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六对醛基苯氧基环三磷腈的合成及其热性能研究

         

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 hexachlorocyclot-riphosphazene(HCCP) and 4-hydroxybenzaldehyde, and characterized by means of infrared spectrometer (IR) , nuclear magnetic resonance (NMR), elemental analysis, differential scanning calorimetry(DSC) and thermo-gravimetry (TG). The influences of the reactive solvent, type and particle size of deacid reagent, molar ratio of p-hydroxybenzaldehyde to HCCP, reaction timed) 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 heter-ocyclic compound with perfect heat-resistance and thermal stability, and it is a promising candidate applied in insulating materials and flame retardant materials.

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