摘要
以4,4′-二氨基二苯甲烷和2,4-二氯-6-苯基-1,3,5-三嗪为原料,无水碳酸钠为催化剂,二氧六环为溶剂合成了一种新型的含三嗪环的二胺单体(2,4-二氨基-[N,N′-二(4′-对氨基苄基苯)]-6-苯基-1,3,5-三嗪)。利用正交试验优化了该合成实验的反应条件,最佳实验条件为:反应温度160℃,反应回流时间4 h,4,4′-二氨基二苯甲烷的用量为2,4-二氯-6-苯基-1,3,5-三嗪物质的量的8倍,无水碳酸钠的用量为2,4-二氯-6-苯基-1,3,5-三嗪物质的量的3倍,在此最优条件下进行实验,产率可高达95. 56%。使用DSC分析仪器测定了该二胺单体的熔点为183. 59℃,并通过红外光谱和核磁共振氢谱表征了该二胺单体的特征官能团振动吸收峰、化学位移和质子峰面积及峰面积比值,确定了该二胺单体的结构。
A novel triazine-eontaining dianine monomer 2, 4-dianino-[N, N＇-bis （4＇-p-aminobenzylphenyl） ]- 6-phenyl-1, 3, 5-triazine was synthesized with 4, 4＇-diaminodiphenyhnethane and 2, 4-dichloro- 6-phenyl-1, 3, 5-triazine as materials, with the anhydrous sodium carbonate as catalyst and dioxane as solvent. Orthogonal experiments were designed to optimize the reaction conditions for the synthetic experiment. The suitable experimental conditions were as follows, the reaction temperature was 160 ℃, the reaction reflux time was 4 h, the amount of 4, 4＇-diaminodiphenyl methane was 8 times as the amount of 2, 4-dichloro-6-phenyl- 1, 3, 5-triazine, the amount of anhydrous sodium carbonate was 3 times as the amount of 2, 4-dichloro-6-phenyl- i, 3, 5-triazine material. When the experiments were performed under these suitable conditions, the yield could reach as high as 95.56%. The melting point of the diamine monomer was determined to be 183. 59 ℃ with DSC （differential scanning calorimeter） , characteristic vibration absoqotion peaks of functional groups of the diamine monomer were characterized by FT-IR spectrum, chemical characterized by IH-NMR spectrum. The structure shift and proton peak area and peak area ratio were of the diamine monomer was determined.
作者
汪聪茜
胡昌智
胡思前
WANG Congqian;HU Changzhi;HU Siqian(Key Laboratory of Optoelectronic Chemical Materials and Devices,Ministry of Education,School of Chemical and Environmental Engineering,Jianghan University,Wuhan 430056,Hubei,China)
出处
《江汉大学学报（自然科学版）》
2018年第6期499-503,共5页
Journal of Jianghan University：Natural Science Edition
基金
国家高技术研究发展计划"863"项目(2015AA03340)
武汉市人才培养计划项目(20141822)
光电化学材料与器件教育部重点实验室(江汉大学)开放基金项目(JDGO-201711)
