CN101462966A - Purification method for exquisite o-phenylenediamine - Google Patents
Purification method for exquisite o-phenylenediamine Download PDFInfo
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- CN101462966A CN101462966A CN 200810249693 CN200810249693A CN101462966A CN 101462966 A CN101462966 A CN 101462966A CN 200810249693 CN200810249693 CN 200810249693 CN 200810249693 A CN200810249693 A CN 200810249693A CN 101462966 A CN101462966 A CN 101462966A
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Abstract
The invention discloses a purification method for refinery o-phenylenediamine. The aim of separation and purification of o-phenylenediamine is realized by gas-liquid mass transfer of rising materials in efficient filling materials; the o-phenylenediamine condensate liquid after separation and purification enters a flaker material disk groove to flake under the protection of nitrogen, so as to obtain flake-shaped products of refinery o-phenylenediamine; compared with traditional process route, the positive effects of the method lie in that: the stability and reliability of the operation is improved, material consumption and energy consumption are reduced, wherein, the unit consumption of crude product is reduced by 8% and the energy consumption is reduced by 30%, the reliability of product quality is improved, the first pass percent is increased to 100% from 92% of the traditional process, and the product content is increased to over 99.5% from 99%.
Description
Technical field:
The present invention relates to a kind of O-Phenylene Diamine and be the processing method of elaboration from the crude product purification.
Background technology:
O-Phenylene Diamine is important fine-chemical intermediate, main application is for producing the raw material of higher effective and lower toxic pesticide " derosal ", " thiophanate ", such agricultural chemicals is a broad spectrum internal-suction type sterilant, can be used for preventing and treating wheat scab, rice sheath blight disease, the sweet potato black spot, the Powdery Mildew of canker of apple fruit and many crops, gray mold, anthrax and sclerotium disease etc.O-Phenylene Diamine also is a dyestuff intermediate, is used for the production of vat dyes and cationic dyestuff, and can make fur dyes and preparation photographic developer, tensio-active agent etc.O-Phenylene Diamine can be used to produce antioxidant MB; Medicine dibazol and rust-preventive agent benzotriazole.
The technology of domestic production exquisite o-phenylenediamine is mainly taked at present: crude product (about 92%) O-Phenylene Diamine is dropped in the distillation tower, ebuillition of heated is through long distillation extraction then, qualified feed liquid is injected (water of the inside and the mixing liquid of antioxidant) crystallization in the water tank crystallizer, then clean facilities is put into the moisture eliminator inner drying and drawn product later on.Traditional production technique adopts the heating of bubble still formula tower still, its tube wall is overheated because of fouling, therefore the easy coking of heated material, and traditional thermal oil circulating condensing system process is longer, equipment is numerous and diverse, and floor space is big, and stable operation is poor, management is difficulty comparatively, so the exquisite o-phenylenediamine quality product of producing with this method is difficult to stablize.
At the problem that exists in the above-mentioned operational path, the object of the present invention is to provide the method for purification of the exquisite o-phenylenediamine that a kind of energy consumption is low, constant product quality is high
The objective of the invention is to be achieved through the following technical solutions, a kind of method of purification of exquisite o-phenylenediamine, mainly may further comprise the steps: a, behind the crude product O-Phenylene Diamine solid materials input material still, closure material still, under the micro-vacuum state, with low-pressure steam indirect heating material, 110 ℃-120 ℃ of control feed temperatures, after feed liquid is all melted, suction rectifying tower still; B, material in the rectifying tower still is slowly heated with thermal oil, keep tower still temperature at 180 ℃-195 ℃, tower still pressure-controlling is at 3.9-5.3Kpa, tower top temperature is at 140 ℃-160 ℃, under this operating mode, the rising material carries out the gas-liquid mass transfer exchange in high efficiency packing, reach the purpose of separating the purification O-Phenylene Diamine; C, the O-Phenylene Diamine phlegma that separates after purifying enter flaker charging tray groove, at nitrogen pressure 20-100mmH
2The O protection is the knot sheet down, obtains exquisite o-phenylenediamine knot flaked product.
Before the charging of rectifying tower still, start the overhead condenser hot water pump, overhead condenser is played circulation, 70 ℃-90 ℃ of maintenance heat exit of pump water temperatures.
Rectifying overhead distillate in early stage is impure more, carries out smart crystallization after collecting, and returning of the exquisite o-phenylenediamine material still that obtains after the centrifuge dehydration is applied mechanically.
The O-Phenylene Diamine phlegma that separates after purifying enters flaker charging tray groove, ties sheet under nitrogen protection, obtains exquisite o-phenylenediamine knot flaked product, and its knot sheet thickness can be adjusted arbitrarily between 0.2mm-1.5mm according to customer requirement.
The present invention compares with traditional operational path, and the positively effect that it possessed is presented as:
1, improved the stability of operation, reliability.
2, reduced material consumption and energy consumption, compared with traditional technology, the crude product unit consumption has reduced by 8%, and energy consumption has reduced by 30%.
3, the stability of quality product improves, and first-time qualification rate brings up to 100% by 92% of traditional technology.Product content is brought up to present more than 99.5% by original 99%.
Description of drawings:
Accompanying drawing is a process flow diagram of the present invention
Embodiment:
Shown in accompanying drawing, provide following three groups of embodiment, so that understand and illustrate the effect of content of the present invention and actual use better.
Embodiment one:
After 5 tons of inputization material of crude product O-Phenylene Diamine still sealing with content 92%, under the micro-vacuum state, with low-pressure steam indirect heating material, 110 ℃ of control feed temperatures, melted three hours, treat that feed liquid all melts, utilize potential difference will melt good crude product liquid fully then and put into rectifying still, when rectifying tower still feed liquid liquid level reaches 85%, stop charging, slowly heat with thermal oil then, keep tower still temperature about 180 ℃, pressure-controlling is at 3.9Kpa, and tower top temperature is opened vacuum pump being pumped into negative pressure 80Kpa in the tower still after 20 minutes about 140 ℃, open cooling-water pump and cool off, water temperature is controlled at 75 ℃.System enters the total reflux state like this, waits next pot from the cat head extraction part foreshot material pot of evolving in about two hours, uses the O-Phenylene Diamine phlegma that so obtained in about 6-8 hours separating after the purification again, qualified liquiform product is injected flaker, at nitrogen pressure 20mmH
29 hours knot sheets are carried out in the O protection down again, and common property goes out 4.26 tons of products.
Embodiment two:
After the sealing of 5.5 tons of inputization material of content 92% crude product O-Phenylene Diamine still, under the micro-vacuum state, with low-pressure steam indirect heating material, 120 ℃ of control feed temperatures, melted three hours, treat that feed liquid all melts, utilize potential difference will melt good crude product liquid fully then and put between the rectifying still, when rectifying tower still feed liquid liquid level reaches 85%, stop charging, use heat-conducting oil heating then, keep tower still temperature about 190 ℃, pressure-controlling is at 4.5Kpa, and tower top temperature is opened vacuum pump being pumped into negative pressure 90Kpa in the tower still after 20 minutes about 150 ℃, open cooling-water pump and cool off, water temperature is controlled at 85 ℃.System enters the total reflux state like this, waits next pot from the cat head extraction part foreshot material pot of evolving in about two hours, uses the O-Phenylene Diamine phlegma that so obtained in about 6-8 hours separating after the purification again, qualified liquiform product is injected flaker, at nitrogen pressure 60mmH
210 hours knot sheets are carried out in the O protection down again, and common property goes out 4.75 tons of products.
Embodiment three:
After the sealing of 5 tons of inputization material of content 92% crude product O-Phenylene Diamine still, under the micro-vacuum state, with low-pressure steam indirect heating material, 120 ℃ of control feed temperatures, melted three hours, treat that feed liquid all melts, utilize potential difference will melt good crude product liquid fully then and put into rectifying still, when rectifying tower still feed liquid liquid level reaches 85%, stop charging, slowly heat with thermal oil then, keep tower still temperature about 195 ℃, pressure-controlling is at 5.3Kpa, and tower top temperature is opened vacuum pump being pumped into negative pressure 100Kpa in the tower still after 20 minutes about 160 ℃, open cooling-water pump and cool off, water temperature is controlled at 90 ℃.System enters the total reflux state like this, waited next pot from the cat head extraction part foreshot material pot of evolving in about two hours, use the O-Phenylene Diamine phlegma that so obtained in about 6-8 hours separating after the purification again, qualified liquiform product is injected flaker, at nitrogen pressure 100mmH
29 hours knot sheets are carried out in the O protection down again, and common property goes out 4.72 tons of products.
Claims (4)
1, the method for purification of exquisite o-phenylenediamine, it is characterized in that: mainly comprise following processing condition and step, a, with behind the crude product O-Phenylene Diamine solid materials input material still, closure material still, under the micro-vacuum state, with low-pressure steam indirect heating material, 110 ℃-120 ℃ of control feed temperatures, after feed liquid is all melted, suction rectifying tower still; B, material in the rectifying tower still is slowly heated with thermal oil, keep tower still temperature at 180 ℃-195 ℃, tower still pressure-controlling is at 3.9-5.3Kpa, tower top temperature is at 140 ℃-160 ℃, under this operating mode, the rising material carries out the gas-liquid mass transfer exchange in high efficiency packing, reach the purpose of separating the purification O-Phenylene Diamine; C, the O-Phenylene Diamine phlegma that separates after purifying enter flaker charging tray groove, at nitrogen pressure 20-100mmH
2The O protection is the knot sheet down, obtains exquisite o-phenylenediamine knot flaked product.
2, the method for purification of exquisite o-phenylenediamine according to claim 1 is characterized in that: before the charging of rectifying tower still, start the overhead condenser hot water pump, overhead condenser is played circulation, 70 ℃-90 ℃ of maintenance heat exit of pump water temperatures.
3, the method for purification of exquisite o-phenylenediamine according to claim 1 is characterized in that: rectifying overhead distillate in early stage is impure more, carries out smart crystallization after collecting, and returning of the exquisite o-phenylenediamine material still that obtains after the centrifuge dehydration is applied mechanically.
4, the method for purification of exquisite o-phenylenediamine according to claim 1 is characterized in that: its knot sheet thickness can be adjusted arbitrarily between 0.2mm-1.5mm as requested.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 200810249693 CN101462966B (en) | 2008-12-31 | 2008-12-31 | Purification method for exquisite o-phenylenediamine |
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| CN 200810249693 CN101462966B (en) | 2008-12-31 | 2008-12-31 | Purification method for exquisite o-phenylenediamine |
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| CN101462966A true CN101462966A (en) | 2009-06-24 |
| CN101462966B CN101462966B (en) | 2013-03-20 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2448084C1 (en) * | 2010-12-22 | 2012-04-20 | Открытое акционерное общество "Каустик" (ОАО "Каустик") | Method of purifying technical 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 |
| CN102757351A (en) * | 2012-07-18 | 2012-10-31 | 如皋市金陵化工有限公司 | Method for continuously purifying and refining ortho toludiamine |
| CN103435495A (en) * | 2013-05-08 | 2013-12-11 | 如皋市金陵化工有限公司 | Purification process for o-phenylenediamine |
| CN104557728A (en) * | 2014-12-22 | 2015-04-29 | 江苏扬农化工集团有限公司 | Method for preparing carbendazol from o-phenylenediamine rectification residues |
| CN106810504A (en) * | 2016-11-30 | 2017-06-09 | 南通波涛化工有限公司 | A kind of preparation method of 4 methyl benzotriazazole |
| 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 |
| CN107286024A (en) * | 2017-06-06 | 2017-10-24 | 青岛科技大学 | A kind of edulcoration purification process of m-phenylene diamine (MPD) |
| CN107286023A (en) * | 2017-06-06 | 2017-10-24 | 青岛科技大学 | A kind of purification process of m-phenylene diamine (MPD) |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1274665C (en) * | 2004-06-29 | 2006-09-13 | 浙江大学 | Process and apparatus for producing o-phenylenediamine |
-
2008
- 2008-12-31 CN CN 200810249693 patent/CN101462966B/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2448084C1 (en) * | 2010-12-22 | 2012-04-20 | Открытое акционерное общество "Каустик" (ОАО "Каустик") | Method of purifying technical 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 |
| CN102757351B (en) * | 2012-07-18 | 2014-04-16 | 如皋市金陵化工有限公司 | Method for continuously purifying and refining ortho-toluene diamine |
| CN102757351A (en) * | 2012-07-18 | 2012-10-31 | 如皋市金陵化工有限公司 | Method for continuously purifying and refining ortho toludiamine |
| CN103435495B (en) * | 2013-05-08 | 2016-03-09 | 如皋市金陵化工有限公司 | The purifying technique of O-Phenylene Diamine |
| CN103435495A (en) * | 2013-05-08 | 2013-12-11 | 如皋市金陵化工有限公司 | Purification process for o-phenylenediamine |
| CN104557728A (en) * | 2014-12-22 | 2015-04-29 | 江苏扬农化工集团有限公司 | Method for preparing carbendazol from o-phenylenediamine rectification residues |
| CN104557728B (en) * | 2014-12-22 | 2017-05-03 | 江苏扬农化工集团有限公司 | Method for preparing carbendazol from o-phenylenediamine rectification residues |
| CN106810504A (en) * | 2016-11-30 | 2017-06-09 | 南通波涛化工有限公司 | A kind of preparation method of 4 methyl benzotriazazole |
| CN107286024A (en) * | 2017-06-06 | 2017-10-24 | 青岛科技大学 | A kind of edulcoration purification process of m-phenylene diamine (MPD) |
| CN107286023A (en) * | 2017-06-06 | 2017-10-24 | 青岛科技大学 | A kind of purification process of m-phenylene diamine (MPD) |
| CN107286023B (en) * | 2017-06-06 | 2018-07-20 | 青岛科技大学 | A kind of purification process of m-phenylene diamine (MPD) |
| 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 |
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| CN101462966B (en) | 2013-03-20 |
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Denomination of invention: Purification method for exquisite o-phenylenediamine Effective date of registration: 20130608 Granted publication date: 20130320 Pledgee: Bengbu high tech SME financing Company Limited by Guarantee Pledgor: Anhui Juyuan Chemical Co., Ltd. Registration number: 2013990000361 |
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Granted publication date: 20130320 Termination date: 20161231 |