CN106748808A - A kind of environment-friendly preparation method of 2,6 dichloro paranitroanilinum - Google Patents
A kind of environment-friendly preparation method of 2,6 dichloro paranitroanilinum Download PDFInfo
- Publication number
- CN106748808A CN106748808A CN201610998905.1A CN201610998905A CN106748808A CN 106748808 A CN106748808 A CN 106748808A CN 201610998905 A CN201610998905 A CN 201610998905A CN 106748808 A CN106748808 A CN 106748808A
- Authority
- CN
- China
- Prior art keywords
- organic solvent
- paranitroanilinum
- environment
- filtrate
- friendly preparation
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/68—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton
- C07C209/74—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton by halogenation, hydrohalogenation, dehalogenation, or dehydrohalogenation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of environment-friendly preparation method of 2,6 dichloro paranitroanilinum, it is comprised the following steps：（a）To organic solvent is added in reaction vessel, paranitroanilinum is subsequently added, stirring is warming up to 50 ~ 70 DEG C and is incubated 1 ~ 3 hour；（b）Again to being passed through chlorine reaction to terminal in the reaction vessel, press filtration after cooling；（c）Filtrate is applied mechanically；Filter cake reclaims the organic solvent, then pressure-filteration drying after being beaten with water using steam distillation.Reacted instead of hydrochloric acid medium by using organic solvent; and subsequently filtrate is being applied mechanically, organic solvent is being reclaimed using steam distillation; discharge this avoid hydrochloric acid medium to environment without polluting, and organic solvent and filtrate all realize recovery, very environmentally friendly；Prior can be that the purity of product is controlled, and improve the quality of product.
Description
Technical field
The invention belongs to chemical assistant field, and in particular to the environment-friendly preparation method of one kind 2,6- dichloro paranitroanilinum.
Background technology
At present, the preparation method of 2,6- dichloros paranitroanilinum mainly has two kinds：（1）By 3,4,5- trichloronitrobenzenes in height
Pressure kettle mesohigh ammonolysis and obtain, the preparation technology equipment investment greatly, it is necessary to using high-tension apparatus, with danger；The technique mesh
It is preceding also only in the theoretic discussion stage, few industrialization, its main application is still processing the trichlorine nitro of accessory substance 3,4,5-
For the purpose of benzene；（2）Paranitroanilinum leads to chlorine reaction in hydrochloric acid medium and forms, and product appearance prepared by the method is in dark yellow,
Quality is universal 94% or so；More headache, the substantial amounts of acid mother liquid waste water of preparation technology generation, cause to environment
Influence.In today of environmentally friendly pay attention to day by day, 2, the 6- dichloro paranitroanilinum preparation methods for developing environmental protection have great importance.
The content of the invention
A kind of environmental protection of 2,6- dichloros paranitroanilinum is provided the invention aims to overcome the deficiencies in the prior art
Preparation method.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：A kind of environmental protection system of 2,6- dichloros paranitroanilinum
Preparation Method, it is comprised the following steps：
（a）To organic solvent is added in reaction vessel, paranitroanilinum is subsequently added, it is small that stirring is warming up to 50 ~ 70 DEG C of insulations 1 ~ 3
When；
（b）Again to being passed through chlorine to reaction end in the reaction vessel, press filtration after cooling；
（c）Filtrate is applied mechanically；Filter cake reclaims the organic solvent after being beaten with water using steam distillation, then pressure-filteration drying is
Can.
Optimally, the organic solvent is one or more mixture of composition in Benzene Chloride, o-dichlorohenzene and DMF.
Further, the ratio of the organic solvent and the nitroaniline is 10 ~ 15L：1kg.
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：Solvent method of the present invention 2,
The environment-friendly preparation method of 6- dichloro paranitroanilinum, is reacted by using organic solvent instead of hydrochloric acid medium, and follow-up
Filtrate is applied mechanically, organic solvent is reclaimed using steam distillation, the discharge this avoid hydrochloric acid medium to environment without making
Into pollution, and organic solvent and filtrate all realize recovery, are emitted no waste water in preparation, very environmentally friendly；More importantly
The purity of product can be controlled, outward appearance is gorgeous, Functionality, quality and appealing design, product content improves the matter of product up to more than 97%
Amount.
Specific embodiment
The present invention is further described below in conjunction with embodiment.
Embodiment 1
The present embodiment provides the environment-friendly preparation method of one kind 2,6- dichloro paranitroanilinum, and it is comprised the following steps：
（a）To Benzene Chloride 7000L is added in the enamel reaction still of 10000L, paranitroanilinum 500kg is subsequently added, stirring heats up
2 hours are incubated to 60 DEG C；
（b）At this temperature, chlorination reaction is carried out to being slowly passed through chlorine in enamel reaction still（Chlorine is passed through for existing routine
Parameter, as long as not making reaction extreme heat emission）；When logical chlorine dose reaches the 90% of theoretical molar amount, it is necessary in the mistake of logical chlorine
Many sub-samplings in journey, in system to be titrated during p-nitrophenyl amine content≤1%, stop ventilation, then be incubated 2 hours（During whole chlorination
Between at ten hours or so；The amount of chlorine for being passed through 50% in first 3 hours；The middle 4 small times are passed through 40% amount of chlorine；Lead within last 3 hours
Enter 10% amount of chlorine；Molar content）；Press filtration after cooling；
（c）Filtrate is applied to next group；Filter cake reclaims organic solvent, then pressure-filteration drying after being beaten with water using steam distillation
Obtain product.
Product quality
Outward appearance：It is golden yellow；
2,6- dichloro paranitroanilinum purity 97.2%.
Embodiment 2
The present embodiment provides the environment-friendly preparation method of one kind 2,6- dichloro paranitroanilinum, and it is comprised the following steps：
（a）To adding DMF in the enamel reaction still of 10000L（Dimethylformamide）5000L, is subsequently added paranitroanilinum
500kg, stirring is warming up to 70 DEG C and is incubated 1 hour；
（b）At this temperature, chlorination reaction is carried out to being passed through chlorine in enamel reaction still；When logical chlorine dose reaches theoretical molar amount
When 90%, it is desirable to many sub-samplings in logical chlorine process；In system to be titrated during p-nitrophenyl amine content≤1%, stop ventilation, then
Insulation 2 hours（Logical chlorine process reference implementation example 1）；Press filtration after cooling；
（c）Filtrate is applied to next group；Filter cake reclaims organic solvent, then pressure-filteration drying after being beaten with water using steam distillation
Obtain product.
Product quality
Outward appearance：It is golden yellow；
2,6- dichloros paranitroanilinum 97.0%.
Embodiment 3
The present embodiment provides the environment-friendly preparation method of one kind 2,6- dichloro paranitroanilinum, and it is comprised the following steps：
（a）To adding DMF in the enamel reaction still of 10000L（Dimethylformamide）7500L, is subsequently added paranitroanilinum
500kg, stirring is warming up to 50 DEG C and is incubated 3 hours；
（b）At this temperature, chlorination reaction is carried out to being passed through chlorine in enamel reaction still；When logical chlorine dose reaches theoretical molar amount
When 90%, it is desirable to many sub-samplings during logical chlorine；In system to be titrated during p-nitrophenyl amine content≤1%, stop logical
Gas, then it is incubated 2 hours（Logical chlorine process reference implementation example 1）；Press filtration after cooling；
（c）Filtrate is applied to next group；Filter cake reclaims organic solvent, then pressure-filteration drying after being beaten with water using steam distillation
Obtain product.
Product quality
Outward appearance：It is golden yellow；
2,6- dichloros paranitroanilinum 96.8%.
Comparative example 1
The present embodiment provides the preparation method of one kind 2,6- dichloro paranitroanilinum, and it is comprised the following steps：
（a）To addition watery hydrochloric acid 7000L in the enamel reaction still of 10000L（Mass concentration is 30%）, it is subsequently added p-nitrophenyl
Amine 500kg, stirring is warming up to 60 DEG C and is incubated 2 hours；
（b）At this temperature, chlorination reaction is carried out to being passed through chlorine in enamel reaction still；When logical chlorine dose reaches theoretical molar amount
When 90%, it is desirable to many sub-samplings during logical chlorine；In system to be titrated during p-nitrophenyl amine content≤1%, stop logical
Gas, then it is incubated 2 hours（Logical chlorine process reference implementation example 1）；Press filtration after cooling；
（c）Filtrate is applied to next group；After filter cake is beaten with water, washing to neutral re-dry obtains product.
Product quality
Outward appearance：Dark yellow；
2,6- dichloros paranitroanilinum 94.3%
The above embodiments merely illustrate the technical concept and features of the present invention, its object is to allow person skilled in the art's energy
Solution present disclosure much of that is simultaneously implemented according to this, and it is not intended to limit the scope of the present invention, all according to spirit of the invention
The equivalent change or modification that essence is made, should all be included within the scope of the present invention.
Claims (3)
1. one kind 2, the environment-friendly preparation method of 6- dichloro paranitroanilinum, it is characterised in that it is comprised the following steps：
（a）To organic solvent is added in reaction vessel, paranitroanilinum is subsequently added, it is small that stirring is warming up to 50 ~ 70 DEG C of insulations 1 ~ 3
When；
（b）Again to being passed through chlorine to reaction end in the reaction vessel, press filtration after cooling；
（c）Filtrate is applied mechanically；Filter cake reclaims the organic solvent after being beaten with water using steam distillation, then pressure-filteration drying is
Can.
2. the environment-friendly preparation method of 2,6- dichloros paranitroanilinum according to claim 1, it is characterised in that：It is described organic
Solvent is one or more mixture of composition in Benzene Chloride, o-dichlorohenzene and DMF.
3. the environment-friendly preparation method of 2,6- dichloros paranitroanilinum according to claim 1 and 2, it is characterised in that：It is described
The ratio of organic solvent and the nitroaniline is 10 ~ 15L：1kg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610998905.1A CN106748808A (en) | 2016-11-14 | 2016-11-14 | A kind of environment-friendly preparation method of 2,6 dichloro paranitroanilinum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610998905.1A CN106748808A (en) | 2016-11-14 | 2016-11-14 | A kind of environment-friendly preparation method of 2,6 dichloro paranitroanilinum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106748808A true CN106748808A (en) | 2017-05-31 |
Family
ID=58973598
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610998905.1A Pending CN106748808A (en) | 2016-11-14 | 2016-11-14 | A kind of environment-friendly preparation method of 2,6 dichloro paranitroanilinum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106748808A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108285189A (en) * | 2018-04-11 | 2018-07-17 | 银川百泓新材料科技有限公司 | A kind of method of extraction by steam distillation o-dichlorohenzene |
| CN108586264A (en) * | 2018-04-08 | 2018-09-28 | 苏州市罗森助剂有限公司 | The production technology of 2,6- dichloro paranitroanilinum |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4935561A (en) * | 1984-06-02 | 1990-06-19 | Hoechst Aktiengesellschaft | Process for isomerizing monochlorotoluenes or dichlorotoluenes |
| US5068443A (en) * | 1990-06-01 | 1991-11-26 | Noram Chemical Company | Process for the manufacture of 2,6-dichloro-4-nitroaniline |
| US5145958A (en) * | 1989-10-04 | 1992-09-08 | Bayer Aktiengesellschaft | Process for the preparation of 2,4- or 2,6-dihalogeno-aniline |
| CN101143829A (en) * | 2007-10-16 | 2008-03-19 | 南通市东昌化工有限公司 | Method for producing 2,6-dichloro-4-trifluoromethylaniline |
-
2016
- 2016-11-14 CN CN201610998905.1A patent/CN106748808A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4935561A (en) * | 1984-06-02 | 1990-06-19 | Hoechst Aktiengesellschaft | Process for isomerizing monochlorotoluenes or dichlorotoluenes |
| US5145958A (en) * | 1989-10-04 | 1992-09-08 | Bayer Aktiengesellschaft | Process for the preparation of 2,4- or 2,6-dihalogeno-aniline |
| US5068443A (en) * | 1990-06-01 | 1991-11-26 | Noram Chemical Company | Process for the manufacture of 2,6-dichloro-4-nitroaniline |
| CN101143829A (en) * | 2007-10-16 | 2008-03-19 | 南通市东昌化工有限公司 | Method for producing 2,6-dichloro-4-trifluoromethylaniline |
Non-Patent Citations (1)
| Title |
|---|
| 李薇雅，金阳: "2 ,6- 二氯- 4- 硝基苯胺的合成工艺研究", 《印染助剂》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108586264A (en) * | 2018-04-08 | 2018-09-28 | 苏州市罗森助剂有限公司 | The production technology of 2,6- dichloro paranitroanilinum |
| CN108586264B (en) * | 2018-04-08 | 2020-12-15 | 苏州市罗森助剂有限公司 | Production process of 2, 6-dichloro-p-nitroaniline |
| CN108285189A (en) * | 2018-04-11 | 2018-07-17 | 银川百泓新材料科技有限公司 | A kind of method of extraction by steam distillation o-dichlorohenzene |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104910020A (en) | Method for recovering dimethylamine from sucralose production wastewater | |
| CN104230724A (en) | Preparation method of diethylene monoisopropanolamine | |
| CN106748808A (en) | A kind of environment-friendly preparation method of 2,6 dichloro paranitroanilinum | |
| CN107674005A (en) | A kind of preparation method of high-concentration naphthalene sulfonic acid formaldehyde condensation products | |
| CN101734667B (en) | Process for producing precipitated white carbon black by silicon tetrachloride | |
| CN108996807A (en) | A method of with nitrogen phosphorus in modified steel scoria-zeolite absorption degradation sanitary sewage | |
| CN105669384B (en) | The method that one kind catalyzes and synthesizes high 44 ' content of isomer Bisphenol F | |
| CN105170046B (en) | A kind of DMP Neutralisation treatment methods | |
| CN107056124B (en) | A kind of preparation method of cement grinding aid | |
| CN106810412A (en) | A kind of production method of the method and Dispersant MF for improving sulfonating reaction efficiency | |
| CN103086384B (en) | Method for preparing white carbon black from red mud | |
| CN105330545A (en) | Method for recycling oxalic acid from triazine ring cyclization mother liquor dreg with tin chloride as catalyst | |
| CN109437812B (en) | Heat-insulating coating and preparation method thereof | |
| CN105220552B (en) | Using the method for the asymmetric Gemini ionic liquid extracts cellulose of imidazoles | |
| CN106083549B (en) | A method of preparing diisobutyl ketone | |
| CN106745074A (en) | A kind of method for preparing sodium fluoride | |
| CN113264864A (en) | Preparation method of N, N' -m-phenylene bismaleimide | |
| CN101492234B (en) | Production process for urban sewage water, sewage sludge dehydrating agent and method of use thereof | |
| CN106939086B (en) | A kind of purification process of aged resin | |
| CN104557728A (en) | Method for preparing carbendazol from o-phenylenediamine rectification residues | |
| CN108912802A (en) | Bentonite activity thickens anti-settling rheological agent and preparation method thereof | |
| CN107880628A (en) | A kind of anodic electrophoresis paint and its manufacture method containing efficient drier | |
| CN102942479A (en) | Method for preparing propylene glycol methyl ether acetate through two-step coupling reaction | |
| CN108715581A (en) | A kind of preparation method of 2- nitryl-4-thiamphenicol benzoic acids | |
| CN104250036A (en) | Phosphorus removal compound flocculating agent prepared from red mud and preparation method and use method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170531 |