一种具有不对称结构含磷二胺单体的合成

Synthesis of a Phosphorus-Containing Diamine Monomer with Asymmetric Structure

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。

A new phosphorus-containing diamine monomer with asymmetric structure was synthesizedwith 4-aminoacetophenone,2,6-diethylaniline and DOPO by one step,and the p - toluenesulfonicacid as catalyst. This article also explored the suitable conditions for synthesis of the diamine monomerthrough orthogonal experiments,the reaction temperature was 130 ℃,the reaction time was 20 h,theamount of 2,6-diethylaniline was 3 times of DOPO molar quantity,the amount of p - toluenesulfonicacid 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 monomerwere characterized by infrared spectrum and proton peaks were characterized by nuclear magneticresonance hydrogen spectrum.