{"title":"利用先进的光谱技术重新研究含有 APP/季戊四醇/zeolite-4A的阻燃聚丙烯的膨胀机理","authors":"Matthieu Caron , Karima Ben Tayeb , Serge Bourbigot , Gaëlle Fontaine","doi":"10.1016/j.polymdegradstab.2024.111040","DOIUrl":null,"url":null,"abstract":"<div><div>The mixture of ammonium polyphosphate (APP) and pentaerythritol (PER) is a very efficient flame retardant (FR) intumescent system suitable for polyolefins such as polypropylene (PP). The mechanisms of intumescence of this FR system in this polymer was investigated using different spectroscopic techniques including continuous wave (CW) electron paramagnetic resonance (EPR) spectroscopy and solid state nuclear magnetic resonance (NMR) technique. In this work, the intumescence mechanism of PP/APP/PER formulations with and without 4A is revisited. The intumescent system was in-depth investigated using NMR, CW EPR and pulsed EPR. The CW EPR technique confirmed that free radicals are mainly generated during the intumescence of the system between 250 and 350 °C. Thanks to the pulsed EPR and solid state NMR, it was evidenced that a key structural shift from a predominantly carbonaceous residue to a predominantly phosphorated residue. Besides, it was also evidenced that zeolite 4A totally collapses during extrusion of PP/APP/PER formulations reacting with APP to generate aluminophosphates. Then, silicophosphates are generated between 350 and 400 °C. Both alumino- and silicophosphates contribute to protect aromatic structures in the residue at high temperatures.</div></div>","PeriodicalId":406,"journal":{"name":"Polymer Degradation and Stability","volume":"230 ","pages":"Article 111040"},"PeriodicalIF":6.3000,"publicationDate":"2024-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Re-examination of the intumescence mechanism of fire retarded PP with APP/pentaerythritol/zeolite-4A using advanced spectroscopic techniques\",\"authors\":\"Matthieu Caron , Karima Ben Tayeb , Serge Bourbigot , Gaëlle Fontaine\",\"doi\":\"10.1016/j.polymdegradstab.2024.111040\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>The mixture of ammonium polyphosphate (APP) and pentaerythritol (PER) is a very efficient flame retardant (FR) intumescent system suitable for polyolefins such as polypropylene (PP). The mechanisms of intumescence of this FR system in this polymer was investigated using different spectroscopic techniques including continuous wave (CW) electron paramagnetic resonance (EPR) spectroscopy and solid state nuclear magnetic resonance (NMR) technique. In this work, the intumescence mechanism of PP/APP/PER formulations with and without 4A is revisited. The intumescent system was in-depth investigated using NMR, CW EPR and pulsed EPR. The CW EPR technique confirmed that free radicals are mainly generated during the intumescence of the system between 250 and 350 °C. Thanks to the pulsed EPR and solid state NMR, it was evidenced that a key structural shift from a predominantly carbonaceous residue to a predominantly phosphorated residue. Besides, it was also evidenced that zeolite 4A totally collapses during extrusion of PP/APP/PER formulations reacting with APP to generate aluminophosphates. Then, silicophosphates are generated between 350 and 400 °C. Both alumino- and silicophosphates contribute to protect aromatic structures in the residue at high temperatures.</div></div>\",\"PeriodicalId\":406,\"journal\":{\"name\":\"Polymer Degradation and Stability\",\"volume\":\"230 \",\"pages\":\"Article 111040\"},\"PeriodicalIF\":6.3000,\"publicationDate\":\"2024-10-15\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Polymer Degradation and Stability\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0141391024003835\",\"RegionNum\":2,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"POLYMER SCIENCE\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Polymer Degradation and Stability","FirstCategoryId":"92","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0141391024003835","RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"POLYMER SCIENCE","Score":null,"Total":0}
Re-examination of the intumescence mechanism of fire retarded PP with APP/pentaerythritol/zeolite-4A using advanced spectroscopic techniques
The mixture of ammonium polyphosphate (APP) and pentaerythritol (PER) is a very efficient flame retardant (FR) intumescent system suitable for polyolefins such as polypropylene (PP). The mechanisms of intumescence of this FR system in this polymer was investigated using different spectroscopic techniques including continuous wave (CW) electron paramagnetic resonance (EPR) spectroscopy and solid state nuclear magnetic resonance (NMR) technique. In this work, the intumescence mechanism of PP/APP/PER formulations with and without 4A is revisited. The intumescent system was in-depth investigated using NMR, CW EPR and pulsed EPR. The CW EPR technique confirmed that free radicals are mainly generated during the intumescence of the system between 250 and 350 °C. Thanks to the pulsed EPR and solid state NMR, it was evidenced that a key structural shift from a predominantly carbonaceous residue to a predominantly phosphorated residue. Besides, it was also evidenced that zeolite 4A totally collapses during extrusion of PP/APP/PER formulations reacting with APP to generate aluminophosphates. Then, silicophosphates are generated between 350 and 400 °C. Both alumino- and silicophosphates contribute to protect aromatic structures in the residue at high temperatures.
期刊介绍：
Polymer Degradation and Stability deals with the degradation reactions and their control which are a major preoccupation of practitioners of the many and diverse aspects of modern polymer technology.
Deteriorative reactions occur during processing, when polymers are subjected to heat, oxygen and mechanical stress, and during the useful life of the materials when oxygen and sunlight are the most important degradative agencies. In more specialised applications, degradation may be induced by high energy radiation, ozone, atmospheric pollutants, mechanical stress, biological action, hydrolysis and many other influences. The mechanisms of these reactions and stabilisation processes must be understood if the technology and application of polymers are to continue to advance. The reporting of investigations of this kind is therefore a major function of this journal.
However there are also new developments in polymer technology in which degradation processes find positive applications. For example, photodegradable plastics are now available, the recycling of polymeric products will become increasingly important, degradation and combustion studies are involved in the definition of the fire hazards which are associated with polymeric materials and the microelectronics industry is vitally dependent upon polymer degradation in the manufacture of its circuitry. Polymer properties may also be improved by processes like curing and grafting, the chemistry of which can be closely related to that which causes physical deterioration in other circumstances.
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