CN106220471A - The method purifying tetrafluoroethene from pyrolysis gas - Google Patents
The method purifying tetrafluoroethene from pyrolysis gas Download PDFInfo
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- CN106220471A CN106220471A CN201610651043.5A CN201610651043A CN106220471A CN 106220471 A CN106220471 A CN 106220471A CN 201610651043 A CN201610651043 A CN 201610651043A CN 106220471 A CN106220471 A CN 106220471A
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- tetrafluoroethene
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- tower
- lightness
- pyrolysis gas
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of method purifying tetrafluoroethene from pyrolysis gas, use lightness-removing column and treating column, lightness-removing column overhead condenser and tower reactor reboiler, treating column overhead condenser and tower reactor reboiler；Pyrolysis gas material liquid containing tetrafluoroethene enters the top of lightness-removing column, sloughing fluoroform, the light component of perfluoroethane, tower reactor logistics enters the middle part for the treatment of column, and tower reactor sloughs difluoromethane, monochlorodifluoromethane, hexafluoropropene heavy constituent, tower top sloughs light component, and side line obtains tetrafluoroethene product.Lightness-removing column tower top operation pressure is 1100 1600Kpa, and reflux ratio is 0.5 3, and theoretical stage is 50 100 altogether.Described treating column tower top operation pressure is 1000 1500Kpa, and reflux ratio is 0.5 3, and theoretical stage is 50 100 altogether.The present invention uses continuous operation, reduces the energy consumption of system.Produce tetrafluoroethene product purity >=99.999%, difluoromethane≤0.0005%.
Description
Technical field
The method that the present invention relates to isolated and purified tetrafluoroethene, a kind of separating high-purity from the pyrolysis gas processed
The method of tetrafluoroethene, belongs to the isolated and purified field of tetrafluoroethene.
Background technology
Tetrafluoroethene is that current volume of production is maximum, is also fluorochemical monomer most important, most widely used.Tetrafluoroethene also known as
Freon-11 14, English name Tetraflouoroethylene, No. CSA is 116-14-3, and molecular formula is C2F4, chemical formula CF2
=CF2, relative molecular mass is 100.02.
Tetrafluoroethene belongs to no color or smell gas, is inflammable, explosive compressible gas and liquid gas.Molten point-142.5
DEG C, boiling point-76.3 DEG C, water insoluble, it is heavier than air.Relative density 1.519, critical temperature 33.3 DEG C, critical pressure
3.92MPa, burning-point 620 DEG C.It is dissolved in acetone, ethanol.Flammability limit is 11%-60% (volume), and ignition temperature only has 180 DEG C,
In the presence of aerobic, it is easily formed unstable explosive peroxide.
Tetrafluoroethene, is called for short TFE, is monomer and the intermediate of fluorochemical of fluoropolymer.Four fluorine ethylenes are made
For the one of fluoropolymer monomer, producer typically will not direct marketing, but produce polytetrafluoroethyl-ne through follow-up polymerization process
Alkene (PTFE), fluorubber, other Novel hot plastics, engineering plastics etc., or for produce other fluorine monomer such as perfluoropropene with
And extinguishing chemical etc..Therefore to ensure the quality of subsequent product, the purity requirement for monomer tetrafluoroethene is the highest.
The method being presently available for industrial monochlorodifluoromethane (R22) pyrolysis system four fluorine ethylenes mainly has two kinds:
Thermal cracking and steam dilution pyrolysis, the pyrolysis gas that both approaches generates, impurity is a lot of, except product tetrafluoroethene and the most anti-
Outside the R22 answered, the most a small amount of low-boiling-point substance and high-boiling components, such as difluoromethane (CH2F2), fluoroform (CHF3), trifluoro second
Alkene (C2HF3), dichlorodifluoromethane (CF2Cl2), perfluoropropene (HFP), chlorotetrafluoroethane (CHClFCF3), carbon monoxide
(CO) etc..The highly purified tetrafluoroethylene monomer of high-quality to be obtained, it is necessary to pyrolysis gas is separated, current tetrafluoroethene pure
The method changing commonly used rectification separating-purifying.
At present, domestic and international tetrafluoroethene rectification segregation apparatus is formed (1# crude tower, 2# lightness-removing column and 3# rectification by three towers
Tower).Pyrolysis gas after treatment, enters 1# crude tower, and 1# tower is mainly (including tetrafluoro second less than tetrafluoroethene boiling point
Alkene) the Light ends Component seperation high with than tetrafluoroethene boiling point out, low boiling component is discharged into 2# lightness-removing column from tower top, and
2# tower is discharged (not including tetrafluoroethene) more low-boiling than tetrafluoroethene component from tower top, the restructuring containing tetrafluoroethene of the 2# tower reactor
Dividing then entrance 3# rectifying column to carry out rectification, qualified tetrafluoroethene is collected to tetrafluoroethene finished product from 3# tower top or side line position, tower top
Groove.
Tetrafluoroethene purity ＜ 99.99% that this process unit produces, and energy consumption is higher.
In order to improve the purity of tetrafluoroethene, it is thus achieved that high performance fluorine-containing polymer, in the present invention, tetrafluoroethene rectification divides
Using two-tower process from device, pyrolysis gas after treatment, after entrance lightness-removing column separates with rectifying column rectification, obtains highly purified
Tetrafluoroethene finished product.
Summary of the invention
It is an object of the invention to provide a kind of method that highly efficient distilling purifies tetrafluoroethene from the pyrolysis gas processed, obtain
Obtain the purity tetrafluoroethene product more than 99.999%, and obtain good yield.
It is an object of the invention to complete by following technical solution:
A kind of method purifying tetrafluoroethene from pyrolysis gas, uses lightness-removing column and treating column, and it is cold that lightness-removing column is provided with tower top
Condenser and tower reactor reboiler, treating column is provided with overhead condenser and tower reactor reboiler；Pyrolysis gas material liquid containing tetrafluoroethene enters
Entering the top of lightness-removing column, slough fluoroform, the light component of perfluoroethane, tower reactor logistics enters the middle part for the treatment of column, and tower reactor is sloughed
Difluoromethane, monochlorodifluoromethane, hexafluoropropene heavy constituent, tower top sloughs light component, and its side line obtains purity and is more than
99.999% tetrafluoroethene product.
Described lightness-removing column and treating column are preferably packed tower.
Described lightness-removing column tower top operation pressure be 1100～1600Kpa, reflux ratio is 0.5～3, theoretical stage be altogether 50～
100.
Described treating column tower top operation pressure be 1000～1500Kpa, reflux ratio is 0.5～3, theoretical stage be altogether 50～
100。
Described pyrolysis gas predominant amount is: fluoroform 0-0.35%, perfluoroethane 0.001-0.05%, tetrafluoroethene
40-60%, difluoromethane 0.1-1%, monochlorodifluoromethane 30-45%, hexafluoropropene 8.6-14.9%.
In the rectification separating technology of the present invention, containing tetrafluoroethene material liquid by with treating column bottom flow out still liquid warp
Feed preheater carries out heat exchange, and relative to traditional rectification separating technology, process total energy consumption reduces about about 15%.
The invention have the advantage that
(1) present invention uses continuous operation, and the most whole invention uses thermal coupling rectification separating technology, reduces system
Energy consumption.
(2) present invention is packed tower because of two towers, so separation efficiency is more efficient, reduces pressure drop and tower reactor still simultaneously
Temperature.
(3) present invention process production tetrafluoroethene product purity >=99.999%, difluoromethane≤0.0005%, process
Product recovery rate is more than 75%.The visible present invention can be effectively improved tetrafluoroethene product purity, it is ensured that the performance indications of product.
Accompanying drawing explanation
The process flow diagram of Fig. 1: the present invention.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but the present invention is not limited to this.
Using the connected mode of accompanying drawing 1, lightness-removing column 3 is provided with overhead condenser 4 and tower reactor reboiler 7, and treating column 9 is provided with tower
Top condenser 10 and tower reactor reboiler 14.After feed preheater 2 heat exchange, lightness-removing column is entered by pipeline containing tetrafluoroethene material liquid 1
The top of 3, sloughs light component 6, and its tower reactor logistics 8 enters the middle part for the treatment of column 9, and tower reactor sloughs heavy constituent 15, and tower top is sloughed gently
Component 12, its side line obtains purity more than 99.999% tetrafluoroethene product 13.
Embodiment 1:
Processing the purification containing tetrafluoroethene raw material of 2300kg per hour, feed composition is as follows: fluoroform 0.08%, six
Fluoroethane 0.002%, tetrafluoroethene 45%, difluoromethane 0.418%, monochlorodifluoromethane 39.5%, hexafluoropropene 15%.
Technological process each tower operating condition
Note: after raw material heat exchange, inlet temperature of stabilizer is 4 DEG C
The azophenlyene product leading indicator produced under above-mentioned process conditions is as follows:
| Leading indicator | |
| Product purity | 99.9991% |
| Perfluoroethane content | 0.0009% |
| Product recovery rate | 77.8% |
Embodiment 2:
Processing the purification containing tetrafluoroethene raw material of 2300kg per hour, feed composition is as follows: fluoroform 0.1%, six
Fluoroethane 0.0015%, tetrafluoroethene 51.2%, difluoromethane 0.0985%, monochlorodifluoromethane 38.2%, hexafluoropropene
10.4%.
Technological process each tower operating condition
| Lightness-removing column | Treating column | |
| Tower type | Packed tower | Packed tower |
| Wire feeding | Stainless steel cloth structured packing | Stainless steel cloth structured packing |
| Theoretical stage | 80 | 80 |
| Tower top operation pressure (absolute pressure)/Kpa | 1300 | 1200 |
| Reflux ratio | 1.1 | 1.1 |
Note: after raw material heat exchange, inlet temperature of stabilizer is 4 DEG C
The tetrafluoroethene product leading indicator produced under above-mentioned process conditions is as follows:
| Leading indicator | |
| Product purity | 99.9992% |
| Perfluoroethane content | 0.0008% |
| Product recovery rate | 76.5% |
Embodiment 3:
Processing the purification containing tetrafluoroethene raw material of 2300kg per hour, feed composition is as follows: fluoroform 0.35%, six
Fluoroethane 0.05%, tetrafluoroethene 60%, difluoromethane 1%, monochlorodifluoromethane 30%, hexafluoropropene 8.6%.
Technological process each tower operating condition
Note: after raw material heat exchange, inlet temperature of stabilizer is 4 DEG C
The tetrafluoroethene product leading indicator produced under above-mentioned process conditions is as follows:
| Leading indicator | |
| Product purity | 99.9992% |
| Perfluoroethane content | 0.0008% |
| Product recovery rate | 78.0% |
As seen from the above table, the present invention is feasible, and the not only technological operation of whole separation process is simple, energy consumption is less,
And separation efficiency is the highest.
The method purifying tetrafluoroethene from pyrolysis gas that the present invention proposes, is retouched by preferred embodiment
Stating, person skilled substantially can be to rectification and purification method as herein described in without departing from present invention, spirit and scope
It is modified or suitably changes and combine realizing the technology of the present invention.Special needs to be pointed out is, all similar replacements and
Changing apparent to those skilled in the art, they are considered as being included in present invention spirit, scope and content
In.
Claims (5)
1. the method purifying tetrafluoroethene from pyrolysis gas, is characterized in that using lightness-removing column and treating column, and lightness-removing column is provided with
Overhead condenser and tower reactor reboiler, treating column is provided with overhead condenser and tower reactor reboiler；Pyrolysis gas containing tetrafluoroethene is former
Feed liquid enters the top of lightness-removing column, sloughs fluoroform, the light component of perfluoroethane, and tower reactor logistics enters the middle part for the treatment of column, tower
Still sloughs difluoromethane, monochlorodifluoromethane, hexafluoropropene heavy constituent, and tower top sloughs light component, and its side line obtains purity and is more than
99.999% tetrafluoroethene product.
2. the method for claim 1, is characterized in that described lightness-removing column and treating column are packed tower.
3. the method for claim 1, is characterized in that lightness-removing column tower top operation pressure is 1100～1600Kpa, reflux ratio
Being 0.5～3, theoretical stage is 50～100 altogether.
4. the method for claim 1, is characterized in that treating column tower top operation pressure is 1000～1500Kpa, reflux ratio
Being 0.5～3, theoretical stage is 50～100 altogether.
5. the method for claim 1, is characterized in that pyrolysis gas predominant amount is: fluoroform 0-0.35%, hexafluoro second
Alkane 0.001-0.05%, tetrafluoroethene 40-60%, difluoromethane 0.1-1%, monochlorodifluoromethane 30-45%, hexafluoropropene
8.6-14.9%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610651043.5A CN106220471A (en) | 2016-08-09 | 2016-08-09 | The method purifying tetrafluoroethene from pyrolysis gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610651043.5A CN106220471A (en) | 2016-08-09 | 2016-08-09 | The method purifying tetrafluoroethene from pyrolysis gas |
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| CN106220471A true CN106220471A (en) | 2016-12-14 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106866357A (en) * | 2017-01-24 | 2017-06-20 | 福建三农化学农药有限责任公司 | A kind of tetrafluoroethene process for purification |
| CN111282305A (en) * | 2020-03-16 | 2020-06-16 | 上海化工研究院有限公司 | Device for rectifying and purifying fluorine-containing solvent by continuous lateral line discharging |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110034740A1 (en) * | 2008-04-25 | 2011-02-10 | Asahi Glass Company, Limited | Method for purifying tetrafluoroethylene |
| CN202415404U (en) * | 2011-12-21 | 2012-09-05 | 天津市泰旭物流有限公司 | Device for preparing tetrafluoroethylene by using monochlorodifluoromethane water vapor dilution pyrolysis method |
-
2016
- 2016-08-09 CN CN201610651043.5A patent/CN106220471A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110034740A1 (en) * | 2008-04-25 | 2011-02-10 | Asahi Glass Company, Limited | Method for purifying tetrafluoroethylene |
| CN202415404U (en) * | 2011-12-21 | 2012-09-05 | 天津市泰旭物流有限公司 | Device for preparing tetrafluoroethylene by using monochlorodifluoromethane water vapor dilution pyrolysis method |
Non-Patent Citations (2)
| Title |
|---|
| 孙旻灏: "四氟乙烯装置精馏提纯的计算机模拟和优化", 《中国优秀硕士学位论文数据库 工程科技I辑》 * |
| 朱顺根: "四氟乙烯的纯化", 《化工生产与技术》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106866357A (en) * | 2017-01-24 | 2017-06-20 | 福建三农化学农药有限责任公司 | A kind of tetrafluoroethene process for purification |
| CN111282305A (en) * | 2020-03-16 | 2020-06-16 | 上海化工研究院有限公司 | Device for rectifying and purifying fluorine-containing solvent by continuous lateral line discharging |
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Address after: 301800 Tianjin city Baodi Plastic Industrial Zone No. 2 Fuyilu Applicant after: TIANJIN ZENITH OIL&GAS ENGINEERING CO., LTD. Address before: Rong Yuan Road 300384 Tianjin city Nankai District Huayuan Industrial Park No. 1 Tian Hotel Room 507 building A Applicant before: TIANJIN ZENITH OIL&GAS ENGINEERING CO., LTD. |
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Application publication date: 20161214 |
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