CN116443826A - System for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride - Google Patents
System for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride Download PDFInfo
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- CN116443826A CN116443826A CN202310466877.9A CN202310466877A CN116443826A CN 116443826 A CN116443826 A CN 116443826A CN 202310466877 A CN202310466877 A CN 202310466877A CN 116443826 A CN116443826 A CN 116443826A
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- tower
- pipeline
- absorption tower
- desorption
- solvent
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- QKCGXXHCELUCKW-UHFFFAOYSA-N n-[4-[4-(dinaphthalen-2-ylamino)phenyl]phenyl]-n-naphthalen-2-ylnaphthalen-2-amine Chemical compound C1=CC=CC2=CC(N(C=3C=CC(=CC=3)C=3C=CC(=CC=3)N(C=3C=C4C=CC=CC4=CC=3)C=3C=C4C=CC=CC4=CC=3)C3=CC4=CC=CC=C4C=C3)=CC=C21 QKCGXXHCELUCKW-UHFFFAOYSA-N 0.000 title claims abstract description 61
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000012535 impurity Substances 0.000 title claims abstract description 22
- 238000010521 absorption reaction Methods 0.000 claims abstract description 84
- 239000002904 solvent Substances 0.000 claims abstract description 66
- 238000003795 desorption Methods 0.000 claims abstract description 53
- 238000003860 storage Methods 0.000 claims abstract description 14
- 238000011084 recovery Methods 0.000 claims abstract description 10
- 238000007599 discharging Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 abstract description 8
- 238000010924 continuous production Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 239000006096 absorbing agent Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- GVGCUCJTUSOZKP-UHFFFAOYSA-N nitrogen trifluoride Chemical compound FN(F)F GVGCUCJTUSOZKP-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/083—Compounds containing nitrogen and non-metals and optionally metals containing one or more halogen atoms
- C01B21/0832—Binary compounds of nitrogen with halogens
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention discloses a system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride, and belongs to the technical field of nitrogen trifluoride preparation. The technical proposal is as follows: comprises an absorption tower and a desorption rectifying tower which are connected through pipelines; the absorption tower is connected with an absorption tower feeding pipeline carbon tetrafluoride and light component discharge pipeline and solvent inlet absorption tower pipeline; a diaphragm compressor is arranged on the feeding pipe of the absorption tower and is connected with the feeding pipe of the compressor, and an absorption tower top condenser is arranged at the top of the absorption tower; the desorption rectifying tower is provided with a desorption rectifying tower top condenser, a solvent recovery pipeline and a desorption rectifying tower reboiler, the desorption rectifying tower top condenser is connected with a nitrogen trifluoride discharging pipeline, one end of the solvent recovery pipeline, which is far away from the desorption rectifying tower, is connected with a solvent storage tank, and an outlet of the solvent storage tank is communicated with a solvent inlet absorption tower pipeline. The method can realize industrialized continuous production for removing carbon tetrafluoride as an impurity in nitrogen trifluoride.
Description
Technical Field
The invention relates to the technical field of nitrogen trifluoride preparation, in particular to a system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride.
Background
The purity of the main stream nitrogen trifluoride in the current market is 4.6N purity (NF 3 is more than or equal to 99.996VOL, and CF4 is less than 30 ppmv), and as the semiconductor chip continuously breaks through and advances forward, especially breaks through the process of 7nm to 5nm and 3nm, the 4.6N grade nitrogen trifluoride can not meet the chip supporting requirement, so that the reject ratio is greatly improved. In the panel industry as well, NF3 purity requirements are increasing as OLED screens mature in technology and are being popularized on a large scale.
The main impurity affecting the purity of nitrogen trifluoride is carbon tetrafluoride, which is difficult to separate by conventional rectification methods because it differs from nitrogen trifluoride by 1 ℃ in boiling point and the mixture of the two forms an azeotrope over a wide temperature and pressure range. The reduction of the carbon tetrafluoride content in nitrogen trifluoride is the key for improving the purity of nitrogen trifluoride, which is also the key point of technical attack of nitrogen trifluoride manufacturers at home and abroad.
Regarding the method for separating the carbon tetrafluoride impurity from the nitrogen trifluoride, various enterprises at home and abroad are researching and developing different schemes and publishing related literature data, but no report on practical industrial application exists.
Disclosure of Invention
The invention provides a system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride, which can realize industrialized continuous production for removing the impurity carbon tetrafluoride in the nitrogen trifluoride, break through the production technology of the high-purity nitrogen trifluoride, realize large-scale production of the high-purity nitrogen trifluoride, reduce the content of the impurity carbon tetrafluoride in the nitrogen trifluoride to within 3ppmv, and maximally receive raw material gas with the CF4 content within 2500 ppmv.
The technical scheme of the invention is as follows: a system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride comprises an absorption tower and a desorption rectifying tower which are connected through pipelines; the absorption tower is connected with an absorption tower feeding pipeline, a carbon tetrafluoride and light component discharge pipeline and a solvent inlet absorption tower pipeline; a diaphragm compressor is arranged on the feeding pipe of the absorption tower and is connected with the feeding pipe of the compressor, and an absorption tower top condenser is arranged at the top of the absorption tower; the desorption rectifying tower is provided with a desorption rectifying tower top condenser, a solvent recovery pipeline and a desorption rectifying tower reboiler, the desorption rectifying tower top condenser is connected with a nitrogen trifluoride discharging pipeline, one end of the solvent recovery pipeline, which is far away from the desorption rectifying tower, is connected with a solvent storage tank, an outlet of the solvent storage tank is communicated with a solvent inlet absorption tower pipeline through a solvent circulating pump inlet pipeline, and a solvent circulating pump is arranged on the solvent inlet absorption tower pipeline.
Preferably, the absorption tower kettle adopts a horizontal tower kettle, and a tube array heat exchanger is arranged in the tower kettle.
Preferably, the absorption tower feeding pipeline is arranged in the middle of the absorption tower body, and the solvent feeding pipeline is arranged at the upper part of the absorption tower body.
Preferably, the device further comprises a controller and a flowmeter, wherein the flowmeter is arranged on the feeding pipeline of the absorption tower and the solvent feeding pipeline of the absorption tower, and the flowmeter is electrically connected with the controller.
Preferably, the desorption rectifying tower top condenser is arranged at the tower top position of the desorption rectifying tower, and the desorption rectifying tower reboiler is arranged at the tower bottom position of the desorption rectifying tower.
Preferably, the top and the bottom of the absorption tower and the top and the bottom of the desorption rectifying tower are provided with pressure transmitters, and the pressure transmitters are electrically connected with a controller and used for monitoring the pressure of the top and the bottom of the absorption tower.
Preferably, the absorption tower, the desorption rectifying tower and the solvent storage tank are all provided with liquid level transmitters, and the liquid level transmitters are electrically connected with the controller and used for monitoring liquid level changes in the absorption tower and the desorption rectifying tower.
Preferably, a temperature sensor is arranged on the tower body of the absorption tower and the desorption rectifying tower, and the temperature sensor is electrically connected with the controller and is used for monitoring the temperature distribution and change of each packing layer in the absorption tower and the desorption rectifying tower.
Preferably, the method further comprises an absorption tower solvent self-circulation pipeline, wherein the absorption tower solvent circulation pipeline is connected with the inlet of the solvent circulation pump.
Compared with the prior art, the invention has the following beneficial effects:
1. the removal of carbon tetrafluoride as an impurity in nitrogen trifluoride can be realized, and industrial large-scale production can be realized;
the purity of the produced nitrogen trifluoride can reach 5.5N purity (the nitrogen trifluoride is more than or equal to 99.9995 percent vol and the CF4 is less than or equal to 3 ppmv);
2. the system can receive and process crude nitrogen trifluoride product with serious exceeding carbon tetrafluoride, and the purity of the processed nitrogen trifluoride product can reach the purity standard of 5.5N; the method is used in combination with the existing nitrogen trifluoride production system, can be used for recycling high carbon tetrafluoride materials under abnormal conditions, improves the production yield of nitrogen trifluoride and reduces the production cost;
3. compared with other schemes, the invention has high automation degree and lower running cost.
Drawings
Fig. 1 is a schematic structural view of the present invention.
In the figure, 1, a compressor feed line; 2. a diaphragm compressor; 3. a feed line to the absorber; 4. an absorption tower; 5. an absorber overhead condenser; 6. solvent enters the absorption tower pipeline; 7. carbon tetrafluoride and light component discharge line; 8. a solvent circulation pump; 9. a solvent self-circulation pipeline of the absorption tower; 10. a solvent circulation cooler; 11. an inlet line of a solvent circulation pump; 12. a solvent storage tank; 13. a desorption rectifying tower; 14. a condenser at the top of the desorption rectification column; 15. nitrogen trifluoride discharge line; 16. a desorption rectifying tower reboiler; 17. solvent recovery line.
Detailed Description
Example 1
As shown in fig. 1, the present embodiment provides a system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride, comprising an absorption column 4 and a desorption rectifying column 13 which are connected by a pipeline; the tower kettle of the absorption tower 4 adopts a horizontal tower kettle, and a tubular heat exchanger is arranged in the tower kettle; the absorption tower 4 is connected with an absorption tower feeding pipeline 3, a carbon tetrafluoride and light component discharge pipeline 7 and a solvent feeding absorption tower pipeline 6; the absorption tower feeding pipeline 3 is arranged in the middle of the absorption tower body, and the solvent feeding absorption tower pipeline 6 is arranged at the upper part of the absorption tower 4; the absorption tower feeding pipeline 3 is provided with a diaphragm compressor 2, the diaphragm compressor 2 is connected with the compressor feeding pipeline 1, and the top of the absorption tower 4 is provided with an absorption tower top condenser 5; the desorption rectifying tower 13 is provided with a desorption rectifying tower top condenser 14, a solvent recovery pipeline 17 and a desorption rectifying tower reboiler 16, the desorption rectifying tower top condenser 14 is connected with a nitrogen trifluoride discharging pipeline 15, the desorption rectifying tower top condenser 14 is arranged at the tower top position of the desorption rectifying tower 13, and the desorption rectifying tower reboiler 16 is arranged at the tower bottom position of the desorption rectifying tower 13; one end of the solvent recovery pipeline 17, which is far away from the desorption rectifying tower 13, is connected with a solvent storage tank 12, an outlet of the solvent storage tank 12 is communicated with a solvent inlet absorption tower pipeline 6 through a solvent circulating pump inlet pipeline 11, and a solvent circulating pump 8 is arranged on the solvent inlet absorption tower pipeline 6;
the device also comprises a controller and a flowmeter, wherein the flowmeter is arranged on the absorption tower feeding pipeline 3 and the solvent feeding absorption tower pipeline 6, and the flowmeter is electrically connected with the controller; the tower top and the tower bottom of the absorption tower 4 and the tower top and the tower bottom of the desorption rectifying tower 13 are respectively provided with a pressure transmitter, and the pressure transmitters are electrically connected with a controller and are used for monitoring the pressure of the tower top and the tower bottom; the absorption tower 4, the desorption rectifying tower 13 and the solvent storage tank 12 are all provided with liquid level transmitters, and the liquid level transmitters are electrically connected with a controller and are used for monitoring the liquid level change in the absorption tower 4 and the desorption rectifying tower 13; a temperature sensor is arranged on the tower body of the absorption tower 4 and the desorption rectifying tower 13, and the temperature sensor is electrically connected with a controller and is used for monitoring the temperature distribution and change of each packing layer in the absorption tower 4 and the desorption rectifying tower 13; the absorption tower solvent self-circulation pipeline 9 is connected with the inlet of the solvent circulation pump 8 and is used for self-circulation of the absorption tower 4.
The working process comprises the following steps:
the nitrogen trifluoride containing carbon tetrafluoride impurity enters the absorption tower 4 from the middle position of the absorption tower 4 after entering the diaphragm compressor 2 through the compressor feeding pipeline 1 to be compressed and boosted, the solvent in the solvent storage tank 12 is firstly cooled to a certain temperature through the solvent circulating cooler 10 after being boosted by the solvent circulating pump 8, then enters the absorption tower 4 from the upper part of the absorption tower 4 to be sprayed, tower internals such as structured packing and a distributor are arranged in the absorption tower 4, after the mixture of carbon tetrafluoride and nitrogen trifluoride fully contacts with the solvent on the surface of the packing in the absorption tower 4, the carbon tetrafluoride and other impurities with lower boiling points are gradually collected at the top of the absorption tower 4 and are periodically discharged from the carbon tetrafluoride and light component discharge pipeline 7, the nitrogen trifluoride enters the tower kettle of the absorption tower 4 along with the solvent, the nitrogen trifluoride enters the desorption rectifying tower 13 through the pipeline to be separated, the nitrogen trifluoride is extracted from the tower kettle of the desorption rectifying tower 13, and the solvent without nitrogen trifluoride is recycled in the solvent storage tank 12 through the solvent recovery pipeline 17.
The system for preparing high-purity nitrogen trifluoride by adopting the continuous absorption, analysis and separation of impurity carbon tetrafluoride is used for preparing high-purity nitrogen trifluoride, the feed composition is shown in table 1, and the material data produced by a nitrogen trifluoride discharge line 15 is shown in table 2.
TABLE 1
TABLE 2
Example 2
Unlike example 1, the feed gas was different from example 1, the other conditions were exactly the same as in example 1, the feed composition was shown in Table 3, and the data of the material produced in nitrogen trifluoride discharge line 15 was shown in Table 4.
TABLE 3 Table 3
TABLE 4 Table 4
Example 3
Unlike example 1, the feed gas was different from example 1, the other conditions were exactly the same as in example 1, the feed composition was shown in Table 5, and the data of the material produced in nitrogen trifluoride discharge line 15 was shown in Table 6.
TABLE 5
TABLE 6
Example 4
Unlike example 1, the feed gas was different from example 1, the other conditions were exactly the same as in example 1, the feed composition was shown in Table 7, and the data of the material produced in nitrogen trifluoride discharge line 15 was shown in Table 8.
TABLE 7
TABLE 8
Example 5
Unlike example 1, the feed gas was different from example 1, the other conditions were exactly the same as in example 1, the feed composition was as shown in Table 9, and the data of the material produced in nitrogen trifluoride discharge line 15 was as shown in Table 10.
TABLE 9
Table 10
As shown in the tables 1-10, the system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride can receive and treat crude nitrogen trifluoride product with serious exceeding standard of carbon tetrafluoride, and multiple batches of nitrogen trifluoride gases with different CF4 contents are respectively injected, so that the purity of the produced nitrogen trifluoride can reach 5.5N purity (the nitrogen trifluoride is more than or equal to 99.9995%vol and the CF4 is less than or equal to 3 ppmv).
Although the present invention has been described in detail by way of preferred embodiments with reference to the accompanying drawings, the present invention is not limited thereto. Various equivalent modifications and substitutions for embodiments of the invention may be made by those skilled in the art without departing from the spirit and scope of the invention, and these modifications and substitutions are intended to be within the scope of the invention. Therefore, the protection scope of the invention is subject to the protection scope of the claims.
Claims (9)
1. The system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride is characterized by comprising an absorption tower (4) and a desorption rectifying tower (13) which are connected through pipelines;
the absorption tower (4) is connected with an absorption tower feeding pipeline (3), a carbon tetrafluoride and light component discharge pipeline (7) and a solvent feeding absorption tower pipeline (6); a diaphragm compressor (2) is arranged on the absorption tower feeding pipeline (3), the diaphragm compressor (2) is connected with the compressor feeding pipeline (1), and an absorption tower top condenser (5) is arranged at the top of the absorption tower (4);
the desorption rectifying tower (13) is provided with a desorption rectifying tower top condenser (14), a solvent recovery pipeline (17) and a desorption rectifying tower reboiler (16), the desorption rectifying tower top condenser (14) is connected with a nitrogen trifluoride discharging pipeline (15), one end, far away from the desorption rectifying tower (13), of the solvent recovery pipeline (17) is connected with a solvent storage tank (12), an outlet of the solvent storage tank (12) is communicated with a solvent inlet absorbing tower pipeline (6) through a solvent circulating pump inlet pipeline (11), and a solvent circulating pump (8) is arranged on the solvent inlet absorbing tower pipeline (6).
2. The system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride as claimed in claim 1, wherein a horizontal tower kettle is adopted as a tower kettle of the absorption tower (4), and a tube array heat exchanger is arranged in the tower kettle.
3. The system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride as claimed in claim 1, wherein the absorption tower feeding pipeline (3) is arranged in the middle of the tower body of the absorption tower (4), and the solvent feeding absorption tower pipeline (6) is arranged in the upper part of the tower body of the absorption tower (4).
4. The system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating carbon tetrafluoride as claimed in claim 1, further comprising a controller and a flowmeter, wherein the flowmeter is arranged on the absorption tower feeding pipeline (3) and the solvent feeding absorption tower pipeline (6), and the flowmeter is electrically connected with the controller.
5. The system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride as claimed in claim 4, wherein a desorption rectifying tower top condenser (14) is arranged at the tower top position of the desorption rectifying tower (13), and a desorption rectifying tower reboiler (16) is arranged at the tower bottom position of the desorption rectifying tower (13).
6. The system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating carbon tetrafluoride as claimed in claim 4, wherein the top and bottom of the absorbing tower (4) and the top and bottom of the stripping and rectifying tower (13) are provided with pressure transmitters, and the pressure transmitters are electrically connected with a controller.
7. The system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating carbon tetrafluoride as claimed in claim 4, wherein the absorption tower (4), the desorption rectifying tower (13) and the solvent storage tank (12) are all provided with liquid level transmitters, and the liquid level transmitters are electrically connected with the controller.
8. The system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating carbon tetrafluoride as claimed in claim 4, wherein a temperature sensor is arranged on the body of the absorption tower (4) and the desorption rectifying tower (13), and the temperature sensor is electrically connected with the controller.
9. The system for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride as claimed in claim 4, further comprising an absorption tower solvent self-circulation pipeline (9), wherein the absorption tower solvent circulation pipeline (9) is connected with an inlet of a solvent circulation pump (8).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310466877.9A CN116443826A (en) | 2023-04-27 | 2023-04-27 | System for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310466877.9A CN116443826A (en) | 2023-04-27 | 2023-04-27 | System for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride |
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| CN116443826A true CN116443826A (en) | 2023-07-18 |
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| CN202310466877.9A Pending CN116443826A (en) | 2023-04-27 | 2023-04-27 | System for preparing high-purity nitrogen trifluoride by continuously absorbing, resolving and separating impurity carbon tetrafluoride |
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|---|---|---|---|---|
| CN104587799A (en) * | 2015-01-26 | 2015-05-06 | 上海梅思泰克环境股份有限公司 | Device and method for processing complex organic waste gas components and recycling resources |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104587799A (en) * | 2015-01-26 | 2015-05-06 | 上海梅思泰克环境股份有限公司 | Device and method for processing complex organic waste gas components and recycling resources |
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