双基阻燃剂DOPS-TEAIC的合成及阻燃环氧树脂的性能  

Synthesis of Flame Retardant DOPS-TEAIC with Double Functional Groups and Its Properties of Flame Retardant Epoxy Resin

作　　者：胥秋 侯泽明 宦宣英 祁钰昭 许松江 宝冬梅[1] 高成涛[2] 邹光龙[1] 张玉鹏 文竹 Qiu Xu;Zeming Hou;Xuanying Huan;Yuzhao Qi;Songjiang Xu;Dongmei Bao;Chengtao Gao;Guanglong Zou;Yupeng Zhang;Zhu Wen(School of Chemical Engineering,Guizhou Minzu University,Guiyang 550025,China;National Engineering Research Center for Compounding and Modification of Polymer Materials,Guiyang 550014,China)

机构地区：[1]贵州民族大学化学工程学院,贵州贵阳550025 [2]国家复合改性聚合物材料工程技术研究中心,贵州贵阳550014

出　　处：《高分子材料科学与工程》2024年第9期74-85,共12页Polymer Materials Science & Engineering

基　　金：国家自然科学基金资助项目(51863004);贵州省省级科技计划项目(CXTD[2021]005,黔科合成果(2023)一般051,黔科合支撑[2024]一般048)。

摘　　要：以9,10-二氢-9-氧杂-10-磷杂菲-10-硫化物(DOPS)与三(2-丙烯酰氧乙基)异氰脲酸酯(TEAIC)为原料,合成了一种新型双基阻燃剂三(2-(9,10-二氢-9-氧杂-10-磷杂菲-10-硫化物)-丙酸乙酯基)三嗪三酮(DOPS-TEAIC)。采用傅里叶变换红外光谱、核磁共振和质谱确定其结构,并将其应用于环氧树脂(EP)制备了EP/DOPS-TEAIC。采用热重分析、垂直燃烧、极限氧指数、锥形量热、热重-红外光谱联用和热裂解-气相色谱/质谱联用等手段研究了阻燃剂DOPS-TEAIC对EP的热稳定性、阻燃性能及热降解行为的影响,并深入分析了其阻燃机理。结果表明,阻燃剂DOPS-TEAIC能够提高EP的热稳定性、残炭量和阻燃性能,降低其热释放速率峰值(PHRR)和平均热释放速率(av-HRR)。当DOPS-TEAIC的质量分数为10.0%时,EP/DOPS-TEAIC的LOI值提高至33.4%,达到UL-94 V-0级,其PHRR和av-HRR值比纯EP分别降低了34.2%和22.8%。阻燃剂DOPS-TEAIC主要通过稀释作用和自由基猝灭作用在气相发挥阻燃作用。A novel flame retardant with double functional groups tris(2-(9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-sulfide)-ethyl propionate-based)triazine-trione(DOPS-TEAIC)was synthesized from 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-sulfide(DOPS)with tris(2-acryloxyethyl)isocyanurate(TEAIC).Its structure was determined by Fourier transform infrared spectroscopy,nuclear magnetic resonance and mass spectrometry,and it was applied in epoxy resin(EP)to prepare EP/DOPS-TEAIC.The effects of DOPS-TEAIC on the thermal stability,flame retardancy and thermal degradation behavior of EP were studied by thermogravimetric analysis,vertical combustion,limiting oxygen index,cone calorimeter,thermogravimetric-infrared spectroscopy and pyrolysis gas chromatography-mass spectrometry,and the flame retarding mechanism was deeply analyzed.The results show that flame retardant DOPS-TEAIC can improve the thermal stability,char residue content and flame retardancy of EP,and reduce its peak heat release rate(PHRR)and average heat release rate(av-HRR).When the mass fraction of DOPS-TEAIC is 10.0%,the LOI value of EP/DOPS-TEAIC increases to 33.4%,reaching UL-94 V-0 level,and its PHRR and av-HRR values are decreased by 34.2%and 22.8%respectively,compared to pure EP.The flame retardant DOPS-TEAIC plays a flame retardant role in gas phase mainly through dilution and free radical quenching.

关 键 词：9 10-二氢-9-氧杂-10-磷杂菲-10-硫化物 三嗪三酮 环氧树脂 阻燃性能 阻燃机理 

分 类 号：TQ323.5[化学工程—合成树脂塑料工业]