Synthesis and flame-retardant analysis of a novel P/N containing flame retardant on epoxy resin composites

IF 2 4区 材料科学 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Fire and Materials Pub Date : 2024-01-26 DOI:10.1002/fam.3200
Vishal Soni, Jai Bhagwan Dahiya
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引用次数: 0

Abstract

A new reactive flame-retardant N′-(1-(4-hydroxyphenyl)-1-(6-oxido-6H-dibenzo[c,e][1,2]oxaphosphinin-6-yl)ethyl) benzohydrazide (DOPO-BD) was synthesized via a two-step reaction involving the Schiff base reaction between benzohydrazide and 4-hydroxy acetophenone, followed by a reaction between the imine-based condensation product and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO). The chemical structure of DOPO-BD was well characterized by Fourier transform infrared spectra (FTIR), 1H, 13C, 31P NMR, and high-resolution mass spectrometry (HRMS). The DOPO-BD was utilized as a reactive flame retardant and co-hardener in DGEBA/DDS. The epoxy composites of varying phosphorus weight percentages were synthesized. UL-94 and LOI tests were used to investigate the flammability of composites. The epoxy composites retained good transparency, which was measured by UV–vis spectroscopy. Thermogravimetric analysis (TGA) observed an increase in the thermal stability of epoxy composites in a higher temperature range with increased char yield. In the UL-94 and LOI tests, EP/DOPO-BD(1.5%P) sample gave a V-0 rating and 30% LOI value. The cone calorimeter test indicated a decrease in total heat released (THR), peak of heat release rate (pHRR), and total smoke production (TSP) for EP/DOPO-BD(1.5%P) in comparison with epoxy (EP). The mechanical properties and glass transition temperature (Tg) of the epoxy composites were determined by Dynamic mechanical analysis (DMA), which showed an increase in storage modulus and a decrease in Tg.

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新型环氧树脂复合材料阻燃剂 P/N 的合成与阻燃性分析
一种新型活性阻燃剂 N′-(1-(4-羟基苯基)-1-(6-氧代-6H-二苯并[c,e][1,2]氧磷杂环庚烷-6-基)乙基) 苯酰肼 (DOPO-BD) 是通过苯酰肼与 4-羟基苯乙酮之间的希夫碱反应,然后通过亚胺基缩合产物与 9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物 (DOPO) 的两步反应合成的、随后,亚胺基缩合产物与 9,10-二氢-9-氧杂-10-磷菲-10-氧化物(DOPO)发生反应。傅立叶变换红外光谱(FTIR)、1H、13C、31P NMR 和高分辨质谱(HRMS)对 DOPO-BD 的化学结构进行了表征。DOPO-BD 在 DGEBA/DDS 中用作活性阻燃剂和共硬化剂。合成了不同磷重量百分比的环氧树脂复合材料。采用 UL-94 和 LOI 测试来研究复合材料的可燃性。环氧树脂复合材料保持了良好的透明度,并通过紫外可见光谱进行了测量。热重分析(TGA)表明,随着炭产量的增加,环氧树脂复合材料在较高温度范围内的热稳定性有所提高。在 UL-94 和 LOI 测试中,EP/DOPO-BD(1.5%P) 样品的 V-0 级和 LOI 值分别为 30%。锥形量热仪测试表明,与环氧树脂(EP)相比,EP/DOPO-BD(1.5%P)的总释放热量(THR)、热释放率峰值(pRR)和总产烟量(TSP)均有所下降。通过动态力学分析(DMA)测定了环氧树脂复合材料的力学性能和玻璃化转变温度(Tg),结果表明储存模量增加,Tg 下降。
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来源期刊
Fire and Materials
Fire and Materials 工程技术-材料科学:综合
CiteScore
4.60
自引率
5.30%
发文量
72
审稿时长
3 months
期刊介绍: Fire and Materials is an international journal for scientific and technological communications directed at the fire properties of materials and the products into which they are made. This covers all aspects of the polymer field and the end uses where polymers find application; the important developments in the fields of natural products - wood and cellulosics; non-polymeric materials - metals and ceramics; as well as the chemistry and industrial applications of fire retardant chemicals. Contributions will be particularly welcomed on heat release; properties of combustion products - smoke opacity, toxicity and corrosivity; modelling and testing.
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