摘要
本文通过甲基膦酸和无水哌嗪反应制备中间体二甲基膦酸哌嗪,将其与新戊二醇进行酯化反应,制备出新型单分子膨胀阻燃剂甲基膦酸-哌嗪-新戊二醇齐聚物(MPPNGO),通过傅里叶红外光谱(FTIR)对其结构进行了表征。通过热重分析(TGA)对阻燃剂MPPNGO的热稳定性及成炭性能进行了表征。测试结果表明,合成物MPPNGO的起始分解温度为233.1℃,在600oC时的残炭量为12 wt%,表明MPPNGO具有良好的热稳定性,可以满足聚乙烯(PE)的加工要求。将阻燃剂MPPNGO添加到PE中制备阻燃PE材料。通过极限氧指数(LOI)和垂直燃烧(UL-94)对材料的阻燃性能进行了表征;通过TGA对阻燃PE的热降解行为进行了分析,通过FTIR对阻燃PE的残炭进行了分析。结果表明:当MPPNGO添加17 wt%时,3.2mm的样品达到了UL-94 V-0级,LOI为23.7%,表明MPPNGO阻燃性能优异。TGA测试表明:MPPNGO的加入促进了材料的提前降解和成炭,提高了材料在高温时的热稳定性。残炭的FTIR测试表明,阻燃PE材料燃烧后,阻燃剂中的磷以磷氧化物的形式留在了炭层中,起到了加固炭层的作用,有利于材料阻燃性能的提高。
In this paper,the intermediate of dimethylphosphonic acid piperazine was firstly prepared from the original materials of methylphosphonic acid and anhydrous piperazine,then the prepared intermediatereacted with neopentyl glycol by the esterification,and the novel single molecular intumescent flame retardant methylphosphonic acid-piperazine-neopentyl glycol oligomer(MPPNGO)was obtained.The structure was characterized by Fourier transform infrared spectroscopy(FTIR).The thermal stability and charring performance of the flame retardants were investigated by thermogravimetric analysis(TGA).The results indicate that the initial thermal decomposition temperature of MPPNGO is 233.1 oC,and the char residue at 600℃is 12 wt%,which reveals that the obtained MPPNGO possess excellent thermal stability and charring ability,and the flame retardant can meet the processing requirements of polyethylene(PE).The prepared MPPNGO were incorporated into PE by melt-mixing to prepare flame retardant PE thermoplastics,then the flame retardancy of the PE composites wasinvestigated by limiting oxygen index(LOI)and vertical buming(UL-94)tests,,the thermal decomposition behaviorof materials wasinvestigated by thermogravimetric analysis(TGA),the char residue was characterized by Fourier transform infrared spectroscopy(FTIR).The results reveal that the samples with the thickness of 3.2 mm can pass UL-94 V-0 flammability ratingwhen the total loading amount IFR is 17 wt%and the LOI value is 23.7%,which indicates that theprepared MPPNGO possesses high flame retardant efficiency for PE materials.The results of thermogravimetric analysis(TGA)show that the addition.of MPPNGO can promote the degradation and carbonization of the materials and improve.the thermal stability of PE thermoplastics at high temperature.The FTIR of the char residue reveals that phosphorus in flame retardants remain in the char layer by the formation of phosphorus oxides,which effectively reinforces the char layer.Consequently,the flame retardancy of the PE composites were enhanced.
作者
张建鑫
高春鹏
ZHANG Jianxin;GAO Chunpeng(Harbin FRP Institute Co.,Ltd,Harbin 150028)
出处
《纤维复合材料》
CAS
2018年第4期16-20,共5页
Fiber Composites
关键词
单分子膨胀阻燃剂
阻燃
聚乙烯
热降解
single molecular intumescent flame retardant
fire retardant
polyethylene
thermal decomposition
