| 1,4-二(5,5-二甲基-1,3-二氧杂己内磷酰亚胺基)苯的合成 |
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| 引用本文： | 彭治汉,欧育湘. 1,4-二(5,5-二甲基-1,3-二氧杂己内磷酰亚胺基)苯的合成[J]. 精细化工, 1999, 16(1): 20-23 |
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| 作者姓名： | 彭治汉 欧育湘 |
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| 作者单位： | 北京理工大学国家阻燃材料专业实验室,北京,100081 |
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| 摘 要： | 对以新戊二醇、三氯氧磷和对苯二胺为原料，在三乙胺和４ Ｎ，Ｎ 二甲胺基吡啶（ＤＭＡＰ）催化作用下合成１，４ 二（５，５ 二甲基 １，３ 二氧杂己内磷酰亚胺基）苯（ＮＢＰＡＮ）的反应进行了研究。讨论了ＤＭＡＰ对该反应的作用机制，合成收率达８２．７％。并用元素分析、ＩＲ和１ＨＮＭＲ表征了产物的结构。热重分析表明ＮＢＰＡＮ的起始分解温度为２８０℃，并在２８０～３１０℃迅速炭化，成炭率达３５．５８％。
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| 关 键 词： | 环状磷酸酯；磷酰亚胺；磷酰化；膨胀阻燃剂 |
| 文章编号： | 1003-5214(1999)01-0020-23 |
Synthesis of 1,4-Bis(5,5-dimethyl-1,3-dioxacyclophosphorimide) benzene |
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| PENG Zhihan,OU Yuxiang. Synthesis of 1,4-Bis(5,5-dimethyl-1,3-dioxacyclophosphorimide) benzene[J]. Fine Chemicals, 1999, 16(1): 20-23 |
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| Authors: | PENG Zhihan OU Yuxiang |
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| Abstract: | Bis(5,5 dimethyl 1,3 dioxacyclophosphorimide)benzene is synthesized by the intermedia of phosphorylation reaction of neopentyl alcohol and POCl 3,and p phenyldiamine in the presence of Et 3N and 4 N,N methylaminopyridine.The total synthetic yield is about 82.7%.The outstanding catalysis of DMAP is studied . The structure of NBPAN is confirmed by elementary analysis ,IR and 1 HNMR.The result of thermogravimetry shows that the beginning temperature of NBPAN decomposition is above 280℃,and rapidly carbonized between 280℃ and 310℃.The char yield is about 35.58% at 500℃. |
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| Keywords: | cyclic phosphate phosphorimide phosphorylation intumescent flame retardant |
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