CN102617353A - Preparation method of 3, 4-dichloronitrobenzene - Google Patents
Preparation method of 3, 4-dichloronitrobenzene Download PDFInfo
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- CN102617353A CN102617353A CN 201210063171 CN201210063171A CN102617353A CN 102617353 A CN102617353 A CN 102617353A CN 201210063171 CN201210063171 CN 201210063171 CN 201210063171 A CN201210063171 A CN 201210063171A CN 102617353 A CN102617353 A CN 102617353A
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- dichloronitrobenzene
- preparation
- chlorination reaction
- chlorine
- nitrochloro
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Abstract
The invention relates to a preparation method of 3, 4-dichloronitrobenzene. According to the method, chlorine gas is introduced into para-nitrochloro-benzene at 100 DEG C to 105 DEG C under the condition of anhydrous ferric chloride existence for taking chlorination reaction to obtain the 3, 4-dichloronitrobenzene. Particularly, the chlorination reaction is always carried out under the infrared microwave irradiation, after the chlorination reaction is completed, reaction materials are neutralized, washed and delaminated to obtain 3, 4-dichloronitrobenzene crude products, and the crude products are further rectified to obtain 3, 4-dichloronitrobenzene finished products. The yield of the target products 3, 4-dichloronitrobenzene obtained according to the method provide by the invention is improved, and the purity is improved.
Description
Technical field
the present invention relates to a kind of 3, the preparation method of 4-dichloronitrobenzene.
Background technology
3, the 4-dichloronitrobenzene is the important intermediate of organic synthesis, is widely used in making fluorochlorobenzene amine, fluorine chloronitrobenzene and 3,4-dichlorphenamide bulk powder.Existing 3, the production of 4-dichloronitrobenzene has technology to be: para-nitrochloro-benzene under 100 ℃ ~ 105 ℃ of temperature, feeds chlorine and carries out chlorination reaction in the presence of the catalyzer FERRIC CHLORIDE ANHYDROUS.After chlorination reaches certain degree of depth, stop logical chlorine; Wash then, layering obtains 3,4-dichloronitrobenzene bullion.With 3,4-dichloronitrobenzene bullion carries out rectifying and promptly gets 3,4-dichloronitrobenzene finished product.The chlorination degree of depth is being strict controlled under the condition between 65% ~ 70%, this production technique gained 3, in the 4-dichloronitrobenzene finished product, the content of by product polychloride is generally 3% ~ 5%.And when chlorination degree of depth control bad, the by product polychloride can be doubled and redoubled.Therefore, adopt this explained hereafter 3, the 4-dichloronitrobenzene, operation is difficult for, and energy consumption is big, and yield is low, and the production capacity of unit equipment is little, and production cost is high.
Summary of the invention
technical problem to be solved by this invention is the deficiency that overcomes prior art, provides a kind of improved 3, the preparation method of 4-dichloronitrobenzene.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
are a kind of 3, the preparation method of 4-dichloronitrobenzene, and this method makes para-nitrochloro-benzene in the presence of FERRIC CHLORIDE ANHYDROUS, under 100 ℃ ~ 105 ℃ of temperature; Feeding chlorine carries out chlorination reaction and obtains 3, the 4-dichloronitrobenzene, and particularly, said chlorination reaction is carried out under the irradiation of infrared microwave always; Chlorination reaction neutralizes to reaction mass after finishing, washing, and layering obtains 3; The bullion of 4-dichloronitrobenzene, the further rectifying of bullion promptly gets 3,4-dichloronitrobenzene finished product.
preferably, the power that is used to produce the instrument of said infrared microwave is more than the 10KW.
Preferably, the feeding flow of chlorine is 30m
3
/ h ~ 50 m
3
/ h, the logical chlorine time is 5 ~ 10 hours
Because adopt the enforcement of above technical scheme, the present invention compared with prior art has following advantage:
according to the present invention, under the irradiation of infrared microwave, the selectivity of chlorination reaction is good especially, polychloride content considerably less (being lower than 2%), therefore, and target product 3, the yield of 4-dichloronitrobenzene improves, and purity improves.
Embodiment
Embodiment 1
3 of present embodiment, the preparation method of 4-dichloronitrobenzene is specific as follows: in 3000 liters chlorination reaction still, add 3000kg fused para-nitrochloro-benzene and 100kg FERRIC CHLORIDE ANHYDROUS; Be warmed up to 100 ℃; Open infrared microwave generator (power 10KW), open the recycle pump of carrying reaction mass, guarantee normal after; Open logical chlorine valve, chlorine flowrate 35m
3
/ h, logical chlorine stops logical chlorine after 8 hours, and the sampling analysis group of products becomes: 3,4-dichloronitrobenzene 80.2%; Para-nitrochloro-benzene 18.3%; Polychloride 1.5%.
Embodiment 2
3 of present embodiment, the preparation method of 4-dichloronitrobenzene is specific as follows: in 3000 liters chlorination reaction still, add 3000kg fused para-nitrochloro-benzene and 100kg FERRIC CHLORIDE ANHYDROUS; Be warmed up to 100 ℃; Open infrared microwave generator (power 10KW), open the recycle pump of carrying reaction mass, guarantee normal after; Open logical chlorine valve, chlorine flowrate 46m
3
/ h, logical chlorine stops logical chlorine after 6 hours, and the sampling analysis group of products becomes: 3,4-dichloronitrobenzene 79.2%; Para-nitrochloro-benzene 19.1%; Polychloride 1.7%.
Embodiment 3
3 of present embodiment, the preparation method of 4-dichloronitrobenzene is specific as follows: in 3000 liters chlorination reaction still, add 3000kg fused para-nitrochloro-benzene and 100kg FERRIC CHLORIDE ANHYDROUS; Be warmed up to 100 ℃; Open infrared microwave generator (power 10KW), open the recycle pump of carrying reaction mass, guarantee normal after; Open logical chlorine valve, chlorine flowrate 30m
3
/ h, logical chlorine stops logical chlorine after 10 hours, and the sampling analysis group of products becomes: 3,4-dichloronitrobenzene 80.4%; Para-nitrochloro-benzene 18.0%; Polychloride 1.6%.
Comparative example 1
3 of this example, the preparation method of 4-dichloronitrobenzene is specific as follows: in 3000 liters chlorination reaction still, add 3000kg fused para-nitrochloro-benzene and 100kg FERRIC CHLORIDE ANHYDROUS, be warmed up to 100 ℃, open logical chlorine valve, chlorine flowrate 35m
3
/ h, logical chlorine stops logical chlorine after 8 hours, and the sampling analysis group of products becomes: 3,4-dichloronitrobenzene 65.7%; Para-nitrochloro-benzene 29.8%; Polychloride 4.5%.
are visible with embodiment 1 to 3 contrast with comparative example 1, and the chlorination degree of depth of Comparative Examples 1 is low, and polychloride is many, and this yield is low, and therefore, production cost is high.
More than the present invention has been done detailed description; Its purpose is to let the personage that is familiar with this art can understand content of the present invention and implements; Can not limit protection scope of the present invention with this; All equivalences of doing according to spirit of the present invention change or modify, and all should be encompassed in protection scope of the present invention
Claims (3)
1. one kind 3, the preparation method of 4-dichloronitrobenzene, this method makes para-nitrochloro-benzene in the presence of FERRIC CHLORIDE ANHYDROUS, under 100 ℃ ~ 105 ℃ of temperature; Feeding chlorine carries out chlorination reaction and obtains 3, and the 4-dichloronitrobenzene is characterized in that: said chlorination reaction is carried out under the irradiation of infrared microwave always, after chlorination reaction finishes; Reaction mass is neutralized, washing, layering obtains 3; The bullion of 4-dichloronitrobenzene, the further rectifying of bullion promptly gets 3,4-dichloronitrobenzene finished product.
2. according to claim 13, the preparation method of 4-dichloronitrobenzene is characterized in that: the power that is used to produce the instrument of said infrared microwave is more than the 10KW.
3. according to claim 13, the preparation method of 4-dichloronitrobenzene is characterized in that: the feeding flow of chlorine is 30m
3/ h ~ 50 m
3/ h, the logical chlorine time is 5 ~ 10 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210063171 CN102617353B (en) | 2012-03-12 | 2012-03-12 | Preparation method of 3, 4-dichloronitrobenzene |
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| CN 201210063171 CN102617353B (en) | 2012-03-12 | 2012-03-12 | Preparation method of 3, 4-dichloronitrobenzene |
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|---|---|
| CN102617353A true CN102617353A (en) | 2012-08-01 |
| CN102617353B CN102617353B (en) | 2013-07-10 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875384A (en) * | 2012-10-16 | 2013-01-16 | 江苏扬农化工集团有限公司 | Method for separating 3, 4-dichloronitrobenzene crystallization mother liquor through extractive distillation |
| CN105418433A (en) * | 2015-11-17 | 2016-03-23 | 山东沾化天九化工有限公司 | Method and device for producing 3,4-dichloronitrobenzene through continuous kettle type reaction |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134712A (en) * | 2007-10-08 | 2008-03-05 | 浙江省常山长盛化工有限公司 | Preparation method of 2,4-dichloro fluorobenzene |
-
2012
- 2012-03-12 CN CN 201210063171 patent/CN102617353B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134712A (en) * | 2007-10-08 | 2008-03-05 | 浙江省常山长盛化工有限公司 | Preparation method of 2,4-dichloro fluorobenzene |
Non-Patent Citations (2)
| Title |
|---|
| 《新疆师范大学学报》 20050331 高军军 微波催化技术在有机合成中的作用 40-44 1-3 第24卷, 第1期 * |
| 《连云港职业大学学报》 19981231 张荣成 2，4-二氯氟苯的合成 42-43 1-3 第十一卷, 第4期 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875384A (en) * | 2012-10-16 | 2013-01-16 | 江苏扬农化工集团有限公司 | Method for separating 3, 4-dichloronitrobenzene crystallization mother liquor through extractive distillation |
| CN105418433A (en) * | 2015-11-17 | 2016-03-23 | 山东沾化天九化工有限公司 | Method and device for producing 3,4-dichloronitrobenzene through continuous kettle type reaction |
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| CN102617353B (en) | 2013-07-10 |
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