CN107963971A - A kind of method that 2,5- dichloronitrobenzenes are prepared using continuous nitrification technique - Google Patents
A kind of method that 2,5- dichloronitrobenzenes are prepared using continuous nitrification technique Download PDFInfo
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- CN107963971A CN107963971A CN201711500446.0A CN201711500446A CN107963971A CN 107963971 A CN107963971 A CN 107963971A CN 201711500446 A CN201711500446 A CN 201711500446A CN 107963971 A CN107963971 A CN 107963971A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/08—Preparation of nitro compounds by substitution of hydrogen atoms by nitro groups
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Abstract
The method that one kind prepares 2,5 dichloronitrobenzenes using continuous nitrification technique, its step are as follows：Sulfuric acid, nitric acid, acid is applied mechanically in being continuously added to after 1.35: 1: 1.46 ratio mixing in the first nitrification pot together with paracide；The temperature of three series connection nitrification pots of control, residence time of material, makes material reach successively in next pot by overflow；After the continuous nitrification reaction in three nitrification pots, isolated diluted acid and acid itrated compound, acid itrated compound is neutralized, washing, obtains 2.5 dichloronitrobenzene of crude product, then obtain more than 99.8% 2.5 dichloronitrobenzene of sterling by rectifying；The spent acid isolated it is a part of it is concentrated recycle, another part makes fertiliser containing magnesium and is used.Due to using continuous nitrification technology, nitrify step by step, successive reaction, so easy to operate, easily controllable, labor intensity is low, and side reaction is few, high income, without there is spent acid generation, production is more had continuity, stability, more adapts to automatic mass production.
Description
First, technical field：
It is especially a kind of to be prepared using continuous nitrification technique the present invention relates to the method that one kind prepares 2,5- dichloronitrobenzenes
The method of 2,5- dichloronitrobenzenes.
2nd, background technology：
2,5- dichloronitrobenzenes, as nitrogen fertilizer potentiating agent, have fixed nitrogen function of fertilizer retention, it is also possible to make dyestuff, pesticide, antioxygen
The intermediate of agent.In dye industry, for the bright red base GG of azoic dyes, red base 3GL, Fast Red RC base etc., 2,5- can be also prepared
Dichloroaniline is as dyestuff intermediate.It is the centre of herbicide dicamba and quizalofop-ethyl as pesticide intermediate in pesticide industry
Body.The primary raw material of 2,5- dichloronitrobenzenes or synthetic antibacterial agents triclosan, therefore, domestic production 2,5- dichloronitrobenzenes city
Field has a extensive future.
At present, domestic production 2,5 dichloronitrobenzenes mainly use batch production process, are to make bottom acid, addition pair with sulfuric acid
Dichloro-benzenes, is then added dropwise nitric acid, the mixed acid nitrification that sulfuric acid is prepared, by keeping the temperature, being layered, neutralizing, washing and dehydration obtains 2,5-
Dichloronitrobenzene product.Batch production process produces 2,5- dichloronitrobenzenes, and there is technological process is long, process units is more, spent acid
The problems such as treating capacity is big, waste water is how low with production capacity, and labor intensity is big.
3rd, the content of the invention：
In order to solve the deficiencies in the prior art, 2,5- are prepared using continuous nitrification technique the object of the present invention is to provide one kind
The method of dichloronitrobenzene.The production process of this method is to cancel nitration mixture to prepare, and simplifies technological process, realizes nitration reaction
Serialization, nitrification liquid separation serialization and spent acid extraction serialization.
Achieving the object of the present invention the technical solution of use is：One kind prepares 2,5- dichloro nitros using continuous nitrification technique
The method of benzene, its step are as follows：
Step 1, the preparation of nitration mixture：The sulfuric acid that concentration is 92.5% is added to nitration mixture kettle, concentration is 98% nitric acid, dense
Spend and apply mechanically acid for 75%-78%；Three kinds of acid in sulfuric acid in nitration mixture kettle: nitric acid: apply mechanically the ratio of acid=1.35: 1: 1.46
Mix stand-by；
Step 2, the paracide that purity is 99.54% is continuously added in first nitrification pot, meanwhile, nitration mixture is also connected
It is continuous to add in the first nitrification pot；The additional proportion of paracide and nitration mixture is 1.86: 1；
Step 3: the temperature of three series connection nitrification pots of control, residence time of material, makes material reach successively next by overflow
In pot；
Step 4: by three nitrification pots continuous nitrification react, realized in the 3rd nitrification pot continuous isolated
Diluted acid and acid itrated compound, upper strata acidity itrated compound are neutralized with 30% sodium carbonate, washed, and obtain crude product 2.5- dichloronitrobenzenes；
Step 5: crude product 2.5- dichloronitrobenzenes send rectification section rectifying, more than 99.8% sterling 2.5- dichloro nitre is obtained
Ji Benqu gas phase hydrogenations workshop section；The spent acid isolated it is a part of it is concentrated recycle, another part makes fertiliser containing magnesium and is used.
The acid of applying mechanically is made of sulfuric acid 76%, nitric acid 1.5% and water.
The temperature of three nitrification pots controls between 56 DEG C -57 DEG C, 61 DEG C -63 DEG C, 66 DEG C -68 DEG C successively；Thing
When expecting that the residence time is small for 3 in each nitrification pot.
The beneficial effects of the invention are as follows：Due to using three nitrification pot arranged in series, nitrify step by step at different temperature,
Successive reaction, so easy to operate, easily controllable, labor intensity is low, and side reaction is few, high income, without there is spent acid generation, makes production
More there is continuity, stability, more adapt to automatic mass production.
4th, embodiment：
A kind of method that 2,5- dichloronitrobenzenes are prepared using continuous nitrification technique of the invention, its step are as follows：Step 1,
The preparation of nitration mixture：The sulfuric acid that concentration is 92.5% is added to nitration mixture kettle, concentration is 98% nitric acid, and concentration is 75%-78%'s
Apply mechanically acid；Three kinds of acid in sulfuric acid in nitration mixture kettle: nitric acid: the ratio mixing for applying mechanically acid=1.35: 1: 1.46 is stand-by；Described
Acid is applied mechanically to be made of sulfuric acid 76%, nitric acid 1.5% and water.The paracide that purity is 99.54%, is continuously added to the by step 2
In one nitrification pot, meanwhile, nitration mixture is also continuously added in the first nitrification pot；The additional proportion of paracide and nitration mixture is 1.86:
1.Step 3: the temperature of three series connection nitrification pots of control, residence time of material；The temperature of three nitrification pots is controlled 56 successively
Between DEG C -57 DEG C, 61 DEG C -63 DEG C, 66 DEG C -68 DEG C；Material it is each nitrification pot in the residence time for 3 it is small when, make thing by overflow
Material reaches in next pot successively.Step 4: by three nitrification pots continuous nitrification react, the 3rd nitrification pot in realize connect
Continue isolated diluted acid and acid itrated compound, upper strata acidity itrated compound is neutralized with 30% sodium carbonate, washed, and obtains crude product 2.5- dichloros
Nitrobenzene.Step 5: crude product 2.5- dichloronitrobenzenes send rectification section rectifying, more than 99.8% sterling 2.5- dichloro nitros are obtained
Ben Qu gas phase hydrogenations workshop section；The spent acid isolated it is a part of it is concentrated recycle, another part makes fertiliser containing magnesium and is used.
This method uses continuous nitrification technology, makes the production of 2.5 dichloronitrobenzenes more have continuity, stability, more
Adapt to automatic mass production.
Claims (3)
1. the method that one kind prepares 2,5- dichloronitrobenzenes using continuous nitrification technique, its step are as follows：
Step 1, the preparation of nitration mixture：The sulfuric acid that concentration is 92.5% is added to nitration mixture kettle, concentration is 98% nitric acid, and concentration is
75%-78%'s applies mechanically acid；Three kinds of acid in sulfuric acid in nitration mixture kettle: nitric acid: apply mechanically the ratio mixing of acid=1.35: 1: 1.46
It is stand-by；
Step 2, the paracide that purity is 99.54% is continuously added in first nitrification pot, meanwhile, nitration mixture is also continuously added
Enter in the first nitrification pot；The additional proportion of paracide and nitration mixture is 1.86: 1；
Step 3: the temperature of three series connection nitrification pots of control, residence time of material, makes material reach next pot successively by overflow
In；
Step 4: by three nitrification pots continuous nitrification react, realize continuous isolated diluted acid in the 3rd nitrification pot
With acid itrated compound, upper strata acidity itrated compound is neutralized with 30% sodium carbonate, washed, and obtains crude product 2.5- dichloronitrobenzenes；
Step 5: crude product 2.5- dichloronitrobenzenes send rectification section rectifying, more than 99.8% sterling 2.5- dichloronitrobenzenes are obtained
Go to gas phase hydrogenation workshop section；The spent acid isolated it is a part of it is concentrated recycle, another part makes fertiliser containing magnesium and is used.
2. a kind of method that 2,5- dichloronitrobenzenes are prepared using continuous nitrification technique as claimed in claim 1, its feature are existed
In：The acid of applying mechanically is made of sulfuric acid 76%, nitric acid 1.5% and water.
3. a kind of method that 2,5- dichloronitrobenzenes are prepared using continuous nitrification technique as claimed in claim 1, its feature are existed
In：The temperature of three nitrification pots controls between 56 DEG C -57 DEG C, 61 DEG C -63 DEG C, 66 DEG C -68 DEG C successively；Material is every
When the residence time is 3 small in a nitrification pot.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711500446.0A CN107963971A (en) | 2017-12-23 | 2017-12-23 | A kind of method that 2,5- dichloronitrobenzenes are prepared using continuous nitrification technique |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552180A (en) * | 2020-12-17 | 2021-03-26 | 沧源华彧工贸有限公司 | Method for producing mixed dinitrobenzene by low-acid continuous nitration of nitrobenzene |
| CN112661648A (en) * | 2020-12-30 | 2021-04-16 | 中海油天津化工研究设计院有限公司 | Process method for co-producing sulfur magnesium fertilizer by isooctyl nitrate |
| CN112778136A (en) * | 2021-01-11 | 2021-05-11 | 南通江山农药化工股份有限公司 | 2, 5-dichloronitrobenzene and micro-channel continuous synthesis process thereof |
| CN115433091A (en) * | 2021-10-18 | 2022-12-06 | 江苏隆昌化工有限公司 | Method for synthesizing 2, 5-dichloronitrobenzene through continuous flow tubular reaction |
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| CN104649910A (en) * | 2013-11-25 | 2015-05-27 | 江苏扬农化工集团有限公司 | Method capable of recycling acids for preparing 2,5-dichloronitrobenzene (DCNB) through continuous nitration |
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- 2017-12-23 CN CN201711500446.0A patent/CN107963971A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104649910A (en) * | 2013-11-25 | 2015-05-27 | 江苏扬农化工集团有限公司 | Method capable of recycling acids for preparing 2,5-dichloronitrobenzene (DCNB) through continuous nitration |
Non-Patent Citations (1)
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| 刘东等: "连续硝化制备2,5-二氯硝基苯的工艺研究", 《农药》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552180A (en) * | 2020-12-17 | 2021-03-26 | 沧源华彧工贸有限公司 | Method for producing mixed dinitrobenzene by low-acid continuous nitration of nitrobenzene |
| CN112552180B (en) * | 2020-12-17 | 2023-08-11 | 沧源华彧工贸有限公司 | Method for producing mixed dinitrobenzene by low-acid continuous nitration of nitrobenzene |
| CN112661648A (en) * | 2020-12-30 | 2021-04-16 | 中海油天津化工研究设计院有限公司 | Process method for co-producing sulfur magnesium fertilizer by isooctyl nitrate |
| CN112778136A (en) * | 2021-01-11 | 2021-05-11 | 南通江山农药化工股份有限公司 | 2, 5-dichloronitrobenzene and micro-channel continuous synthesis process thereof |
| CN112778136B (en) * | 2021-01-11 | 2023-07-14 | 南通江山农药化工股份有限公司 | 2, 5-dichloronitrobenzene and microchannel continuous synthesis process thereof |
| CN115433091A (en) * | 2021-10-18 | 2022-12-06 | 江苏隆昌化工有限公司 | Method for synthesizing 2, 5-dichloronitrobenzene through continuous flow tubular reaction |
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