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CN103524350A - Recovery method for 5-clorine-2-nitroaniline - Google Patents

Recovery method for 5-clorine-2-nitroaniline Download PDF

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Publication number
CN103524350A
CN103524350A CN201310525796.8A CN201310525796A CN103524350A CN 103524350 A CN103524350 A CN 103524350A CN 201310525796 A CN201310525796 A CN 201310525796A CN 103524350 A CN103524350 A CN 103524350A
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CN
China
Prior art keywords
nitroaniline
recovery method
chloro
clorine
fenbendazole
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201310525796.8A
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Chinese (zh)
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CN103524350B (en
Inventor
陈荣
朱志勇
王琳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Baozhong Baoda Pharmaceutical Co.,Ltd.
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JIANGSU BAOZONG BAODA PHARMACEUTICAL CO Ltd
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Priority to CN201310525796.8A priority Critical patent/CN103524350B/en
Publication of CN103524350A publication Critical patent/CN103524350A/en
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Abstract

The invention discloses a recovery method for 5-clorine-2-nitroaniline. The recovery method for the 5-clorine-2-nitroaniline is characterized in that waste dissolved out of a mother solution in the fenbendazole ammoniation step is added in solvent, the warming and backflow process is conducted for half an hour, thermal filtering is conducted, filter liquor is cooled and crystallized, and a crystal substance is obtained; the crystal substance is dissolved again and is cooled naturally, seed crystal is added in the solution, crystallization, filtering, washing and drying are conducted, and pure 5-clorine-2-nitroaniline is obtained. The recovery method for the 5-clorine-2-nitroaniline is compact and efficient, safe to operate, and suitable for industrial production.

Description

A kind of recovery method of 5-chloro-2-nitroaniline
Technical field
The present invention relates to reclaim in a kind of waste of separating out the method for 5-chloro-2-nitroaniline from the mother liquor of fenbendazole ammonification step.
Background technology
5-chloro-2-nitroaniline is purposes intermediate very widely, particularly as the key intermediate of fenbendazole.Fenbendazole, has another name called fenbendazole, and chemistry 5-thiophenyl benzimidazolyl-2 radicals-Urethylane by name, is a kind of anti-parasite medicine of broad-spectrum high efficacy for animals.Fenbendazole is used to kill animal gastrointestinal tract parasite, it not only has height anthelmintic activity to animal gastrointestinal tract roundworm, hookworm, whipworm, part tapeworm and strongylid, and part bronchial tree and lung parasite (cat lung worm and lung fluke) are also had to preferably curative effect.It is wide that fenbendazole has expelling parasite spectrum, and toxicity is low, better tolerance, the advantage such as safety range is wide, good palatability.
The discarded mother liquor of fenbendazole ammonification step, after cooling, having a large amount of solids separates out, the solid the inside that this part is separated out has comprised a lot of impurity and product 5-chloro-2-nitroaniline, general recovery makes product reach standard, all directly doing solid waste processes, both waste resource, to environmental protection, brought pressure again.
Summary of the invention
The object of the present invention is to provide a kind of recovery method of 5-chloro-2-nitroaniline, aim to provide a kind of succinct efficient, make it operational safety, more meet suitability for industrialized production.
For solving the problems of the technologies described above, the technical solution used in the present invention is: by the waste of separating out in the mother liquor of fenbendazole ammonification step, add solvent, temperature rising reflux half an hour, after heat filtering, filtrate crystallisation by cooling is obtained to crystallisate, crystallisate is dissolved again, and naturally cooling, adds crystal seed, crystallization, filtration, washing, dry to obtain sterling 5-chloro-2-nitroaniline, concrete steps are as follows:
(1) waste is added in the solvent of 3 to 5 times of amounts, temperature rising reflux half an hour, tolerant filtering not, crystallisation by cooling, filtration washing, dries to obtain crystallisate.Solvent is selected from following methyl alcohol, ethanol, toluene, dimethylbenzene, preferably ethanol.
(2) crystallisate crystallization for the first time being obtained, dissolves again, naturally cooling, and solution, by clarifying while becoming muddy, adds crystal seed by the time, crystallization, filtration, washing, dries to obtain the 5-chloro-2-nitroaniline of sterling.
Beneficial effect of the present invention: the recovery method that the present invention selects, succinct efficient, operational safety, is applicable to suitability for industrialized production.
Embodiment
Following type reaction is used for illustrating the present invention, within the simple replacement of the present invention being done those skilled in the art or improvement etc. all belong to the technical scheme that the present invention protects.
Embodiment 1
Step 1: in 1000 milliliters of four-hole boiling flasks with thermometer and whipping appts, open and stir, add successively 150g to contain waste, add 500g ethanol, temperature rising reflux half an hour, filtered while hot, by filtrate crystallisation by cooling, filter, wash, dry and to obtain crystallisate 102g.
Step 2: previous step is obtained in four-hole boiling flask that crystallisate 102g adds 1000 milliliters, add again 300g ethanol, temperature rising reflux half an hour, reflux complete, naturally cooling adds a small amount of crystal seed, after waiting crystallization when liquid starts to become muddiness, filter, wash, dry and to obtain the 5-chloro-2-nitroaniline 81.6g of sterling, total recovery is 54.4%.
Embodiment 2
Step 1: in 1000 milliliters of four-hole boiling flasks with thermometer and whipping appts, open and stir, add successively 100g to contain waste, add 350g ethanol, temperature rising reflux half an hour, filtered while hot, by filtrate crystallisation by cooling, filter, wash, dry and to obtain crystallisate 75g.
Step 2: previous step is obtained in four-hole boiling flask that crystallisate 75g adds 1000 milliliters, add again 300g ethanol, temperature rising reflux half an hour, reflux complete, naturally cooling adds a small amount of crystal seed, after waiting crystallization when liquid starts to become muddiness, filter, wash, dry and to obtain the 5-chloro-2-nitroaniline 58.9g of sterling, total recovery is 58.9%.
Embodiment 3
Step 1: in 2000 milliliters of four-hole boiling flasks with thermometer and whipping appts, open and stir, add successively 200g to contain waste, add 700g ethanol, temperature rising reflux half an hour, filtered while hot, by filtrate crystallisation by cooling, filter, wash, dry and to obtain crystallisate 146g.
Step 2: previous step is obtained in four-hole boiling flask that crystallisate 146g adds 1000 milliliters, add again 500g ethanol, temperature rising reflux half an hour, reflux complete, naturally cooling adds a small amount of crystal seed, after waiting crystallization when liquid starts to become muddiness, filter, wash, dry and to obtain the 5-chloro-2-nitroaniline 115g of sterling, total recovery is 57.5%.

Claims (4)

1. a recovery method for 5-chloro-2-nitroaniline, is characterized in that: described method comprises the following steps in order:
(1) by the waste of separating out in the mother liquor of fenbendazole ammonification step, add solvent, temperature rising reflux half an hour, after heat filtering, filtrate crystallisation by cooling is obtained to crystallisate;
(2) crystallisate is dissolved again, naturally cooling, adds crystal seed, crystallization, filtration, washing, dries to obtain sterling 5-chloro-2-nitroaniline.
2. the recovery method of a kind of 5-chloro-2-nitroaniline according to claim 1, is characterized in that: described solvent is methyl alcohol, ethanol, dimethylbenzene, toluene.
3. the recovery method of a kind of 5-chloro-2-nitroaniline according to claim 1 and 2, is characterized in that: described solvent is ethanol.
4. the recovery method of a kind of 5-chloro-2-nitroaniline according to claim 1, is characterized in that: the waste of separating out in the mother liquor of described fenbendazole ammonification step and the mass ratio of solvent are 1:3-5.
CN201310525796.8A 2013-10-31 2013-10-31 Recovery method for 5-clorine-2-nitroaniline Active CN103524350B (en)

Priority Applications (1)

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Application Number Priority Date Filing Date Title
CN201310525796.8A CN103524350B (en) 2013-10-31 2013-10-31 Recovery method for 5-clorine-2-nitroaniline

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CN103524350A true CN103524350A (en) 2014-01-22
CN103524350B CN103524350B (en) 2015-03-25

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101244878A (en) * 2008-02-25 2008-08-20 南京大学 Treatment for wastewater in para-nitraniline production and method for resource recovery and use
CN102241635A (en) * 2011-04-28 2011-11-16 江苏宝众宝达药业有限公司 Preparation method for anthelmintic benzimidazole fenbendazole
CN103242237A (en) * 2013-05-10 2013-08-14 常州亚邦齐晖医药化工有限公司 New preparation method for anthelmintic fenbendazole

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101244878A (en) * 2008-02-25 2008-08-20 南京大学 Treatment for wastewater in para-nitraniline production and method for resource recovery and use
CN102241635A (en) * 2011-04-28 2011-11-16 江苏宝众宝达药业有限公司 Preparation method for anthelmintic benzimidazole fenbendazole
CN103242237A (en) * 2013-05-10 2013-08-14 常州亚邦齐晖医药化工有限公司 New preparation method for anthelmintic fenbendazole

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
钟红梅等: "从邻氯苯甲醛废水中回收邻氯苯甲酸的研究", 《广东化工》, vol. 35, no. 11, 31 December 2008 (2008-12-31) *

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Address after: 226500 No.10, Yuejiang Road, Changjiang Town, Rugao City, Nantong City, Jiangsu Province

Patentee after: Jiangsu Baozhong Baoda Pharmaceutical Co.,Ltd.

Address before: 226500 No.10, Yuejiang Road, Changjiang Town, Rugao City, Nantong City, Jiangsu Province

Patentee before: JIANGSU BAOZONG & BAODA PHARMACHEM Co.,Ltd.