双环膦酸酯的合成、表征及其阻燃RPUF的热解动力学分析

邓杰, 孙佳鑫, 赵泽熙, 孙泽营, 孙才英*

化工新型材料 ›› 2023, Vol. 51 ›› Issue (9) : 184 -189.

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化工新型材料 ›› 2023, Vol. 51 ›› Issue (9) : 184-189. DOI: 10.19817/j.cnki.issn1006-3536.2023.09.034
科学研究

双环膦酸酯的合成、表征及其阻燃RPUF的热解动力学分析

    邓杰, 孙佳鑫, 赵泽熙, 孙泽营, 孙才英*
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Synthesis and characterization of bicyclic phosphonate and its pyrolysis kinetics analysis of flame retardant RPUF

  • Deng Jie, Sun Jiaxin, Zhao Zexi, Sun Zeying, Sun Caiying
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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]BF4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。

Abstract

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]BF4.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

Key words

cyclic phosphate / rigid polyurethane / organic synthesis / flame retardancy / thermal decomposition kinetics

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双环膦酸酯的合成、表征及其阻燃RPUF的热解动力学分析[J]. 化工新型材料, 2023, 51(9): 184-189 DOI:10.19817/j.cnki.issn1006-3536.2023.09.034

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