CN116081574A - Method for removing carbon dioxide in hydrogen chloride - Google Patents
Method for removing carbon dioxide in hydrogen chloride Download PDFInfo
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- CN116081574A CN116081574A CN202211504340.9A CN202211504340A CN116081574A CN 116081574 A CN116081574 A CN 116081574A CN 202211504340 A CN202211504340 A CN 202211504340A CN 116081574 A CN116081574 A CN 116081574A
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- Prior art keywords
- hydrogen chloride
- carbon dioxide
- nacl solution
- saturated nacl
- tower
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 74
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 57
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910000041 hydrogen chloride Inorganic materials 0.000 title claims abstract description 57
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 37
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 19
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 11
- 239000000460 chlorine Substances 0.000 claims abstract description 8
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 8
- -1 chlorine ions Chemical class 0.000 claims abstract description 8
- 238000010517 secondary reaction Methods 0.000 claims abstract description 8
- 239000002274 desiccant Substances 0.000 claims description 19
- 239000003463 adsorbent Substances 0.000 claims description 18
- 239000002808 molecular sieve Substances 0.000 claims description 17
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 17
- 229910021536 Zeolite Inorganic materials 0.000 claims description 15
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 15
- 239000010457 zeolite Substances 0.000 claims description 15
- 238000001179 sorption measurement Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 3
- 239000000428 dust Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical class [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000005247 gettering Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0718—Purification ; Separation of hydrogen chloride by adsorption
-
- 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
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Separation Of Gases By Adsorption (AREA)
- Drying Of Gases (AREA)
Abstract
The invention discloses a method for removing carbon dioxide in hydrogen chloride, which comprises the following steps: step one: after hydrogen chloride is filtered and compressed, the hydrogen chloride enters the bottom of a first-stage reaction tower filled with saturated NaCL solution, the saturated NaCL solution in the first-stage reaction tower is contacted with the first-stage reaction tower, and the chlorine ions are saturated in the solution, so that the hydrogen chloride can not be dissolved again, and carbon dioxide is fused into the saturated NaCL solution; step two: the hydrogen chloride filtered by the primary carbon dioxide enters the bottom of a secondary reaction tower filled with a saturated NaCL solution, the saturated NaCL solution in the secondary reaction tower is contacted with the saturated NaCL solution, and the chlorine ions are saturated in the solution, so that the hydrogen chloride can not be dissolved again, and the carbon dioxide is fused into the saturated NaCL solution; and step three. In the invention, the hydrogen chloride is contacted with the saturated NaCL solution in the first-stage reaction tower and the second-stage reaction tower, and the chloride ions are saturated in the solution, so that the hydrogen chloride can not be dissolved again, and the carbon dioxide is fused into the saturated NaCL solution.
Description
Technical Field
The invention relates to the technical field of hydrogen chloride processing, in particular to a method for removing carbon dioxide in hydrogen chloride.
Background
The electronic grade high-purity hydrogen chloride is an important material for processes such as silicon wafer etching, passivation, epitaxy, gas phase polishing, gettering and cleaning treatment in integrated circuit production, and can also be used in the fields of metal smelting, photoconductive communication, scientific research and the like. With the development of large-scale integrated circuits, the requirement on the purity of hydrogen chloride is higher and higher, and besides the purity of more than 99.999%, the requirement on the content of impurities in the hydrogen chloride is more and more severe, and particularly the content of hydrocarbon and carbon oxides is required to be strictly limited so as to prevent C from forming in the silicon wafer processing process. In the past, the China mostly imports electronic grade hydrogen chloride from countries such as America, japanese and the like, but in recent years, the development of chemical gases required by the electronic industry in China has not been broken through and developed in technology.
Disclosure of Invention
The present invention provides a method for removing carbon dioxide from hydrogen chloride to overcome the above-mentioned technical problems of the prior art.
The technical scheme of the invention is realized as follows:
according to one aspect of the present invention, a method for removing carbon dioxide from hydrogen chloride is provided.
The method for removing carbon dioxide in hydrogen chloride comprises the following steps:
step one: after hydrogen chloride is filtered and compressed, the hydrogen chloride enters the bottom of a first-stage reaction tower filled with saturated NaCL solution, the saturated NaCL solution in the first-stage reaction tower is contacted with the first-stage reaction tower, and the chlorine ions are saturated in the solution, so that the hydrogen chloride can not be dissolved again, and carbon dioxide is fused into the saturated NaCL solution;
step two: the hydrogen chloride filtered by the primary carbon dioxide enters the bottom of a secondary reaction tower filled with a saturated NaCL solution, the saturated NaCL solution in the secondary reaction tower is contacted with the saturated NaCL solution, and the chlorine ions are saturated in the solution, so that the hydrogen chloride can not be dissolved again, and the carbon dioxide is fused into the saturated NaCL solution;
step three: then, hydrogen chloride subjected to secondary filtration enters the bottom of a primary drying tower filled with a drying agent, and is subjected to adsorption to remove most of water, and then is discharged from the top of the tower to be subjected to deep dehydration;
step four: then, entering the bottom of a secondary drying tower, removing trace moisture, and then, discharging from the top of the tower, wherein the moisture content in the removed hydrogen chloride is less than 0.5ppm;
step five: then enters from the bottom of an adsorption tower 5 filled with the adsorbent, and comes out from the top of the tower after adsorbing and removing carbon dioxide and trace moisture, wherein the content of carbon dioxide after adsorption is less than 2ppm.
Wherein the drying agent in the third step and the fourth step and the adsorbent in the fifth step are zeolite molecular sieves.
Wherein the drying agent in the third step and the fourth step is a 13X zeolite molecular sieve, and the adsorbent in the fifth step is an SSZ-13 zeolite molecular sieve.
Wherein the drying agent in the third step and the fourth step and the adsorbent in the fifth step are treated by high-temperature chlorine gas at 200 ℃ for two hours.
Wherein, hydrogen chloride in the first step is filtered and compressed and then enters the first-stage reaction tower at the pressure of 0.3-0.6MPa and the normal temperature at the flow of 1-5M 3/h.
The beneficial effects are that:
in the invention, the hydrogen chloride is contacted with saturated NaCL solution in the first-stage reaction tower and the second-stage reaction tower, and the chloride ions are saturated in the solution, so that the hydrogen chloride can not be dissolved again, and the carbon dioxide is fused into the saturated NaCL solution;
the drying agent and the adsorbent used in the invention are treated by chlorine gas at the high temperature of 200 ℃ for 2 hours, so that the dust rate is reduced after the treatment, the strength is enhanced, and the drying and adsorption requirements can be met;
the adsorbent can be 5A, 13X, SSZ-13 zeolite molecular sieve and other adsorbents, preferably SSZ-13 zeolite molecular sieve, and SSZ-13 has good carbon dioxide adsorption performance and is easy to regenerate;
the drying agent of the invention can be a 3A, 5A, 13X type zeolite molecular sieve, preferably a 13X molecular sieve drying agent, which does not react with hydrogen chloride, has high water absorption capacity and enough strength, can not bring metal ions and dust into hydrogen chloride gas, and is easy to regenerate;
according to the water content of different raw material products and the purity requirement of the products, multistage physical drying can be arranged to fully remove the water in the raw materials.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a process flow diagram of a method for removing carbon dioxide from hydrogen chloride according to an embodiment of the invention;
fig. 2 is a schematic flow chart of the steps of a method for removing carbon dioxide from hydrogen chloride according to an embodiment of the invention.
In the figure:
1. a first-stage reaction tower; 2. a second-stage reaction tower; 3. a first-stage drying tower; 4. a first-stage drying tower; 5. an adsorption tower.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which are derived by a person skilled in the art based on the embodiments of the invention, fall within the scope of protection of the invention.
According to an embodiment of the present invention, a method for removing carbon dioxide from hydrogen chloride is provided.
As shown in fig. 1, a method for removing carbon dioxide from hydrogen chloride according to an embodiment of the present invention includes the following steps:
step S101, hydrogen chloride enters the bottom of a first-stage reaction tower 1 filled with saturated NaCL solution after being filtered and compressed, the saturated NaCL solution in the first-stage reaction tower 1 is contacted with the first-stage reaction tower, and the chlorine ions are saturated in the solution, so that the hydrogen chloride can not be dissolved any more, and carbon dioxide is fused into the saturated NaCL solution;
step S103, hydrogen chloride filtered by primary carbon dioxide enters the bottom of a secondary reaction tower 2 filled with saturated NaCL solution, the saturated NaCL solution in the secondary reaction tower 2 is contacted with the saturated NaCL solution, and the chlorine ions are saturated in the solution, so that the hydrogen chloride cannot be dissolved again, and the carbon dioxide is fused into the saturated NaCL solution;
step S105, step three: then, hydrogen chloride subjected to secondary filtration enters the bottom of a primary drying tower 3 filled with a drying agent, and is subjected to adsorption to remove most of water, and then is discharged from the top of the tower to be subjected to deep dehydration;
step S107, entering the bottom of the secondary drying tower 4, removing trace moisture, and then discharging from the top of the tower, wherein the moisture content in the removed hydrogen chloride is less than 0.5ppm;
step S109, entering from the bottom of the adsorption tower 5 filled with the adsorbent, adsorbing and removing carbon dioxide and trace moisture, and then exiting from the top of the tower, wherein the content of carbon dioxide after adsorption is less than 2ppm.
Wherein the drying agent in the third step and the fourth step and the adsorbent in the fifth step are zeolite molecular sieves.
Wherein the drying agent in the third step and the fourth step is a 13X zeolite molecular sieve, and the adsorbent in the fifth step is an SSZ-13 zeolite molecular sieve.
Wherein the drying agent in the third step and the fourth step and the adsorbent in the fifth step are treated by high-temperature chlorine gas at 200 ℃ for two hours.
Wherein, hydrogen chloride in the first step is filtered and compressed and then enters the first-stage reaction tower 1 at the pressure of 0.3-0.6MPa and the normal temperature at the flow rate of 1-5M 3/h.
In summary, by means of the above technical solution of the present invention, hydrogen chloride contacts with the saturated NaCL solution in both the first-stage reaction tower 1 and the second-stage reaction tower 2, and since chloride ions are saturated in the solution, hydrogen chloride cannot be dissolved any more, and carbon dioxide is dissolved into the saturated NaCL solution;
the drying agent and the adsorbent used in the invention are treated by chlorine gas at the high temperature of 200 ℃ for 2 hours, so that the dust rate is reduced after the treatment, the strength is enhanced, and the drying and adsorption requirements can be met;
the adsorbent can be 5A, 13X, SSZ-13 zeolite molecular sieve and other adsorbents, preferably SSZ-13 zeolite molecular sieve, and SSZ-13 has good carbon dioxide adsorption performance and is easy to regenerate;
the drying agent of the invention can be a 3A, 5A, 13X type zeolite molecular sieve, preferably a 13X molecular sieve drying agent, which does not react with hydrogen chloride, has high water absorption capacity and enough strength, can not bring metal ions and dust into hydrogen chloride gas, and is easy to regenerate;
according to the water content of different raw material products and the purity requirement of the products, multistage physical drying can be arranged to fully remove the water in the raw materials.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (5)
1. A method for removing carbon dioxide from hydrogen chloride, comprising:
step one: after hydrogen chloride is filtered and compressed, the hydrogen chloride enters the bottom of a first-stage reaction tower (1) filled with saturated NaCL solution, the saturated NaCL solution in the first-stage reaction tower (1) is contacted with the first-stage reaction tower, the chlorine ions are saturated in the solution, the hydrogen chloride can not be dissolved any more, and carbon dioxide is fused into the saturated NaCL solution;
step two: the hydrogen chloride filtered by the primary carbon dioxide enters the bottom of a secondary reaction tower (2) filled with a saturated NaCL solution, the saturated NaCL solution in the secondary reaction tower (2) is contacted with the saturated NaCL solution, and the chlorine ions are saturated in the solution, so that the hydrogen chloride can not be dissolved again, and the carbon dioxide is fused into the saturated NaCL solution;
step three: then, hydrogen chloride subjected to secondary filtration enters the bottom of a primary drying tower (3) filled with a drying agent, and is subjected to adsorption to remove most of water, and then is discharged from the top of the tower to be subjected to deep dehydration;
step four: then, entering the bottom of a secondary drying tower (4), removing trace moisture, and then, discharging from the top of the tower, wherein the moisture content in the removed hydrogen chloride is less than 0.5ppm;
step five: then enters from the bottom of an adsorption tower (5) filled with the adsorbent, and comes out from the top of the tower after adsorbing and removing carbon dioxide and trace moisture, wherein the content of carbon dioxide after adsorption is less than 2ppm.
2. The method of claim 1, wherein the desiccant in the third step, the desiccant in the fourth step, and the adsorbent in the fifth step are zeolite molecular sieves.
3. The method of claim 2, wherein the desiccant in both the third and fourth steps is a 13X zeolite molecular sieve and the adsorbent in the fifth step is an SSZ-13 zeolite molecular sieve.
4. A method for removing carbon dioxide from hydrogen chloride according to claim 3, wherein the drying agent in both of said third and fourth steps and the adsorbent in said fifth step are treated with high temperature chlorine gas at 200 ℃ for two hours.
5. The method for removing carbon dioxide from hydrogen chloride according to claim 4, wherein hydrogen chloride in said step one is filtered and compressed, and then enters the first-stage reaction tower at a flow rate of 1-5M 3/h under a pressure of 0.3-0.6MPa and at normal temperature.
Priority Applications (1)
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CN202211504340.9A CN116081574A (en) | 2022-11-28 | 2022-11-28 | Method for removing carbon dioxide in hydrogen chloride |
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CN202211504340.9A CN116081574A (en) | 2022-11-28 | 2022-11-28 | Method for removing carbon dioxide in hydrogen chloride |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106422656A (en) * | 2016-11-30 | 2017-02-22 | 广东广山新材料有限公司 | Hydrogen chloride gas purification method |
CN107324283A (en) * | 2017-07-07 | 2017-11-07 | 天津市职业大学 | A kind of method of recycling treatment iron-contained industrial waste hydrochloric acid |
CN108946772A (en) * | 2018-09-27 | 2018-12-07 | 山东泰和水处理科技股份有限公司 | A method of pure Lithium Carbonate is prepared by lithium ore |
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2022
- 2022-11-28 CN CN202211504340.9A patent/CN116081574A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106422656A (en) * | 2016-11-30 | 2017-02-22 | 广东广山新材料有限公司 | Hydrogen chloride gas purification method |
CN107324283A (en) * | 2017-07-07 | 2017-11-07 | 天津市职业大学 | A kind of method of recycling treatment iron-contained industrial waste hydrochloric acid |
CN108946772A (en) * | 2018-09-27 | 2018-12-07 | 山东泰和水处理科技股份有限公司 | A method of pure Lithium Carbonate is prepared by lithium ore |
Non-Patent Citations (3)
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廖清江: "《无机药物化学》", 30 April 1957, 人民卫生出版社, pages: 34 * |
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