季膦萘磺酸盐离子液体与甲基膦酸二甲酯协同阻燃环氧树脂  

Synergistic Flame-retardant Epoxy Resin Using Quaternary Phosphate Naphthalene Sulfonate Ionic Liquid and Dimethyl Methylphosphonate

作　　者：张璐[1,2] 刘杰[2] 娄生辉[2] 江惠 王松 李三喜[1] 唐涛[2] 张爱玲[1] ZHANG Lu;LIU Jie;LOU Shenghui;JIANG Hui;WANG Song;LI Sanxi;TANG Tao;ZHANG Ailing(School of Environmental and Chemical Engineering,Shenyang University of Technology,Shenyang 110870,China;State Key Laboratory of Polymer Physics and Chemistry,Changchun Institute of Applied Chemistry,Chinese Academy of Sciences,Changchun 130022,China)

机构地区：[1]沈阳工业大学环境与化学工程学院,沈阳110870 [2]中国科学院长春应用化学研究所高分子物理与化学国家重点实验室,长春130022

出　　处：《高等学校化学学报》2024年第4期159-168,共10页Chemical Journal of Chinese Universities

基　　金：国家自然科学基金(批准号:22075274,51991353,51991350)资助。

摘　　要：合成了一种新型季膦萘磺酸盐室温离子液体[TBP]NS,利用傅里叶变换红外光谱(FTIR)和核磁共振波谱(1H NMR和31P NMR)确定了其结构,并将其与甲基膦酸二甲酯(DMMP)复配用于制备阻燃环氧树脂.阻燃性能测试结果表明,当在环氧树脂(EP)中加入质量分数为6%的[TBP]NS和4%的DMMP时,所得阻燃环氧树脂EP/4%[TBP]NS/6%DMMP的极限氧指数达到31.2%, UL-94垂直燃烧通过V-0级别.与纯环氧树脂相比,该阻燃环氧树脂的峰值热释放速率(PHRR)降低了59%,总热释放(THR)降低了43%,峰值CO释放速率(PCOP)降低了41%,残炭率升高了97%.[TBP]NS和DMMP在氧指数、垂直燃烧和锥形量热测试中均展现出优异的协同阻燃作用,并且表现出良好的炭化能力和降热效果.在力学性能方面,与单纯加入DMMP的环氧树脂相比,EP/4%[TBP]NS/6%DMMP的拉伸强度、断裂伸长率和弯曲强度均有提高.A novel room temperature ionic liquid of quaternary phosphate naphthalene sulfonate([TBP]NS)was synthesized.The structure of[TBP]NS was determined by Fourier transform infrared spectroscopy(FTIR)and nuclear magnetic resonance spectroscopy(1H NMR and 31P NMR).[TBP]NS was combined with dimethyl methylphosphonate(DMMP)to prepare flame-retardant epoxy resin.The flame-retardant results showed that when 6%(mass fraction)of[TBP]NS and 4%(mass fraction)of DMMP were added into epoxy resin(EP),the limiting oxygen index of the flame-retardant EP reached 31.2%,and EP/6%[TBP]NS/4%DMMP passed the UL-94 vertical combustion V-0 level. Compared with pure EP, the EP/6%[TBP]NS/4%DMMP showed a 59% reduction in peak heat release rate(PHRR), a 43% reduction in total heat release rate(THR), a 41% reduction in peak carbon monoxide release rate(PCOP), and a 97% increase in char yield. [TBP]NS and DMMP showed excellent synergistic flame retardancy in both the gaseous phase and the condensed phase, and good charring ability and heat reduction effect. In terms of mechanical properties, the tensile strength, elongation at break and bending strength of the EP/6%[TBP]NS/4%DMMP were all improved compared with those of the EP with DMMP alone.

关 键 词：环氧树脂 液体阻燃剂 离子液体 甲基膦酸二甲酯 

分 类 号：O631[理学—高分子化学]