CN1035324C - Process for production of 2,6-dichlorophenol by using O-chlorophenol - Google Patents
Process for production of 2,6-dichlorophenol by using O-chlorophenol Download PDFInfo
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- CN1035324C CN1035324C CN95101733A CN95101733A CN1035324C CN 1035324 C CN1035324 C CN 1035324C CN 95101733 A CN95101733 A CN 95101733A CN 95101733 A CN95101733 A CN 95101733A CN 1035324 C CN1035324 C CN 1035324C
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- chloro phenol
- ortho chloro
- solvent
- present
- tetrachloride
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Abstract
The present invention relates to a method for utilizing o-chlorophenol to produce 2, 6-dichloro phenol. The existing old methods have the defects of complicated technology, high cost and serious pollution. The present invention adopts a method that catalysts are added into solvent of tetrachloride to generate chlorination reaction at a certain temperature, and o-chlorophenol is utilized to produce 2, 6-dichloro phenol in one step, so that the defects of the prior art are overcome. The present invention has the advantages of simple technology, low cost, little pollution, etc. and is suitable for industrial production.
Description
The present invention relates to a kind of method of producing the 2.6-chlorophenesic acid by ortho chloro phenol.
2.6-chlorophenesic acid is important medicine " diclofenac ", " EBP-II " and pesticide intermediate, method by ortho chloro phenol production 2.6-chlorophenesic acid is at present: with the ortho chloro phenol earlier sulfonation, and post chlorization reaction, hydrolysis under alkaline condition again, after carry out rectifying again and make its reaction formula:
This processing method exists complex process, and the consumption sulfuric acid amount is big, alkali consumption height, the defective that wastewater discharge is many.
The purpose of this invention is to provide and a kind ofly produce the short-cut method of 2.6-chlorophenesic acid, thereby overcome the deficiencies in the prior art part from the ortho chloro phenol single step reaction.
The processing method that adopts for the present invention that achieves the above object is: in agitator glass there-necked flask and exhaust emissions absorption unit are housed, add an amount of tetrachloride solvent and ortho chloro phenol earlier, under stirring state, add the appropriate amount of catalysts Diisopropylamine, heating and insulation feed a certain amount of chlorine again and react in certain temperature range, stop logical chlorine, urge and catch hydrogenchloride, and then material entered carry out fractionation in the rectifying tower, can obtain the 2.6-chlorophenesic acid.
Solvent for use tetrachloride of the present invention is zellon or tetracol phenixin, and the weight ratio of solvent and ortho chloro phenol is 10-20: 1, the weight percent of Diisopropylamine and ortho chloro phenol is 0.3-1%, the amount of chlorine that feeds and the weight ratio of ortho chloro phenol are 0.5-0.8: 1, and the heat tracing temperature is 70-110 ℃.
In sum, the method that the present invention proposes promptly in specific solvent, adds special catalyzer, at a certain temperature, carry out introduce chlorine gas to make reaction, and then carry out rectifying, this shows, advantages such as it is simple that the present invention has technology, and material consumption is few, and cost is low, and blowdown is few.
Below in conjunction with embodiment the present invention is done detailed explanation.
In agitator glass there-necked flask and exhaust emissions absorption unit are housed, add zellon 200 grams and ortho chloro phenol 20 grams earlier, under stirring state, add catalyzer Diisopropylamine 0.1 gram, heating and insulation are at 75-85 ℃, and logical chlorine reacts, and logical chlorine dose is 15 grams, stop logical oxygen, urge and catch hydrogenchloride 0.5-1 hour, and then material is entered rectifying tower carry out fractionation, can obtain 2.6-chlorophenesic acid 14-16 gram (content 98%), about selectivity 80%, reaction conversion ratio is more than 95%.In addition, 2.4-chlorophenesic acid 1-2 gram, 2.4.6--Trichlorophenol 2-3 gram, its chemical equation is:
The present invention compared with prior art has following characteristics:
1, the present invention's one one-step chlorination reaction, and old technology three-step reaction just can obtain, So technology of the present invention is simple, equipment investment is few, adapts to industrial production.
2, material consumption of the present invention is few, the solvent recoverable, so cost is low, And old technology consumption sulfuric acid amount is big, and the alkali consumption height can't be recycled.
3, the three wastes of the present invention are few, except in the chlorination process HCl toxic emission arranged, and do not have Other waste material, and wastewater flow rate is big in the old technological reaction process, particularly hydrolytic process In, produce 1: 10 waste water.
Claims (5)
1, a kind of method by ortho chloro phenol production 2,6-chlorophenesic acid, it is characterized in that in container that agitator is housed and exhaust emissions absorption unit, add an amount of tetrachloride solvent and ortho chloro phenol earlier, under stirring state, add the proper catalyst Diisopropylamine again, and the weight percent of Diisopropylamine and ortho chloro phenol is 0.3～1%, heating and insulation are in certain temperature range, feed again after a certain amount of chlorine reacts, stop logical chlorine, urge and catch hydrogenchloride, and then material entered carry out fractionation in the rectifying tower, can obtain 2, the 6-chlorophenesic acid.
2, method according to claim 1 is characterized in that the solvent tetrachloride is zellon or tetracol phenixin.
3, method according to claim 1 and 2, the weight ratio that it is characterized in that solvent and ortho chloro phenol is 10-20: 1.
4, method according to claim 1 and 2 is characterized in that the weight ratio of logical chlorine dose and ortho chloro phenol is 0.5-0.8: 1.
5, method according to claim 1 and 2 is characterized in that the heat tracing temperature is 75-110 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95101733A CN1035324C (en) | 1995-02-16 | 1995-02-16 | Process for production of 2,6-dichlorophenol by using O-chlorophenol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95101733A CN1035324C (en) | 1995-02-16 | 1995-02-16 | Process for production of 2,6-dichlorophenol by using O-chlorophenol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1129207A CN1129207A (en) | 1996-08-21 |
| CN1035324C true CN1035324C (en) | 1997-07-02 |
Family
ID=5074068
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95101733A Expired - Fee Related CN1035324C (en) | 1995-02-16 | 1995-02-16 | Process for production of 2,6-dichlorophenol by using O-chlorophenol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1035324C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106083532A (en) * | 2016-05-03 | 2016-11-09 | 灌云金安化工有限公司 | The process units of a kind of high-purity 2,6 chlorophenesic acid and production technology thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4094913A (en) * | 1977-01-07 | 1978-06-13 | Velsicol Chemical Corporation | Process for the preparation of 2,5-dichlorophenol |
| JPS5540613A (en) * | 1978-09-14 | 1980-03-22 | Sumitomo Chem Co Ltd | Preparation of 2, 6-dichloro-4-alkylphenol |
-
1995
- 1995-02-16 CN CN95101733A patent/CN1035324C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4094913A (en) * | 1977-01-07 | 1978-06-13 | Velsicol Chemical Corporation | Process for the preparation of 2,5-dichlorophenol |
| JPS5540613A (en) * | 1978-09-14 | 1980-03-22 | Sumitomo Chem Co Ltd | Preparation of 2, 6-dichloro-4-alkylphenol |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1129207A (en) | 1996-08-21 |
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