CN100376523C - Method and equipment for recovering F22 and hexafluoro propylene in tetrafluoroethylene production - Google Patents
Method and equipment for recovering F22 and hexafluoro propylene in tetrafluoroethylene production Download PDFInfo
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- CN100376523C CN100376523C CNB2006101662885A CN200610166288A CN100376523C CN 100376523 C CN100376523 C CN 100376523C CN B2006101662885 A CNB2006101662885 A CN B2006101662885A CN 200610166288 A CN200610166288 A CN 200610166288A CN 100376523 C CN100376523 C CN 100376523C
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Abstract
This invention relates to a process of recover di-fluorine- monochloromethane and hexafluoro-propylene (HFP) from Tetrafluoroethylene production. The feature is using F22, C3F6 membrane. It used F22, C3F6 membrane replace azeotropic tower, HFP absorber, resolution tower to recover exhaust residue of di-fluorine- monochloromethane(F22) and HFP (C3F6). This invention has high recovery rate, can reduce energy consumption and costs. The invention also provides equipment of achieving the aforementioned method.
Description
Technical field:
The invention belongs to the fluorine chemical field, relate to and reclaim difluorochloromethane (F22) in the tetrafluoroethylene production technique and separate R 1216 (C with reclaiming
3F
6) method and apparatus.
Background technology:
Tetrafluoroethylene is present turnout maximum, most important fluorochemical monomer, and it is the tetrafluoroethylene raw material, is the comonomer of many fluorinated copolymers, also is the intermediate of multiple fluorochemicals.The tetrafluoroethylene production level has been represented the level of the organic fluorine industrial development of a country.
Among the product that tetrafluoroethylene sees Ruff in 1933 etc. the earliest when tetrafluoro-methane is carried out thermolysis in carbon arc.But realize that really industrialization is after finding tetrafluoroethylene, equaled to propose in 1945 difluorochloromethane prepares tetrafluoroethylene by pyrolysis method by J.D.Park.Because the raw material of this path of preparing tetrafluoroethylene is easy to get, method is simple, technology reaches its maturity, is convenient to industrial production, so this method is widely adopted.
At present in the TFE monomer production technique for guaranteeing the higher yields of tetrafluoroethylene, F22 is incomplete cracked in scission reaction, so this part has neither part nor lot in cracked F22 and needs recycling.
Difluorochloromethane (CHClF
2, being called for short F22) and the pyrolytic reaction equation is as follows:
CHClF
2→ C
2F
4(volume ratio: 45-50%)+C
3F
6(volume ratio: 3-5%)+CHClF
2(volume ratio: 40-45%)+other
The chemical process of difluorochloromethane pyrolytic reaction is very complicated, and pyrolysis product has more than 30 component.Principal product is a tetrafluoroethylene, and by product comprises R 1216, Perfluorocyclobutane, Vcon, trifluorochloroethylene, methyl chlorofluoride and Fluorine containing olefine, also has hydrogenchloride, carbon monoxide, hydrogen fluoride etc. in addition.
At present, the difluorochloromethane that still uses in the industrialization technology of making tetrafluoroethylene has two kinds: blank pipe pyrolysis and overheated steam dilution pyrolysis.
No matter make tetrafluoroethylene with the difluorochloromethane pyrolysis, be blank pipe pyrolysis or overheated steam dilution pyrolysis, and these by products all exist.
Therefore, the separation of pyrolysis gas is an important component part during tetrafluoroethylene is produced.Mainly comprise: (1) tetrafluoroethylene monomer is purified; (2) recovery of difluorochloromethane; (3) separation and the recovery of useful component (as R 1216) in the by product; (4) processing of raffinate spent acid.
In the traditional technology, splitting gas enters the raffinate tower by the low tower that boils, rectifying tower, TFE recovery tower, in the raffinate tower, realizes separating of raffinate and light constituent, light constituent mainly contain F22, C
3F
6, light component is discharged by cat head and is entered azeotrope column.In azeotrope column, reclaim the F22 of 90%-95%, also have small part F22 and C
3F
6Form azeotrope, pass through C again
3F
6Absorption tower, Analytic Tower carry out to the separation of F22 and to C
3F
6Recovery.Adopt traditional technology to have drawbacks such as energy consumption height, the rate of recovery are low, complicated operation.
In the process of venting one's spleen with traditional rectificating method heat of dissociation, can form the azeotrope that difluorochloromethane and R 1216 are formed, azeotrope is impossible in addition isolating by conventional distillation or rectifying means.But in the tetrafluoroethylene production process, difluorochloromethane must be separated with R 1216.Otherwise, carry out pyrolytic reaction if difluorochloromethane circulated with the azeotrope of R 1216, R 1216 forms the macromole product easily when pyrolysis, block reactive system and after-treatment system, cause frequent unplanned parking, the unsafe factor of aggrandizement apparatus.If difluorochloromethane and R 1216 are directly discharged atmosphere, can cause the tetrafluoroethylene yield to descend, the unit cost of production raises, and causes environmental pollution.
R 1216 is one of basic material of organic fluorine industry, and it is widely used in the production of viton, fluoroplastics, perfluoro propene oxid, heptafluoro-propane, fluorine surfactant.Therefore reclaim R 1216 and be used, turn waste into wealth, good environmental protection effect and economic benefit are arranged.Patent RU2063952 (1996) and patent RU2211209 (2003) disclose the method that reclaims R 1216, but have that the R 1216 quality product is not high, shortcomings such as complex procedures, contaminate environment and cost height, be not suitable for industrialization and use.
Chinese patent application 200610021004.3 discloses a kind of recovery method of perfluoro propylene, especially from containing perfluoro propylene (C
3F
6) and difluorochloromethane (CHClF
2) reclaim the method for perfluoro propylene in the tetrafluoroethylene production technique of azeotrope, it is served as reasons and contains perfluoro propylene (C at least
3F
6) and difluorochloromethane (CHClF
2) the mixture of raw material azeotrope in obtain the purpose mixture, this purpose mixture is the perfluoro propylene mixture that contains the greater concn perfluoro propylene, this method comprises predistillation, extracting rectifying and main rectification step, and the F22 of recovery is more than or equal to 97.8% (volume ratio); The perfluoro propylene quality reaches 99.99% (volume ratio).This invented technology long flow path, equipment is many, complicated operation.
Chinese patent application 200610038442.0 discloses a kind of difluorochloromethanazeotropic azeotropic hexafluoropropene and has separated and recovery method, in envrionment temperature, under self pressure, difluorochloromethane-R 1216 azeotropic mixture is passed through the gas delivery membrane module with gaseous state, obtain the infiltration gas that is mainly difluorochloromethane and the residual air of oozing that is mainly R 1216 of two strands of destroyed azeotropic ratios by the gas delivery membrane module, to ooze the condenser liquefaction of residual air process and collect condensate storage, enter rectifying tower then, obtain pure R 1216 from the tower still after the rectifying, from a small amount of azeotropic mixture of recovered overhead; After reclaiming pure R 1216, the a small amount of azeotropic mixture that reclaims in the rectifying is returned original low pressure gas holder in the tetrafluoroethylene production equipment together together with infiltration gas, and enter original distillation system in the tetrafluoroethylene production equipment, carry out normal rectifying separation and reclaim the difluorochloromethane process.Above-mentioned traditional technology technical process is longer, and complicated operation brings a lot of inconvenience to actual production.
Summary of the invention:
The purpose of this invention is to provide reclaim in the low tetrafluoroethylene production technique of a kind of separation efficiency height, energy consumption difluorochloromethane with separate R 1216 technical process.
The inventor after repeated discussions with experiment, finally adopted a kind of F22 of utilization, C
3F
6The technical process of separatory membrane replaces azeotrope column, R 1216 absorption tower, Analytic Tower.This film is the composite membrane that is made of supporting layer, fine and close effective separating layer, has high-throughput, highly selective and excellent solvent-resistance energy.Isolating main component from the raffinate column overhead is F22 and C
3F
6Gas mixture, gas mixture enters the film recovery process, wherein F22 is than C
3F
6See through F22, C Deng non-condensable gas
3F
6The speed of separatory membrane is fast, so per-meate side F22 enriching and recovering, the gas of retentate side enters the second road separatory membrane, the infiltration gas of the second road film returns the first road film by compressor, ooze residual air and enter the 3rd road film, the infiltration gas of the 3rd road film returns the second road film by compressor, oozes residual air and then enters the R 1216 treatment system.F22, C
3F
6Separatory membrane satisfies the needs of Separation and Recovery F22 in the tetrafluoroethylene production process fully.
Reclaim difluorochloromethane and the method for separating R 1216 in the tetrafluoroethylene production technique provided by the invention, it is characterized in that having used a kind of F22, C
3F
6Separatory membrane.
Described F22, C
3F
6The composite membrane of separatory membrane for being made of supporting layer, fine and close effective separating layer has high-throughput, highly selective and excellent solvent-resistance energy.
Reclaim difluorochloromethane and the technical process that separates R 1216 in the tetrafluoroethylene production technique, key step comprises:
The raffinate cat head exhaust → first road separatory membrane → second road separatory membrane → the 3rd road separatory membrane → R 1216 is handled.
Reclaim difluorochloromethane and the method for separating R 1216 in the tetrafluoroethylene production technique of the present invention, concrete processing step is as follows:
1) gas mixture that distills out of the raffinate column overhead of tetrafluoroethylene enters the Membrane recovery unit MRU first road separatory membrane, obtains permeating gas and oozes residual air; Infiltration gas returns the monomer workshop and participates in cracking again;
2) ooze residual air and enter the second road separatory membrane.The F22 that oozes in the residual air obtains secondary separation here, obtains second permeation gas and secondary and oozes residual air; Second permeation gas returns the first road film to be separated again;
3) secondary oozes residual air and enters the 3rd road separatory membrane, and secondary oozes residual air and obtains three times here and separate, and obtains three infiltration gas and oozes residual air three times; Three times infiltration gas returns the second road film, oozes residual air and enters the thick storage tank of R 1216 for three times.
Preferably, to distill out main component be F22 and C to tetrafluoroethylene raffinate column overhead
3F
6Gas mixture.The content of F22 is 80%-85%, and the content of C3F6 is 8%-12%, all the other component concentration 3%-12%.
The gas mixture that tetrafluoroethylene raffinate column overhead distills out enters the Membrane recovery unit MRU first road separatory membrane, obtains permeating gas and oozes residual air.Be rich in F22 in the infiltration gas, F22 purity can reach 96%-99%, oozes to be rich in C3F6 in the residual air, and C3F6 purity can reach 86%-90%, and infiltration gas returns the monomer workshop and participates in cracking again.
Ooze residual air and enter the second road separatory membrane.The F22 that oozes in the residual air obtains secondary separation here, obtains second permeation gas and secondary and oozes residual air; The gas of per-meate side is rich in its purity of F22 can reach 86%-92%, and the gas of retentate side is rich in C3F6, and C3F6 purity can reach 86%-90%.Second permeation gas returns the first road film to be separated again.
Secondary oozes residual air and enters the 3rd road separatory membrane, oozes residual air and obtains three separation here, obtains three infiltration gas and oozes residual air three times; The gas of per-meate side is rich in F22, and purity is 75%-80%, and three times infiltration gas returns the second road film; The gas of retentate side is rich in C3F6 purity can reach 86%-90%, oozes residual air three times to enter the thick storage tank of R 1216, carries out the rectifying of R 1216.
The present invention also provides a kind of enforcement device of the present invention, comprising:
Three Membrane recovery unit MRUs are used to separate F22 and C
3F
6Gas mixture; Obtain oozing residual air and infiltration gas by Membrane recovery unit MRU;
A mixture conduit is used for carrying F22 and C to Membrane recovery unit MRU
3F
6Gas mixture.
Three infiltration feed channel are used to carry the infiltration gas that is separated the F22 that contains 96%-99% that obtains by Membrane recovery unit MRU.
Three ooze the residual air pipeline, are used to carry by Membrane recovery unit MRU separate C that obtain, that contain 86%-90%
3F
6Ooze residual air.
Two condensers are respectively applied for condensation infiltration feed channel and ooze the infiltration gas of residual air pipe-line transportation and ooze residual air.
Two surge tanks are respectively applied for the gas-pervious storage of oozing of second and third road film.
Two compressors, the infiltration gas that is used for the second road film turns back to the first road film; The infiltration gas of the 3rd road film returns the second road film.
A kind of F22, C have been used in this technical process
3F
6Separatory membrane is installed in after the raffinate tower, replaces azeotrope column, R 1216 absorption tower and R 1216 Analytic Tower, and the ability that film device is handled gas mixture is 100-130NM
3/ H, the purity of the F22 that is recovered to is 96%-99%.This technology, outstanding advantage are with F22, C
3F
6Separatory membrane replaces azeotrope column.Azeotrope column energy consumption height, the requirement that discontented podomere can lower consumption.And F22, C
3F
6The separatory membrane installation costs is low, does not have energy consumption substantially, rate of recovery height; Satisfied that modern industry is efficient, less energy-consumption and free of contamination demand for development, the energy make full use of and environment protection aspect demonstrate great potential.
Description of drawings
Fig. 1 is a device sketch of the present invention.Wherein: 1: the material inlet pipeline; 2; The first road membrane separation unit; 3: the second road membrane separation units; 4: the three road membrane separation units; 5: ooze residual air and reclaim condenser; 6: three times infiltration gas reclaims compressor; 7: three times infiltration gas reclaims surge tank (2#); 8: ooze the residual air recycling pipeline; 9: second permeation gas reclaims compressor; 10: second permeation gas reclaims surge tank (1#); 11: infiltration gas reclaims condenser; 12: infiltration gas recycling pipeline.
Embodiment;
Following examples are to further specify of the present invention, but the present invention is not limited thereto.
Embodiment 1
With 5000 tons of devices is example, and this technical process is positioned at after the raffinate tower, and the exhaust of raffinate cat head enters the first road F22, C
3F
6Separatory membrane, the infiltration gas that sees through the first road film are that main its purity can reach 96%-99% with the difluorochloromethane, and this part infiltration gas is recycled to monomer workshop low pressure gas holder and participates in cracking once more after the 1# condenser condenses, ooze residual air and then enter the second road separatory membrane.At 86%-92%, this part infiltration gas returns the first road film by 1# surge tank and compressor and carries out secondary separation, oozes residual air and continues to enter the 3rd road separatory membrane through difluorochloromethane purity in the infiltration gas of the second road separatory membrane.The purity that sees through difluorochloromethane in the infiltration gas of the 3rd road film is 75%-80%, and this part infiltration gas returns the second road F22, C by 2# surge tank and compressor
3F
6Separatory membrane carries out secondary separation.The 3rd road film ooze C in the residual air
3F
6Purity at 86%-90%, the residual air of oozing of the 3rd road film enters C then through the condensation of 2# condenser
3F
6Thick storage tank carries out the R 1216 distillation operation then.
In 5000 tons of monomer devices, azeotropic Tata still quantity of steam 350kg/ hour-600kg/ hour, so Mei Nian steam consumption is 3000 tons-5000 tons, 120 yuan of steam per ton, the expense of steam is 360,000-600,000, unit cooler is power consumption 200KW per hour, annual power consumption expense is about 860,000-890,000, R 1216 absorption tower, the used extraction agent constantly loss in use of Analytic Tower, annual loss of extractant expense is 2.5 ten thousand-30,000, and annual energy charge adds up to 124.5 ten thousand-1,520,000.In the traditional technology, the processing power of azeotrope column is 450kg/h-500kg/h, and the recovery purity of F22 is 85%-95%.
A kind of F22, C have been used in this technical process
3F
6Separatory membrane is installed in after the raffinate tower, replaces azeotrope column, R 1216 absorption tower and R 1216 Analytic Tower, and the ability that film device is handled gas mixture is 30-50NM
3/ H, the purity of the F22 that is recovered to is 96%-99%.This technology, outstanding advantage are with F22, C
3F
6Separatory membrane replaces azeotrope column.Azeotrope column energy consumption height, the requirement that discontented podomere can lower consumption.And F22, C
3F
6Separatory membrane does not have energy consumption substantially, and ten thousand yuan/year of installation and maintenance cost average out to 40-60 are well below the input of azeotrope column.This film energy consumption is low, rate of recovery height; Satisfied that modern industry is efficient, less energy-consumption and free of contamination demand for development, the energy make full use of and environment protection aspect demonstrate great potential.
Claims (6)
1. reclaim difluorochloromethane and the method for separating R 1216 in a tetrafluoroethylene production technique, it is characterized in that, used F22, C
3F
6Separatory membrane; Described F22, C
3F
6The composite membrane of separatory membrane for constituting by supporting layer, fine and close effective separating layer; Comprise the following steps:
1) gas mixture that distills out of the raffinate column overhead of tetrafluoroethylene enters the Membrane recovery unit MRU first road separatory membrane, obtains permeating gas and oozes residual air; Infiltration gas returns the monomer workshop and participates in cracking again;
2) ooze residual air and enter the second road separatory membrane, the F22 that oozes in the residual air obtains secondary separation here, obtains second permeation gas and secondary and oozes residual air; Second permeation gas returns the first road film to be separated again;
3) secondary oozes residual air and enters the 3rd road separatory membrane, and secondary oozes residual air and obtains three times here and separate, and obtains three infiltration gas and oozes residual air three times; Three times infiltration gas returns the second road film, oozes residual air three times to enter the thick storage tank of R 1216, carries out the rectifying of R 1216.
2. reclaim difluorochloromethane and the method for separating R 1216 in the tetrafluoroethylene production technique as claimed in claim 1, it is characterized in that the content of F22 is 80%-85% in the gas mixture that the raffinate column overhead of the tetrafluoroethylene described in the step 1) distills out, C
3F
6Content be 8%-12%, all the other component concentration 3%-12%.
3. reclaim difluorochloromethane and the method for separating R 1216 in the tetrafluoroethylene production technique as claimed in claim 1, it is characterized in that be rich in F22 in the infiltration gas that obtains in the step 1), F22 purity reaches 96%-99%, oozes to be rich in C in the residual air
3F
6, C
3F
6Purity reaches 86%-90%.
4. reclaim difluorochloromethane and the method for separating R 1216 in the tetrafluoroethylene production technique as claimed in claim 1, it is characterized in that step 2) in the second permeation gas that obtains be rich in F22, F22 purity reaches 86%-92%; Secondary oozes residual air and is rich in C
3F
6, C
3F
6Purity reaches 86%-90%.
5. reclaim difluorochloromethane and the method for separating R 1216 in the tetrafluoroethylene production technique as claimed in claim 1, it is characterized in that three infiltration gas that obtain in the step 3) are rich in F22, purity is 75%-80%; Ooze residual air three times and be rich in C
3F
6, purity reaches 86%-90%.
6. realize reclaiming in the described tetrafluoroethylene production technique of claim 1 equipment of two fluoro-methyl chloride and the method for separating R 1216, comprising:
Three Membrane recovery unit MRUs are used to separate F22 and C
3F
6Gas mixture; Obtain oozing residual air and infiltration gas by Membrane recovery unit MRU;
A mixture conduit is used for carrying F22 and C to Membrane recovery unit MRU
3F
6Gas mixture;
Three infiltration feed channel are used to carry by Membrane recovery unit MRU and separate the infiltration gas that obtains;
Three ooze the residual air pipeline, are used to carry by Membrane recovery unit MRU separate the residual air of oozing that obtains;
Two condensers are respectively applied for condensation infiltration feed channel and ooze the infiltration gas of residual air pipe-line transportation and ooze residual air;
Two surge tanks are respectively applied for the gas-pervious storage of oozing of second and third road film;
Two compressors, the infiltration gas that is used for the second road film turns back to the first road film; The infiltration gas of the 3rd road film returns the second road film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101662885A CN100376523C (en) | 2006-12-25 | 2006-12-25 | Method and equipment for recovering F22 and hexafluoro propylene in tetrafluoroethylene production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101662885A CN100376523C (en) | 2006-12-25 | 2006-12-25 | Method and equipment for recovering F22 and hexafluoro propylene in tetrafluoroethylene production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN100999436A CN100999436A (en) | 2007-07-18 |
| CN100376523C true CN100376523C (en) | 2008-03-26 |
Family
ID=38258273
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101662885A Active CN100376523C (en) | 2006-12-25 | 2006-12-25 | Method and equipment for recovering F22 and hexafluoro propylene in tetrafluoroethylene production |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102267851B (en) * | 2011-06-07 | 2013-12-25 | 上海三爱富新材料股份有限公司 | Separation method of hexafluoropropylene and monochlorodifluoromethane (F22) mixture |
| CN104788283B (en) * | 2015-03-12 | 2016-08-24 | 福建三农化学农药有限责任公司 | A kind of hexafluoropropene produces two-wire rectificating method and the rectifying device of cracking gas |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1027435A (en) * | 1963-02-28 | 1966-04-27 | Osaka Kinzoku Kogyo Company Lt | Recovery of tetrafluoroethylene and hexafluoropropene |
| CN1830929A (en) * | 2006-02-22 | 2006-09-13 | 常熟三爱富中昊化工新材料有限公司 | Method for separating and recovery difluorochloromethane azeotropic hexafluoropropene |
| CN1872824A (en) * | 2006-05-26 | 2006-12-06 | 中昊晨光化工研究院 | Method for recovering perfluoro propylene from technique of producing tetrafluoroethlene |
-
2006
- 2006-12-25 CN CNB2006101662885A patent/CN100376523C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1027435A (en) * | 1963-02-28 | 1966-04-27 | Osaka Kinzoku Kogyo Company Lt | Recovery of tetrafluoroethylene and hexafluoropropene |
| CN1830929A (en) * | 2006-02-22 | 2006-09-13 | 常熟三爱富中昊化工新材料有限公司 | Method for separating and recovery difluorochloromethane azeotropic hexafluoropropene |
| CN1872824A (en) * | 2006-05-26 | 2006-12-06 | 中昊晨光化工研究院 | Method for recovering perfluoro propylene from technique of producing tetrafluoroethlene |
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| CN100999436A (en) | 2007-07-18 |
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