摘要
以无水哌嗪、DOPO、四氯化碳为原料制备了磷氮阻燃剂6,6’-(哌嗪-1,4-二基)双(6H-二苯并[c,e][1,2]氧杂磷苯-6-氧化物)(PiP-DOPO),通过红外光谱与核磁共振对其结构进行了表征。将其用于阻燃环氧树脂,通过热重分析(TG)对PiP-DOPO与环氧树脂复合材料的热性能进行了表征,通过氧指数(LOI)、垂直燃烧(UL94)及锥形量热测试对环氧树脂复合材料的阻燃性能进行了表征,通过扫描电镜(SEM)对环氧树脂复合材料残炭形貌进行了表征。结果表明,当体系中磷的质量分数为1.50%时,TG测试表明,600℃时体系残炭量由23.02%(EP-0)增加至25.23%(EP-3)(N2氛围),LOI为27.5,UL94测试为V-0级,最大热释放速率(PHRR)由622.8kW/m2降至325.0kW/m2,总热释放量(THR)由121.8 MJ/m2降至76.8 MJ/m2,SEM表明PiP-DOPO的加入能够明显改变环氧体系残炭的表面形貌,PiPDOPO对环氧树脂有良好的阻燃效果。
The phosphorus-nitrogen flame retardant 6,6′-（piperazine-1,4-diyl）bis（6 H-dibenzo[c,e][1,2]oxophosphate-6-oxide）PiP-DOPO was synthesized using piperazine,9,10-2 H-9-oxa-10-phospaphenanthrene-10-oxide（DOPO）and carbon tetrachloride as raw materials.Its structure was characterized by FT-IR and1 H-NMR,and PiP-DOPO was used to flame retarded epoxy resin（EP）.The thermal properties of PiP-DOPO and cured products were investigated by TGA,flame retardant properties were characterized by limit oxygen index（LOI）,vertical burning test（UL 94）and cone calorimeter test（CCT）,and the residual carbon morphology was investigated by SEM.The results show that when the phosphorus content is 1.50%in the EP system,the carbon residue rate could reach 25.23% from 23.02%（pure EP）at 600 ℃（in N2 atmosphere）,the LOI reaches 27.5,the UL 94 passes V-0 level,the PHRR is 325.0 kW/m^2,THR is 76.8 MJ/m^2.And the SEM result reveals that the addition of PiP-DOPO can obviously improve the carbon residue morphology after combustion.So,the PiP-DOPO can enhance the flame retardant properties of epoxy resin.
作者
王志国
梁兵
刘徐越
Zhiguo Wang;Bing Liang;Xuyue Liu(School of Materials Science and Engineering,Shenyang University of Chemical Technology,Shenyang 110142,China)
出处
《高分子材料科学与工程》
EI
CAS
CSCD
北大核心
2018年第8期149-153,160,共6页
Polymer Materials Science & Engineering
基金
国家国际科技合作与交流专项资助项目(2013DFA51200)
辽宁省科学技术计划项目(2015304002)
关键词
环氧树脂
阻燃
磷氮阻燃剂
复合材料
热性能
epoxy resin
flame retardance
phosphorus nitrogen flame retardant
composites
thermal properties
