CN116081574A - Method for removing carbon dioxide in hydrogen chloride - Google Patents

Method for removing carbon dioxide in hydrogen chloride Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
hydrogen chloride
carbon dioxide
nacl solution
saturated nacl
tower
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202211504340.9A
Other languages
Chinese (zh)
Inventor
李飞明
栗鹏伟
孙芳
邹小英
王睿燕
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Ruiheng Electronic Material Co ltd
Original Assignee
Zhejiang Ruiheng Electronic Material Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhejiang Ruiheng Electronic Material Co ltd filed Critical Zhejiang Ruiheng Electronic Material Co ltd
Priority to CN202211504340.9A priority Critical patent/CN116081574A/en
Publication of CN116081574A publication Critical patent/CN116081574A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00Halogens; Halogen acids
    • C01B7/01Chlorine; Hydrogen chloride
    • C01B7/07Purification ; Separation
    • C01B7/0706Purification ; Separation of hydrogen chloride
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00Halogens; Halogen acids
    • C01B7/01Chlorine; Hydrogen chloride
    • C01B7/07Purification ; Separation
    • C01B7/0706Purification ; Separation of hydrogen chloride
    • C01B7/0718Purification ; Separation of hydrogen chloride by adsorption
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02CCAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00Capture or disposal of greenhouse gases
    • Y02C20/40Capture 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

Method for removing carbon dioxide in hydrogen chloride
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.
CN202211504340.9A 2022-11-28 2022-11-28 Method for removing carbon dioxide in hydrogen chloride Pending CN116081574A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211504340.9A CN116081574A (en) 2022-11-28 2022-11-28 Method for removing carbon dioxide in hydrogen chloride

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211504340.9A CN116081574A (en) 2022-11-28 2022-11-28 Method for removing carbon dioxide in hydrogen chloride

Publications (1)

Publication Number Publication Date
CN116081574A true CN116081574A (en) 2023-05-09

Family

ID=86205338

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202211504340.9A Pending CN116081574A (en) 2022-11-28 2022-11-28 Method for removing carbon dioxide in hydrogen chloride

Country Status (1)

Country Link
CN (1) CN116081574A (en)

Citations (3)

* Cited by examiner, † Cited by third party
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Title
廖清江: "《无机药物化学》", 30 April 1957, 人民卫生出版社, pages: 34 *
杨宇: ""S+V"教学法构建及其在初三化学实验教学中的应用", 《中国优秀硕士学位论文全文数据库 社会科学Ⅱ辑》, 15 February 2023 (2023-02-15), pages 27 *
郑学裕: "抓好联系 促进生成", 《中学化学教学参考》, 10 October 2012 (2012-10-10), pages 37 *

Similar Documents

Publication Publication Date Title
TWI691359B (en) Method for pressure swing adsorption, purification and reuse of full-pressure waste hydrogen gas in semiconductor process
CN113353958B (en) Clean production process of hexafluorophosphate
EP1334758B1 (en) Gas separating and purifying method and its apparatus
CN114133314B (en) Purification device and purification process of electronic grade trifluoromethane
JP2023535850A (en) Separation of HF/HCl Containing Etching Exhaust Gas by FTrPSA and Recovery, Recycling and Reuse Method
KR101812532B1 (en) Purification process of nitrous oxide
CN112591711B (en) High-purity high-yield FTrPSA separation and purification extraction method for HF/HCl mixed gas
CN116081574A (en) Method for removing carbon dioxide in hydrogen chloride
CN116062756A (en) Process and device for preparing ultra-high purity carbonyl sulfide from industrial carbonyl sulfide
CN103626129A (en) Preparation method for electronic-grade high-purity chlorine from industrial liquid chlorine
CN216336618U (en) Recovery of CO from chemical process2System for preparing nitrogen from waste gas
JP2003246611A (en) Helium purifying apparatus
JP4132614B2 (en) Purification method of high purity NF3 gas
CN112758961B (en) Lithium chloride production process and system thereof
JPS6022919A (en) Pressure increasing method of adsorption tower in three-tower pressure swinging method
CN108190894B (en) acid washing circulation process of high-purity quartz sand
JPH0489387A (en) Inert gas recovering device for single crystal pulling up device
CN116459788B (en) Disilane purifying agent and preparation method and application thereof
CN114873568B (en) Electronic grade SF 6 Rectification pretreatment system
CN115722027A (en) Method and device for recovering nitrogen trifluoride from dry etching tail gas
CN221739920U (en) Ultra-high purity purification system for electronic grade semiconductor byproduct hydrogen
CN112624050B (en) FTrPSA separation and purification method for HCl gas containing low-concentration HF through deep defluorination and drying
JPS60156548A (en) Collecting agent of carbon monoxide and its manufacture
KR101952945B1 (en) Method for recorvering nitrous oxide
JPWO2022127019A5 (en)

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination