二苯甲酮亚胺的合成的合成工艺研究.doc

二苯甲酮亚胺的合成的合成工艺研究 ? 摘要 ? 二苯甲酮亚胺是一种重要的化学中间体，潜在着巨大的经济效益和广阔的市场前景。因而如何提高其产物的纯度成为关键的问题，本文就这问题作一探讨，研究了多种合成的方法及工艺的改进路线，对实验室和工业生产的工艺条件及要求进行对照，逐一比较它们之间的优缺点。最后选取了由P.L.Pickard 和T.L.Tolbert提出的用格氏试剂和腈的复合反应，再用无水甲醇分解复合产物，从而得到二苯甲酮亚胺的这条工艺改进路线。实验结果表明在室内相对湿度小于65%条件下，制备格氏试剂的成功几率较高，最后产率高达61%~81%，此反应条件温和、合理、环境友善，可以成为实验室制取二苯甲酮亚胺普遍所采用的方法。 关键词：格氏试剂；二苯甲酮亚胺；无水甲醇；副反应 ? ? ? ? ? ? ? ? ? ? ? ? Abstract ? Diphenyl ketimine, an important chemical middleware, has whopping economic benefit and wide market prospect. So how to improve its production purity becomes important, and it is discussed in this paper. Here, kinds of synthesis methods and technical improvement ways are researched, and the technical requirement of laboratory producing and the ones of industrial producing are also compared. Finally, the technical improvement way proposed by P.L. Pickard and T.L.Tolbert is selected. First make Grignard reagent and nitril composite reaction, then decomposing synthetical producetion with anhydrous methanol, and finally get diphenyl ketimine. As the experiment results show, when the indoor relative humidity under 65 percent, the success probability of producing Grignard reagent is very high, the produce yield is as high as 61 percent to 81 percent. Because the reaction condition is mild, reasonable and moderate, this method is always used to produce dipheny1 ketimine in laboratory. Key words: Grignard reagent；diphenyl ketimine；anhydrous methanol；side reaction ? 目录 ? 1. 绪 论……………………………………………………………………………… 1.1 二苯甲酮亚胺的物化性质和用途…………………………………………… 1.2 工艺路线的研究及比较……………………………………………………… 1.2.1 工艺路线的研究………………………………………………………… 1.2.2 各条工艺路线的优缺点比较…………………………………………… 2. 格氏试剂的概况…………………………………………………………………… 2.1 格氏试剂的总体概况………………………………………………………… 2.2 格氏试剂的机理……………………………………………………………… 2.3 格氏试剂的化学性质………………………………………………………… 2.4 格氏试剂的制备要点和注意点……………………………………………… 3. 实验部分………………………………………………………………………… 3.1 原料及设备…………………………………………………………………… 3.1.1 原料……………………………………………………………………… 3.1.2 仪器设备………………………………………………………………… 3.2 工艺路线及测试……………………………………………………………… 3.2.