CN106278903B - Thick nitro-chlorobenzene washs production method - Google Patents
Thick nitro-chlorobenzene washs production method Download PDFInfo
- Publication number
- CN106278903B CN106278903B CN201510251307.3A CN201510251307A CN106278903B CN 106278903 B CN106278903 B CN 106278903B CN 201510251307 A CN201510251307 A CN 201510251307A CN 106278903 B CN106278903 B CN 106278903B
- Authority
- CN
- China
- Prior art keywords
- washing
- separator
- organic phase
- chlorobenzene
- nitro
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of thick nitro-chlorobenzenes to wash production method.After nitration reaction, nitration product and spent acid enter nitrator-separator separation, and the organic phase after separation carries out alkali cleaning in static mixer successively and washing, obtained organic phase carry out subsequent processing again.Alkali cleaning and washing are carried out using static mixer, due to making washing process realize pipeline, equipment investment can be reduced；And washings series connection is washed for thick nitro-chlorobenzene, can not only reduce the dosage of water, but also washing effect improves；For complete unit in addition to delivery pump, without motion object is less prone to failure, can increase effective production time.
Description
Technical field
The present invention relates to a kind of chemical products production methods, and in particular to be that Chlorobenzene Nitration is produced nitro-chlorobenzene and produced
Thick nitro-chlorobenzene in journey refines the production method of depickling, dephenolize.
Background technology
Nitro-chlorobenzene is important industrial chemicals, different with dividing by paranitrochlorobenzene, o-nitrochlorobenzene, 3 kinds of m-chloronitrobenzene
Structure body forms.Nitro-chlorobenzene can be reacted with the nitration mixture being made of sulfuric acid and nitric acid progress liquid-phase nitration to be made by chlorobenzene,
It nitrifies in obtained crude product containing residual acid and dangerous phenol by-product can be brought to subsequent production.Nitro-chlorobenzene is washed
Journey is with certain density lye come the residual acid in neutralized crude nitro-chlorobenzene, and so that phenols is reacted with alkali and generate phenates.Phenates
It is soluble easily in water, then washed, to realize depickling and dephenolize, obtain smart nitro-chlorobenzene.
The alkali cleaning of domestic traditional nitro-chlorobenzene, washing process are operated continuously frequently with autoclave, flow be first wash, then
Then alkali cleaning is washed again, equipment therefor is that more stirred autoclaves are used in series, the series connection of generally three kettles, water, lye and nitrification
Object counter-current flow.Such production method carries out mixing, washing using a water, and not only a water consumption is big, and generation is given up containing phenol
Water is more, and equipment number of units is more, investment is high, takes up a large area, and operation and control is complicated, and washing effect is not easy to ensure.
Invention content
The purpose of the present invention is to provide a kind of small investment, the thick nitro-chlorobenzene that installation area is small, washing effect is good is washed
Wash technique.Nitro-chlorobenzene washing is carried out using the present invention, due to making washing process realize pipeline, equipment investment can be reduced；And
Washings are used in series, and wastewater flow rate is small, and washing effect is good.
Technical solution of the invention is：Thick nitro-chlorobenzene from nitrator-separator, with aqueous slkali and from 2# points
Secondary water from device outlet, in 1# static mixers, cocurrent hybrid reaction, the by-product phenols in thick nitro-chlorobenzene and residual
Acid be neutralized and it is most of enter inorganic phase, the material after neutralization enters 1# separators, and upper layer spent lye sends to post-processing, under
The thick nitro-chlorobenzene of layer is with a water from 3# separator outlets, the cocurrent mixing, washing in 2# static mixers, most of sodium
Salt enters water phase, and material enters 2# separators after washing, isolates upper layer secondary water and removes 1# static mixers, lower coarse nitroxyl chloride
Benzene washes cocurrent mixing, washing in static mixer with process water in 3#, and remaining sodium salt travels further into water phase, material after washing
Into 3# separators, isolates the water of upper layer one time and 2# static mixers, lower layer's organic phase is gone further to be refining to obtain smart nitroxyl chloride
Benzene.
Wherein, material cocurrent mixes, and organic phase is 1 with inorganic phase molar ratio:1~2:1, preferably organic phase is matched with inorganic phase
Than being 4:3~5:3.
Wherein, nitrator-separator of the present invention and alkali cleaning separator be selected from gravity separator, cyclone separator or
Assemble separator, preferably gravity separator, residence time of material is 10 min-30 min.
Wherein, the lye of washing process is sodium hydrate aqueous solution, and the mass fraction of sodium hydrate aqueous solution is 5%-45%,
It is preferred that the mass fraction of sodium hydrate aqueous solution is 30%-40%, the flow-rate ratio of lye and organic phase is 15:1-50:1.
Wherein, washing and lock out operation temperature are 35-75 DEG C.
The present invention has the following advantages：
1. compared with multi-floating bodies countercurrent washing technology, is washed using static mixing tubular type, equipment investment can be saved；
2. washings series connection is washed for thick nitro-chlorobenzene, it is possible to reduce the dosage of water, and washing effect is good；
3. complete unit, in addition to transporting pump, without motion structure is less prone to failure, can increase effective production time.
Description of the drawings
Fig. 1 is the process flow diagram of the embodiment of the present invention.
Specific implementation mode
Following embodiment technological process is referring to attached drawing 1.
Embodiment 1：
The thick nitro-chlorobenzene 9.3m of 75 DEG C of temperature3/ h, 0.3 m of sodium hydroxide of 20% concentration3/ h and secondary water enter diameter
The 1# static mixers of 150mm, long 2m, control pressure 0.2MPa, it is laggard in 1# static mixers to be sufficiently mixed neutralization reaction
Enter 1# separators, residence time of material is 10min in 1# separators, and upper layer inorganic phase goes salkali waste to handle, lower layer's organic phase and 3#
Water of separator outlet enters cocurrent mixing, washing in 2# static mixers, control pressure 0.2MPa, the material after washing
Into 2# separators, residence time of material is 10min in 2# separators, and the water phase on upper layer enters 1# static mixers, lower layer
Organic phase and 5.4 m of Fresh process water3/ h enters 3# static mixer mixing, washings, and the material after washing enters 3# separators,
3# separator upper waters go 2# static mixers, lower layer's organic phase to remove nitro-chlorobenzene rectifier unit.
Embodiment 2：
The thick nitro-chlorobenzene 9.3m of 75 DEG C of temperature3/ h, 0.2 m of sodium hydroxide of 30% concentration3/ h and secondary water enter diameter
The 1# static mixers of 150mm, long 2m, control pressure 0.2MPa, it is laggard in 1# static mixers to be sufficiently mixed neutralization reaction
Enter 1# separators, residence time of material is 20min in 1# separators, and upper layer inorganic phase goes salkali waste to handle, lower layer's organic phase and 3#
Water of separator outlet enters cocurrent mixing, washing in 2# static mixers, control pressure 0.2MPa, the material after washing
Into 2# separators, residence time of material is 20min in 2# separators, and the water phase on upper layer enters 1# static mixers, lower layer
Organic phase and 6.4 m of Fresh process water3/ h enters 3# static mixer mixing, washings, and the material after washing enters 3# separators,
3# separator upper waters go 2# static mixers, lower layer's organic phase to remove nitro-chlorobenzene rectifier unit.
Embodiment 3：
The thick nitro-chlorobenzene 10.8m of temperature 70 C3/ h, 0.3 m of sodium hydroxide of 30% concentration3/ h and secondary water enter diameter
The 1# static mixers of 150mm, long 2m, control pressure 0.2MPa, it is laggard in 1# static mixers to be sufficiently mixed neutralization reaction
Enter 1# separators, residence time of material is 20min in 1# separators, and upper layer inorganic phase goes salkali waste to handle, lower layer's organic phase and 3#
Water of separator outlet enters cocurrent mixing, washing in 2# static mixers, control pressure 0.2MPa, the material after washing
Into 2# separators, residence time of material is 20min in 2# separators, and the water phase on upper layer enters 1# static mixers, lower layer
Organic phase and 6.5 m of Fresh process water3/ h enters 3# static mixer mixing, washings, and the material after washing enters 3# separators,
3# separator upper waters go 2# static mixers, lower layer's organic phase to remove nitro-chlorobenzene rectifier unit.
Embodiment 4：
The thick nitro-chlorobenzene 10.8m of temperature 70 C3/ h, 0.3 m of sodium hydroxide of 40% concentration3/ h and secondary water enter diameter
The 1# static mixers of 150mm, long 2m, control pressure 0.2MPa, it is laggard in 1# static mixers to be sufficiently mixed neutralization reaction
Enter 1# separators, residence time of material is 30min in 1# separators, and upper layer inorganic phase goes salkali waste to handle, lower layer's organic phase and 3#
Water of separator outlet enters cocurrent mixing, washing in 2# static mixers, control pressure 0.2MPa, the material after washing
Into 2# separators, residence time of material is 30min in 2# separators, and the water phase on upper layer enters 1# static mixers, lower layer
Organic phase and 7.6 m of Fresh process water3/ h enters 3# static mixer mixing, washings, and the material after washing enters 3# separators,
3# separator upper waters go 2# static mixers, lower layer's organic phase to remove nitro-chlorobenzene rectifier unit.
Embodiment 5：
The thick nitro-chlorobenzene 10.8m of temperature 70 C3/ h, 0.5 m of sodium hydroxide of 40% concentration3/ h and secondary water enter diameter
The 1# static mixers of 150mm, long 2m, control pressure 0.2MPa, it is laggard in 1# static mixers to be sufficiently mixed neutralization reaction
Enter 1# separators, residence time of material is 30min in 1# separators, and upper layer inorganic phase goes salkali waste to handle, lower layer's organic phase and 3#
Water of separator outlet enters cocurrent mixing, washing in 2# static mixers, control pressure 0.2MPa, the material after washing
Into 2# separators, residence time of material is 30min in 2# separators, and the water phase on upper layer enters 1# static mixers, lower layer
Organic phase and 7.4 m of Fresh process water3/ h enters 3# static mixer mixing, washings, and the material after washing enters 3# separators,
3# separator upper waters go 2# static mixers, lower layer's organic phase to remove nitro-chlorobenzene rectifier unit.
Sodium salt content the results are shown in Table 1 in thick nitro-chlorobenzene after above example washing.
Sodium salt content in 1 thick nitro-chlorobenzene of table
| Sample | Sodium salt content/ppm after washing |
| Embodiment 1 | 1.5 |
| Embodiment 2 | 1.3 |
| Embodiment 3 | 1.2 |
| Embodiment 4 | 1.5 |
| Embodiment 5 | 1.6 |
Except the various embodiments described above, embodiment of the present invention is also very much, all using equivalent or equivalence replacement technical side
Case, in protection scope of the present invention.
Although describing the present invention in above illustration, but it is to be understood that, the details is only used for
For example, those skilled in the art can make it in the spirit and scope that the claim without departing substantially from the present invention is limited
It changes.
Claims (4)
1. a kind of thick nitro-chlorobenzene washs production method, it is characterised in that：Alkali cleaning and washing, material are carried out using static mixer
Cocurrent mixes, and organic phase is 1 with inorganic phase molar ratio:1~2:1, lye is sodium hydrate aqueous solution, sodium hydrate aqueous solution
Mass fraction is 5%-45%, and the flow-rate ratio of lye and organic phase is 15:1-50:1, and washings series connection is used for thick nitro-chlorobenzene
Washing, detailed process are：After nitration reaction, nitration product and spent acid enter nitrator-separator separation, the thick nitre isolated
Base chlorobenzene and aqueous slkali and the secondary water from 2# separator outlets, in 1# static mixers, cocurrent is sufficiently mixed in progress
And reaction, the material after neutralization enter 1# separators, upper layer goes out inorganic phase, and lower layer goes out organic phase, lower layer's organic phase with come from 3#
Water of separator outlet, in 2# static mixers, cocurrent is sufficiently mixed washing, and material enters 2# separators after washing,
The upper layer secondary water isolated goes 1# static mixers, lower layer's organic phase to be washed in static mixer in 3# with process water, cocurrent
It is sufficiently mixed washing, material enters 3# separators after washing, isolates the water of upper layer one time and goes 2# static mixers, lower layer's organic phase
It goes further to be refining to obtain smart nitro-chlorobenzene；The residence time is 10-30 min, washing and lock out operation to material in the separator
Temperature is 35-75 DEG C.
2. according to the method described in claim 1, it is characterized in that organic phase and inorganic matched are 4:3~5:3.
3. according to the method described in claim 1, it is characterized in that separator be selected from gravity separator, cyclone separator or
Assemble separator.
4. according to the method described in claim 3, it is characterized in that separator uses gravity separator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510251307.3A CN106278903B (en) | 2015-05-18 | 2015-05-18 | Thick nitro-chlorobenzene washs production method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510251307.3A CN106278903B (en) | 2015-05-18 | 2015-05-18 | Thick nitro-chlorobenzene washs production method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106278903A CN106278903A (en) | 2017-01-04 |
| CN106278903B true CN106278903B (en) | 2018-09-25 |
Family
ID=57631907
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510251307.3A Active CN106278903B (en) | 2015-05-18 | 2015-05-18 | Thick nitro-chlorobenzene washs production method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106278903B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111389324A (en) * | 2020-04-20 | 2020-07-10 | 湖北东方化工有限公司 | System and method for mixed washing and separation of nitro compounds |
| CN111848325B (en) * | 2020-07-14 | 2023-05-09 | 中国石油化工股份有限公司 | Method and system for alkaline washing of cumene raw material by CHPPO device |
| CN111807920A (en) * | 2020-07-14 | 2020-10-23 | 中国石油化工股份有限公司 | Method and system for deacidifying cumene raw material of CHPPO (chlorinated Polypropylene oxide) device |
| CN115286511A (en) * | 2022-07-19 | 2022-11-04 | 安徽东至广信农化有限公司 | Efficient production process of nitrochlorobenzene |
| CN115138271B (en) * | 2022-07-20 | 2024-03-15 | 山东旭锐新材股份有限公司 | Continuous micro-washing system and method for brominated polystyrene solution |
| CN115286512A (en) * | 2022-07-25 | 2022-11-04 | 安徽东至广信农化有限公司 | Process for purifying nitration product |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101607911A (en) * | 2009-07-07 | 2009-12-23 | 扬州大学 | The washing impurity-removing technology of crude nitrochlorobenzene products after chlorobenzene thermal insulation nitration |
| CN102070457A (en) * | 2011-02-15 | 2011-05-25 | 河南洛染股份有限公司 | Method for continuously preparing dinitrochlorobenzene |
| CN103664629A (en) * | 2012-09-10 | 2014-03-26 | 中国石油化工股份有限公司 | Nitrobenzene washing and separating system |
-
2015
- 2015-05-18 CN CN201510251307.3A patent/CN106278903B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101607911A (en) * | 2009-07-07 | 2009-12-23 | 扬州大学 | The washing impurity-removing technology of crude nitrochlorobenzene products after chlorobenzene thermal insulation nitration |
| CN102070457A (en) * | 2011-02-15 | 2011-05-25 | 河南洛染股份有限公司 | Method for continuously preparing dinitrochlorobenzene |
| CN103664629A (en) * | 2012-09-10 | 2014-03-26 | 中国石油化工股份有限公司 | Nitrobenzene washing and separating system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106278903A (en) | 2017-01-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106278903B (en) | Thick nitro-chlorobenzene washs production method | |
| CN106278902B (en) | A kind of method for reducing sodium salt content in thick nitrobenzene | |
| CN107013924A (en) | Incineration of refuse flyash processing equipment and processing method | |
| CN103664629B (en) | A kind of nitrobenzene washing, separation system | |
| JP2017520559A5 (en) | ||
| CN101607911B (en) | Washing impurity-removing technology of crude nitrochlorobenzene products after chlorobenzene thermal insulation nitration | |
| CN106892792A (en) | A kind of method for continuously synthesizing and its synthesis device of 3,4 2 chlorobenzotrifluoride | |
| CN113248385A (en) | Method for reducing alkali consumption of acidic nitrobenzene | |
| CN106186435B (en) | Integrated treatment and the reuse method of a kind of Benzene Chloride waste liquid and waste residue | |
| CN103980126A (en) | Separation method of nitrochlorobenzene | |
| CN107286066A (en) | A kind of technique and system of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram | |
| CN104474875B (en) | Process the method for the waste gas containing hydrogen sulfide, Carbon bisulfide and corresponding device | |
| CN206328320U (en) | A kind of high purity caprolactam refining plant | |
| CN210215055U (en) | Processing apparatus of sodium sulfate waste liquid in coal tar production process | |
| CN108341399A (en) | A kind of production of chlorohydrination epoxides hypochlorous acid preparation facilities and its application method | |
| CN114085381B (en) | Gas phase dimethyl dichlorosilane hydrolysis process | |
| CN211487152U (en) | Device for treating tail gas discharged in disorganized mode in DMF (dimethyl formamide) wastewater recovery process | |
| CN202315644U (en) | Chlorine absorption device during production of trichloroiminocyanuric acid | |
| CN104891443B (en) | The gas-liquid of a kind of pure chlorine dioxide is automatically separated preparation facilities and preparation method | |
| CN103130296A (en) | Treatment process of industrial organic wastewater containing acetate | |
| CN203820680U (en) | System for continuously producing concentrate hydrosilicone oil | |
| CN110054338A (en) | The processing unit and application method of sodium sulfate waste liquid in a kind of coal tar oil production process | |
| CN202988883U (en) | Waste acid and waste saline water treatment system combining inorganic synthesis with reverse osmosis | |
| CN207204074U (en) | A kind of modified reactor | |
| CN114569929B (en) | Decomposition device and decomposition method for chloroethylene rectification residual liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee after: China Petroleum & Chemical Corp. Patentee after: SINOPEC NANJING CHEMICAL RESEARCH INSTITUTE Co.,Ltd. Address before: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee before: China Petroleum & Chemical Corp. Patentee before: Nanhua Group Research Institute |
|
| CP01 | Change in the name or title of a patent holder |