| 引用本文: | 张君营,张志永,冷洋,李晓丽.HVPA-DOPO与二乙基次膦酸铝协同阻燃环氧树脂研究[J].材料科学与工艺,2025,33(3):21-28.DOI:10.11951/j.issn.1005-0299.20230336. |
| ZHANG Junying,ZHANG Zhiyong,LENG Yang,LI Xiaoli.HVPAP-DOPO and aluminum diethylphosphinate synergistic flame retardant epoxy resin[J].Materials Science and Technology,2025,33(3):21-28.DOI:10.11951/j.issn.1005-0299.20230336. |
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| 摘要: |
| 为了获得一种阻燃性能良好的环氧树脂固化物,本文以六氯环三磷腈、香草醛、乙醇胺和9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)为原料合成了一种新型阻燃剂六-(N-羟乙基氨基-DOPO-次甲基-2-甲氧基-苯氧基)-环三磷腈(HVPA-DOPO),通过傅里叶变换红外(FT-IR)与核磁共振波谱(1H-NMR和31P-NMR)进行了结构表征。将其与二乙基次膦酸铝(ADP)复配后用于环氧树脂阻燃,利用热重分析(TG)研究了复合材料的稳定性。通过极限氧指数(LOI)、垂直燃烧(UL-94)、锥形量热测试研究了材料的阻燃性能,利用扫描电镜(SEM)观察了炭层的形貌。研究表明,在环氧树脂中加入HVPA-DOPO和ADP,800 ℃下复合材料的残炭量增加到19%,LOI达到33.1%并通过UL-94 V-0级,热释放速率峰值(PHRR)和总热释放(THR)分别降低到450.6 kW/m2和70.9 MJ/m2,扫描电镜(SEM)测试说明复配阻燃体系能形成膨胀致密的炭层,所有测试结果表明二种阻燃剂复配提高了环氧树脂的阻燃性能。 |
| 关键词: 环氧树脂 环三磷腈大分子 DOPO ADP 阻燃性能 |
| DOI：10.11951/j.issn.1005-0299.20230336 |
| 分类号:TQ323.5 |
| 文献标识码:A |
| 基金项目:国家自然科学基金资助项目(52103251). |
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| HVPAP-DOPO and aluminum diethylphosphinate synergistic flame retardant epoxy resin |
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ZHANG Junying, ZHANG Zhiyong, LENG Yang, LI Xiaoli
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(Heilongjiang Key Laboratory of Molecular Design and Preparation of Flame Retarded Materials, College of Chemistry, Chemical Engineering and Resource Utilization, Northeast Forestry University, Harbin 150040, China)
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| Abstract: |
| In order to obtain an epoxy resin curing material with good flame retardancy, a novel flame retardant hexa-(N-hydroxyethylamino-DOPO-methylene-2-methoxy-phenoxy)-cyclotriphosphazene(HVPA-DOPO) was synthesized from phosphonitrilic chloride trimer, vanillin, ethanolamine and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO). Its structure was characterized by Fourier transform infrared (FT-IR) and nuclear magnetic resonance spectroscopy (1H-NMR and 31P-NMR). Then HVPA-DOPO and aluminum diethylphosphonate (ADP) were combined to flame retard epoxy resin. The thermal stability was studied by thermogravimetric analysis (TG), and the flame retardant properties of the flame retarded composite were investigated through limiting oxygen index (LOI), UL-94 vertical combustion and cone calorimetry. The morphology of the carbon layers was observed by scanning electron microscopy (SEM). The results show that the addition of HVPA-DOPO and ADP to epoxy resin increases the residual char of the composites to 19% at 800 °C, while the LOI reaches 33.1% and passes UL-94 V-0. The peak heat release rate (PHRR) and total heat release rate (THR) decrease to 450.6 kW/m2 and 70.9 MJ/m2 respectively. SEM tests indicate that the compound flame retardants forms an expanded and dense carbon layer. The test results indicate that the combination of the two flame retardants enhances the flame retardancy of the epoxy resin. |
| Key words: epoxy resin cyclotriphosphazene macromolecule DOPO ADP flame retardant properties |
