CN116812876A - Preparation method of sulfuryl fluoride - Google Patents
Preparation method of sulfuryl fluoride Download PDFInfo
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- CN116812876A CN116812876A CN202310864519.3A CN202310864519A CN116812876A CN 116812876 A CN116812876 A CN 116812876A CN 202310864519 A CN202310864519 A CN 202310864519A CN 116812876 A CN116812876 A CN 116812876A
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- fluoride
- sulfuryl
- preparing
- anhydrous hydrogen
- sulfuryl fluoride
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- 239000005935 Sulfuryl fluoride Substances 0.000 title claims abstract description 53
- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 33
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 28
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 24
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- BRCWHGIUHLWZBK-UHFFFAOYSA-K bismuth;trifluoride Chemical group F[Bi](F)F BRCWHGIUHLWZBK-UHFFFAOYSA-K 0.000 claims abstract description 14
- 238000003682 fluorination reaction Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 5
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 18
- 235000003270 potassium fluoride Nutrition 0.000 claims description 9
- 239000011698 potassium fluoride Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 abstract description 3
- 239000000376 reactant Substances 0.000 abstract description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract 1
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 6
- -1 artworks Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- LNKQQZFLNUVWQQ-UHFFFAOYSA-N 1-chloro-2,2-bis(4'-chlorophenyl)ethylene Chemical compound C=1C=C(Cl)C=CC=1C(=CCl)C1=CC=C(Cl)C=C1 LNKQQZFLNUVWQQ-UHFFFAOYSA-N 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 3
- 239000013067 intermediate product Substances 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- ZEIYBPGWHWECHV-UHFFFAOYSA-N nitrosyl fluoride Chemical compound FN=O ZEIYBPGWHWECHV-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 1
- HXELGNKCCDGMMN-UHFFFAOYSA-N [F].[Cl] Chemical group [F].[Cl] HXELGNKCCDGMMN-UHFFFAOYSA-N 0.000 description 1
- ZJPPTKRSFKBZMD-UHFFFAOYSA-N [Li].FS(=N)F Chemical compound [Li].FS(=N)F ZJPPTKRSFKBZMD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012025 fluorinating agent Substances 0.000 description 1
- 239000002316 fumigant Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- PNQBEPDZQUOCNY-UHFFFAOYSA-N trifluoroacetyl chloride Chemical compound FC(F)(F)C(Cl)=O PNQBEPDZQUOCNY-UHFFFAOYSA-N 0.000 description 1
- 210000002268 wool Anatomy 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
- C01B17/00—Sulfur; Compounds thereof
- C01B17/46—Compounds containing sulfur, halogen, hydrogen, and oxygen
-
- 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
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of fluoride engineering and discloses a preparation method of sulfuryl fluoride; the method comprises the following steps: adding liquid sulfuryl chloride into anhydrous hydrogen fluoride with dissolved catalyst, and stirring to perform fluorination reaction to generate mixed gas containing sulfuryl fluoride gas and hydrogen chloride gas; the catalyst is bismuth trifluoride; the dosage of the bismuth trifluoride is 0.1-2% of the anhydrous hydrogen fluoride. The reactants of the invention are all liquid, the liquid homogeneous reaction rate is high, the byproducts are few, and the yield is high; the catalyst is not deactivated.
Description
Technical Field
The invention relates to the technical field of fluorine chemical industry, in particular to a preparation method of sulfuryl fluoride.
Background
Sulfuryl fluoride (SO) 2 F 2 ) Is colorless and odorless gas at normal temperature and pressure, has chemical inertness and is easy to decompose at high temperature. The application is the most widely used as a kind of fumigationThe steam agent has the advantages of small dosage, strong permeability and quick desorption, does not corrode metals, wool, cotton fabrics, plastics, artworks, leather and the like, does not affect the color, and does not destroy the ozone layer of the atmosphere when being used as a pesticide, a bactericide and a fumigant, so that the sulfuryl fluoride is widely applied in the fields.
In recent years, sulfuryl fluoride has begun to be used as a raw material for synthesizing lithium difluorosulfimide. The lithium bis (fluorosulfonyl) imide is a novel lithium salt electrolyte material of a lithium ion battery with wide application prospect, and can improve the cycle performance and the multiplying power performance of the power battery in the power battery. Therefore, sulfuryl fluoride has very good development prospect in the field of lithium ion batteries.
The preparation method of the sulfuryl fluoride mainly comprises the following steps: a direct fluorination method using sulfur dioxide and fluorine gas as main raw materials, an anhydrous hydrofluoric acid method using sulfur dioxide, chlorine and anhydrous hydrofluoric acid as raw materials, a nitrosyl fluoride method using sulfur dioxide and nitrosyl fluoride as main raw materials, a sulfuryl chloride fluorination method for synthesizing sulfuryl fluoride by fluorinating sulfuryl chloride, a fluorosulfonic acid method using fluorosulfonic acid and barium chloride as main raw materials, and the like. Among them, sulfuryl chloride fluorination is one of the more common processes. For example, U.S. Pat. No. 3, process for the production of sulfuryl fluoride,79 discloses that ammonium bifluoride is used to fluorinate sulfuryl chloride to generate sulfuryl fluoride at 90-150 ℃, but the reaction yield is low, only 59%. Chinese patent publication No. CN102351681B, "a method for continuously synthesizing trifluoroacetyl chloride and sulfuryl fluoride", uses hydrogen fluoride to fluoride sulfuryl chloride under the action of palladium/carbon catalyst, and makes them react at 150-160 deg.c to produce sulfuryl fluoride, but the catalyst is easy to deactivate, its catalytic efficiency is low and its catalyst cost is high. Chinese patent publication No. CN103864022B, a method for preparing sulfuryl fluoride, uses potassium fluoride as fluorinating agent, the potassium fluoride is suspended and dispersed in organic solvent in the form of solid particles, and makes fluorine-chlorine exchange reaction with liquid sulfuryl chloride under stirring, but the solid and liquid react, the contact is limited, the reaction is slower, the fluorination is insufficient, and the byproduct sulfuryl chloride fluoride (SO 2 ClF) is more.
Disclosure of Invention
The invention aims to overcome the defects and provide a preparation method of sulfuryl fluoride.
In order to achieve the above purpose, the invention is implemented according to the following technical scheme:
a method for preparing sulfuryl fluoride, comprising the following steps: adding liquid sulfuryl chloride into anhydrous hydrogen fluoride with dissolved catalyst, and stirring to perform fluorination reaction to generate mixed gas containing sulfuryl fluoride gas and hydrogen chloride gas; the reaction equation of the fluorination reaction is as follows:
SO 2 Cl 2 +2HF→SO 2 F 2 ↑+2HCl↑。
preferably, the catalyst is bismuth trifluoride; the dosage of the bismuth trifluoride is 0.1-2% of the anhydrous hydrogen fluoride.
Preferably, potassium fluoride is also added to the anhydrous hydrogen fluoride of the dissolved catalyst; the dosage of the potassium fluoride is 2-5% of the anhydrous hydrogen fluoride by mass. The use of potassium fluoride allows for higher reaction yields.
Preferably, the liquid sulfuryl chloride is added in an amount of less than 30% by mass of the anhydrous hydrogen fluoride.
Preferably, the liquid sulfuryl chloride is added dropwise; the addition amount of the liquid sulfuryl chloride per minute is 0.2-2% of the mass of the anhydrous hydrogen fluoride.
Too fast addition of liquid sulfuryl chloride can lead to insufficient fluorination reaction, and the intermediate product sulfuryl chloride fluoride can be carried by sulfuryl fluoride gas to escape, so that the impurity content is increased.
Preferably, the reaction temperature of the fluorination reaction is-5 to 5 ℃.
Too high a reaction temperature will lead to the evolution of the intermediate sulfuryl fluoride as a gas to form impurities (sulfuryl fluoride boiling point 7 ℃), too low a reaction temperature will reduce the reaction rate.
Preferably, the mixed gas is washed with water and then dehydrated to obtain pure sulfuryl fluoride.
Preferably, the water removal is cold trap water removal; the cold trap temperature is-50 to-10 ℃.
The lower the cold trap temperature, the better the water removal effect, but too low a temperature will result in the target product sulfuryl fluoride also being liquefied.
Preferably, the water removal is performed by using activated alumina.
Preferably, the water removal is performed by rectification.
The catalyst in the invention is not deactivated, and new hydrogen fluoride is supplied to the residual liquid, wherein the dissolved catalyst can be reused for a plurality of times.
Compared with the prior art, the invention has the beneficial effects that:
the reactants of the invention are all liquid, the liquid homogeneous reaction rate is high, the byproducts are few, and the yield is high; the catalyst is not deactivated.
Detailed Description
A method for preparing sulfuryl fluoride, comprising the following steps:
slowly adding liquid sulfuryl chloride into anhydrous hydrogen fluoride of the dissolved catalyst bismuth trifluoride, controlling the reaction temperature to be between 5 ℃ below zero and 5 ℃, stirring to generate a mixed gas containing sulfuryl fluoride gas and hydrogen chloride gas, washing the mixed gas by a water washing tower to remove hydrogen chloride and a small amount of hydrogen fluoride, and liquefying and separating impurity water by a cold trap to obtain pure sulfuryl fluoride.
The fluorination reaction of the sulfuryl chloride is SO 2 Cl 2 +2HF→SO 2 F 2 ↑+2HCl↑。
The dosage of the catalyst bismuth trifluoride is 0.1-2% of the anhydrous hydrogen fluoride.
The anhydrous hydrogen fluoride with the mass of 2 to 5 percent of that of potassium fluoride is added into the anhydrous hydrogen fluoride with the dissolved catalyst bismuth trifluoride, so that the reaction yield is higher.
The addition amount of the liquid sulfuryl chloride is less than 30% of the anhydrous hydrogen fluoride; the addition amount of the liquid sulfuryl chloride per minute is 0.2-2% of the mass of the anhydrous hydrogen fluoride, the excessive addition can lead to insufficient fluorination reaction, the intermediate product sulfuryl chloride fluoride is carried by sulfuryl fluoride gas to escape, and the impurity content is increased.
The reaction temperature is controlled to be between 5 ℃ below zero and 5 ℃, so that the intermediate product sulfuryl fluoride can escape in a gas form to form impurities (the boiling point of the sulfuryl fluoride is 7 ℃), and the reaction rate can be reduced when the temperature is too low;
the temperature of the cold trap is-50 to-10 ℃, the lower the temperature is, the better the water removal effect is, but the too low temperature can lead to the liquefaction of the target product sulfuryl fluoride; wherein the cold trap water removal can be replaced by activated alumina water removal or rectification method water removal.
The invention is further described in terms of specific examples, illustrative examples and illustrations of which are provided herein to illustrate the invention, but are not to be construed as limiting the invention.
Example 1:
a method for preparing sulfuryl fluoride, comprising the following steps:
in an environment of minus 5 ℃, 200g of anhydrous hydrogen fluoride and 0.2g of bismuth trifluoride are added into a reaction kettle internally lined with polytetrafluoroethylene, stirring is carried out for dissolution, sulfuryl chloride is dropwise added at the speed of 0.4g/min for 10min, stirring is carried out for full reaction for 30min, gas generated by the reaction is collected, 4.59g of mixed gas is obtained, water washing and water removal are carried out by a cold trap at minus 30 ℃ to obtain 2.61g of sulfuryl fluoride gas, the yield is 86.4%, and the purity is 98.2%.
Example 2:
a method for preparing sulfuryl fluoride, comprising the following steps:
in the environment of 5 ℃, 200g of anhydrous hydrogen fluoride, 4g of bismuth trifluoride and stirring for dissolution are added into a reaction kettle internally lined with polytetrafluoroethylene, liquid sulfuryl chloride is dripped at the speed of 4g/min for 10min, the mixture is stirred for 30min again, gas generated by the reaction is collected to obtain 48.90g of mixed gas, 28.28g of sulfuryl fluoride gas is obtained through water washing and water removal by a cold trap at minus 30 ℃, and the yield is 93.5% and the purity is 96.8%.
In the embodiment, the dropping speed of the liquid sulfuryl chloride is higher, so that impurity sulfuryl chloride fluoride is increased, and the purity of the product is slightly lower.
Example 3
A method for preparing sulfuryl fluoride, comprising the following steps:
in an environment of 0 ℃, 200g of anhydrous hydrogen fluoride and 2.1g of bismuth trifluoride are added into a reaction kettle internally lined with polytetrafluoroethylene, liquid sulfuryl chloride is dripped at the speed of 2g/min for 10min under stirring, gas generated by the reaction is collected after the reaction is fully reacted for 30min, 24.30g of mixed gas is obtained, and then 13.93g of sulfuryl fluoride gas is obtained through water washing and water removal by a cold trap at minus 30 ℃, wherein the yield is 92.1%, and the purity is 98.3%.
Example 4:
a method for preparing sulfuryl fluoride, comprising the following steps:
in an environment of minus 5 ℃, 200g of anhydrous hydrogen fluoride and 0.2g of bismuth trifluoride and 6g of potassium fluoride are added into a reaction kettle internally lined with polytetrafluoroethylene, liquid sulfuryl chloride is dripped at the speed of 0.4g/min for 10min by stirring and dissolving, the gas generated by the reaction is collected after the reaction is fully stirred for 30min to obtain 4.79g of mixed gas, and 2.76g of sulfuryl fluoride gas is obtained by water washing and water removal by a cold trap at minus 30 ℃, the yield is 91.4%, and the purity is 98.2%.
Comparative example 1:
the procedure of example 4 was repeated except that the catalyst bismuth trifluoride was not used in the comparative example. The entire reaction did not proceed and no sulfuryl fluoride product was collected.
The technical scheme of the invention is not limited to the specific embodiment, and all technical modifications made according to the technical scheme of the invention fall within the protection scope of the invention.
Claims (10)
1. A preparation method of sulfuryl fluoride is characterized in that: the method comprises the following steps: adding liquid sulfuryl chloride into anhydrous hydrogen fluoride with dissolved catalyst, and stirring to perform fluorination reaction to generate mixed gas containing sulfuryl fluoride gas and hydrogen chloride gas; the reaction equation of the fluorination reaction is as follows:
SO 2 Cl 2 +2HF→SO 2 F 2 ↑+2HCl↑。
2. the method for preparing sulfuryl fluoride according to claim 1, wherein: the catalyst is bismuth trifluoride; the dosage of the bismuth trifluoride is 0.1-2% of the anhydrous hydrogen fluoride.
3. The method for preparing sulfuryl fluoride according to claim 1, wherein: potassium fluoride is also added into the anhydrous hydrogen fluoride of the dissolved catalyst; the dosage of the potassium fluoride is 2-5% of the anhydrous hydrogen fluoride by mass.
4. The method for preparing sulfuryl fluoride according to claim 1, wherein: the addition amount of the liquid sulfuryl chloride is less than 30 percent of the mass of the anhydrous hydrogen fluoride.
5. The method for preparing sulfuryl fluoride according to claim 1, wherein: the liquid sulfuryl chloride is added dropwise; the addition amount of the liquid sulfuryl chloride per minute is 0.2-2% of the mass of the anhydrous hydrogen fluoride.
6. The method for preparing sulfuryl fluoride according to claim 1, wherein: the reaction temperature of the fluorination reaction is-5 to 5 ℃.
7. The method for preparing sulfuryl fluoride according to claim 1, wherein: and (3) washing the mixed gas with water, and then removing water to obtain pure sulfuryl fluoride.
8. The method for preparing sulfuryl fluoride according to claim 7, wherein: the water removal is cold trap water removal; the cold trap temperature is-50 to-10 ℃.
9. The method for preparing sulfuryl fluoride according to claim 7, wherein: the water is removed by adopting activated alumina.
10. The method for preparing sulfuryl fluoride according to claim 7, wherein: the water removal adopts rectification water removal.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102351681A (en) * | 2011-08-16 | 2012-02-15 | 浙江大学 | Method for continuously synthesizing trifluoroacetyl chloride and sulfuryl fluoride |
CN107188138A (en) * | 2017-05-02 | 2017-09-22 | 惠州市大道新材料科技有限公司 | A kind of preparation method of pair of fluorine sulfimide lithium |
CN114477100A (en) * | 2022-01-29 | 2022-05-13 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride by sulfuryl chloride fluorination method |
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2023
- 2023-07-14 CN CN202310864519.3A patent/CN116812876B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102351681A (en) * | 2011-08-16 | 2012-02-15 | 浙江大学 | Method for continuously synthesizing trifluoroacetyl chloride and sulfuryl fluoride |
CN107188138A (en) * | 2017-05-02 | 2017-09-22 | 惠州市大道新材料科技有限公司 | A kind of preparation method of pair of fluorine sulfimide lithium |
CN114477100A (en) * | 2022-01-29 | 2022-05-13 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride by sulfuryl chloride fluorination method |
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