CN100540517C - The method of separating trifluoroethylene during tetrafluoroethylene is produced - Google Patents
The method of separating trifluoroethylene during tetrafluoroethylene is produced Download PDFInfo
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- CN100540517C CN100540517C CN 200710115900 CN200710115900A CN100540517C CN 100540517 C CN100540517 C CN 100540517C CN 200710115900 CN200710115900 CN 200710115900 CN 200710115900 A CN200710115900 A CN 200710115900A CN 100540517 C CN100540517 C CN 100540517C
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Abstract
The invention belongs to the fluorine chemical field, the method of separating trifluoroethylene in a kind of tetrafluoroethylene production is provided, its concrete processing step is as follows: the material gas that tetrafluoroethylene reclaims cat head directly enters rectifying tower, tetrafluoroethylene in the material gas, trifluoro-ethylene and other component are separated, tetrafluoroethylene, trifluoro-ethylene in the material gas are assembled at cat head, and all the other components are returned system behind the tetrafluoroethylene recovery tower by the tower still; Tetrafluoroethylene, trifluoro-ethylene mixture enter extraction tower, utilize extraction agent that trifluoro-ethylene is absorbed, trifluoro-ethylene enters Analytic Tower with extraction agent, in Analytic Tower, trifluoro-ethylene is separated from extraction liquid by steam heating, trifluoro-ethylene is assembled at the Analytic Tower cat head, enters the trifluoro-ethylene storage tank then.The present invention has realized the high efficiency separation to trifluoro-ethylene, has realized the controllability of Paratetrafluoroethylene quality, has shown great potential aspect environment protection.
Description
Technical field
The invention belongs to the fluorine chemical field, relate to the method and apparatus of separating trifluoroethylene in the tetrafluoroethylene production technique.
Background technology
Trifluoro-ethylene is a kind of by product that produces during tetrafluoroethylene monomer is produced.At present, the technology of the difluorochloromethane manufacturing tetrafluoroethylene of industrialization use has two kinds: blank pipe pyrolysis and overheated steam dilution cracking.The flow process that the present invention relates to belongs to overheated steam dilution cracking.
Water vapour dilutes cracking transformation efficiency height, by product is less relatively, productive rate is high, and it has become one of industrial important method of producing tetrafluoroethylene.The domestic water vapor dilution cracking process that generally adopts of China is produced at present, the main by product of water vapor dilution cracking process has trifluoro-ethylene, methylene fluoride, R 1216, trifluoro-chloroethane etc., these by products have very big influence to polymer properties, in present technology, methylene fluoride, R 1216, trifluoro-chloroethane etc. have obtained effective separation.And trifluoro-ethylene is because its boiling point and tetrafluoroethylene are very approaching, and simple rectifying is difficult to they are separated, and therefore never has a good treatment process.
In the domestic current technology, after splitting gas is handled by low boil tower, rectifying tower, tetrafluoroethylene recovery tower, raffinate tower etc., component such as trifluoro-ethylene and tetrafluoroethylene reclaims cat head from tetrafluoroethylene and gets back to lp system in front, so circulation, along with the accumulation of time, the content of trifluoro-ethylene in system can increase day by day, and the trifluoro-ethylene content in the tetrafluoroethylene is increased, and have influence on polymer properties, the resistance to chemical corrosion of polymkeric substance, dielectric properties are descended.
In order to guarantee the quality of tetrafluoroethylene, the content of trifluoro-ethylene reaches certain degree in system, just take the method that tetrafluoroethylene reclaims the material gas emptying of cat head is come trifluoro-ethylene content in the reduction system, so a part of tetrafluoroethylene is by emptying, cause the increase of unit consumption, simultaneously environment has been caused certain pollution.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, disclose a kind of technical process of separating trifluoroethylene from the tetrafluoroethylene production process.
Because most trifluoro-ethylene reclaims cat head through tetrafluoroethylene and returns lp system, and tetrafluoroethylene to reclaim the trifluoro-ethylene concentration of cat head the highest, so this technical process is after tetrafluoroethylene reclaims cat head, thereby guarantees the quality of tetrafluoroethylene; Trifluoro-ethylene, tetrafluoroethylene boiling point are more approaching, and therefore simple rectifying is difficult to realize the separation to the two; In the material component of tetrafluoroethylene recovery cat head various ingredients such as difluorochloromethane, C2ClF5, trifluoro-ethylene, tetrafluoroethylene are arranged, simple extraction, parsing separate will make these wastage of material.Adopted a kind of three tower separation processes flow processs through test of many times and demonstration: material gas is gone into rectifying tower from the jacking of tetrafluoroethylene recovery tower, rectifying by rectifying tower, trifluoro-ethylene in the material gas, tetrafluoroethylene are separated from cat head, and useful components such as difluorochloromethane are returned original system from the tower still; Trifluoro-ethylene, tetrafluoroethylene enter extraction tower from rectifying tower top, because the tetrafluoroethylene molecule is a non-polar molecule, therefore the trifluoro-ethylene molecule is a polar molecule, has used a kind of polarity extracting agent that trifluoro-ethylene is absorbed in extraction tower and is stored in the tower still, and tetrafluoroethylene returns lp system by cat head; Extraction liquid enters Analytic Tower by the pressure reduction of extraction tower and Analytic Tower by the extraction tower still, resolves by heating, and the trifluoro-ethylene that is extracted the agent absorption is discharged, and enters the trifluoro-ethylene storage tank by cat head again.
The technical process of separating trifluoroethylene mainly comprises in the tetrafluoroethylene production technique: tetrafluoroethylene reclaims cat head exhaust → rectifying tower → extraction tower → Analytic Tower → trifluoro-ethylene storage tank.
The method of separating trifluoroethylene during tetrafluoroethylene of the present invention is produced, step is as follows:
1) the material gas of tetrafluoroethylene recovery cat head directly enters rectifying tower, by rectifying, tetrafluoroethylene in the material gas, trifluoro-ethylene and other component are separated, tetrafluoroethylene, trifluoro-ethylene in the material gas more than 90% are assembled at cat head, and all the other components are returned system behind the tetrafluoroethylene recovery tower by the tower still;
2) tetrafluoroethylene of rectifying tower top, trifluoro-ethylene mixture enter extraction tower, utilize extraction agent that trifluoro-ethylene is absorbed in extraction tower, and tetrafluoroethylene is assembled at cat head, and turn back to continuation participation rectifying in the lp system; Trifluoro-ethylene enters Analytic Tower with extraction agent;
3) extraction liquid of extraction tower still enters Analytic Tower, by steam heating trifluoro-ethylene is separated from extraction liquid in Analytic Tower, and trifluoro-ethylene is assembled at the Analytic Tower cat head, enters the trifluoro-ethylene storage tank then.
Preferably, the rectification temperature of rectifying tower is cat head-15～+ 15 ℃ in the step 1), 10～50 ℃ of tower stills; Liquid-gas ratio is 3～20: 1.Preferred, liquid-gas ratio is 7～10: 1.
Preferably, step 2) extraction agent in is a polarity extracting agent, is selected from acetone, methyl alcohol, methyl-2-pyrrolidone, ethyl propionate, DMF or amine.Preferable methyl pyrrolidone, amine or methyl alcohol.
Preferably, the steam heating temperature in the step 3) is 30～100 ℃.
Tetrafluoroethylene reclaims the again rectifying of the material gas of cat head through rectifying tower, tetrafluoroethylene that can 90% in the material is above, trifluoro-ethylene is separated, make tetrafluoroethylene, the gas mixture of trifluoro-ethylene is assembled in rectifying tower top, enter extraction tower by rectifying tower top, in extraction tower, pass through efficient extraction agent with tetrafluoroethylene, trifluoro-ethylene in the trifluoro-ethylene gas mixture extracts, tetrafluoroethylene is then assembled at the extraction cat head, can reach more than 95% by the tetrafluoroethylene purity after absorbing, simultaneously, the extraction liquid that contains trifluoro-ethylene enters the Analytic Tower of back, utilize steam that extraction tower is heated, trifluoro-ethylene in the extraction liquid is discharged, the trifluoro-ethylene concentration of resolving cat head is more than 90%, goes into the trifluoro-ethylene storage tank through the Analytic Tower jacking.The impurity trifluoro-ethylene that will influence the tetrafluoroethylene quality by above-mentioned flow process is separated.
The method of separating trifluoroethylene is characterized in having adopted a kind of three-column process flow in the tetrafluoroethylene production technique provided by the invention.Three-column process flow is made up of rectifying tower, extraction tower, Analytic Tower three parts, is characterized in that good separating effect, flow process are simple and easy to realize.
A kind of three-column process flow has been used in this technical process behind the tetrafluoroethylene recovery tower; trifluoro-ethylene in the system is separated; the effect of its separating trifluoroethylene can reach more than 90%; the advantage that the present invention gives prominence to is to have broken through the situation of in the domestic current technology trifluoro-ethylene not being carried out high efficiency separation; realized the controllability of Paratetrafluoroethylene quality; improve the phenomenon of arbitrarily discharging trifluoro-ethylene during tetrafluoroethylene is produced, aspect environment protection, shown great potential.
Description of drawings
Fig. 1 is a general flow chart of the present invention, and wherein 1 is rectifying tower, and 2 is extraction tower, and 3 is Analytic Tower, and 4 is recycle pump, and 5 is the trifluoro-ethylene storage tank
Embodiment
Below explanation is concrete enforcement of the present invention, but the present invention is not limited thereto.
Embodiment 1:
As shown in Figure 1, this device is implemented on 3000 tons of tetrafluoroethylene production equipments, after this technology is positioned at the tetrafluoroethylene recovery tower, material gas is gone into tower 1 from the jacking of tetrafluoroethylene recovery tower, the tower top temperature of tower 1 is-15～+ 15 ℃, and tower still temperature is 10～50 ℃, and liquid-gas ratio is 3～20: 1; By the separation of tower 1, the tetrafluoroethylene more than 90%, trifluoro-ethylene in the material gas to be separated, useful components such as difluorochloromethane are returned original system from the tower still;
Trifluoro-ethylene, tetrafluoroethylene are assembled on tower 1 top, go into extraction tower 2 by tower 1 jacking, extraction by extraction tower 2, trifluoro-ethylene in tetrafluoroethylene, the trifluoro-ethylene gas mixture is extracted out, because the tetrafluoroethylene molecule is a non-polar molecule, therefore the trifluoro-ethylene molecule is a polar molecule, has used a kind of polarity extracting agent that trifluoro-ethylene is absorbed in extraction tower 2 and is stored in the tower still; Extraction agent is a polarity extracting agent, is selected from a kind of in acetone, methyl alcohol, methyl-2-pyrrolidone, ethyl propionate, DMF or the amine.Preferable methyl pyrrolidone, amine or methyl alcohol.Above-mentioned polarity extracting agent all can well get a desired effect.
Tetrafluoroethylene is returned by cat head and continues to participate in rectifying in the lp system of 3000 tons of tetrafluoroethylene production equipments; Trifluoro-ethylene enters Analytic Tower 3 with extraction agent, and the pressure reduction by extraction tower 2 and Analytic Tower 3 is pressed into Analytic Tower 3 with extraction liquid, utilizes steam heating tower 3 that the trifluoro-ethylene in the extraction liquid is discharged, and the steam heating temperature is 30～100 ℃; The trifluoro-ethylene that discharges is gathered in the cat head of Analytic Tower 3, enters trifluoro-ethylene storage tank 5 by cat head again.
By effective recovery with separate, it is stable that the quality of tetrafluoroethylene has obtained, near and guaranteed that polymer properties is stable; Stopped the waste of emptying, reduced unit consumption of product simultaneously material.
Embodiment 2:
Implement on 3000 tons of tetrafluoroethylene production equipments, after this technology was positioned at the tetrafluoroethylene recovery tower, material gas was gone into tower 1 from the jacking of tetrafluoroethylene recovery tower, and the tower top temperature of tower 1 is-15～+ 15 ℃, and tower still temperature is 10～50 ℃, and liquid-gas ratio is 7～10: 1; By the separation of tower 1, the tetrafluoroethylene more than 90%, trifluoro-ethylene in the material gas to be separated, useful components such as difluorochloromethane are returned original system from the tower still; Other are with embodiment 1.
Claims (4)
1. the method for separating trifluoroethylene during a tetrafluoroethylene is produced, step is as follows:
1) the material gas of tetrafluoroethylene recovery cat head directly enters rectifying tower, by rectifying, tetrafluoroethylene in the material gas, trifluoro-ethylene and other component are separated, tetrafluoroethylene, trifluoro-ethylene in the material gas more than 90% are assembled at cat head, and all the other components are returned system behind the tetrafluoroethylene recovery tower by the tower still;
2) tetrafluoroethylene of rectifying tower top, trifluoro-ethylene mixture enter extraction tower, utilize extraction agent that trifluoro-ethylene is absorbed in extraction tower, and tetrafluoroethylene is assembled at cat head, and turn back to continuation participation rectifying in the lp system; Trifluoro-ethylene enters Analytic Tower with extraction agent; Described extraction agent is a polarity extracting agent, is selected from acetone, methyl alcohol, methyl-2-pyrrolidone, ethyl propionate or DMF;
3) extraction liquid of extraction tower still enters Analytic Tower, by steam heating trifluoro-ethylene is separated from extraction liquid in Analytic Tower, and trifluoro-ethylene is assembled at the Analytic Tower cat head, enters the trifluoro-ethylene storage tank then.
2. the method for separating trifluoroethylene is characterized in that the tower top temperature of rectifying tower is-15～15 ℃ in the step 1) during tetrafluoroethylene as claimed in claim 1 was produced, and tower still temperature is 10～50 ℃; Liquid-gas ratio is 3～20: 1.
3. the method for separating trifluoroethylene is characterized in that liquid-gas ratio is 7～10: 1 during tetrafluoroethylene as claimed in claim 2 was produced.
4. the method for separating trifluoroethylene is characterized in that the steam heating temperature in the step 3) is 30～100 ℃ during tetrafluoroethylene as claimed in claim 1 was produced.
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| CN 200710115900 CN100540517C (en) | 2007-12-29 | 2007-12-29 | The method of separating trifluoroethylene during tetrafluoroethylene is produced |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101550061B (en) * | 2009-05-13 | 2012-01-04 | 上海三爱富新材料股份有限公司 | Trifluoroethylene recovery method and device thereof |
| WO2014178352A1 (en) * | 2013-04-30 | 2014-11-06 | 旭硝子株式会社 | Composition containing trifluoroethylene |
| CN106316779B (en) * | 2016-08-18 | 2019-02-05 | 山东东岳高分子材料有限公司 | A method of recycling high-purity trifluoro-ethylene from tetrafluoroethene by-product |
| CN109879720B (en) * | 2017-12-06 | 2021-01-29 | 中昊晨光化工研究院有限公司 | Method and equipment for separating and recovering difluoro dichloromethane in tetrafluoroethylene production |
| CN111689835A (en) * | 2019-03-13 | 2020-09-22 | 中昊晨光化工研究院有限公司 | Preparation of C by cracking F222F4System and method for recovering trifluoroethylene in process |
| CN111039748B (en) * | 2019-12-31 | 2022-06-07 | 山东华夏神舟新材料有限公司 | Method for separating trifluoroethylene from tetrafluoroethylene cracking gas |
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Non-Patent Citations (2)
| Title |
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| 四氟乙烯的生产与工艺（二）. 朱顺根.有机氟工业，第2期. 1997 |
| 四氟乙烯的生产与工艺（二）. 朱顺根.有机氟工业，第2期. 1997 * |
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