CN102001658B - Novel method for purifying gaseous phosgene - Google Patents
Novel method for purifying gaseous phosgene Download PDFInfo
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- CN102001658B CN102001658B CN2010105453423A CN201010545342A CN102001658B CN 102001658 B CN102001658 B CN 102001658B CN 2010105453423 A CN2010105453423 A CN 2010105453423A CN 201010545342 A CN201010545342 A CN 201010545342A CN 102001658 B CN102001658 B CN 102001658B
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Abstract
The invention relates to a method for purifying gaseous phosgene, comprising the following steps of: (1) adding trichloromethane lower than a phosgene overflow port of a luminescence kettle in the luminescence kettle; (2) introducing gaseous phosgene into the luminescence kettle; (3) continuously liquefying at low temperature until liquid state phosgene overflows, wherein the uncondensed noncondensable gas circularly returns to a last work procedure to be mixed with coal gas and then synchronized into the gaseous phosgene with carbon monoxide; and (4) opening a phosgene gasification kettle jacket for heating oil, opening an overflow valve of the luminescence kettle after the liquid state phosgene in the luminescence kettle reaches the overflow port and obtaining the required phosgene by gasifying the liquid state phosgene which automatically flows into the phosgene gasification kettle under the condition of gravity. According to the invention, by using the technical scheme of continuously liquefying the phosgene under the condition of low temperature and then continuously gasifying at a certain temperature, the noncondensable gas can be removed and residual gas can be recycled. The weight percentage of the purified gaseous phosgene is improved to over 99.0 percent from 90-92 percent; and in addition, the carbon monoxide in the gaseous phosgene can be fully recycled.
Description
Technical field
The present invention relates to the gaseous phosgene purification techniques, refer in particular to a kind of the solution, the method that the gaseous phosgene that makes the utilization ratio of carbon monoxide obtain abundant raising is simultaneously purified because of the continuous product quality problem of phosgene impurity effect matter.
Background technology
Phosgene is carbamate chemicals for agriculture and one of multiple fine chemical product and medicine intermediate synthesis material, and the future that has a wide range of applications, particularly gaseous phosgene are solid-state relatively, and it is low to have use cost, the characteristics that reaction impurities is few.Chlorine and carbon monoxide synthetic route are mainly walked by each manufacturer at present; Its phosgene volume content is all between 70～75%; Mass content is between 90～92%, and wherein noncondensable gas is more, to after state the production of product and be processed with certain influence; And noncondensable gas all is to absorb through tail gas to handle, and wasted resource.Patent of invention 00806122 has been reported the route with the synthetic phosgene of chlorine and carbon monoxide, but does not see that the report of purifying after pair phosgene liquefaction and tail gas being recycled is arranged.
Summary of the invention
The objective of the invention is to improve and innovate, a kind of method of easy and simple to handle, gaseous phosgene purification that energy consumption is low and economic and practical is provided to shortcoming that exists in the background technology and problem.
The present invention includes following steps:
1) at first in the cold light still, adds the trichloromethane that is lower than cold light still phosgene riser, and cold light still temperature is controlled at 0～-5 ℃;
2) in the cold light still, feed gaseous phosgene, Tong Guangkou is located at below the trichloromethane liquid level, can adopt logical light distributor, and heat interchanging area is 20M
2
3) through continuous low temperature liquefaction, overflow until liquid light, operation and coal gas were mixed before the noncondensable gas that wherein is not condensed was circulated back to, again with carbon monoxide synthetic gas attitude phosgene;
4) open phosgene gasification still chuck deep fat at last; The control hot oil temperature is between 60～80 ℃; Treat that liquid phosgene is opened cold light still surplus valve after reaching riser in the cold light still, liquid light gasifies from flowing to phosgene gasification still under gravity condition, obtains required phosgene; Promptly purifying finishes, and supplies subsequent processing to use.
The gaseous phosgene volume percent content that the present invention fed is 70～75%, and mass percentage content is 90～92%, and all the other are carbon monoxide, carbonic acid gas, water etc.
Cold light still of the present invention is volume 1～1.5M
3The chuck enamel still, the condensing surface on the cold light still is set to graphite condenser.
Phosgene gasification still of the present invention is the enamel still of jacketed, and volume is 3 M
3
Cold light still of the present invention and phosgene gasification still vertical parallax are more than 8M.
The phosgene quality percentage composition that the inventive method is purified is more than 99.0%, and the carbon monoxide recovery utilization rate is more than 90%.
Advantage of the present invention and beneficial effect:
The present invention utilizes liquefaction continuously under the phosgene coldcondition, gasifies continuously in certain temperature then, removes non-condensable gases, and residual air is recycled.The quality percentage composition of the gaseous phosgene after purifying through the inventive method is brought up to more than 99.0% from 90～92%, and the carbon monoxide in the gaseous phosgene is recycled fully.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1:
In the cold light still, add the 300L trichloromethane; Control cold light still temperature is at-3 ℃, and feeding volume content is 72%, and mass content is 91.3% phosgene; Through continuous low temperature liquefaction; And keep hot oil temperature in the time of 68 ℃, to gasify, and the back gaseous phosgene mass content that obtains gasifying is 99.3%, the carbon monoxide recovery utilization rate reaches 92.5%.
Embodiment 2:
In the cold light still, add the 300L trichloromethane; Control cold light still temperature is at-4 ℃, and feeding volume content is 71%, and mass content is 91.0% phosgene; Through continuous low temperature liquefaction; And keep hot oil temperature in the time of 72 ℃, to gasify, and the back gaseous phosgene mass content that obtains gasifying is 99.5%, the carbon monoxide recovery utilization rate reaches 94.6%.
Embodiment 3:
In the cold light still, add the 300L trichloromethane; Control cold light still temperature is at-5 ℃, and feeding volume content is 75%, and mass content is 92.0% phosgene; Through continuous low temperature liquefaction; And keep hot oil temperature in the time of 78 ℃, to gasify, and the back gaseous phosgene mass content that obtains gasifying is 99.7%, the carbon monoxide recovery utilization rate reaches 96.5%.
Embodiment of the present invention only is the description that preferred implementation of the present invention is carried out; Be not that design of the present invention and scope are limited; Under the prerequisite that does not break away from design philosophy of the present invention, engineering technical personnel make technical scheme of the present invention in this area various modification and improvement all should fall into protection scope of the present invention; The technology contents that the present invention asks for protection all is documented in claims.
Claims (6)
1. the gaseous phosgene method of purifying is characterized in that may further comprise the steps:
1) at first in the cold light still, adds the trichloromethane that is lower than cold light still phosgene riser, and cold light still temperature is controlled at 0～-5 ℃;
2) in the cold light still, feed gaseous phosgene, Tong Guangkou is located at below the trichloromethane liquid level, adopts logical light distributor, and heat interchanging area is 20M
2
3) through continuous low temperature liquefaction, overflow until liquid phosgene, operation and coal gas were mixed before the noncondensable gas that wherein is not condensed was circulated back to, again with carbon monoxide synthetic gas attitude phosgene;
4) open phosgene gasification still chuck deep fat at last; The control hot oil temperature is between 60～80 ℃; Treat that liquid phosgene is opened cold light still surplus valve after reaching riser in the cold light still, liquid phosgene gasifies from flowing to phosgene gasification still under gravity condition, obtains required phosgene; Promptly purifying finishes, and supplies subsequent processing to use.
2. the method that gaseous phosgene according to claim 1 is purified is characterized in that the gaseous phosgene volume percent content that feeds is 70～75%, and mass percentage content is 90～92%, and all the other are carbon monoxide, carbonic acid gas, water etc.
3. the method that gaseous phosgene according to claim 1 is purified is characterized in that described cold light still is volume 1～1.5M
3The chuck enamel still, on the cold light still graphite condenser is set.
4. the method that gaseous phosgene according to claim 1 is purified is characterized in that described phosgene gasification still is the enamel still of jacketed, and volume is 3M
3
5. the method that gaseous phosgene according to claim 1 is purified is characterized in that described cold light still and phosgene gasification still vertical parallax is more than 8M.
6. the method that gaseous phosgene according to claim 1 is purified is characterized in that the phosgene quality percentage composition that this method is purified is more than 99.0%, and the carbon monoxide recovery utilization rate is more than 90%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105453423A CN102001658B (en) | 2010-11-16 | 2010-11-16 | Novel method for purifying gaseous phosgene |
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| CN2010105453423A CN102001658B (en) | 2010-11-16 | 2010-11-16 | Novel method for purifying gaseous phosgene |
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| CN102001658A CN102001658A (en) | 2011-04-06 |
| CN102001658B true CN102001658B (en) | 2012-07-11 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102897747B (en) * | 2012-10-24 | 2015-03-11 | 无锡东恒新能源科技有限公司 | Carbon nanotube purification system |
| EP3024783A1 (en) | 2013-07-26 | 2016-06-01 | SABIC Global Technologies B.V. | Method and apparatus for producing high purity phosgene |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000505035A (en) * | 1996-02-21 | 2000-04-25 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | Method for producing phosgene |
| US20050025693A1 (en) * | 2003-07-30 | 2005-02-03 | General Electric Company | Processes and systems for making phosgene |
| CN101348252A (en) * | 2008-04-25 | 2009-01-21 | 甘肃银光化学工业集团有限公司 | Phosgene recovery method for toluene diisocyanate production process |
| CN101445238A (en) * | 2007-11-29 | 2009-06-03 | 拜尔材料科学股份公司 | Phosgene production process for reducing CO emission |
-
2010
- 2010-11-16 CN CN2010105453423A patent/CN102001658B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000505035A (en) * | 1996-02-21 | 2000-04-25 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | Method for producing phosgene |
| US20050025693A1 (en) * | 2003-07-30 | 2005-02-03 | General Electric Company | Processes and systems for making phosgene |
| CN101445238A (en) * | 2007-11-29 | 2009-06-03 | 拜尔材料科学股份公司 | Phosgene production process for reducing CO emission |
| CN101348252A (en) * | 2008-04-25 | 2009-01-21 | 甘肃银光化学工业集团有限公司 | Phosgene recovery method for toluene diisocyanate production process |
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Denomination of invention: A kind of method for gaseous phosgene purification Effective date of registration: 20220801 Granted publication date: 20120711 Pledgee: Hunan Linxiang rural commercial bank Limited by Share Ltd. Pledgor: HUNAN GOFAR FINE CHEMICAL TECH. CO.,LTD. Registration number: Y2022980011705 |
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