame retardant that is a chemical analog of diglycidyl ether of bisphenol A (DGEBA), as well as its incorporation as a matrix into carbon fiber laminates. Carbon fiber composites, if used for structural applications in mass transport vehicles (aircraft, trains), will require some aspects of improved fire performance to be used safely in those applications. The first phase of work involved the development of two separate synthesis routes to produce the flame retardant monomer, referred to as Phosphorus-DGEBA or simply P-DGEBA. The second step was to determine the viability of the compound's polymerization behavior through various experimental mixing formulations and curing conditions with an aliphatic amine curing agent. Differential scanning calorimetry (DSC) was used to evaluate the curing behavior of P-DGEBA when mixed with DGEBA and an aliphatic amine curing agent and dynamic mechanical analysis (DMA) was used to observe the glass transition temperature (Tg) of the carbon fiber composites. Thermogravimetric analysis (TGA) was also used to investigate the thermal stability and thermal degradation behaviors of the P-DGEBA/DGEBA blends. The final step included the fabrication of composites and their flammability testing using a cone calorimeter. DMA testing for P-DGEBA measured a Tgthat was 10 °C higher than a DGEBA based carbon fiber composite, and DSC studies found that the P-DGEBA / DGEBA blend polymerized well with the amine curing agent. The TGA, MCC, and cone calorimeter data yielded mixed results with TGA and MCC suggesting a more condensed phase / char formation flame retardant activity for P-DGEBA, while cone calorimeter suggested a more vapor phase flame retardant activity. Overall, the P-DGEBA shows some promise as a reactive FR for epoxy + carbon fiber composites, but more study is needed.