1,2,4-三氯苯的純化和利用

制藥工程論文編號:ZY121    論文字數:7100,頁數:26

目  錄
中文摘要 I
英文摘要 II
目錄 III
1. 緒論 1
 1.1 前言 1
 1.2 研究現狀 7
 1.3論文研究內容及意義 7
2. 實驗部分 8
 2.1 實驗儀器和試劑 8
 2.1.1 實驗儀器 8
 2.1.2 實驗試劑 8
 2.2 實驗操作步驟 9
 2.2.1 廢液的精餾 9
 2.2.2 精餾粗產物洗滌 9
 2.2.3 廢液和精餾產物的硝化 9
 2.2.4 硝化產物還原 10
3. 結果與討論 10
 3.1 蒸餾餾分氣相色譜分析 10
 3.2 洗滌產物氣相色譜分析 17
 3.3 硝化劑用量對反應的影響 17
 3.4 不同還原劑對反應的影響 19
 3.5 討論 19
4．總結與展望 20
 4.1 總結 20
 4.2 展望 20
致謝 21
參考文獻 22

摘要：對2,4-二氯氟苯生產過程中所產生的廢液三氯苯進行回收處理。通過廢液分析可知其主要成分為2,4-二氯氟苯，并含有一定量的1,2,4-三氯苯及少量同分異構的三氯苯和多氯苯。首先通過精餾得到純度為98%的2,4-二氯氟苯和純度為88%的1,2,4-三氯苯，用洗潔精洗滌88%的1,2,4-三氯苯粗品，再用純水清洗并干燥得到純度為95%的1,2,4-三氯苯粗品，然后對95%的1,2,4-三氯苯進行硝化，得到99%的2,4,5-三氯硝基苯，并將所得產品還原成2,4,5-三氯苯胺。實驗考察了不同的硝化方法、硝化劑的用量對反應的影響，研究結果表明：當粗產品用量為35ml、發煙硝酸為80ml時進行硝化，提純后得到34.046g 2,4,5-三氯硝基苯，純度為99.4%，而其還原產物2,4,5-三氯苯胺的純度可達到99%。

關鍵詞：2,4-二氯氟苯，1,2,4-三氯苯,提純,硝化,還原，2,4,5-三氯苯胺

Abstract: This topic was about recycling of trichlorobezene from the preparation of 2,4-dichlorofluobezene. As the analysis of the recycling liquid showed, 2,4-dichlorofluobezene was the main part, and there was also some 1,2,4-trichlorobenzene and a little of isomers of trichlorobenzene and polychlorobezene. Firstly, 2,4-dichlorofluobezene and 1,2,4-trichlorobenzene were gained by distiling with the purity of 98% and 88%, respectively. Then 1,2,4-trichlorobenzene with the purity of 95% was got by cleaning with detergent and water. Thirdly, 2,4,5-trichloronitrobenzene was prepared by nitration from 1,2,4-trichlorobenzene, with the purity of 99%. finally, 1,2,4-trichlorobenzene was converted to 2,4,5-trichloroaniline by reduction. Different methods of nitration and amount of nitrating reagent were tested in this article. As the result showed, when nitration took place with 35ml of 1,2,4-trichlorobenzene and 80ml of fuming nitric acid, 36.046g of 2,4,5-trichloronitrobenzene was gained, with the purity of 99,4%, and the purity of its reducing production could reached 99%.

Key words:  2,4-dichlorofluorobenzene, 1,2,4-trichlorobenzene, Purification, nitration, reduction, 2,4,5-Trichloroaniline