CN114470866B - Method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride - Google Patents
Method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride Download PDFInfo
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- CN114470866B CN114470866B CN202210092081.7A CN202210092081A CN114470866B CN 114470866 B CN114470866 B CN 114470866B CN 202210092081 A CN202210092081 A CN 202210092081A CN 114470866 B CN114470866 B CN 114470866B
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- fluoride
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- hydrogen fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/10—Oxidants
- B01D2251/108—Halogens or halogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/20—Halogens or halogen compounds
- B01D2257/204—Inorganic halogen compounds
- B01D2257/2047—Hydrofluoric acid
Abstract
The invention discloses a method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride, which comprises the following steps: firstly, pumping negative pressure of a mixing kettle, then introducing a crude trifluoromethanesulfonyl fluoride liquid, and adding an extracting agent to obtain a mixture; introducing nitrogen into the mixing kettle, then transferring the mixture into a rectifying tower for rectification, discharging heavy component impurities, and distilling out light component trifluoromethanesulfonyl fluoride; then introducing the evaporated light component trifluoromethanesulfonyl fluoride into an adsorption tower to be adsorbed by adopting an adsorbent to obtain a refined trifluoromethanesulfonyl fluoride gas, and condensing the refined trifluoromethanesulfonyl fluoride gas into liquid in a refined tank. In the invention, the extracting agent is adopted, and the relative volatility between the hydrogen fluoride and the trifluoromethanesulfonyl fluoride is changed by utilizing the action between the hydrogen fluoride and the extracting agent, so that most of the hydrogen fluoride can be removed; after the rectification process, the content of hydrogen fluoride in the trifluoromethanesulfonyl fluoride is low, and the hydrogen fluoride is removed by using the adsorbent, so that collapse of the adsorbent is avoided.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride.
Background
The crude trifluoromethanesulfonyl fluoride liquid usually contains hydrogen fluoride impurities, and the trifluoromethanesulfonyl fluoride and the hydrogen fluoride can form an azeotrope, so that the hydrogen fluoride cannot be removed cleanly by the traditional rectification method. And because the crude trifluoromethanesulfonyl fluoride liquid contains high content of hydrogen fluoride, the adsorbent is directly adopted to adsorb the hydrogen fluoride, so that the collapse of the adsorbent is caused. Therefore, it is important to develop a method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride, which overcomes the shortcomings of the prior art. The method utilizes the action between the hydrogen fluoride and the extracting agent, thereby changing the relative volatility between the hydrogen fluoride and the trifluoromethanesulfonyl fluoride, removing most of the hydrogen fluoride and facilitating the subsequent rectification process.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride, which is characterized by comprising the following steps:
s1, firstly, pumping negative pressure of a mixing kettle, then transferring crude trifluoromethanesulfonyl fluoride liquid in a crude product tank into the mixing kettle, adding an extracting agent, and stirring at the temperature of-40 ℃ to-25 ℃ to obtain a mixture;
s2, introducing nitrogen into the mixing kettle in the S1, pressing the mixture obtained in the S1 into a rectifying tower for rectification, evaporating out light component trifluoromethanesulfonyl fluoride, discharging heavy component impurities into a hydrogen fluoride recovery tank, wherein the temperature of the tower kettle of the rectifying tower is 10-30 ℃, the temperature of a rectifying column is 5-19 ℃, and the reflux ratio is 5-10;
and S3, introducing the light component trifluoromethanesulfonyl fluoride steamed out in the S2 into an adsorption tower, adsorbing by an adsorbent to obtain refined trifluoromethanesulfonyl fluoride gas with the hydrogen fluoride content of less than or equal to 20ppm, and introducing the refined trifluoromethanesulfonyl fluoride gas into a refined tank to be condensed into liquid.
Preferably, the mass fraction of the hydrogen fluoride in the crude trifluoromethanesulfonyl fluoride liquid in S1 is 5wt% to 10wt%.
Preferably, the negative pressure in S1 is-0.07 MPa to-0.01 MPa.
Preferably, the dosage ratio of the crude trifluoromethanesulfonyl fluoride liquid to the extracting agent in the mixture in S1 is 100mL: (2-5) g.
Preferably, the stirring time in S1 is 2h to 10h.
Preferably, the extracting agent in S1 is one or more of sodium fluoride, potassium bifluoride, and sodium bifluoride.
Preferably, the heavy component impurity in S2 is a hydrogen fluoride liquid containing an extractant.
Preferably, the pressure of the nitrogen introduced into the S2 is 0.01MPa to 0.05MPa.
Preferably, the adsorbent in S3 is sodium fluoride spherical particles or potassium fluoride spherical particles, and the particle size of the adsorbent is 10-25 mm.
Preferably, the temperature of the refined product tank in S3 is-50 ℃ to-35 ℃.
Compared with the prior art, the invention has the following advantages:
1. the invention changes the relative volatility between the hydrogen fluoride and the trifluoromethanesulfonyl fluoride by adding the extracting agent and utilizing the action between the hydrogen fluoride and the extracting agent, and can remove most of the hydrogen fluoride; and then rectifying is carried out, the content of hydrogen fluoride in the rectified trifluoromethanesulfonyl fluoride is lower, the hydrogen fluoride can be more easily removed by using the adsorbent, collapse of the adsorbent is avoided, and in the purification process, no three wastes are generated, so that the method is simple in process, lower in cost and capable of being popularized and used.
2. Heavy component impurities after rectification are discharged into a hydrogen fluoride recovery tank, hydrogen fluoride volatilized by adsorbent regeneration in an adsorption tower is collected in the hydrogen fluoride recovery tank, the recovered hydrogen fluoride can be directly used for electrolyzing a raw material for preparing trifluoromethanesulfonyl fluoride, and an extracting agent in the hydrogen fluoride recovery tank can be used for electrolyzing a conductive agent in the raw material.
3. The adsorbent adopts potassium fluoride or sodium fluoride because potassium fluoride and sodium fluoride are converted into potassium bifluoride and sodium bifluoride after absorbing hydrogen fluoride, and potassium bifluoride and sodium bifluoride are converted into potassium fluoride and sodium fluoride after regeneration, so that the potassium fluoride and the sodium fluoride can be recycled.
The technical solution of the present invention will be described in further detail by examples.
Detailed Description
Example 1
The method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride in the present example includes the following steps:
s1, firstly, pumping negative pressure of a mixing kettle, wherein the negative pressure is-0.07 MPa, then transferring a crude trifluoromethanesulfonyl fluoride liquid in a crude product tank into the mixing kettle, adding a sodium fluoride extracting agent, and stirring for 2 hours at the temperature of-25 ℃ to obtain a mixture;
the mass fraction of hydrogen fluoride in the crude trifluoromethanesulfonyl fluoride liquid in the S1 is 5wt%; the dosage ratio of the crude trifluoromethanesulfonyl fluoride liquid to the extractant in the mixture in S1 is 100mL:2g of the total weight of the mixture;
s2, introducing nitrogen into the mixing kettle in the S1, pressing the mixture obtained in the S1 into a rectifying tower for rectification, evaporating out light component trifluoromethanesulfonyl fluoride, discharging heavy component impurities into a hydrogen fluoride recovery tank, wherein the temperature of the tower kettle of the rectifying tower is 10 ℃, the temperature of a rectifying column is 5 ℃, and the reflux ratio is 10; the nitrogen provides positive pressure, the mixture is pressed into the rectifying tower, and the reaction in the rectifying tower is not influenced even if the nitrogen enters the rectifying tower;
the pressure of the nitrogen in the S2 is 0.01MPa; the heavy component impurity is hydrogen fluoride liquid containing sodium fluoride;
s3, introducing the light component trifluoromethanesulfonyl fluoride steamed out in the S2 into an adsorption tower, adsorbing by an adsorbent to obtain refined trifluoromethanesulfonyl fluoride gas with the hydrogen fluoride content of 10ppm, and introducing the refined trifluoromethanesulfonyl fluoride gas into a refined tank to be condensed into liquid;
in S3, the adsorbent is sodium fluoride spherical particles, and the particle size of the adsorbent is 10-25 mm; the temperature of the fine product tank is-50 ℃.
Example 2
The method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride of the present example includes the following steps:
s1, firstly, pumping negative pressure of a mixing kettle, wherein the negative pressure is-0.04 MPa, then transferring crude trifluoromethanesulfonyl fluoride liquid in a crude product tank into the mixing kettle, adding a potassium fluoride extracting agent, and stirring for 7 hours at the temperature of-32 ℃ to obtain a mixture;
the mass fraction of hydrogen fluoride in the crude trifluoromethanesulfonyl fluoride liquid in the S1 is 7wt%; the dosage ratio of the crude trifluoromethanesulfonyl fluoride liquid to the extractant in the mixture in S1 is 100mL:3g of the total weight of the mixture;
s2, introducing nitrogen into the mixing kettle in the S1, pressing the mixture obtained in the S1 into a rectifying tower for rectification, evaporating out light component trifluoromethanesulfonyl fluoride, discharging heavy component impurities into a hydrogen fluoride recovery tank, wherein the temperature of the tower kettle of the rectifying tower is 20 ℃, the temperature of a rectifying column is 12 ℃, and the reflux ratio is 7;
the pressure of the nitrogen in the S2 is 0.03MPa; the heavy component impurity is hydrogen fluoride liquid containing potassium fluoride;
s3, introducing the light component trifluoromethanesulfonyl fluoride steamed out in the S2 into an adsorption tower, adsorbing by an adsorbent to obtain refined trifluoromethanesulfonyl fluoride gas with the hydrogen fluoride content of 15ppm, and introducing the refined trifluoromethanesulfonyl fluoride gas into a refined tank to be condensed into liquid;
the adsorbent in S3 is potassium fluoride spherical particles, and the particle size of the adsorbent is 10-25 mm; the temperature of the fine product tank is-40 ℃.
Example 3
The method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride of the present example includes the following steps:
s1, firstly, pumping negative pressure to a mixing kettle, wherein the negative pressure is-0.01 MPa, then transferring crude trifluoromethanesulfonyl fluoride liquid in a crude product tank into the mixing kettle, adding a potassium bifluoride extracting agent, and stirring for 10 hours at the temperature of-40 ℃ to obtain a mixture;
the mass fraction of hydrogen fluoride in the crude trifluoromethanesulfonyl fluoride liquid in the S1 is 10wt%; the dosage ratio of the crude trifluoromethanesulfonyl fluoride liquid to the extractant in the mixture in S1 is 100mL:5g of the total weight of the mixture;
s2, introducing nitrogen into the mixing kettle in the S1, pressing the mixture obtained in the S1 into a rectifying tower for rectification, evaporating out light component trifluoromethanesulfonyl fluoride, discharging heavy component impurities into a hydrogen fluoride recovery tank, wherein the temperature of the tower kettle of the rectifying tower is 30 ℃, the temperature of the rectifying tower is 19 ℃, and the reflux ratio is 5;
the pressure of the nitrogen in the S2 is 0.05MPa; the heavy component impurity is hydrogen fluoride liquid containing potassium fluoride;
s3, introducing the light component trifluoromethanesulfonyl fluoride steamed out in the S2 into an adsorption tower, adsorbing by an adsorbent to obtain refined trifluoromethanesulfonyl fluoride gas with the hydrogen fluoride content of 18ppm, and introducing the refined trifluoromethanesulfonyl fluoride gas into a refined tank to be condensed into liquid;
the adsorbent in S3 is spherical particles of potassium fluoride, and the particle size of the adsorbent is 10-25 mm; the temperature of the fine product tank is-35 ℃.
Example 4
S1, firstly, pumping negative pressure of a mixing kettle, wherein the negative pressure is-0.03 MPa, then transferring a crude trifluoromethanesulfonyl fluoride liquid in a crude product tank into the mixing kettle, adding a sodium fluoride extracting agent, and stirring for 6 hours at the temperature of-30 ℃ to obtain a mixture;
the mass fraction of hydrogen fluoride in the crude trifluoromethanesulfonyl fluoride liquid in the S1 is 6wt%; the dosage ratio of the crude trifluoromethanesulfonyl fluoride liquid to the extractant in the mixture in S1 is 100mL:4g of the total weight of the mixture;
s2, introducing nitrogen into the mixing kettle in the S1, pressing the mixture obtained in the S1 into a rectifying tower for rectification, evaporating out light component trifluoromethanesulfonyl fluoride, discharging heavy component impurities into a hydrogen fluoride recovery tank, wherein the temperature of the tower kettle of the rectifying tower is 25 ℃, the temperature of a rectifying column is 15 ℃, and the reflux ratio is 8;
the pressure of the nitrogen in the S2 is 0.04MPa; the heavy component impurity is hydrogen fluoride liquid containing sodium fluoride;
s3, introducing the light component trifluoromethanesulfonyl fluoride steamed out in the S2 into an adsorption tower, adsorbing by an adsorbent to obtain refined trifluoromethanesulfonyl fluoride gas with the hydrogen fluoride content of 12ppm, and introducing the refined trifluoromethanesulfonyl fluoride gas into a refined tank to be condensed into liquid;
in S3, the adsorbent is sodium fluoride spherical particles, and the particle size of the adsorbent is 10-25 mm; the temperature of the fine product tank is-40 ℃.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (8)
1. A method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride is characterized by comprising the following steps:
s1, firstly, pumping negative pressure of a mixing kettle, then transferring a crude trifluoromethanesulfonyl fluoride liquid in a crude tank into the mixing kettle, adding an extracting agent, and stirring at the temperature of-40 ℃ to-32 ℃ to obtain a mixture; the dosage ratio of the crude trifluoromethanesulfonyl fluoride liquid to the extractant in the mixture is 100mL: (2-5) g; the extracting agent is potassium fluoride, potassium bifluoride or sodium bifluoride;
s2, introducing nitrogen into the mixing kettle in the S1, pressing the mixture obtained in the S1 into a rectifying tower for rectification, evaporating out light component trifluoromethanesulfonyl fluoride, discharging heavy component impurities into a hydrogen fluoride recovery tank, wherein the temperature of a kettle of the rectifying tower is 20-30 ℃, the temperature of a rectifying column is 12-19 ℃, and the reflux ratio is 7-10;
and S3, introducing the light component trifluoromethanesulfonyl fluoride steamed out in the S2 into an adsorption tower, adsorbing by an adsorbent to obtain refined trifluoromethanesulfonyl fluoride gas with the hydrogen fluoride content of less than or equal to 20ppm, and introducing the refined trifluoromethanesulfonyl fluoride gas into a refined tank to be condensed into liquid.
2. The method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride according to claim 1, wherein the mass fraction of hydrogen fluoride in the crude trifluoromethanesulfonyl fluoride liquid in S1 is 7 to 10wt%.
3. The method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride according to claim 1, wherein the negative pressure in S1 is in the range of-0.04 MPa to-0.01 MPa.
4. The method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride according to claim 1, wherein the stirring time in S1 is 7 to 10 hours.
5. The method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride as claimed in claim 1, wherein the heavy component impurity in S2 is a hydrogen fluoride liquid containing an extractant.
6. The method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride according to claim 1, wherein the pressure of the nitrogen gas introduced into S2 is 0.01MPa to 0.05MPa.
7. The method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride according to claim 1, wherein the adsorbent in S3 is spherical sodium fluoride particles or spherical potassium fluoride particles, and the particle size of the adsorbent is 10mm to 25mm.
8. The method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride according to claim 1, wherein the temperature of the fine tank in S3 is in a range of-40 ℃ to-35 ℃.
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| JP2009102294A (en) * | 2007-10-02 | 2009-05-14 | Central Glass Co Ltd | Method for purification of trifluoromethanesulfonyl fluoride |
| CN101790500A (en) * | 2007-05-25 | 2010-07-28 | 纳幕尔杜邦公司 | Process for the separation of fluorocarbons using ionic liquids |
| JP2010173959A (en) * | 2009-01-29 | 2010-08-12 | Central Glass Co Ltd | Method for purifying trifluoromethanesulfonyl fluoride |
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| CN108276315A (en) * | 2017-12-29 | 2018-07-13 | 中国船舶重工集团公司第七八研究所 | A kind of purification process of trifluoromethanesulfonic acid |
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| US8598378B2 (en) * | 2008-03-14 | 2013-12-03 | University Of Hawaii | Methods and compositions for extraction and transesterification of biomass components |
| JP2013170129A (en) * | 2012-02-20 | 2013-09-02 | Mitsubishi Materials Corp | Method for separating perfluoroalkanesulfonyl fluoride gas |
| FR3003570B1 (en) * | 2013-03-20 | 2016-01-29 | Renault Sas | SPECIFIC SULFONATE COMPOUNDS FOR USE AS ELECTROLYTE SOLVENT FOR LITHIUM BATTERIES |
| CN112390230A (en) * | 2020-11-20 | 2021-02-23 | 苏州金宏气体股份有限公司 | Purification method and purification system of chlorine trifluoride |
| CN216023237U (en) * | 2021-11-03 | 2022-03-15 | 中船(邯郸)派瑞特种气体股份有限公司 | Purification device of hydrogen fluoride in trifluoromethanesulfonyl fluoride |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101790500A (en) * | 2007-05-25 | 2010-07-28 | 纳幕尔杜邦公司 | Process for the separation of fluorocarbons using ionic liquids |
| JP2009102294A (en) * | 2007-10-02 | 2009-05-14 | Central Glass Co Ltd | Method for purification of trifluoromethanesulfonyl fluoride |
| JP2010173959A (en) * | 2009-01-29 | 2010-08-12 | Central Glass Co Ltd | Method for purifying trifluoromethanesulfonyl fluoride |
| CN104387300A (en) * | 2014-11-11 | 2015-03-04 | 中国船舶重工集团公司第七一八研究所 | Purification method of trifluoromathanesulfonyl fluoride |
| CN108276315A (en) * | 2017-12-29 | 2018-07-13 | 中国船舶重工集团公司第七八研究所 | A kind of purification process of trifluoromethanesulfonic acid |
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