CN115650822A - Method and device for extracting trifluoromethane from trifluoromethane waste gas - Google Patents

Method and device for extracting trifluoromethane from trifluoromethane waste gas Download PDF

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Publication number
CN115650822A
CN115650822A CN202211527223.4A CN202211527223A CN115650822A CN 115650822 A CN115650822 A CN 115650822A CN 202211527223 A CN202211527223 A CN 202211527223A CN 115650822 A CN115650822 A CN 115650822A
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trifluoromethane
tower
waste gas
finished product
extracting
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CN202211527223.4A
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侯绪芬
巩向金
王伟
崔坤伟
甘明哲
王鑫
崔安刚
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Shandong Dongyue Chemical Co ltd
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Shandong Dongyue Chemical Co ltd
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Abstract

The invention belongs to the technical field of trifluoromethane waste gas utilization, and particularly relates to a method and a device for extracting trifluoromethane from trifluoromethane waste gas. The method for extracting the trifluoromethane comprises the following steps: (1) Introducing the trifluoromethane waste gas into a buffer tank for buffering, and then introducing the trifluoromethane waste gas into a compressor for pressurizing; (2) And after the pressurized trifluoromethane waste gas enters an oil separator and is separated, the pressurized trifluoromethane waste gas enters a degassing tower from an upper feed inlet, the discharge of the bottom of the degassing tower is carried out to a rectifying tower, after the trifluoromethane is rectified in the rectifying tower, a trifluoromethane finished product with the purity of over 99.9 percent is discharged from the top of the rectifying tower to a finished product condenser for condensation, and the condensed liquid-phase trifluoromethane enters a finished product tank. The method has the advantages of low investment cost, short flow, simple operation, no introduction of other raw materials, conversion of the trifluoromethane from the production waste gas into the finished product, purity of over 99.9 percent and utilization of fluorine resources.

Description

Method and device for extracting trifluoromethane from trifluoromethane waste gas
Technical Field
The invention belongs to the technical field of trifluoromethane waste gas utilization, and particularly relates to a method and a device for extracting trifluoromethane from trifluoromethane waste gas.
Background
Trifluoromethane (R23) is a by-product of the process for the production of dichlorochloromethane (R22) and is a greenhouse gas (GWP value 14800). At present, the R23 industrial treatment method mainly comprises incineration and plasma treatment, but the treatment cost and equipment investment are high, and a large amount of fluorine resources are wasted. If the compound can be reasonably utilized, such as converted into a product or other useful compounds, not only has important economic benefits, but also solves the problem of environmental pollution.
Patent CN111960916A provides a method for implementing R23 resource utilization by using R23 as raw material and fluorinating chloroalkane in the presence of catalyst. Patent CN107216233A provides a method for utilizing R23 resources, which is to prepare important fluorine-containing monomers such as tetrafluoroethylene, hexafluoropropylene and the like with high added value by subjecting R23 to gas phase reaction cracking without using a catalyst. The common problem in the prior R23 resource utilization technology is that the cracking temperature is high and the number of byproducts is large.
Patent CN209721995U provides a refining plant of accessory substance R23 that produces in the purification recovery R22 industrial production, absorb through hydrochloric acid absorption tower, in the gas holder of keeping in after processing through water scrubber, caustic wash tower in proper order, the gas in the gas holder gets the R23 crude product through getting into the compression piece-rate system after cooling drying system handles again, R23 produces the R23 product after the rectification system is gone through to the R23 crude product, but the flow is comparatively complicated, involve multiple equipment.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method and the device for extracting the trifluoromethane from the trifluoromethane waste gas have the advantages of low investment cost, short flow, simple operation, no introduction of other raw materials, conversion of the trifluoromethane from the production waste gas into a finished product, purity of over 99.9 percent and utilization of fluorine resources.
The method for extracting the trifluoromethane from the trifluoromethane waste gas comprises the following steps:
(1) Conveying the trifluoromethane waste gas to a compressor through a pipeline for pressurization;
(2) And after the pressurized trifluoromethane waste gas enters an oil separator and is separated, the pressurized trifluoromethane waste gas enters a degassing tower from an upper feed inlet, the discharge of the bottom of the degassing tower is carried out to a rectifying tower, after the trifluoromethane is rectified in the rectifying tower, a trifluoromethane finished product with the purity of over 99.9 percent is discharged from the top of the rectifying tower to a finished product condenser for condensation, and the condensed liquid-phase trifluoromethane enters a finished product tank.
In the present invention, the components of the trifluoromethane exhaust gas mainly include trifluoromethane, nitrogen, oxygen, carbon monoxide, carbon dioxide, methane, hydrogen fluoride, chlorotrifluoromethane, bromotrifluoromethane, monochlorodifluoromethane, dichlorodifluoromethane and water.
In the step (1), the pressure of the trifluoromethane waste gas is increased to 2.0 to 4.3MPa through a compressor.
In the step (2), the pressure of the degassing tower is 2.0 to 4.3MPa, the temperature of a tower kettle is 10 to 25 ℃, the temperature of a tower top is 0 to 25 ℃, and the liquid level is 400 to 720mm.
In the step (2), the pressure of the rectifying tower is 2.0 to 4.3MPa, the temperature of the tower kettle is 30 to 75 ℃, the temperature of the tower top is 0 to 25 ℃, and the liquid level is 600 to 960mm.
In the step (2), the degassing tower, the rectifying tower and the finished product condenser are all condensed by saline water with the temperature of minus 10 to minus 15 ℃.
In the step (2), the pressure of the finished product tank is less than or equal to 3.0MPa, and the liquid level is less than or equal to 1800mm.
Discharging light components (nitrogen, oxygen, carbon monoxide, carbon dioxide, methane and the like) in the waste gas through the top of the degassing tower; and discharging heavy components (trifluoromonochloromethane, trifluoromonobromomethane, difluoromonochloromethane, difluorodichloromethane, hydrogen fluoride, water and the like) in the waste gas through the tower kettle of the rectifying tower.
The device for extracting the trifluoromethane from the trifluoromethane waste gas comprises a compressor, an oil separator, a degassing tower, a rectifying tower, a finished product condenser and a finished product tank which are sequentially connected.
The compressor is connected with a trifluoromethane waste gas inlet pipe, and the finished product groove is connected with a trifluoromethane finished product discharge pipe.
And the top of the degassing tower is connected with a non-condensing exhaust pipe.
And the bottom of the rectifying tower is connected with a heavy component discharge pipe.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method and a device for extracting trifluoromethane from trifluoromethane waste gas, which have the advantages of low investment cost, short flow, simple operation and no introduction of other raw materials, converts the trifluoromethane from the production waste gas into a finished product, ensures that the purity is over 99.9 percent, utilizes fluorine resources, reduces the incineration treatment cost, is green and environment-friendly, and ensures that the trifluoromethane waste gas is recycled.
Drawings
FIG. 1 is a schematic view of an apparatus for extracting trifluoromethane from trifluoromethane waste gas according to the present invention;
in the figure: 1. a compressor; 2. an oil separator; 3. a degassing tower; 4. a rectifying tower; 5. a finished product condenser; 6. a finished product groove; 7. a trifluoromethane waste gas inlet pipe; 8. the exhaust pipe is not condensed; 9. a heavies discharge pipe; 10. and a finished trifluoromethane product discharge pipe.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
As shown in fig. 1, the apparatus for extracting trifluoromethane from trifluoromethane waste gas according to the present invention comprises a compressor 1, an oil separator 2, a degassing tower 3, a rectifying tower 4, a finished product condenser 5 and a finished product tank 6, which are connected in sequence; the compressor 1 is connected with a trifluoromethane waste gas inlet pipe 7, and the finished product groove 6 is connected with a trifluoromethane finished product discharge pipe 10; the top of the degassing tower 3 is connected with a non-condensing exhaust pipe 8; the bottom of the rectifying tower 4 is connected with a heavy component discharge pipe 9.
Example 2
The apparatus of example 1 was used to extract trifluoromethane from trifluoromethane off-gas by the following method:
the original R23 crude gas entering the incinerator for treatment is conveyed to a compressor for pressurization, and the outlet pressure of the compressor is controlled to be 2.0MPa. The pressurized R23 crude product enters an oil separator for separation, and then is discharged from the upper part to enter a degassing tower, the pressure of the degassing tower is controlled at 2.0MPa, the internal temperature of a tower kettle is controlled at 25 ℃, the temperature of the top of the tower is controlled at 10 ℃, and the liquid level of the tower kettle is controlled at 600mm. When the liquid level of the kettle of the degassing tower reaches 400mm, a discharge valve at the bottom of the degassing tower is opened, the material is stably supplied to the rectifying tower, the top of the degassing tower is opened for exhausting, and a discharge valve at the top of the degassing tower is opened. Discharging from the bottom of the degassing tower to a rectifying tower, performing mass and heat transfer exchange in the rectifying tower, controlling the pressure of the rectifying tower at 2.0MPa, the internal temperature of the tower kettle at 35 ℃, and the temperature of the top of the tower at 10 ℃. When the liquid level of the rectifying tower is 600mm, steam is started, the top of the rectifying tower discharges to a finished product condenser for condensation, and the condensed liquid-phase material enters an R23 finished product groove.
Wherein, the degassing tower, the rectifying tower and the finished product condenser are all condensed by brine with the temperature of minus 10 ℃, the temperature and the pressure in the tower are controlled within the specified range, and the components at the top of the tower are sampled and analyzed to obtain the R23 finished product with the purity of 99.95 percent.
Example 3
The apparatus of example 1 was used to extract trifluoromethane from trifluoromethane off-gas by the following method:
the original R23 crude gas entering the incinerator for treatment is conveyed to a compressor for pressurization, and the outlet pressure of the compressor is controlled to be 3.0MPa. And (3) separating the pressurized R23 crude product in an oil separator, discharging from the upper part, and feeding into a degassing tower, wherein the pressure of the degassing tower is controlled at 3.0MPa, the internal temperature of a tower kettle is controlled at 10 ℃, the temperature of the top of the tower is controlled at 0 ℃, and the liquid level of the tower kettle is controlled at 720mm. When the liquid level of the kettle of the degassing tower reaches 400mm, a discharge valve at the bottom of the degassing tower is opened to stably supply materials to the rectifying tower, and a discharge valve at the top of the degassing tower is opened to exhaust gases. Discharging from the bottom of the degassing tower to a rectifying tower, performing mass and heat transfer exchange in the rectifying tower, controlling the pressure of the rectifying tower at 3.0MPa, the internal temperature of the tower kettle at 55 ℃, and the temperature at the top of the tower at 0 ℃. When the liquid level of the rectifying tower is 650mm, steam is started, the top of the rectifying tower discharges to a finished product condenser for condensation, and the condensed liquid-phase material enters an R23 finished product tank.
Wherein, the degassing tower, the rectifying tower and the finished product condenser are all condensed by brine with the temperature of-15 ℃, the temperature and the pressure in the tower are controlled within the specified range, and the components at the top of the tower are sampled and analyzed to obtain the R23 finished product with the purity of 99.92 percent.
Example 4
The apparatus of example 1 was used to extract trifluoromethane from trifluoromethane off-gas by the following method:
original R23 crude gas entering the incinerator for treatment is switched to a buffer tank for buffering, then enters a compressor for pressurization, and the outlet pressure of the compressor is controlled to be 4.3MPa. The pressurized R23 crude product enters an oil separator for separation, and then is discharged from the upper part to enter a degassing tower, the pressure of the degassing tower is controlled to be 4.3MPa, the internal temperature of a tower kettle is controlled to be 20 ℃, the temperature of the top of the tower is controlled to be 15 ℃, and the liquid level of the tower kettle is controlled to be 700mm. When the liquid level of the kettle of the degassing tower reaches 400mm, a discharge valve at the bottom of the degassing tower is opened, the material is stably supplied to the rectifying tower, the top of the degassing tower is opened for exhausting, and a discharge valve at the top of the degassing tower is opened. Discharging from the bottom of the degassing tower to a rectifying tower, performing mass and heat transfer exchange in the rectifying tower, controlling the pressure of the rectifying tower at 4.3MPa, the internal temperature of the tower kettle at 75 ℃ and the temperature of the top of the tower at 20 ℃. When the liquid level of the rectifying tower is 600mm, steam is started, the top of the rectifying tower discharges to a finished product condenser for condensation, and the condensed liquid-phase material enters an R23 finished product groove.
Wherein, the degassing tower, the rectifying tower and the finished product condenser are all condensed by brine with the temperature of-12 ℃, the temperature and the pressure in the tower are controlled within the specified range, and the components at the top of the tower are sampled and analyzed to obtain the R23 finished product with the purity of 99.96 percent.
Example 5
The apparatus of example 1 was used to extract trifluoromethane from trifluoromethane off-gas by the following method:
original R23 crude product gas entering the incinerator for treatment is switched to a buffer tank for buffering, then enters a compressor for pressurization, and the outlet pressure of the compressor is controlled to be 4.3MPa. The pressurized R23 crude product enters an oil separator, is separated, and then is discharged from the upper part to enter a degassing tower, wherein the pressure of the degassing tower is controlled at 4.3MPa, the internal temperature of a tower kettle is controlled at 25 ℃, the temperature of the top of the tower is controlled at 25 ℃, and the liquid level of the tower kettle is controlled at 600mm. When the liquid level of the kettle of the degassing tower reaches 400mm, a discharge valve at the bottom of the degassing tower is opened to stably supply materials to the rectifying tower, and a discharge valve at the top of the degassing tower is opened to exhaust gases. Discharging from the bottom of the degassing tower to a rectifying tower, performing mass and heat transfer exchange in the rectifying tower, controlling the pressure of the rectifying tower at 4.3MPa, the internal temperature of the tower kettle at 45 ℃ and the temperature of the top of the tower at 25 ℃. When the liquid level of the rectifying tower is 800mm, steam is started, the top of the rectifying tower discharges to a finished product condenser for condensation, and the condensed liquid-phase material enters an R23 finished product tank.
Wherein, the degassing tower, the rectifying tower and the finished product condenser are all condensed by brine with the temperature of 15 ℃ below zero, the temperature and the pressure in the tower are controlled within the specified range, and the components at the top of the tower are sampled and analyzed to obtain the R23 finished product with the purity of 99.95 percent.
Example 6
The apparatus of example 1 was used to extract trifluoromethane from trifluoromethane off-gas by the following method:
original R23 crude gas entering the incinerator for treatment is switched to a buffer tank for buffering, then enters a compressor for pressurization, and the outlet pressure of the compressor is controlled to be 4.3MPa. The pressurized R23 crude product enters an oil separator, is separated, and then is discharged from the upper part to enter a degassing tower, wherein the pressure of the degassing tower is controlled at 4.3MPa, the internal temperature of a tower kettle is controlled at 25 ℃, the temperature of the top of the tower is controlled at 10 ℃, and the liquid level of the tower kettle is controlled at 600mm. When the liquid level of the kettle of the degassing tower reaches 400mm, a discharge valve at the bottom of the degassing tower is opened to stably supply materials to the rectifying tower, and a discharge valve at the top of the degassing tower is opened to exhaust gases. Discharging from the bottom of the degassing tower to a rectifying tower, performing mass and heat transfer exchange in the rectifying tower, controlling the pressure of the rectifying tower at 4.3MPa, the internal temperature of the tower kettle at 55 ℃, and the temperature at the top of the tower at 10 ℃. When the liquid level of the rectifying tower is 960mm, steam is started, the top of the rectifying tower is discharged to a finished product condenser for condensation, and the condensed liquid-phase material enters an R23 finished product tank.
Wherein, the degassing tower, the rectifying tower and the finished product condenser are all condensed by brine with the temperature of minus 10 ℃, the temperature and the pressure in the tower are controlled within the specified range, and the components at the top of the tower are sampled and analyzed to obtain the R23 finished product with the purity of 99.97 percent.

Claims (9)

1. A method for extracting trifluoromethane from trifluoromethane waste gas is characterized in that: the method comprises the following steps:
(1) Conveying the trifluoromethane waste gas to a compressor through a pipeline for pressurization;
(2) And after the pressurized trifluoromethane waste gas enters an oil separator and is separated, the pressurized trifluoromethane waste gas enters a degassing tower from an upper feed inlet, the discharge of the bottom of the degassing tower is carried out to a rectifying tower, after the trifluoromethane is rectified in the rectifying tower, a trifluoromethane finished product with the purity of over 99.9 percent is discharged from the top of the rectifying tower to a finished product condenser for condensation, and the condensed liquid-phase trifluoromethane enters a finished product tank.
2. The method for extracting trifluoromethane from trifluoromethane off-gas according to claim 1, wherein the method comprises the steps of: in the step (1), the pressure of the trifluoromethane waste gas is increased to 2.0 to 4.3MPa by a compressor.
3. The method for extracting trifluoromethane from trifluoromethane off-gas according to claim 1, wherein the method comprises the steps of: in the step (2), the pressure of the degassing tower is 2.0 to 4.3MPa, the temperature of the tower kettle is 10 to 25 ℃, the temperature of the tower top is 0 to 25 ℃, and the liquid level is 400 to 720mm.
4. The method of extracting trifluoromethane from trifluoromethane off-gas according to claim 1, wherein: in the step (2), the pressure of the rectifying tower is 2.0 to 4.3MPa, the temperature of the tower kettle is 30 to 75 ℃, the temperature of the tower top is 0 to 25 ℃, and the liquid level is 600 to 960mm.
5. The method of extracting trifluoromethane from trifluoromethane off-gas according to claim 1, wherein: in the step (2), the degassing tower, the rectifying tower and the finished product condenser are all condensed by saline water with the temperature of minus 10 to minus 15 ℃.
6. A device for extracting trifluoromethane from trifluoromethane waste gas is characterized in that: comprises a compressor (1), an oil separator (2), a degassing tower (3), a rectifying tower (4), a finished product condenser (5) and a finished product tank (6) which are connected in sequence.
7. The apparatus for extracting trifluoromethane from trifluoromethane off-gas according to claim 6, wherein: the compressor (1) is connected with a trifluoromethane waste gas inlet pipe (7), and the finished product groove (6) is connected with a trifluoromethane finished product discharge pipe (10).
8. The apparatus for extracting trifluoromethane from trifluoromethane off-gas according to claim 6, wherein: and the top of the degassing tower (3) is connected with a noncondensable exhaust pipe (8).
9. The apparatus for extracting trifluoromethane from trifluoromethane off-gas according to claim 6, wherein: and the bottom of the rectifying tower (4) is connected with a heavy component discharge pipe (9).
CN202211527223.4A 2022-12-01 2022-12-01 Method and device for extracting trifluoromethane from trifluoromethane waste gas Withdrawn CN115650822A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100999437A (en) * 2006-12-22 2007-07-18 山东东岳化工有限公司 Recovery method of trifluoromethane
CN102101651A (en) * 2011-01-19 2011-06-22 山东东岳化工有限公司 Method and device for refining chlorine hydride byproduct and recovering trifluoromethane in production of monochlorodifluoromethane
CN114133314A (en) * 2021-11-02 2022-03-04 山东东岳化工有限公司 Purification device and purification process for electronic-grade trifluoromethane

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100999437A (en) * 2006-12-22 2007-07-18 山东东岳化工有限公司 Recovery method of trifluoromethane
CN102101651A (en) * 2011-01-19 2011-06-22 山东东岳化工有限公司 Method and device for refining chlorine hydride byproduct and recovering trifluoromethane in production of monochlorodifluoromethane
CN114133314A (en) * 2021-11-02 2022-03-04 山东东岳化工有限公司 Purification device and purification process for electronic-grade trifluoromethane

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Application publication date: 20230131