發(fā)布時(shí)間：2018-05-15 09:17

  本文選題：三聚氰酸 + 胺化　； 參考：《山東大學(xué)》2017年碩士論文

【摘要】：本文首先介紹了三聚氰酸的一些物理化學(xué)性質(zhì)以及作為二氧化碳封存利用產(chǎn)物的特點(diǎn),由其制備帶三嗪環(huán)的性能良好的高分子材料是一條低碳排放的材料工業(yè)路線。探討了胺類化合物的合成方法,并以三聚氰酸為原料合成了帶三嗪環(huán)的胺類化合物并利用多種檢測(cè)方法測(cè)定了其結(jié)構(gòu)。本文章主要對(duì)三聚氰酸的幾種氨/胺化反應(yīng)以及其生成產(chǎn)物做出了實(shí)驗(yàn)研究,主要分為三部分:一是三聚氰酸氨化反應(yīng)及其生成產(chǎn)物的研究,二是三聚氰酸與二乙烯三胺的胺化反應(yīng)研究,三是三聚氰酸和二乙烯三胺反應(yīng)制備低聚物。(1)以三聚氰酸為原料,碳酸銨為氨源,在高壓釜中反應(yīng)并得到了氨化產(chǎn)物,使用高效液相色譜法對(duì)產(chǎn)品進(jìn)行了分析,用酸堿反滴定法滴定氨化產(chǎn)物的產(chǎn)率。實(shí)驗(yàn)結(jié)果表明:在反應(yīng)溫度為290℃,反應(yīng)時(shí)間為4h,SiO2+SnCl2(1:1)為催化劑的條件下,反應(yīng)產(chǎn)物的氨化率最高;從高效液相色譜譜圖中可以看出三聚氰酸氨化產(chǎn)物可能大部分為三聚氰酸一個(gè)氨基取代產(chǎn)物以及三聚氰酸兩個(gè)氨基取代產(chǎn)物。(2)以二乙烯三胺為原料對(duì)三聚氰酸(摩爾比為4:1)進(jìn)行了胺化反應(yīng),實(shí)驗(yàn)結(jié)果表明,在反應(yīng)溫度210℃,反應(yīng)時(shí)間為4小時(shí),選擇5A分子篩催化劑的條件下,三聚氰酸的反應(yīng)程度最高。采用了交替指示劑鹽酸滴定法測(cè)定該反應(yīng)中的伯氨基值的減少量,反應(yīng)前后伯氨基值的減少量越多,反應(yīng)程度越高。用薄層色譜法對(duì)三聚氰酸胺化過(guò)程進(jìn)行跟蹤,得到了三聚氰酸胺化產(chǎn)品,并分別使用了紅外光譜儀、核磁共振儀等儀器對(duì)生成產(chǎn)品表征,從表征圖譜可以看出,三聚氰酸與二乙烯三胺發(fā)生了催化胺化反應(yīng)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為原料(摩爾比為1:1),在230℃不加催化劑的條件下反應(yīng)4小時(shí)得到了低聚合度的反應(yīng)產(chǎn)物。實(shí)驗(yàn)使用了紅外光譜儀、核磁共振氫譜儀、質(zhì)譜等儀器對(duì)生成的低聚合度的產(chǎn)品進(jìn)行了表征,從核磁圖譜上可以看出三聚氰酸與二乙烯三胺不僅發(fā)生了胺化反應(yīng)而且生成了低聚化合物的反應(yīng)產(chǎn)物,從質(zhì)譜圖上可以看出三聚氰酸與二乙烯三胺生成的產(chǎn)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，

本文編號(hào)：1891860