肖滕,刘睿,罗子依,文啸锋,易妮,于雯琪,王玮,刘诚.磷氮阻燃剂DOPO-AN的合成及其阻燃环氧研究[J].井冈山大学自然版,2023,44(3):38-44 |
磷氮阻燃剂DOPO-AN的合成及其阻燃环氧研究 |
Synthesis of Phosphorus-nitrogen Flame Retardant DOPO-AN and ITS flame retardant modified epoxy resin |
投稿时间:2023-01-15 修订日期:2023-03-17 |
DOI:10.3969/j.issn.1674-8085.2023.03.006 |
中文关键词: DOPO 环氧树脂 阻燃性能 热性能 力学性能 |
英文关键词: DOPO epoxy resin flame retardant property thermal property mechanical property |
基金项目:国家自然科学基金项目(21802057,22262015);江西省自然科学基金项目(20224BAB204008,20212BAB213020);江西省教育厅科技计划项目(GJJ2201648) |
作者 | 单位 | E-mail | 肖滕 | 井冈山大学化学化工学院, 江西, 吉安 343009 | | 刘睿 | 井冈山大学化学化工学院, 江西, 吉安 343009 | | 罗子依 | 井冈山大学化学化工学院, 江西, 吉安 343009 | | 文啸锋 | 井冈山大学化学化工学院, 江西, 吉安 343009 | | 易妮 | 井冈山大学化学化工学院, 江西, 吉安 343009 | | 于雯琪 | 井冈山大学化学化工学院, 江西, 吉安 343009 | | 王玮 | 井冈山大学化学化工学院, 江西, 吉安 343009 | | 刘诚 | 井冈山大学化学化工学院, 江西, 吉安 343009 | liucheng@jgsu.edu.cn |
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中文摘要: |
以9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO),2-氨基蒽醌(AN)和多聚甲醛(POM)为原料,通过一锅法合成了一种新型磷氮阻燃剂2-(N,N-二(9,10-二氢-9-氧杂-10-磷杂菲-10基)甲基)氨基蒽醌(DOPO-AN)。利用核磁共振谱(1H-NMR、31P-NMR)、红外光谱(FTIR)对其分子结构进行表征,并将DOPO-AN用于阻燃改性环氧树脂(EP)。运用差示扫描量热法、万能力学试验机、氧指数仪、垂直燃烧仪分别研究了DOPO-AN/EP复合材料的力学性能、热稳定性、阻燃性能。结果表明,阻燃剂DOPO-AN能明显改善环氧树脂的阻燃性和热稳定性。当体系磷元素质量分数为0.67%时(DOPO-AN/EP-8%),800 ℃时残炭率由0.45%增加到7.9%;极限氧指数(LOI)随阻燃剂量的增加而增加,由纯环氧树脂的25.3%提高到30.1%,垂直燃烧UL94等级达到V-0级。力学性能结果表明,环氧树脂的拉伸强度由836 MPa增加至863 MPa,说明DOPO-AN的加入对EP的力学性能影响不大。 |
英文摘要: |
A novel flame retardant, 2-(N, N- bis(9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-yl) methyl) aminoanthraquinone (DOPO-AN), was synthesized by using 9,10-dihydro-9-oxa-10- phosphenanthrene-10-oxide (DOPO), 2-aminoanthraquinone (AN), polyoxymethylene (POM) as the raw materials. Its structure was characterized by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance spectroscopy (1H-NMR, 31P-NMR), and then DOPO-AN was used as the flame retardant to modify epoxy resin (EP). The mechanical properties, thermal properties, flame retardant properties of DOPO-AN/EP composites were investigated respectively. The results showed that the flame retardancy and thermal properties of epoxy resin were obviously improved by DOPO-AN. When the mass fraction of phosphorus was 0.67 wt.% (DOPO-AN/EP-8%), the char yield of DOPO-AN/EP-8% was increased to 7.9% at 800 ℃. The oxygen index (LOI) increased from 25.3% to 30.1% with the increase of DOPO-AN; the vertical combustion grade UL94 reached V-0 level. The results of mechanical property showed that the tensile strength of epoxy resin increased from 836 MPa to 863 MPa, indicating that the mechanical properties of EP unacted on DOPO-AN loading. |
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