双环膦酸酯的合成、表征及其阻燃RPUF的热解动力学分析  

Synthesis and characterization of bicyclic phosphonate and its pyrolysis kinetics analysis of flame retardant RPUF

作　　者：邓杰 孙佳鑫 赵泽熙 孙泽营 孙才英[1] Deng Jie;Sun Jiaxin;Zhao Zexi;Sun Zeying;Sun Caiying(Heilongjiang Key Laboratory Molecular Design and Preparation of Flame Retarded Materials,College of Chemistry,Chemical Engineering and Resource Utilization,Northeast Forestry University,Harbin 150040)

机构地区：[1]东北林业大学化学化工与资源利用学院,黑龙江省阻燃分子设计与制备重点实验室,哈尔滨150040

出　　处：《化工新型材料》2023年第9期184-189,共6页New Chemical Materials

摘　　要：以三羟甲基丙烷和甲基膦酸二甲酯为原料在离子液体[Bmim]BF_(4)催化下合成双环膦酸酯阻燃剂:甲基膦酸二(5-乙基-2-甲基-2-氧代-1,3,2-二氧磷杂环己烷-5-基)甲基酯。用气相色谱跟踪反应进程,柱色谱提纯产物用于表征产品结构。当双环膦酸酯阻燃剂添加量为25%时,硬质聚氨酯泡沫的极限氧指数值由18.8%提高到26.6%,最大热分解速率由6.48%/min降低到4.40%/min。采用Kissinger法和Flynn-Wall-Ozawa法分别计算硬质聚氨酯和阻燃硬质聚氨酯的热分解活化能,并根据计算结果对两者的热分解机理进行了分析。A type of dicyclic phosphate flame retardant:bis((5-ethyl-2-methyl-2-oxido-1,3,2-dioxaphosphinan-5-yl)methyl)methylphosphonate was synthesized from trimethylol propane and dimethyl methylphosphonate catalyzed by ionic liquid[Bmim]BF_(4).The reaction process was tracked by gas chromatography,and the product was purified by column chromatography to characterize the product structure.When the bicyclic phosphonate flame retardant was added at 25%,the limiting oxygen index value of flame retardant rigid polyurethane foam increased from 18.8%to 26.6%,and the maximum thermal decomposition rate decreased from 6.48%·min^(-1) to 4.40%·min^(-1).The activation energies of thermal decomposition of rigid polyurethane foam and flame retardant rigid polyurethane foam were calculated by Kissinger method and Flynn-wall-Ozawa method,respectively,and the thermal decomposition mechanism was analyzed based on the calculation results.

关 键 词：环状磷酸酯 硬质聚氨酯 有机合成 阻燃性能 热分解动力学 

分 类 号：TB332[一般工业技术—材料科学与工程]