摘要
六对醛基苯氧基环三磷腈(HAPCP)是一种重要的无卤高效阻燃剂和精细化工中间体,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)和对羟基苯甲醛为原料制备HAPCP,经红外光谱(IR)、核磁共振(NMR)、元素分析、差热(DSC)和热重(TG)等测试分析手段对产物的结构和热性能进行了表征,并考察了溶剂、缚酸剂、原料配比、反应时间和反应温度对HAPCP收率的影响。结果表明,在四氢呋喃中,以无水碳酸钾为缚酸剂,n(对羟基苯甲醛)∶n(六氯环三磷腈)=7.2∶1,65℃下反应24h,HAPCP的收率可达92.5%。热性能研究表明,HAPCP在N2气氛下的起始分解温度为270℃,800℃时残炭率仍有78.5%,是一种耐热性和热稳定性好的无机-有机杂环化合物,在绝热材料和阻燃材料领域呈现出良好的应用前景。
Hexakis（4-formacylphenoxy） cyclotriphosphazene（HAPCP） was an important efficient halogen free flame retardant and fine chemical intermediate and it has attracted significant attention because of its excellent heat-resistance and flame-resistance.In the study,HAPCP was prepared via the reaction of hexachlorocyclotriphosphazene（HCCP） and 4-hydroxybenzaldehyde,and characterized by means of infrared spectrometer（IR）,nuclear magnetic resonance（NMR）,elemental analysis,differential scanning calorimetry（DSC） and thermogravimetry（TG）.The influences of the reactive solvent,type and particle size of deacid reagent,molar ratio of p-hydroxybenzaldehyde to HCCP,reaction time（t） and reaction temperature（T） on the yield were investigated.The results showed when n（p-hydroxybenzaldehyde）∶n（HCCP）=7.2∶1,T= 65℃,t=24h,tetrahydrofuran as solvent and anhydrous sodium carbonate as deacid reagent,the yield of HAPCP was the highest and amounted up to 92.5%.Thermal analysis results showed that the onset decomposition temperature of HAPCP was 270℃,and the carbon yield at 800℃ was still up to 78.5%.Therefore,HAPCP was an inorganic-organic heterocyclic compound with perfect heat-resistance and thermal stability,and it is a promising candidate applied in insulating materials and flame retardant materials.
出处
《功能材料》
EI
CAS
CSCD
北大核心
2013年第3期396-400,共5页
Journal of Functional Materials
基金
国家教育部"蓝火计划"资助项目(20110941023)
贵州省科学技术基金资助项目(黔科合J字[2011]2074号)
贵州民族大学2012年校级科研资助项目(2012JS008)
关键词
六对醛基苯氧基环三磷腈
合成
热性能
hexakis（4-formacylphenoxy） cyclotriphosphazene
synthesis
thermal properties
