1,2,4-三氯苯的纯化和利用

论文编号:ZY121    论文字数:7100,页数:26

摘要：对2,4-二氯氟苯生产过程中所产生的废液三氯苯进行回收处理。通过废液分析可知其主要成分为2,4-二氯氟苯，并含有一定量的1,2,4-三氯苯及少量同分异构的三氯苯和多氯苯。首先通过精馏得到纯度为98%的2,4-二氯氟苯和纯度为88%的1,2,4-三氯苯，用洗洁精洗涤88%的1,2,4-三氯苯粗品，再用纯水清洗并干燥得到纯度为95%的1,2,4-三氯苯粗品，然后对95%的1,2,4-三氯苯进行硝化，得到99%的2,4,5-三氯硝基苯，并将所得产品还原成2,4,5-三氯苯胺。实验考察了不同的硝化方法、硝化剂的用量对反应的影响，研究结果表明：当粗产品用量为35ml、发烟硝酸为80ml时进行硝化，提纯后得到34.046g 2,4,5-三氯硝基苯，纯度为99.4%，而其还原产物2,4,5-三氯苯胺的纯度可达到99%。

关键词：2,4-二氯氟苯，1,2,4-三氯苯,提纯,硝化,还原，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

目  录
中文摘要 I
英文摘要 II
目录 III
1. 绪论 1
 1.1 前言 1
 1.2 研究现状 7
 1.3论文研究内容及意义 7
2. 实验部分 8
 2.1 实验仪器和试剂 8
 2.1.1 实验仪器 8
 2.1.2 实验试剂 8
 2.2 实验操作步骤 9
 2.2.1 废液的精馏 9
 2.2.2 精馏粗产物洗涤 9
 2.2.3 废液和精馏产物的硝化 9
 2.2.4 硝化产物还原 10
3. 结果与讨论 10
 3.1 蒸馏馏分气相色谱分析 10
 3.2 洗涤产物气相色谱分析 17
 3.3 硝化剂用量对反应的影响 17
 3.4 不同还原剂对反应的影响 19
 3.5 讨论 19
4．总结与展望 20
 4.1 总结 20
 4.2 展望 20
致谢 21
参考文献 22