CN103435495A - Purification process for o-phenylenediamine - Google Patents
Purification process for o-phenylenediamine Download PDFInfo
- Publication number
- CN103435495A CN103435495A CN2013101664081A CN201310166408A CN103435495A CN 103435495 A CN103435495 A CN 103435495A CN 2013101664081 A CN2013101664081 A CN 2013101664081A CN 201310166408 A CN201310166408 A CN 201310166408A CN 103435495 A CN103435495 A CN 103435495A
- Authority
- CN
- China
- Prior art keywords
- phenylene diamine
- product
- phenylenediamine
- crude product
- purifying technique
- 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.)
- Granted
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a purification process for o-phenylenediamine. An o-phenylenediamine crude product is used as a raw material and an ammonolysis and reduction process of o-chloronitrobenzene is employed by the synthesis of o-phenylenediamine. The purification process comprises the steps of transporting a crude product of o-phenylenediamine to a rectification tower kettle to carry out distillation and purification. During the whole rectification process, a vacuum degree is controlled at 6-10 mmHg; and a temperature of the tower kettle is controlled at about 145 +/-3 DEG C. Finally, a proper amount of a protective agent is added in materials of a product; and the materials are flaked under the vacuum or nitrogen protection to obtain a white o-phenylenediamine finished product. The purification process is advantageous in that process is simple; operation is stable and reliable; energy consumption is low; product quality is stable; and product yield is increased.
Description
Technical field
The present invention relates to the purifying technique of O-Phenylene Diamine, belong to the fine chemistry industry preparation field.
Background technology
O-Phenylene Diamine is important organic chemicals, be commonly used for the intermediate of dyestuff, agricultural chemicals, auxiliary agent, sensitive materials etc., for the manufacture of polymeric amide, urethane, derosal and thiophanate, vat scarlet GG, levelling agent, antioxidant MB, also for the preparation of photographic developer, tensio-active agent etc.Along with the development of technique, international and domestic market increases year by year to the demand of exquisite o-phenylenediamine at present.
Take in the benzotriazole making processes that O-Phenylene Diamine is raw material, usually adopt conventional O-Phenylene Diamine crude product to make, need carry out the more processing steps such as pickling, washing, rectifying, decolouring recrystallization to the benzotriazole generated and just meet requirement, not so there will be more impurity to cause content and look number to be difficult to meet high-quality requirement, yet more and more higher to the benzotriazole quality requirements on market, therefore need to purify technique is optimized O-Phenylene Diamine, prepare high-quality benzotriazole.
Summary of the invention
The object of the invention is to, for overcoming the deficiency of O-Phenylene Diamine purifying technique in prior art, provides a kind of process for refining of studying O-Phenylene Diamine.
The present invention adopts following technical scheme to realize:
A kind of purifying technique of O-Phenylene Diamine, it is characterized in that: take the O-Phenylene Diamine crude product as raw material, adopt o-chloronitrobenzene ammonia solution reducing process, technical process is as follows: take the O-Phenylene Diamine crude product as raw material, adopt o-chloronitrobenzene ammonia solution reducing process, technical process is as follows: the crude product O-Phenylene Diamine that will be dissolved in advance in storage tank V1 is delivered in rectifying tower reactor V2 by pump P1, by recycle pump, the P2 condiments being circulated in to thin-film evaporator E1 is heated, produce gas, rise in tower and exchange separation, gas phase is cooling through condenser E2 at tower top, form liquid phase, return in tower and carry out the gas-liquid exchange with the gas phase risen, by reflux ratio controller R1, material is gathered to different cuts, remove front-end volatiles and tar, obtain white O-Phenylene Diamine liquid, finally in the product material, add appropriate protective material, in vacuum or nitrogen protection situation, material is tied to sheet, obtain white O-Phenylene Diamine finished product.
Described crude product O-Phenylene Diamine temperature is controlled 120 ± 2 ℃ and is delivered to the rectifying tower reactor.
Preferably the tower reactor temperature is at 142-148 ℃.
Whole rectifying is tied sheet to material under vacuum, and vacuum tightness is 6-10mmHg.
Described protectant add-on is 0.5%.
Beneficial effect of the present invention: technique is simple, and stable operation is reliable, Energy Intensity Reduction, and constant product quality, product yield improves.
The accompanying drawing explanation
Fig. 1 is the technical process of O-Phenylene Diamine purification system.
In figure, E1 is that reboiler, E2 are that condenser, V1 are that material storaging tank, V2 are that still liquid basin, V7 are that the residual basin of still, V3 are that front-end volatiles tank, V4 are that products pot, V5 are that after cut tank, V6 are that vacuum tank, P1 are that to pass on pump, P2 be still liquid recycle pump, P3 vacuum pump group, R1 reflux ratio control device to raw material.
embodiment:
Below in conjunction with specific embodiment, the present invention is elaborated.
Embodiment 1
Raw material: O-Phenylene Diamine crude product, O-Phenylene Diamine content 90%, the crystallization of outward appearance brown; Protective material, more than 80%, is industrial goods.
Pilot plant:
1) rectifying device: 3600L still kettle, material 304 stainless steels; Φ 600 * 195000mm rectifying tower, packed height 9000mm, material 304 stainless steels;
2) crystallizer: vacuum or nitrogen protection flaker.
The purifying technique of O-Phenylene Diamine is as follows:
During the crude product O-Phenylene Diamine that is dissolved in advance 4 tons of content 90% in storage tank V1 is delivered to the rectifying tower reactor at 120 ± 2 ℃ by pump P1, by recycle pump P2, condiments being circulated in to thin-film evaporator E1 is heated, produce gas, rise in tower and exchange separation by filler, gas phase is cooling through condenser E2 at tower top, form liquid phase, return in tower and carry out the gas-liquid exchange with the gas phase risen, by reflux ratio controller R1, material is gathered to different cuts, remove front-end volatiles and tar, obtain white O-Phenylene Diamine liquid.It is 10mmHg that whole rectifying is controlled vacuum tightness, and the tower reactor temperature, 145 ℃ of left and right, is finally added the 2g protective material in product in material, in the nitrogen protection situation, material is tied to sheet, obtains 3.56 tons of white O-Phenylene Diamine finished products.
By analysis, it is 99.61% that marker method is analyzed content to the O-Phenylene Diamine finished product obtained, and it is 99.8% that normalization method is analyzed content; Outward appearance is white; Do not detect o-Nitraniline and Ortho-Chloro aniline impurity; Product is the small-particle crystallization.
The adjacent rectification yield 90.5% of ash, knot sheet yield 99%, total recovery 85 %.
Embodiment 2
Vacuum tightness in the present embodiment is 6mmHg, and the tower reactor temperature is 130 ℃, and protective material is 1g, and all the other are identical with embodiment 1.
Embodiment 3
Vacuum tightness in the present embodiment is 10mmHg, and the tower reactor temperature is 145 ℃, and protective material is 0.5g, and all the other are identical with embodiment 1.
Embodiment 4
Vacuum tightness in the present embodiment is 15mmHg, and the tower reactor temperature is 162 ℃, and protective material is 0.1g, and all the other are identical with embodiment 1.
The relation that table 1 is rectification yield and temperature, vacuum tightness.
Table 1 rectifying vacuum tightness, temperature, yield information slip
By upper table, seen, along with the increase of vacuum tightness, product content, all more than 99.5%, slightly increase, but product yield is the trend that first rises and reduce afterwards thereupon, and therefore, rectifying vacuum tightness is chosen between 10-6mmHg.
Table 2 is the impact of protection dosage on content and the yield of product.
Table 2 oxidation inhibitor concentration, product yield and content
Upper table shows that the protective material add-on is too much, can cause product purity to reduce, and add-on crosses that I haven't seen you for ages causes product rubescent, does not have provide protection, and it is 0.5% comparatively suitable therefore through experiment, choosing add-on.
The present invention can use without prejudice to the specific form of spirit of the present invention or principal character and summarize; above-mentioned embodiment is only in order to technical scheme of the present invention to be described but not design of the present invention and protection domain are limited; those of ordinary skill of the present invention is modified or is equal to replacement technical scheme of the present invention; and not breaking away from aim and the scope of technical scheme, it all should be encompassed in claim scope of the present invention.
Claims (5)
1. the purifying technique of an O-Phenylene Diamine, it is characterized in that: take the O-Phenylene Diamine crude product as raw material, adopt o-chloronitrobenzene ammonia solution reducing process, technical process is as follows: the crude product O-Phenylene Diamine that will be dissolved in advance in storage tank V1 is delivered in rectifying tower reactor V2 by pump P1, by recycle pump, the P2 condiments being circulated in to thin-film evaporator E1 is heated, produce gas, rise in tower and exchange separation, gas phase is cooling through condenser E2 at tower top, form liquid phase, return in tower and carry out the gas-liquid exchange with the gas phase risen, by reflux ratio controller R1, material is gathered to different cuts, remove front-end volatiles and tar, obtain white O-Phenylene Diamine liquid, finally in the product material, add appropriate protective material, in vacuum or nitrogen protection situation, material is tied to sheet, obtain white O-Phenylene Diamine finished product.
2. the purifying technique of a kind of O-Phenylene Diamine according to claim 1 is characterized in that: crude product O-Phenylene Diamine temperature is controlled 120 ± 2 ℃ and is delivered to the rectifying tower reactor.
3. the purifying technique of a kind of O-Phenylene Diamine according to claim 1, it is characterized in that: the tower reactor temperature is 142-148 ℃.
4. the purifying technique of a kind of O-Phenylene Diamine according to claim 1, it is characterized in that: under vacuum, material is tied to sheet, vacuum tightness is 10-6mmHg.
5. the purifying technique of a kind of O-Phenylene Diamine according to claim 1, it is characterized in that: protectant add-on is 0.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310166408.1A CN103435495B (en) | 2013-05-08 | 2013-05-08 | The purifying technique of O-Phenylene Diamine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310166408.1A CN103435495B (en) | 2013-05-08 | 2013-05-08 | The purifying technique of O-Phenylene Diamine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103435495A true CN103435495A (en) | 2013-12-11 |
| CN103435495B CN103435495B (en) | 2016-03-09 |
Family
ID=49689243
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310166408.1A Active CN103435495B (en) | 2013-05-08 | 2013-05-08 | The purifying technique of O-Phenylene Diamine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103435495B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107286025A (en) * | 2017-07-12 | 2017-10-24 | 安徽广信农化股份有限公司 | A kind of method of carbendazim primary raw material o-phenylenediamine purification |
| CN109879762A (en) * | 2019-03-27 | 2019-06-14 | 宁夏瑞泰科技股份有限公司 | A kind of method of purification of o-phenylenediamine |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2354224A1 (en) * | 1973-10-30 | 1975-10-02 | Hoechst Ag | PROCESS FOR THE PRODUCTION OF AN AMINOBENZENE DERIVATIVE |
| JPH0446259B2 (en) * | 1983-04-26 | 1992-07-29 | Sumitomo Chemical Co | |
| CN1491935A (en) * | 2001-06-15 | 2004-04-28 | 江苏省海安染料化工厂 | Producing metaphenylene diamine by rectifying method |
| CN1594279A (en) * | 2004-06-29 | 2005-03-16 | 浙江大学 | Process and apparatus for producing o-phenylenediamine |
| CN101462966A (en) * | 2008-12-31 | 2009-06-24 | 安徽巨元化工有限公司 | Purification method for exquisite o-phenylenediamine |
| CN102531921A (en) * | 2010-12-24 | 2012-07-04 | 中国石油化工股份有限公司 | Refining and shaping process of p-phenylenediamine |
| CN102633652A (en) * | 2011-02-23 | 2012-08-15 | 江苏康恒化工有限公司 | High-purity o-phenylenediamine preparation method |
-
2013
- 2013-05-08 CN CN201310166408.1A patent/CN103435495B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2354224A1 (en) * | 1973-10-30 | 1975-10-02 | Hoechst Ag | PROCESS FOR THE PRODUCTION OF AN AMINOBENZENE DERIVATIVE |
| JPH0446259B2 (en) * | 1983-04-26 | 1992-07-29 | Sumitomo Chemical Co | |
| CN1491935A (en) * | 2001-06-15 | 2004-04-28 | 江苏省海安染料化工厂 | Producing metaphenylene diamine by rectifying method |
| CN1594279A (en) * | 2004-06-29 | 2005-03-16 | 浙江大学 | Process and apparatus for producing o-phenylenediamine |
| CN101462966A (en) * | 2008-12-31 | 2009-06-24 | 安徽巨元化工有限公司 | Purification method for exquisite o-phenylenediamine |
| CN102531921A (en) * | 2010-12-24 | 2012-07-04 | 中国石油化工股份有限公司 | Refining and shaping process of p-phenylenediamine |
| CN102633652A (en) * | 2011-02-23 | 2012-08-15 | 江苏康恒化工有限公司 | High-purity o-phenylenediamine preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 吕咏梅: "邻苯二胺生产技术进展与市场分析", 《现代农药》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105017027B (en) * | 2015-06-11 | 2017-03-22 | 安徽东至广信农化有限公司 | Material layering process for reduced o-phenylenediamine |
| CN107286025A (en) * | 2017-07-12 | 2017-10-24 | 安徽广信农化股份有限公司 | A kind of method of carbendazim primary raw material o-phenylenediamine purification |
| CN109879762A (en) * | 2019-03-27 | 2019-06-14 | 宁夏瑞泰科技股份有限公司 | A kind of method of purification of o-phenylenediamine |
| CN109879762B (en) * | 2019-03-27 | 2022-02-22 | 宁夏瑞泰科技股份有限公司 | Purification method of o-phenylenediamine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103435495B (en) | 2016-03-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2177501B1 (en) | Method and plant for the production of ethanol amines | |
| CN101006038B (en) | Method for the production of formic acid | |
| CN103435495A (en) | Purification process for o-phenylenediamine | |
| WO2010066674A3 (en) | Method for purifying polymethylols | |
| CA3022388C (en) | Method for preparing azoxystrobin intermediates | |
| CN107344786B (en) | Method for treating ultraviolet absorbent UV-531 production wastewater | |
| CN103242197B (en) | Preparation method of ultraviolet absorbent intermediate etocrilene (ETO) | |
| CN102659563A (en) | Organic extraction phase for extracting lactic acid from heavy phase lactic acid | |
| SA519410230B1 (en) | Process for Purifying (Meth)Acrylic Acid Including A Dividing-Wall Distillation Column | |
| CN104311448A (en) | Preparation method of dinitolmide | |
| CN103635469B (en) | Method for producing tetrahydrofuran | |
| CN104447366A (en) | Preparation method of high-purity 2-amino-3, 5-dibromobenzaldehyde | |
| CN106631813B (en) | A kind of bronopol process for refining | |
| CN103772185B (en) | Device and method for removing moisture and heteroacids in acetic acid | |
| CN105330078B (en) | The catalyst recovery method of B4 workshop sections in pyridiniujm production | |
| US20050080294A1 (en) | Separation of amine from a phenolic compound | |
| CN104262210B (en) | A kind of method extracting paratoluenesulfonic acid sodium salt from Tiamulin synthetic wastewater | |
| CN103706136B (en) | For the double rectification column separation method of purification of methyl tertiary butyl ether(MTBE) in statins building-up process waste liquid-tetrahydrofuran recycling | |
| CN109665993B (en) | Preparation method of anti-aging agent AW | |
| CN109704990B (en) | Refining method of high-purity acetonitrile | |
| CN106957284B (en) | A kind of separating-purifying process for refining of tertiary carbonic acid glycidyl ester crude product | |
| CN115417755A (en) | Purification and cyclization process of 3, 4-dihydroxy-2, 5-hexanedione | |
| CN102516119B (en) | Continuous low-energy consumption acetonitrile refining process | |
| CN105968028B (en) | A kind of acetonitrile continuous negative pressure distillation extraction technique | |
| CN115057784A (en) | Method for treating octyl trichlamide wastewater |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20160526 Address after: 226500, 2, Xiangjiang Road, Changjiang town (Rugao port area), Nantong, Jiangsu, Rugao Patentee after: NANTONG BOTAO CHEMICAL CO., LTD. Address before: Jiang town Rugao City, Jiangsu province 226500 Nantong City Village Liaison Patentee before: Rugao Jinling Chemical Co., Ltd. |