CN101423480A - Production method of 2, 6-dichloro-p-nitroaniline and special reaction kettle thereof - Google Patents
Production method of 2, 6-dichloro-p-nitroaniline and special reaction kettle thereof Download PDFInfo
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- CN101423480A CN101423480A CNA2008101363308A CN200810136330A CN101423480A CN 101423480 A CN101423480 A CN 101423480A CN A2008101363308 A CNA2008101363308 A CN A2008101363308A CN 200810136330 A CN200810136330 A CN 200810136330A CN 101423480 A CN101423480 A CN 101423480A
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- Prior art keywords
- nitroaniline
- reaction kettle
- volume
- dichloro
- production method
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- BIXZHMJUSMUDOQ-UHFFFAOYSA-N dichloran Chemical compound NC1=C(Cl)C=C([N+]([O-])=O)C=C1Cl BIXZHMJUSMUDOQ-UHFFFAOYSA-N 0.000 title abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 25
- TYMLOMAKGOJONV-UHFFFAOYSA-N 4-nitroaniline Chemical compound NC1=CC=C([N+]([O-])=O)C=C1 TYMLOMAKGOJONV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006467 substitution reaction Methods 0.000 claims abstract description 12
- 239000004568 cement Substances 0.000 claims abstract description 7
- 239000000919 ceramic Substances 0.000 claims abstract description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 35
- 239000000460 chlorine Substances 0.000 claims description 35
- 229910052801 chlorine Inorganic materials 0.000 claims description 35
- 239000000463 material Substances 0.000 claims description 14
- 239000006096 absorbing agent Substances 0.000 claims description 8
- 239000003755 preservative agent Substances 0.000 claims description 6
- 230000002335 preservative effect Effects 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 238000005660 chlorination reaction Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 15
- 239000000047 product Substances 0.000 description 10
- 150000001412 amines Chemical class 0.000 description 6
- 210000003298 dental enamel Anatomy 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000005266 casting Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002620 method output Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- GOLXNESZZPUPJE-UHFFFAOYSA-N spiromesifen Chemical compound CC1=CC(C)=CC(C)=C1C(C(O1)=O)=C(OC(=O)CC(C)(C)C)C11CCCC1 GOLXNESZZPUPJE-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a production method of 2, 6-dichloro-p-nitroaniline and a special reaction kettle thereof, wherein the method specifically comprises the following steps: the method comprises the following steps that p-nitroaniline and chlorine gas are subjected to substitution reaction in a concentrated hydrochloric acid medium to generate 2, 6-dichloro-p-nitroaniline, particularly, the substitution reaction is carried out in a large-volume reaction kettle connected with a tail gas absorption tower, the large-volume reaction kettle comprises a kettle body formed by pouring cement, ceramic tiles lined on the inner surface of the kettle body, and the volume of the reaction kettle is more than or equal to 15m3. The adoption of a large-volume reaction kettle can improve the yield, reduce the production cost and reduce the environmental pollution.
Description
Technical field
The invention belongs to the organic synthesis field, particularly relate to a kind of 2, the production method and the specific equipment thereof of 6-dichloro p-Nitroaniline.
Background technology
In the prior art, 2, it is raw material that the production of 6-dichloro p-Nitroaniline is taked with the p-Nitroaniline, feeds the interrupter method production of chlorine in enamel list still, because the enamel volume of present domestic maximum is 15m
3, involve great expense, and because the enamel still shell is an irony, very easily corrosion.Therefore equipment cost occupies larger proportion in producing, and because the operation of single still, not only yields poorly but also in case the chlorine that feeds has improperly slightly, the contents of residual chlorine in the tail gas will exceed standard greatly, and then cause severe contamination to environment.In addition, this method selectivity is relatively poor, can't effectively suppress to forbid the generation of by product polychlorobiphenyl amine.
Summary of the invention
It is a kind of 2 that technical problem to be solved by this invention provides, the production method of 6-dichloro p-Nitroaniline, and this method output height, production cost is low, environmental pollution is little.
The present invention also will provide reactor special-purpose in a kind of aforementioned production method, and its cost is low.
For solving above technical problem, a kind of technical scheme that the present invention takes is:
A kind of 2, the production method of 6-dichloro p-Nitroaniline, substitution reaction takes place and generates 2 in p-Nitroaniline and chlorine in the concentrated hydrochloric acid medium, 6-dichloro p-Nitroaniline, particularly, described substitution reaction is to carry out in being connected with the large-volume reaction kettle of tail gas absorber, and this large-volume reaction kettle comprises that building the still body, the lining that constitute by cement is located at the ceramic tile on the described still body internal surface, and its volume is more than or equal to 15m
3
Because the still body is that cement casting forms, equipment cost is lower, and the volume of still can be accomplished very big, thereby improve output and reduce cost, and in large-volume reaction kettle, feed chlorine, can reduce the effusion of chlorine, thereby reduce environmental pollution.
Above-mentioned 2, the further scheme of the production method of 6-dichloro p-Nitroaniline is: at first add p-Nitroaniline and concentrated hydrochloric acid in described large-volume reaction kettle, be incubated 55～60 ℃, then with 30～70m
3The speed of/h feeds chlorine and carries out substitution reaction in still, so, the operational condition gentleness greatly reduces the generation of forbidding by product polychlorobiphenyl amine, improves the quality of product.
Above-mentioned 2, the production method of 6-dichloro p-Nitroaniline also can be able to further enforcement by following proposal:
(1), a plurality of described large-volume reaction kettle are connected successively, and described tail gas absorber is connected with last reactor;
(2), in above-mentioned each large-volume reaction kettle, add p-Nitroaniline and concentrated hydrochloric acid;
(3), in each large-volume reaction kettle, feed chlorine successively and carry out described substitution reaction, after each substitution reaction finishes, before next large-volume reaction kettle feeds chlorine, the material that fed in the large-volume reaction kettle of chlorine is pumped, pump to continue in the large-volume reaction kettle behind the material to add and dissolved good p-Nitroaniline concentrated hydrochloric acid solution in the dissolution kettle, be serially connected in the back of former last reactor, continue chlorination reaction.To react good material then, and pump from large-volume reaction kettle, to neutral, it is described 2 that oven dry makes, 6-dichloro p-Nitroaniline through press filtration, washing.
Owing to take many still series connection to produce, almost there is not unnecessary chlorine to overflow in the production process, improve production environment greatly, and can improve the speed that chlorine feeds, thereby shorten the production cycle, enhance productivity.The volume of each large-volume reaction kettle is preferably at 40～60m
3Between.
Another technical scheme of the present invention is: a kind of being exclusively used in produces 2, the reactor of 6-dichloro p-Nitroaniline, and it comprises that still body, the lining constructed by cement are located at the ceramic tile on the described still body internal surface.
The volume of this reactor is preferably 15～60m
3
Preferably, aforesaid reaction vessel also comprises the preservative coat of the outside surface that is arranged on the still body.This preservative coat be by being that the epoxy anticorrosion material constitutes, and the mode of taking to apply is coated in the epoxy anticorrosion material on the outside surface of still body and forms described preservative coat.
The cost of this reactor is low, and is used to produce 2, and 6-dichloro p-Nitroaniline has output height, production cost is low, environmental pollution is little advantage.
Embodiment
The present invention will be described in detail below in conjunction with specific embodiment, but be not limited to this.
Among the following embodiment, every reactor that relates to is cement and builds and form, its liner ceramic tile, and outside surface scribbles the epoxy anticorrosion material.The volume of reactor can design arbitrarily according to producing needs.
Example 1
According to 2 of present embodiment, the equipment that the production method of 6-dichloro p-Nitroaniline is used mainly comprises: 1 dissolution kettle (volume 50m
3/ only), 5 placed in-line 50m
3/ reactor only and a shared tail gas absorber that all is communicated with 5 placed in-line reactors.Tail gas absorber is connected with each reactor, available valve opening or disconnection, and tail gas absorber is used for the hydrogen chloride gas that absorption reaction emits and the chlorine of complete reaction not.So reaction unit makes chlorine consumption near theoretical amount, does not have chlorine to be discharged in the atmosphere substantially, thereby reduces environmental pollution.
For convenience of description, above-mentioned 5 reactors are numbered are No. 1 still, No. 2 stills, No. 3 stills, No. 4 stills, No. 5 stills.
According to 2 of present embodiment, the production method of 6-dichloro p-Nitroaniline specifically comprises the steps:
(1), in above-mentioned 5 reactors, drop into 29% HCl 30T and p-Nitroaniline 1.7T respectively, stirred 3 hours.
(2), to No. 1 still with 50m
3The speed of/h feeds chlorine, and the tail gas of No. 1 still feeds in the material of No. 2 stills, and the tail gas of same No. 2 stills feeds No. 3 stills, and the tail gas of No. 3 stills feeds No. 4 stills, and the tail gas of No. 4 stills feeds No. 5 stills, and the tail gas of No. 5 stills inserts tail gas absorber and absorbs.Lead to chlorine after 4 hours, endpoint detection, after terminal point arrived, material was to room temperature in the cooling reactor, and then with this product pump entering plate basket, the press filtration after scouring is dried and is promptly got 2.525T finished product 2,6-dichloro p-Nitroaniline to neutral.After testing, 2,6-dichloro p-Nitroaniline purity is 97.5%, contains polychlorobiphenyl amine 0.8% in the finished product.
(3), treat that No. 1 still material pumps after, pump in No. 1 still having dissolved good material 1.7T p-Nitroaniline, 30T30% hydrochloric acid soln in the dissolution kettle, then No. 2 stills are fed chlorine, circulation successively, promptly No. 1 still tail gas inserts the absorption tower and absorbs.
According to 2 of present embodiment, the production method of 6-dichloro p-Nitroaniline is because the series connection of five stills is produced, therefore logical chlorine speed can suitably be accelerated, the time of logical chlorine shortens relatively, and the probability that produces forbidding by product polychlorobiphenyl amine reduces relatively, so the main content of reaction product is higher.
Embodiment 2
Other condition is with embodiment 1, and changing logical chlorine speed is 67m
3/ h, the logical chlorine time is 3 hours, records in the finished product, 2,6-dichloro p-Nitroaniline purity is 97.4%, contains polychlorobiphenyl amine 0.8% in the finished product.
Embodiment 3
Other condition is with embodiment 1, and changing logical chlorine speed is 40m
3/ h, the logical chlorine time is 5 hours, records in the finished product, 2,6-dichloro p-Nitroaniline purity is 96.5%, contains polychlorobiphenyl amine 1.3% in the finished product.
Comparative Examples (adopting the traditional technology preparation)
Drop into p-Nitroaniline 200Kg in the 5000L enamel reaction still, hydrochloric acid 3400Kg stirs and is warmed up to 50 ℃, slowly feeds chlorine (20m then
3About/h).The logical chlorine time is 10～12 hours.After endpoint detection arrives, cool to 40 ℃, stock is to the plate basket, and is washed to neutrality, must finished product 2, and 6-dichloro p-Nitroaniline 296Kg.
Hydrogen chloride gas that reaction produces and the chlorine that has not reacted absorb step by step with water ring vacuum pump.
The product of giving money as a gift are heavy: 296, and content 97.3%, many chlorine 1.1%.The chlorine consumption is bigger than normal.
Obviously, traditional technology will reach the selectivity identical with the present invention, the speed that then feeds chlorine is very slow, the time of finishing once production needs 10～12 hours at least, even so, still have more chlorine residue and overflow, make that not only production cost rises greatly, and operating environment of pollution.In addition, the advantage aspect output of the present invention also is conspicuous.
Claims (13)
1, a kind of 2, the production method of 6-dichloro p-Nitroaniline, substitution reaction takes place and generates 2 in p-Nitroaniline and chlorine in the concentrated hydrochloric acid medium, 6-dichloro p-Nitroaniline, it is characterized in that: described substitution reaction is carried out in being connected with the large-volume reaction kettle of tail gas absorber, described large-volume reaction kettle comprises that building the still body, the lining that constitute by cement is located at the ceramic tile on the described still body internal surface, and the volume of described large-volume reaction kettle is more than or equal to 15m
3
2, according to claim 1 a kind of 2, the production method of 6-dichloro p-Nitroaniline is characterized in that: at first add p-Nitroaniline and concentrated hydrochloric acid in described large-volume reaction kettle, be incubated 55～60 ℃, then with 30～70m
3The speed of/h feeds chlorine and carries out substitution reaction in still.
3, according to claim 1 a kind of 2, the production method of 6-dichloro p-Nitroaniline is characterized in that: described large-volume reaction kettle has a plurality of, and this production method specifically comprises the steps:
(1), a plurality of described large-volume reaction kettle are connected successively, and described tail gas absorber is connected with last reactor;
(2), in above-mentioned each large-volume reaction kettle, add p-Nitroaniline and concentrated hydrochloric acid;
(3), in each large-volume reaction kettle, feed chlorine successively and carry out described substitution reaction, after each substitution reaction finishes, before next large-volume reaction kettle feeds chlorine, the material that fed in the large-volume reaction kettle of chlorine is pumped, pump to continue in the large-volume reaction kettle behind the material to add and dissolved good p-Nitroaniline concentrated hydrochloric acid solution in the dissolution kettle, be serially connected in the back of former last reactor, continue chlorination reaction.The material that will react good then pumps from large-volume reaction kettle, and to neutral, it is described 2 that oven dry makes, 6-dichloro p-Nitroaniline through press filtration, washing.
4, according to claim 3 a kind of 2, the production method of 6-dichloro p-Nitroaniline is characterized in that: described large-volume reaction kettle is 5.
5, described a kind of 2 according to above-mentioned any claim, the production method of 6-dichloro p-Nitroaniline is characterized in that: the volume of described large-volume reaction kettle is 40～60m
3
6, a kind of being exclusively used in produces 2, and the reactor of 6-dichloro p-Nitroaniline is characterized in that: comprise that still body, the lining constructed by cement are located at the ceramic tile on the described still body internal surface.
7, reactor according to claim 6 is characterized in that: the volume of described reactor is 15～60m
3
8, reactor according to claim 6 is characterized in that: described reactor also comprises the preservative coat of the outside surface that is arranged on described still body.
9, reactor according to claim 8 is characterized in that: described preservative coat is made of the epoxy anticorrosion material.
10, according to Claim 8 or 9 described reactors, it is characterized in that: described preservative coat is coated on the outside surface of described still body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101363308A CN101423480A (en) | 2008-11-27 | 2008-11-27 | Production method of 2, 6-dichloro-p-nitroaniline and special reaction kettle thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101363308A CN101423480A (en) | 2008-11-27 | 2008-11-27 | Production method of 2, 6-dichloro-p-nitroaniline and special reaction kettle thereof |
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| CN101423480A true CN101423480A (en) | 2009-05-06 |
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| CNA2008101363308A Pending CN101423480A (en) | 2008-11-27 | 2008-11-27 | Production method of 2, 6-dichloro-p-nitroaniline and special reaction kettle thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618061A (en) * | 2012-03-12 | 2012-08-01 | 苏州市罗森助剂有限公司 | Preparation method for 2-[N-(2-cyanoethyl)-4-[(2,6-dichloro-4-nitrobenzophenone)azo]anilino]ethyl acetate |
| 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 |
| CN104592042A (en) * | 2014-12-29 | 2015-05-06 | 浙江龙盛集团股份有限公司 | Clean technology for continuously synthesizing 2,4-binitro-6-chloroaniline |
| CN105461571A (en) * | 2014-12-29 | 2016-04-06 | 浙江龙盛集团股份有限公司 | Clean technology for continuously synthesizing 2,6-dichloro-p-nitroaniline |
-
2008
- 2008-11-27 CN CNA2008101363308A patent/CN101423480A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618061A (en) * | 2012-03-12 | 2012-08-01 | 苏州市罗森助剂有限公司 | Preparation method for 2-[N-(2-cyanoethyl)-4-[(2,6-dichloro-4-nitrobenzophenone)azo]anilino]ethyl acetate |
| CN102618061B (en) * | 2012-03-12 | 2013-08-07 | 苏州市罗森助剂有限公司 | Preparation method for 2-[N-(2-cyanoethyl)-4-[(2,6-dichloro-4-nitrobenzophenone)azo]anilino]ethyl acetate |
| 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 |
| 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 |
| CN104592042A (en) * | 2014-12-29 | 2015-05-06 | 浙江龙盛集团股份有限公司 | Clean technology for continuously synthesizing 2,4-binitro-6-chloroaniline |
| CN105461571A (en) * | 2014-12-29 | 2016-04-06 | 浙江龙盛集团股份有限公司 | Clean technology for continuously synthesizing 2,6-dichloro-p-nitroaniline |
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Open date: 20090506 |