香草醛基磷酰胺阻燃剂的分子构建与性能

TQ314.2; 首先以苯基磷酰二氯和1,10-癸二胺单体为原料,采用一步缩合法合成苯基磷酰癸二胺,然后将其分别和含单醛、双醛以及三醛基团的香草醛及其衍生物通过缩合反应分别制得含有席夫碱的香草醛基线性磷酰胺小分子(V1)、线性聚磷酰胺(V2)和支化聚磷酰胺(V3).采用傅里叶变换红外光谱、核磁共振、凝胶渗透色谱和X射线光电子能谱表征它们的结构,并采用热重分析、差示扫描量热仪研究了不同分子结构磷酰胺阻燃剂的热稳定性、热降解行为和成炭性.结果表明,分子结构和磷、氮元素含量会同时影响阻燃剂的热稳定性和成炭性.对于线性结构的阻燃剂V1和V2,其分子量对热稳定性能的影响很大,V2的热稳定性能低于V1;支...

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Published in功能高分子学报 Vol. 36; no. 6; pp. 561 - 569
Main Authors 薛逸娇, 张天辰, 张猛, 宋平安, 周永红
Format Journal Article
LanguageChinese
Published 中国林业科学研究院林产化学工业研究所,南京 210042%南昆士兰大学未来材料中心,农业与环境科学学院,澳大利亚 Springfield 4300 01.12.2023
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ISSN1008-9357
DOI10.14133/j.cnki.1008-9357.20230905001

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Abstract TQ314.2; 首先以苯基磷酰二氯和1,10-癸二胺单体为原料,采用一步缩合法合成苯基磷酰癸二胺,然后将其分别和含单醛、双醛以及三醛基团的香草醛及其衍生物通过缩合反应分别制得含有席夫碱的香草醛基线性磷酰胺小分子(V1)、线性聚磷酰胺(V2)和支化聚磷酰胺(V3).采用傅里叶变换红外光谱、核磁共振、凝胶渗透色谱和X射线光电子能谱表征它们的结构,并采用热重分析、差示扫描量热仪研究了不同分子结构磷酰胺阻燃剂的热稳定性、热降解行为和成炭性.结果表明,分子结构和磷、氮元素含量会同时影响阻燃剂的热稳定性和成炭性.对于线性结构的阻燃剂V1和V2,其分子量对热稳定性能的影响很大,V2的热稳定性能低于V1;支化结构的阻燃剂V3相较于线性结构的阻燃剂成炭性能更好.此外,由于席夫碱的酸解效应,三种香草醛基阻燃剂在乙酸水溶液中分别在4、12、36 h可实现完全降解.
AbstractList TQ314.2; 首先以苯基磷酰二氯和1,10-癸二胺单体为原料,采用一步缩合法合成苯基磷酰癸二胺,然后将其分别和含单醛、双醛以及三醛基团的香草醛及其衍生物通过缩合反应分别制得含有席夫碱的香草醛基线性磷酰胺小分子(V1)、线性聚磷酰胺(V2)和支化聚磷酰胺(V3).采用傅里叶变换红外光谱、核磁共振、凝胶渗透色谱和X射线光电子能谱表征它们的结构,并采用热重分析、差示扫描量热仪研究了不同分子结构磷酰胺阻燃剂的热稳定性、热降解行为和成炭性.结果表明,分子结构和磷、氮元素含量会同时影响阻燃剂的热稳定性和成炭性.对于线性结构的阻燃剂V1和V2,其分子量对热稳定性能的影响很大,V2的热稳定性能低于V1;支化结构的阻燃剂V3相较于线性结构的阻燃剂成炭性能更好.此外,由于席夫碱的酸解效应,三种香草醛基阻燃剂在乙酸水溶液中分别在4、12、36 h可实现完全降解.
Abstract_FL Phenylphosphonic dichloride and 1,10-diaminodecane monomer were used as raw materials to prepare phenylphosphonic diaminodecane by one-step condensation method.Then,vanillin and its derivatives containing monaldehyde,dialdehyde and trialdehyde group were introduced to prepare vanillin-based linear phosphoramide(V1),linear polyphosphoramide(V2)and branched polyphosphoramide(V3)containing Schiff base via condensation reaction.The structures of these three vanillin-based phosphoramide fire retardants were determined by Fourier transform infrared spectroscopy,nuclear magnetic resonance,gel permeation chromatography and X-ray photoelectron spectroscopy,and their thermal stability,thermal degradation behavior and char-forming ability were studied by thermogravimetric analysis and differential scanning calorimeter.The results show that the molecular structure and the content of phosphorus and nitrogen can both affect the thermal stability and carbonization of fire retardants simultaneously.For linear fire retardants V1 and V2,their molecular weight has a great influence on the thermal stability.When molecular weight increases,more C―C chains tend to decompose,so the thermal stability of V2 is lower than that of V1.The branched fire retardant V3 with a high degree of crosslinking has better carbonization properties than linear fire retardants.In addition,due to the acidolysis effect of Schiff base,three kinds of vanillin-based phosphoramide fire retardants can be completely degraded in acetic acid aqueous solution within 4,12 h and 36 h,respectively.
Author 张猛
周永红
宋平安
薛逸娇
张天辰
AuthorAffiliation 中国林业科学研究院林产化学工业研究所,南京 210042%南昆士兰大学未来材料中心,农业与环境科学学院,澳大利亚 Springfield 4300
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Author_FL ZHANG Tianchen
SONG Pingan
ZHOU Yonghong
XUE Yijiao
ZHANG Meng
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DocumentTitle_FL Molecular Construction and Properties of Vanillin-Based Phosphoramide Fire Retardants
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Keywords fire retardant
degradation property
阻燃剂
热稳定性
降解性能
结构-性能关系
香草醛
thermal stability
vanillin
structure-property relationship
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PublicationTitle 功能高分子学报
PublicationTitle_FL Journal of Functional Polymers
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Publisher 中国林业科学研究院林产化学工业研究所,南京 210042%南昆士兰大学未来材料中心,农业与环境科学学院,澳大利亚 Springfield 4300
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