Quantification of Irgafos P-168 and Degradative Profile in Samples of a Polypropylene/Polyethylene Composite Using Microwave, Ultrasound and Soxhlet Extraction Techniques

J. Hernández‐Fernández, Jaime Pérez-Mendoza, Rodrigo Ortega-Toro
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Abstract

In polypropylene/polyethylene composite (C-PP/PE) production, stabilizing additives such as Irgafos P-168 are essential as antioxidant agents. In this study, an investigation was carried out that covers different solid–liquid extraction methods (Soxhlet, ultrasound, and microwaves); various variables were evaluated, such as temperature, extraction time, the choice of solvents, and the type of C-PP/PE used, and the gas chromatography coupled to mass spectrometry (GC-MS) technique was used to quantify the presence of Irgafos P-168 in the C-PP/PE samples. The results revealed that microwave extraction was the most effective in recovering Irgafos P-168. A recovery of 96.7% was achieved when using dichloromethane as a solvent, and 92.83% was achieved when using limonene as a solvent. The ultrasound technique recovered 91.74% using dichloromethane and 89.71% using limonene. The Soxhlet extraction method showed the lowest recovery percentages of 57.39% using dichloromethane as a solvent and 55.76% with limonene, especially when the C-PP/PE was in the form of pellets. The degradation products that obtained the highest degradation percentages were Bis (di-test-butyl phenyl) phosphate and Mono (di-test-butyl phenyl) phosphate using the microwave method with dichloromethane as a solvent and PP in film. Finally, the possible mechanisms for forming the degradation compounds of Irgafos P-168 were postulated.
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利用微波、超声波和索氏提取技术定量聚丙烯/聚乙烯复合材料样品中的伊尔加福斯 P-168 和降解曲线
在聚丙烯/聚乙烯复合材料(C-PP/PE)生产中,Irgafos P-168 等稳定添加剂作为抗氧化剂是必不可少的。本研究对不同的固液萃取方法(索氏提取法、超声波提取法和微波提取法)进行了调查;对温度、萃取时间、溶剂的选择和使用的 C-PP/PE 类型等各种变量进行了评估,并使用气相色谱-质谱联用(GC-MS)技术对 C-PP/PE 样品中的伊尔加福斯 P-168 进行了定量。结果表明,微波萃取是回收伊尔加福斯 P-168 的最有效方法。以二氯甲烷为溶剂的回收率为 96.7%,以柠檬烯为溶剂的回收率为 92.83%。超声波技术使用二氯甲烷的回收率为 91.74%,使用柠檬烯的回收率为 89.71%。索氏提取法的回收率最低,以二氯甲烷为溶剂时为 57.39%,以柠檬烯为溶剂时为 55.76%,尤其是当 C-PP/PE 为颗粒状时。在以二氯甲烷为溶剂、聚丙烯为薄膜的微波法中,降解率最高的降解产物是磷酸二(二试丁基苯基)酯和磷酸单(二试丁基苯基)酯。最后,对 Irgafos P-168 降解化合物的可能形成机制进行了推测。
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