| 引用本文: | 廖庆玲,马福民,付勇军,谭行,曾黎明,冯帮余.含马来酰亚胺结构的DOPO基反应型阻燃剂的合成及其对环氧树脂性能的影响[J].材料科学与工艺,2023,31(3):63-70.DOI:10.11951/j.issn.1005-0299.20220125. |
| LIAO Qingling,MA Fumin,FU Yongjun,TAN Xing,ZENG Liming,FENG Bangyu.Synthesis of DOPO-based reactive flame retardant containing maleimide structure and its effect on epoxy resin[J].Materials Science and Technology,2023,31(3):63-70.DOI:10.11951/j.issn.1005-0299.20220125. |
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| 摘要: |
| 以9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)和N-对羧基苯基马来酰亚胺(pCPMI)为主要原料合成了一种新型的反应型阻燃剂DOPO-pCPMI,利用傅里叶变换红外光谱(FT-IR),核磁共振谱(1H-NMR、31P-NMR)对阻燃剂分子的结构及其组成进行了分析表征。随后将DOPO-pCPMI与环氧树脂预聚,再以4,4’-二氨基二苯基砜(DDS)为固化剂制备DOPO-pCPMI/EP复合材料。通过极限氧指数(LOI)、动态热机械分析(DTMA)、热失重分析研究了复合材料的阻燃性能和热性能。结果表明:当pCPMI的质量分数为6%时,DOPO-pCPMI/EP固化体系综合性能最佳,氧指数由24%提高至33.5%；玻璃化转变温度(Tg)为210 ℃；弯曲强度由90 MPa提升至127 MPa；在氮气气氛下不同组分树脂的浇铸体残炭率不断提高。对燃烧后炭层的红外分析和扫描电子显微镜(SEM)分析表明形成了含马来酰亚胺的刚性炭层,且炭层外部紧凑、完整,内部致密、多孔。 |
| 关键词: DOPO N-对羧基苯基马来酰亚胺 阻燃 环氧树脂 残炭 |
| DOI：10.11951/j.issn.1005-0299.20220125 |
| 分类号:TB332 |
| 文献标识码:A |
| 基金项目:湖北省教育厅指导性项目(B2019225)；湖北理工学院人才引进项目(18XJZ02R). |
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| Synthesis of DOPO-based reactive flame retardant containing maleimide structure and its effect on epoxy resin |
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LIAO Qingling1, MA Fumin1, FU Yongjun1, TAN Xing2, ZENG Liming2, FENG Bangyu3
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(1. School of Materials Science and Engineering, Hubei Polytechnic University, Huangshi 435003, China; 2. School of Materials Science and Engineering, Wuhan University of Technology, Wuhan 430070, China; 3. Huangshi Fuxing Aluminum Co., Ltd., Huangshi 435003, China)
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| Abstract: |
| A novel reactive flame retardant (DOPO-pCPMI) was synthesized by the reaction between N-(p-carboxyphenyl) maleimide and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO). The structure and composition were characterized by FT-IR and nuclear magnetic resonance spectroscopy (1H-NMR and 31P-NMR). Prepolymer was obtained by mixing DOPO-pCPMI with epoxy resin, and then DOPO-pCPMI/EP composites were prepared with 4,4’-diaminodiphenyl sulfone (DDS) as curing agent. The flame retardancy and thermal property of DOPO-pCPMI/EP composites were investigated by limiting oxygen index (LOI), dynamic thermomechanical analysis (DTMA), and thermogravimetric analysis. Results show that when the content of pCPMI was 6%, DOPO-pCPMI/EP composites exhibited the best integrated performances, and LOI increased from 24% to 33.5%. The glass transition temperature (Tg) was 210 ℃. The bending strength increased from 90 MPa to 127 MPa. The char yields of resins with different components in nitrogen atmosphere were increased. The structures of char residues after burning were analyzed by FTIR and SEM. It shows that a rigid char layer containing maleimide was formed. The exterior char residue was compact and complete, and the interior char residue was dense and porous. |
| Key words: DOPO N-(p-carboxyphenyl) maleimide flame retardant epoxy resin char |
