基于环三磷腈/磷酸酯反应型磷-氮阻燃剂的合成、热降解及应用

doi:10.11949/j.issn.0438-1157.20141850

化工学报 ›› 2015, Vol. 66 ›› Issue (5): 1976-1982.DOI: 10.11949/j.issn.0438-1157.20141850

• 材料化学工程与纳米技术 • 上一篇下一篇

基于环三磷腈/磷酸酯反应型磷-氮阻燃剂的合成、热降解及应用

胡文田, 杨荣, 许亮, 宋艳, 李锦春

常州大学材料科学与工程学院, 江苏常州 213000

收稿日期:2014-12-15 修回日期:2015-01-23 出版日期:2015-05-05 发布日期:2015-05-05
通讯作者: 李锦春
基金资助:
国家自然科学基金项目(51473024);江苏省产学研联合创新资金项目(BY2013024-07)。

Synthesis, properties and application of reactive nitrogen-phosphorus flame retardant

HU Wentian, YANG Rong, XU Liang, SONG Yan, LI Jinchun

School of Materials Science and Engineering, Changzhou University, Changzhou 213000, Jiangsu, China

Received:2014-12-15 Revised:2015-01-23 Online:2015-05-05 Published:2015-05-05
Supported by:
supported by the National Natural Science Foundation of China (51473024) and the Industry-Academic Joint Innovative Fund of Jiangsu Province (BY2013024-07).

摘要/Abstract

摘要： 以六氯环三磷腈(HCCP)、对羟基苯甲醛及亚磷酸二乙酯等为原料,成功合成了一种反应型磷-氮膨胀阻燃剂六(4-磷酸二乙酯羟甲基苯氧基)环三磷腈(HPHPCP),HPHPCP结构经傅里叶红外光谱(FTIR)、核磁共振(NMR)证实。热失重(TG/DTG)表明HPHPCP具有较高的热稳定性及良好的成炭性,氮气氛下的起始分解温度为162.7℃,800℃时残炭量大于40%(质量分数);利用HPHPCP的羟基结构,应用于硬质聚氨酯泡沫塑料中,可以显著提高聚氨酯硬泡的阻燃性能,添加30%的HPHPCP就可以使聚氨酯氧指数达到27%。

关键词: 阻燃剂, 合成, 热降解, 硬质聚氨酯泡沫

Abstract: A novel reactive flame retardant named hexakis (4-diethyl phosphate hydroxymethyl phenoxy) cyclotriphosphazene (HPHPCP) was synthesized from hexachlorocyclotriphosphazene (HCCP), p-hydroxy benzaldehyde and diethyl phosphite. Chemical structures of intermediate and HPHPCP were characterized by Fourier-transform infrared spectroscopy (FTIR), proton and 31P nuclear magnetic resonance (NMR). Thermal stability of the HPHPCP was determined via thermogravimetric analysis (TGA). Halogen-free flame-retardant rigid polyurethane foams (RPU) were prepared by using HPHPCP as a reactive flame retardant. The effect of HPHPCP content on the thermal and flame-retardant properties of RPU was investigated with TGA, and limiting oxygen index (LOI). The temperatures of 5%(mass) loss (T_5%) of HPHPCP in nitrogen and air were 162.7℃ and 153.0℃, and the residues at 800℃ of HPHPCP in nitrogen and air were 42.1% and 12.0%(mass), respectively. HPHPCP could enhance thermal stability of RPU. The T_5% of RPU-20%HPHPCP was 193.9℃, 20℃ higher than pure RPU. Moreover, limiting oxygen index (LOI) of RPU increased with increasing HPHPCP, and LOI of RPU-30%HPHPCP was 27%.

Key words: flame retardant, synthesis, thermal degradation, rigid polyurethane foam

中图分类号:

O631

胡文田, 杨荣, 许亮, 宋艳, 李锦春. 基于环三磷腈/磷酸酯反应型磷-氮阻燃剂的合成、热降解及应用[J]. 化工学报, 2015, 66(5): 1976-1982.

HU Wentian, YANG Rong, XU Liang, SONG Yan, LI Jinchun. Synthesis, properties and application of reactive nitrogen-phosphorus flame retardant[J]. CIESC Journal, 2015, 66(5): 1976-1982.

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基于环三磷腈/磷酸酯反应型磷-氮阻燃剂的合成、热降解及应用

Synthesis, properties and application of reactive nitrogen-phosphorus flame retardant

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