CN101143829A - Method for producing 2,6-dichloro-4-trifluoromethylaniline - Google Patents
Method for producing 2,6-dichloro-4-trifluoromethylaniline Download PDFInfo
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- CN101143829A CN101143829A CNA2007101347476A CN200710134747A CN101143829A CN 101143829 A CN101143829 A CN 101143829A CN A2007101347476 A CNA2007101347476 A CN A2007101347476A CN 200710134747 A CN200710134747 A CN 200710134747A CN 101143829 A CN101143829 A CN 101143829A
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- trifluoromethyl aniline
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Abstract
The invention discloses a production method of 2, 6-dichloro-4-trifluoromethylaniline, which ordinally includes reaction, desolventization, vacuum rectification, etc. The invention has the advantages of easy operation and good quality of products, and the purity of products can be over ninety nine point five percent.
Description
Technical field:
The present invention relates to a kind of 2, the production method of 6-dichlor-4-trifluoromethyl aniline.
Background technology:
2, the 6-dichlor-4-trifluoromethyl aniline is a kind of of great value pesticide intermediate, be mainly used in the sharp strength spy of agricultural chemicals of the high-efficiency low-toxicity of synthesizing new, sharp strength spy is the pesticide new variety of actively promoting in recent years with China Ministry of Agriculture in the world, and its range of application is more and more wider.Existing processes complexity, quality product are not good.
Summary of the invention:
The object of the present invention is to provide a kind of good product quality, easy-operating 2, the production method of 6-dichlor-4-trifluoromethyl aniline.
Technical solution of the present invention is:
A kind of 2, the production method of 6-dichlor-4-trifluoromethyl aniline is characterized in that: comprise the following steps: successively
(1) reaction: the p-trifluoromethylaniline raw material is added in the solvent, in reactor, feed chlorine and carry out chlorination reaction generation 2, the mixture of 6-dichlor-4-trifluoromethyl aniline, byproduct hydrochloric acid tail gas is used to reclaim hydrochloric acid;
(2) remove solvent: with 2,6-dichlor-4-trifluoromethyl aniline mixture, remove solvent after, add the alkali neutralization, 2,6-dichlor-4-trifluoromethyl aniline crude product;
(3) rectification under vacuum: with 2,6-dichlor-4-trifluoromethyl aniline crude product send into smart slip device carry out rectification under vacuum refining finished product.
The concrete grammar of step (3) is: with 2,6-dichlor-4-trifluoromethyl aniline crude product pumps into 60～80 ℃ of heating evaporations in the dehydrogenation still kettle, steam lower boiling steam, still material in the dehydrogenation still kettle pumps in the rectifying tower still kettle, under vacuum condition, heat 70～90 ℃ of evaporations, 2, the steam of 6-dichlor-4-trifluoromethyl aniline enters rectifying tower, from overhead collection 2, the 6-dichlor-4-trifluoromethyl aniline is made with extra care finished product.
Solvent in the step (1) is toluene, ethylene dichloride, trichloromethane, glacial acetic acid or tetracol phenixin.The 5-trifluoromethylaniline raw material in the step (1) and the amount ratio of solvent are by weight: 1: 2.5～4.0.
The lower boiling steam that steams enters in the lightness-removing column, advances packing layer under vacuum condition from bottom to top, removes 2, the light constituent in the 6-dichlor-4-trifluoromethyl aniline crude product.
The present invention is easy to operate, good product quality, and product purity reaches more than 99.5%.
The invention will be further described below in conjunction with embodiment.
Embodiment:
A kind of 2, the production method of 6-dichlor-4-trifluoromethyl aniline comprises the following steps: successively
(1) reaction: the p-trifluoromethylaniline raw material is added in the solvent, feed chlorine and carry out chlorination reaction generation 2 in reactor, the mixture of 6-dichlor-4-trifluoromethyl aniline, byproduct hydrochloric acid tail gas are used to reclaim hydrochloric acid and sell;
(2) remove solvent: with 2,6-dichlor-4-trifluoromethyl aniline mixture after precipitation still heating evaporation removes solvent fully, adds the alkali neutralization, gets 2,6-dichlor-4-trifluoromethyl aniline crude product;
(3) rectification under vacuum: with 2,6-dichlor-4-trifluoromethyl aniline crude product pumps into 60～80 ℃ of heating evaporations in the dehydrogenation still kettle, steam lower boiling steam, still material in the dehydrogenation still kettle pumps into the rectifying tower still kettle at the bottom of still, heats 70～90 ℃ of evaporations under vacuum condition, 2, the steam of 6-dichlor-4-trifluoromethyl aniline enters rectifying tower, by packing layer, from overhead collection 2, the 6-dichlor-4-trifluoromethyl aniline is made with extra care finished product from bottom to top.The above-mentioned lower boiling steam that steams enters in the lightness-removing column, advances packing layer under vacuum condition from bottom to top, removes 2, the light constituent in the 6-dichlor-4-trifluoromethyl aniline crude product.
Solvent in the step (1) is toluene (or ethylene dichloride or trichloromethane or glacial acetic acid or a tetracol phenixin.
The 5-trifluoromethylaniline raw material in the step (1) and the amount ratio of solvent are by weight: 1: 2.5～4.0 (routine 1:2.5,1: 3.3,1: 4.0).
Claims (5)
1. one kind 2, the production method of 6-dichlor-4-trifluoromethyl aniline is characterized in that: comprise the following steps: successively
(1) reaction: the p-trifluoromethylaniline raw material is added in the solvent, in reactor, feed chlorine and carry out chlorination reaction generation 2, the mixture of 6-dichlor-4-trifluoromethyl aniline, byproduct hydrochloric acid tail gas is used to reclaim hydrochloric acid;
(2) remove solvent: with 2,6-dichlor-4-trifluoromethyl aniline mixture, remove solvent after, add the alkali neutralization, 2,6-dichlor-4-trifluoromethyl aniline crude product;
(3) rectification under vacuum: with 2,6-dichlor-4-trifluoromethyl aniline crude product send into smart slip device carry out rectification under vacuum refining finished product.
2. according to claim 12, the production method of 6-dichlor-4-trifluoromethyl aniline, it is characterized in that: the concrete grammar of step (3) is: with 2,6-dichlor-4-trifluoromethyl aniline crude product pumps into 60～80 ℃ of heating evaporations in the dehydrogenation still kettle, steam lower boiling steam, still material in the dehydrogenation still kettle pumps in the rectifying tower still kettle, under vacuum condition, heat 70～90 ℃ of evaporations, 2, the steam of 6-dichlor-4-trifluoromethyl aniline enters rectifying tower, from overhead collection 2, the 6-dichlor-4-trifluoromethyl aniline is made with extra care finished product.
3. according to claim 1 and 22, the production method of 6-dichlor-4-trifluoromethyl aniline is characterized in that: the solvent in the step (1) is toluene, ethylene dichloride, trichloromethane, glacial acetic acid or tetracol phenixin.
4. according to claim 1 and 22, the production method of 6-dichlor-4-trifluoromethyl aniline is characterized in that: the 5-trifluoromethylaniline raw material in the step (1) and the amount ratio of solvent are by weight: 1: 2.5～4.0.
5. according to claim 22, the production method of 6-dichlor-4-trifluoromethyl aniline is characterized in that: the lower boiling steam that steams, enter in the lightness-removing column, under vacuum condition, advanced packing layer from bottom to top, removed 2, the light constituent in the 6-dichlor-4-trifluoromethyl aniline crude product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101347476A CN100534975C (en) | 2007-10-16 | 2007-10-16 | Method for producing 2,6-dichloro-4-trifluoromethylaniline |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2007101347476A CN100534975C (en) | 2007-10-16 | 2007-10-16 | Method for producing 2,6-dichloro-4-trifluoromethylaniline |
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| CN101143829A true CN101143829A (en) | 2008-03-19 |
| CN100534975C CN100534975C (en) | 2009-09-02 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863342A (en) * | 2012-10-17 | 2013-01-09 | 湖北美天生物科技有限公司 | Preparation method of high-purity 2, 6-dichloro-4-trifluoromethyl aniline |
| CN103450030A (en) * | 2013-09-05 | 2013-12-18 | 南通市海圣药业有限公司 | Chlorine introducing method of 3,5-dichloro-4-aminotrifluorotoluene and chlorine introducing system applied to chlorine introducing method |
| CN103483207A (en) * | 2013-09-05 | 2014-01-01 | 南通市海圣药业有限公司 | Rectification method for 3,5-dichloro-4-aminotrifluorotoluene as well as light tower system and rectification tower system applied in rectification method of 3,5-dichloro-4-aminotrifluorotoluene |
| CN106748808A (en) * | 2016-11-14 | 2017-05-31 | 苏州市罗森助剂有限公司 | A kind of environment-friendly preparation method of 2,6 dichloro paranitroanilinum |
| CN106866426A (en) * | 2017-02-27 | 2017-06-20 | 浙江巍华化工有限公司 | A kind of method of comprehensive utilization of the trichlorobenzotrifluoride of accessory substance 2,4,5 for producing 3,4,5 trichlorobenzotrifluorides |
| CN114507147A (en) * | 2022-03-16 | 2022-05-17 | 浙江巍华新材料股份有限公司 | Method for preparing 2, 6-dichloro-4-trifluoromethylaniline |
-
2007
- 2007-10-16 CN CNB2007101347476A patent/CN100534975C/en active Active
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863342A (en) * | 2012-10-17 | 2013-01-09 | 湖北美天生物科技有限公司 | Preparation method of high-purity 2, 6-dichloro-4-trifluoromethyl aniline |
| CN103450030A (en) * | 2013-09-05 | 2013-12-18 | 南通市海圣药业有限公司 | Chlorine introducing method of 3,5-dichloro-4-aminotrifluorotoluene and chlorine introducing system applied to chlorine introducing method |
| CN103483207A (en) * | 2013-09-05 | 2014-01-01 | 南通市海圣药业有限公司 | Rectification method for 3,5-dichloro-4-aminotrifluorotoluene as well as light tower system and rectification tower system applied in rectification method of 3,5-dichloro-4-aminotrifluorotoluene |
| WO2015032235A1 (en) * | 2013-09-05 | 2015-03-12 | 南通市海圣药业有限公司 | Rectification method for 3,5-dichloro-4-aminotrifluorotoluene, and light tower system and rectification tower system used in rectification method |
| CN103483207B (en) * | 2013-09-05 | 2015-04-22 | 南通市海圣药业有限公司 | Rectification method for 3,5-dichloro-4-aminotrifluorotoluene as well as light tower system and rectification tower system applied in rectification method of 3,5-dichloro-4-aminotrifluorotoluene |
| CN103450030B (en) * | 2013-09-05 | 2015-05-27 | 南通市海圣药业有限公司 | Chlorine introducing method of 3,5-dichloro-4-aminotrifluorotoluene and chlorine introducing system applied to chlorine introducing method |
| CN106748808A (en) * | 2016-11-14 | 2017-05-31 | 苏州市罗森助剂有限公司 | A kind of environment-friendly preparation method of 2,6 dichloro paranitroanilinum |
| CN106866426A (en) * | 2017-02-27 | 2017-06-20 | 浙江巍华化工有限公司 | A kind of method of comprehensive utilization of the trichlorobenzotrifluoride of accessory substance 2,4,5 for producing 3,4,5 trichlorobenzotrifluorides |
| CN106866426B (en) * | 2017-02-27 | 2018-08-10 | 浙江巍华化工有限公司 | A kind of method of comprehensive utilization for the by-product 2,4,5- trichlorobenzotrifluorides producing 3,4,5-Trichloro-trifluoromethyl-benzene |
| CN114507147A (en) * | 2022-03-16 | 2022-05-17 | 浙江巍华新材料股份有限公司 | Method for preparing 2, 6-dichloro-4-trifluoromethylaniline |
| CN114507147B (en) * | 2022-03-16 | 2024-03-19 | 浙江巍华新材料股份有限公司 | Method for preparing 2, 6-dichloro-4-trifluoromethyl aniline |
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| Publication number | Publication date |
|---|---|
| CN100534975C (en) | 2009-09-02 |
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Address after: 226401 Jiangsu County of Rudong Province town Ma Tang Jianshe Road No. 40-1 Patentee after: Jiangsu YOUPU bio chemical Polytron Technologies Inc Address before: 226401 Jiangsu County of Rudong Province town Ma Tang Jianshe Road No. 40-1 Patentee before: Dongchang Chemical Industry Co., Ltd., Nantong City |
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