六苯氧基环三磷腈的合成及其热稳定性研究  

Research on synthesis and thermal stability of hexa(phenoxy) cyclotriphosphazene

作　　者：宝冬梅[1,2] 刘吉平[2] 谢兵[1] 潘羽[1] 卢运贤 王化彪 

机构地区：[1]贵州民族大学化学与环境科学学院,贵阳550025 [2]北京理工大学材料学院,北京100081

出　　处：《功能材料》2016年第5期165-169,173,共6页Journal of Functional Materials

基　　金：国家自然科学基金资助项目(21362005);贵州省科技厅-贵州民族大学联合基金资助项目(黔科合LH字[2014]7381号);贵州省2014年大学生创新创业训练计划资助项目(201410672004)

摘　　要：六苯氧基环三磷腈(HPCTP)是一种环境友好型阻燃剂,因具有良好的耐热性和阻燃性而备受关注。以六氯环三磷腈(HCCP)、苯酚和氢氧化钠为原料制备HPCTP,经红外光谱(IR)、X射线衍射分析(XRD)、核磁共振(NMR)、元素分析(EA)、质谱分析(MS)、差热(DSC)和热重(TG)等分析手段对产物的结构和热稳定性进行了表征,并考察了反应温度、反应时间和投料比例3个因素对HPCTP收率的影响。结果表明,以THF为溶剂,n(苯酚)∶n(NaOH)=1∶1,n(苯酚)∶n(HCCP)=8∶1,65℃回流反应48h,HPCTP的收率为92.0%。热稳定性研究表明,HPCTP的热稳定性较好,在N_2气氛下的起始分解温度为365℃,适合作为阻燃剂添加到聚合物基材中,而且可以将其应用到对加工温度要求比较高的体系中去。Hexa(phenoxy)cyclotriphosphazene(HPCTP)was an environmentally friendly flame retardant and it has attracted significant attention because of its excellent heat-resistance and flame-resistance.In the study,HPCTP was synthesized by the reaction of hexachlorocyclotriphosphazene(HCCP)with phenol and sodium hydroxide,and characterized by means of infrared spectrometer(IR),X-Ray diffraction(XRD),nuclear magnetic resonance(NMR),elemental analysis(EA),mass spectrometry(MS),differential scanning calorimetry(DSC)and thermogravimetry(TG).The influences of reaction temperature(T),reaction time(t)and raw material ratio on the yield of HPCTP were investigated.The results showed when n(phenol)∶n(sodium hydroxide)=1∶1,n(phenol)∶n(HCCP)=8∶1,T=65℃,t=48h,THF as solvent,the yield of HPCTP was the highest and amounted up to 92.0%.Thermal analysis results showed that the onset decomposition temperature of HPCTP was 365 ℃.Therefore,HPCTP was a flame retardant with perfect thermal stability,and it can be applied in high processing temperature system.

关 键 词：六苯氧基环三磷腈 合成 热稳定性 

分 类 号：O627.5[理学—有机化学]