三聚氰酸胺化反应及其产物研究

发布时间：2018-05-15 09:17

  本文选题：三聚氰酸 + 胺化　； 参考：《山东大学》2017年硕士论文

【摘要】：本文首先介绍了三聚氰酸的一些物理化学性质以及作为二氧化碳封存利用产物的特点,由其制备带三嗪环的性能良好的高分子材料是一条低碳排放的材料工业路线。探讨了胺类化合物的合成方法,并以三聚氰酸为原料合成了带三嗪环的胺类化合物并利用多种检测方法测定了其结构。本文章主要对三聚氰酸的几种氨/胺化反应以及其生成产物做出了实验研究,主要分为三部分:一是三聚氰酸氨化反应及其生成产物的研究,二是三聚氰酸与二乙烯三胺的胺化反应研究,三是三聚氰酸和二乙烯三胺反应制备低聚物。(1)以三聚氰酸为原料,碳酸铵为氨源,在高压釜中反应并得到了氨化产物,使用高效液相色谱法对产品进行了分析,用酸碱反滴定法滴定氨化产物的产率。实验结果表明:在反应温度为290℃,反应时间为4h,SiO2+SnCl2(1:1)为催化剂的条件下,反应产物的氨化率最高;从高效液相色谱谱图中可以看出三聚氰酸氨化产物可能大部分为三聚氰酸一个氨基取代产物以及三聚氰酸两个氨基取代产物。(2)以二乙烯三胺为原料对三聚氰酸(摩尔比为4:1)进行了胺化反应,实验结果表明,在反应温度210℃,反应时间为4小时,选择5A分子筛催化剂的条件下,三聚氰酸的反应程度最高。采用了交替指示剂盐酸滴定法测定该反应中的伯氨基值的减少量,反应前后伯氨基值的减少量越多,反应程度越高。用薄层色谱法对三聚氰酸胺化过程进行跟踪,得到了三聚氰酸胺化产品,并分别使用了红外光谱仪、核磁共振仪等仪器对生成产品表征,从表征图谱可以看出,三聚氰酸与二乙烯三胺发生了催化胺化反应合成了6-二乙烯三胺基-1,3,5-三嗪-2,4(1H,3H)-二酮。(3)以三聚氰酸和二乙烯三胺为原料(摩尔比为1:1),在230℃不加催化剂的条件下反应4小时得到了低聚合度的反应产物。实验使用了红外光谱仪、核磁共振氢谱仪、质谱等仪器对生成的低聚合度的产品进行了表征,从核磁图谱上可以看出三聚氰酸与二乙烯三胺不仅发生了胺化反应而且生成了低聚化合物的反应产物,从质谱图上可以看出三聚氰酸与二乙烯三胺生成的产物的聚合度不高,主要在三聚物。
[Abstract]:In this paper, some physical and chemical properties of cyanuric acid and its characteristics as a product of carbon dioxide sequestration are introduced. It is a low carbon emission material industry route to prepare high molecular materials with good properties with triazine ring. The synthetic method of amines was discussed, and the amines with triazine ring were synthesized from cyanuric acid and their structures were determined by various methods. In this paper, several kinds of ammonia / amination reactions and their formation products of cyanuric acid are studied experimentally, which are divided into three parts: one is the study of amination reaction of cyanuric acid and its products. The second is the amination reaction between tripolycyanic acid and diethylenetriamine, and the third is the reaction of tripolycyanic acid with diethylenetriamine to prepare oligomer. (1) using tripolycyanic acid as raw material, ammonium carbonate as ammonia source, the amination product is obtained in autoclave. The product was analyzed by high performance liquid chromatography and the yield of ammoniated product was titrated by acid-base reverse titration. The results showed that under the conditions of reaction temperature 290 鈩，

本文编号：1891860