CN106316863A - Efficient o-phenylenediamine recovery method - Google Patents
Efficient o-phenylenediamine recovery method Download PDFInfo
- Publication number
- CN106316863A CN106316863A CN201610665496.3A CN201610665496A CN106316863A CN 106316863 A CN106316863 A CN 106316863A CN 201610665496 A CN201610665496 A CN 201610665496A CN 106316863 A CN106316863 A CN 106316863A
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- CN
- China
- Prior art keywords
- phenylenediamine
- salt
- layering
- rectification
- ortho
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/30—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds
- C07C209/32—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups
- C07C209/36—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups by reduction of nitro groups bound to carbon atoms of six-membered aromatic rings in presence of hydrogen-containing gases and a catalyst
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- 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
- C07C209/86—Separation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
Abstract
The invention discloses an efficient o-phenylenediamine recovery method. The efficient o-phenylenediamine recovery method mainly comprises the steps that 1, an ortho-nitroaniline and sodium sulfide solution makes ortho-nitroaniline produce reduction reaction; 2, after system cooling, all the materials in the step 1 are pressed into a layering tank for primary layering; 3, an o-phenylenediamine and salt hydrate at the top of the layering tank is transferred to a heating kettle, the materials in the heating kettle are heated to remove moisture in the materials and make the salt precipitate from the o-phenylenediamine, and then collection is performed; 4, the o-phenylenediamine solution obtained after layering is collected; 5, filtration and rectification are performed, and pure o-phenylenediamine is collected and recovered for standby application. By the adoption of the method, the process including cooling, crystallization, centrifugation and heating during rectification is omitted, energy consumption is reduced, the working time is shortened, the phenomenon that a large amount of salt and water is brought to a rectification process is avoided, rectification residues are decreased, and the follow-up o-phenylenediamine rectification quality and yield are improved.
Description
Technical field
The present invention relates to field of environmental engineering, be specifically related to the efficient recycling method of a kind of o-phenylenediamine.
Background technology
O-phenylenediamine also known as 1,2-diaminobenzene, 1,2-phenylenediamine.From water, precipitation person is that white is to faint yellow foliaceous
Crystallization, from chloroform, precipitation person crystallizes for prism-shaped.Exposed to air is easy to variable color, by leucismus Huang, becomes palm fibre, purpling,
After become black.Relative density 1.2698.Fusing point 103～104 DEG C.Boiling point 256～258 DEG C.It is slightly soluble in cold water, is soluble in heat
Water, ethanol, ether, chloroform and benzene.With mineral acid effect, generate water-soluble salt；Aqueous solution reacts with Carbon bisulfide, generates
2-mercaptobenzimidazole；Add pressure and carbon dioxide reaction, generate benzimidazolone.This product is poisonous, after suction, causes vision to hinder
Hinder, with contact skin, cause inflammation, enter in eye, also cause inflammation.
O-phenylenediamine is a kind of traditional fine-chemical intermediate, is mainly used as pesticide producing, is to prepare carbendazim and first
The raw material of base thiophanate etc., it also has document to report in application pharmaceutically.The synthesis of o-phenylenediamine is mainly with adjacent nitro chlorination
Benzene and ammonia synthesis ortho-nitraniline, then the process route of o-phenylenediamine is become with sodium sulfide reducing.After material reduction through crystallization again
Centrifugal, the big cost of labor intensity is high.Using high temperature lower leaf, material is delivered directly to rectifying still rectification, reduce crystallization, centrifugal,
Melting material operation, has saved recruitment cost, reduces labor intensity.
Summary of the invention
For the deficiencies in the prior art, the invention provides the efficient recycling method of a kind of o-phenylenediamine.
The present invention can be achieved through the following technical solutions:
A kind of efficient recycling method of o-phenylenediamine, its step mainly included is as follows:
(1) adding ortho-nitraniline and ethanol in reactor, stirring makes ortho-nitraniline fully dissolve, adds sulfuration
Sodium solution makes ortho-nitraniline generation reduction reaction, and reaction reduces system temperature to 80-90 DEG C after terminating, described ortho-nitrophenyl
Amine: the weight ratio of sodium sulfide is 1:2；
(2) after system cooling, materials all in step 1 being pressed into layering groove together, layering trench bottom adds coil pipe cooling, liquid
Body is from being layered trench bottom through U-shaped curved inflow collecting tank；
(3) o-phenylenediamine at layering groove top is proceeded to heating kettle with the hydrate of salt, in heating kettle, material is heated up
To 100-120 DEG C, remove moisture therein, collect after making salt separate out from o-phenylenediamine；
(4) after collecting salt, repeating step 2, the operation of 3, the o-phenylenediamine controlling to get rid of is 1:1 with salt ratio, is layered groove
The liquid that top is flowed out is o-phenylenediamine；
(5) by the o-phenylenediamine solution in step 4 with being pumped in filter-pressing cauldron filtration, after removing salt, clear liquid is directly used
Transport pump, to rectifying still rectification, collects pure o-phenylenediamine, reclaims standby.
The invention have the benefit that 1) there is ratio at different temperatures in o-phenylenediamine in o-phenylenediamine reducing solution with saline
The method of double differences, utilizes this difference in specific gravity to carry out physical layering, conservation, also can reach preferable layered effect simultaneously；2) fall is eliminated
Temperature, crystallize, centrifugal, the process heated up again during rectification, save energy consumption, shorten man-hour, it is to avoid substantial amounts of salinity and water band
Enter rectification working process, decrease rectification residue, improve quality and the yield of postorder o-phenylenediamine rectification；3) this layering groove can connect
Continuous layering；4) liquid o-phenylenediamine directly feeds carbendazim rectification, it is to avoid opening temperature thawing, minimizing slags tap, thus be greatly improved
The benefit of enterprise.
Detailed description of the invention:
By embodiment, the detailed description of the invention of the present invention is made an explanation below.
Embodiment
The efficient recycling method of a kind of o-phenylenediamine, its step mainly included is as follows: (1) adds 1 weight in reactor
Amount part ortho-nitraniline and 4 parts by weight of ethanol, stirring makes ortho-nitraniline fully dissolve, adds 2 weight portion sodium sulfide solutions
Ortho-nitraniline generation reduction reaction, reaction is made to reduce system temperature to 80 DEG C after terminating；(2) after system cooling, by step 1
All materials are pressed into layering groove together, and layering trench bottom adds coil pipe cooling, and liquid is collected through U-shaped curved inflow from layering trench bottom
Groove；(3) o-phenylenediamine at layering groove top is proceeded to heating kettle with the hydrate of salt, in heating kettle, material is warming up to 110
DEG C, remove moisture therein, collect after making salt separate out from o-phenylenediamine；(4) after collecting salt, by the mixing of o-phenylenediamine Yu salt
Thing is again transferred to be layered groove, repeats step 2, the operation of 3, until the o-phenylenediamine got rid of and salt ratio are 1:1, is layered groove top
The liquid that portion flows out is o-phenylenediamine；(5) by the o-phenylenediamine solution in step 4 with being pumped in filter-pressing cauldron filtration, remove
After desalting, clear liquid directly with transport pump to rectifying still rectification, collect pure o-phenylenediamine, reclaim standby.
By said method can obtain purity be 97%, yield be the o-phenylenediamine of 99%.
The foregoing is only the section Example of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (1)
1. the efficient recycling method of an o-phenylenediamine, it is characterised in that the step mainly included is as follows:
(1) adding ortho-nitraniline and ethanol in reactor, stirring makes ortho-nitraniline fully dissolve, adds sodium sulfide molten
Liquid makes ortho-nitraniline generation reduction reaction, and reaction reduces system temperature to 80-90 DEG C after terminating, described ortho-nitraniline:
The weight ratio of sodium sulfide is 1:2；
(2) after system cooling, materials all in step 1 being pressed into layering groove together, layering trench bottom adds coil pipe cooling, liquid from
Layering trench bottom is through U-shaped curved inflow collecting tank；
(3) o-phenylenediamine at layering groove top is proceeded to heating kettle with the hydrate of salt, in heating kettle, material is warming up to
100-120 DEG C, remove moisture therein, collect after making salt separate out from o-phenylenediamine；
(4) after collecting salt, repeating step 2, the operation of 3, the o-phenylenediamine controlling to get rid of is 1:1 with salt ratio, is layered groove top
The liquid flowed out is o-phenylenediamine solution；
(5), by the o-phenylenediamine solution in step 4 with being pumped in filter-pressing cauldron filtration, after removing salt, clear liquid is directly defeated with pump
Deliver to rectifying still rectification, collect pure o-phenylenediamine, reclaim standby.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610665496.3A CN106316863A (en) | 2016-08-13 | 2016-08-13 | Efficient o-phenylenediamine recovery method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610665496.3A CN106316863A (en) | 2016-08-13 | 2016-08-13 | Efficient o-phenylenediamine recovery method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106316863A true CN106316863A (en) | 2017-01-11 |
Family
ID=57739298
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610665496.3A Pending CN106316863A (en) | 2016-08-13 | 2016-08-13 | Efficient o-phenylenediamine recovery method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107459049A (en) * | 2017-08-01 | 2017-12-12 | 安徽东至广信农化有限公司 | A kind of phenyl amines organic intermediate ammonolysis Mother liquor Ammonia recovery technique |
| CN108610261A (en) * | 2018-04-27 | 2018-10-02 | 韶关凌化工有限公司 | A kind of synthetic method improving phenylenediamine yields |
| CN108689860A (en) * | 2018-07-18 | 2018-10-23 | 荆门医药工业技术研究院 | A kind of synthetic method preparing 4- butyl benzene -1,2- diamines |
| CN113426150A (en) * | 2021-07-16 | 2021-09-24 | 安徽东至广信农化有限公司 | Rectification device for o-phenylenediamine and use method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2122607A (en) * | 1982-05-12 | 1984-01-18 | Magyar Asvanyolaj Es Foeldgaz | Preparation of o-phenylenediamine |
| WO2005070869A1 (en) * | 2003-12-24 | 2005-08-04 | Council Of Scientific & Industrial Research | Selective hydrogenation of nitrogen containing aromatics |
| CN101200336A (en) * | 2007-12-18 | 2008-06-18 | 赵志军 | Process for zero-discharge treatment of o-phenylenediamine sodium sulfide reduction wastewater |
| CN105017028A (en) * | 2015-07-27 | 2015-11-04 | 江阴市华亚化工有限公司 | Improved synthetic method for preparing o-phenylenediamine by reducing o-nitroaniline |
| CN105017027A (en) * | 2015-06-11 | 2015-11-04 | 安徽东至广信农化有限公司 | Material layering process for reduced o-phenylenediamine |
-
2016
- 2016-08-13 CN CN201610665496.3A patent/CN106316863A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2122607A (en) * | 1982-05-12 | 1984-01-18 | Magyar Asvanyolaj Es Foeldgaz | Preparation of o-phenylenediamine |
| WO2005070869A1 (en) * | 2003-12-24 | 2005-08-04 | Council Of Scientific & Industrial Research | Selective hydrogenation of nitrogen containing aromatics |
| CN101200336A (en) * | 2007-12-18 | 2008-06-18 | 赵志军 | Process for zero-discharge treatment of o-phenylenediamine sodium sulfide reduction wastewater |
| CN105017027A (en) * | 2015-06-11 | 2015-11-04 | 安徽东至广信农化有限公司 | Material layering process for reduced o-phenylenediamine |
| CN105017028A (en) * | 2015-07-27 | 2015-11-04 | 江阴市华亚化工有限公司 | Improved synthetic method for preparing o-phenylenediamine by reducing o-nitroaniline |
Non-Patent Citations (4)
| Title |
|---|
| 上海染化十五厂: "溶剂萃取法处理邻苯二胺废水", 《辽宁化工》 * |
| 张国安 等: "邻苯二胺合成路线浅述", 《农药》 * |
| 杨乔森: "Pd/C催化剂催化邻硝基苯胺加氢制备邻苯二胺", 《工业催化》 * |
| 肖传发: "邻硝基苯胺催化加氢合成邻苯二胺", 《广东化工》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107459049A (en) * | 2017-08-01 | 2017-12-12 | 安徽东至广信农化有限公司 | A kind of phenyl amines organic intermediate ammonolysis Mother liquor Ammonia recovery technique |
| CN108610261A (en) * | 2018-04-27 | 2018-10-02 | 韶关凌化工有限公司 | A kind of synthetic method improving phenylenediamine yields |
| CN108610261B (en) * | 2018-04-27 | 2021-05-14 | 韶关凌一化工有限公司 | Synthetic method for improving yield of phenylenediamine |
| CN108689860A (en) * | 2018-07-18 | 2018-10-23 | 荆门医药工业技术研究院 | A kind of synthetic method preparing 4- butyl benzene -1,2- diamines |
| CN113426150A (en) * | 2021-07-16 | 2021-09-24 | 安徽东至广信农化有限公司 | Rectification device for o-phenylenediamine and use method thereof |
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Application publication date: 20170111 |
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