江汉大学学报(自然科学版) ›› 2016, Vol. 44 ›› Issue (3): 215-218.doi: 10.16389/j.cnki.cn42-1737/n.2016.03.004

• 光电化学材料与器件研究 • 上一篇    下一篇

一种具有不对称结构含磷二胺单体的合成

陈薇a,b,陈妤红a,蔡春飞a,b,代云利a,b,刘继延a,b,胡思前*a,b   

  1. 江汉大学 a. 光电化学材料与器件教育部重点实验室;b. 化学与环境工程学院,湖北 武汉 430056
  • 出版日期:2016-06-28 发布日期:2016-07-21
  • 通讯作者: 胡思前
  • 作者简介:陈薇(1991—),女,硕士生,研究方向:耐热阻燃聚酰亚胺材料。
  • 基金资助:
    国家高技术研究发展计划(863计划)资助项目(2015AA033406);武汉市科技人才培养计划(20141822)

Synthesis of a Phosphorus-Containing Diamine Monomer with Asymmetric Structure

CHEN Weia,b,CHEN Yuhonga,CAI Chunfeia,b,DAI Yunlia,b,LIU Jiyana,b,HU Siqian*a,b   

  1. a. Key Laboratory of Optoelectronic Chemical Materials and Devices,Ministry of Education;b. School of Chemistry and Environmental Engineering,Jianghan University,Wuhan 430056,Hubei,China
  • Online:2016-06-28 Published:2016-07-21
  • Contact: HU Siqian

摘要: 使用DOPO 与4-氨基苯乙酮和2,6-二乙基苯胺为原料,以对甲苯磺酸为催化剂,采用一步法合成了一种新型具有不对称结构含磷二胺单体。设计正交试验探讨出合成该二胺单体的最佳条件,反应温度130 ℃,反应时间20 h,2,6-二乙基苯胺用量为DOPO摩尔量的3倍及对甲苯磺酸的量为DOPO质量用量的4%,收率为60%。用DSC检测其熔点在247.9 ℃,红外光谱和核磁共振氢谱表征含磷二胺单体的特征官能团振动吸收峰和质子峰。

关键词: DOPO, 含磷二胺, 不对称结构

Abstract: A new phosphorus-containing diamine monomer with asymmetric structure was synthesized with 4-aminoacetophenone,2,6-diethylaniline and DOPO by one step,and the p - toluenesulfonic acid as catalyst. This article also explored the suitable conditions for synthesis of the diamine monomer through orthogonal experiments,the reaction temperature was 130 ℃,the reaction time was 20 h,the amount of 2,6-diethylaniline was 3 times of DOPO molar quantity,the amount of p - toluenesulfonic acid was 4% of DOPO quality,and the yield was 60% . The substance′ s melting point is 247. 9 ℃ detected by DSC,characteristic vibration absorption peaks of functional groups of the diamine monomer were characterized by infrared spectrum and proton peaks were characterized by nuclear magnetic resonance hydrogen spectrum.

Key words: DOPO, phosphorus-containing diamine, asymmetric structure

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