CN112724047A - Device and method for preparing trifluoromethanesulfonyl fluoride - Google Patents
Device and method for preparing trifluoromethanesulfonyl fluoride Download PDFInfo
- Publication number
- CN112724047A CN112724047A CN202011475878.2A CN202011475878A CN112724047A CN 112724047 A CN112724047 A CN 112724047A CN 202011475878 A CN202011475878 A CN 202011475878A CN 112724047 A CN112724047 A CN 112724047A
- Authority
- CN
- China
- Prior art keywords
- trifluoromethanesulfonyl
- fluoride
- reactor
- heat exchanger
- trifluoromethanesulfonyl fluoride
- 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.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a device and a method for preparing trifluoromethanesulfonyl fluoride, and belongs to the technical field of preparation of trifluoromethanesulfonyl fluoride. The device comprises a trifluoromethanesulfonyl chloride storage tank, a reactor, a reflux heat exchanger and a trifluoromethanesulfonyl fluoride storage tank, the device is few in equipment, the process flow is simplified, the safety is high, the trifluoromethanesulfonyl fluoride with higher purity can be collected while the trifluoromethanesulfonyl fluoride is reacted, the utilization efficiency of the equipment is greatly improved, and the cost is effectively reduced; the method takes trifluoromethanesulfonyl chloride and potassium fluoride as raw materials and cyclohexanone as a solvent, so that unreacted excessive fluorinating agent and solvent can be conveniently recovered, trifluoromethanesulfonyl fluoride with the purity of over 99.5 vol% can be collected by simple reflux after the reaction at a higher temperature, the product purity is higher, and no hydrogen fluoride or other light component impurities exist, so that the method is suitable for industrial production.
Description
Technical Field
The invention relates to a device and a method for preparing trifluoromethanesulfonyl fluoride, and belongs to the technical field of preparation of trifluoromethanesulfonyl fluoride.
Background
The trifluoromethanesulfonyl fluoride has a boiling point of-21.7 ℃ at normal pressure, is a weak-odor gas at normal temperature, is easy to liquefy, does not react with hydrogen, is insoluble in cold water, hydrogen fluoride and the like, and is easy to hydrolyze under hot water and alkaline conditions. The trifluoromethanesulfonyl fluoride is an important intermediate in the field of fine chemical engineering, and can be used as important raw materials for organic synthesis, pesticide and medicine, ionic liquid, lithium ion electrolyte and the like.
The trifluoromethanesulfonyl fluoride is available in the forms of photolysis, chemical direct fluorination, electrolysis and fluorination of trifluoromethanesulfonyl chloride with potassium fluoride, but at present, the most industrially applicable method is electrolysis. With methanesulfonyl fluoride (CH)3SO2F) Or methanesulfonyl Chloride (CH)3SO2Cl) electrolysis method for producing trifluoromethanesulfonyl fluoride by using methanesulfonyl fluoride or methanesulfonyl Chloride (CH)3SO2Cl) as starting material and excess liquid fluorineThe hydrogen fluoride is subjected to electrochemical fluorination reaction in an electrolytic bath, and the product is trifluoromethanesulfonyl fluoride (CF)3SO2F) Hydrogen (H)2) Carbon tetrafluoride (CF)4) Difluoro Sulfoxide (SOF)2) Carbon dioxide (CO)2) And oxygen difluoride (OF)2) Since hydrogen fluoride is excessive and its saturated vapor pressure is high, a certain amount of Hydrogen Fluoride (HF) gas is included in the produced gas mixture, and the content of impurity gases other than hydrogen is not high, but the use of trifluoromethanesulfonyl fluoride is affected, so that it must be purified.
The patent CN2008801141902 central Pin corporation provides a method for preparing trifluoromethanesulfonyl fluoride by reacting trifluoromethanesulfonyl chloride with potassium fluoride in the presence of water, the purity of the product obtained is about 98.9%. The method has the following problems: 1) the triflic acid and the hydrogen chloride gas are easy to be hydrolyzed to generate, so that equipment is corroded and the operation is dangerous; 2) the purity of the obtained product is not high; 3) the potassium fluoride and the potassium chloride are both dissolved in water, and the potassium fluoride is wrapped by the generated potassium chloride along with the reaction, so that the reaction rate is gradually slowed down, and the reaction efficiency is lower; 4) excessive potassium fluoride and potassium chloride are not suitable to be separated, so that the raw material waste is caused.
Under the protection of nitrogen, the university of Wuhan in patent CN201910273954.2 provides a method for dripping trifluoromethyl sulfonyl chloride into a solution containing potassium fluoride and 18-crown-6, wherein during dripping, a reaction system is placed in an ice water bath, after dripping is finished, the reaction is continued for 2 hours, and a trifluoromethyl sulfonyl fluoride liquid with the purity of about 98 percent can be collected in a cold trap. The method has the following problems: 1) two solvents are adopted, so that the separation is difficult and the pollution is large; 2) the reaction temperature is low, the reaction rate is low, and the reaction time is long; 3) the potassium chloride and potassium fluoride which are generated are not easy to separate; 4) the purity of the obtained product is not high.
The purification method of trifluoromethanesulfonyl fluoride is relatively few, and the following methods have been reported. Study on Synthesis of trifluoromethanesulfonic anhydride (Fanclei, Liuchangyuan. study on Synthesis of trifluoromethanesulfonic anhydride [ J)]Organofluorine industry, 2005 (4): 6) it has been reported that trifluoromethanesulfonyl fluoride is led out from the outlet of the electrolytic cell together with hydrogen and is carried by the hydrogen through a condenserThe hydrogen fluoride cooling reflux returns to the electrolytic cell again, the rest gas enters a water absorber and an alkali washing absorber through a buffer to remove all hydrogen chloride and hydrogen fluoride, then enters a gas storage cabinet through a gas-liquid separator, the gas is pumped out by a hydrogen compressor, enters a freezing dehydrator and then passes through a molecular sieve dryer to remove water brought in the water washing and alkali washing processes, the dried gas flows into a trifluoromethanesulfonyl fluoride storage tank through cryogenic liquefaction, and hydrogen which is not condensed and liquefied is discharged. The method for separating and refining trifluoromethanesulfonyl fluoride reported in patent CN200810243626.X comprises the following steps: cooling and condensing the electrochemical fluorination gas-phase product of the methanesulfonyl fluoride to condense hydrogen fluoride into a liquid phase, then carrying out gas-liquid separation, washing and absorbing the gas-phase material by a carbonate aqueous solution to remove the hydrogen fluoride, carrying out gas-liquid separation, then adding a dehydrating agent into the gas-phase material, dehydrating and drying, carrying out gas-solid separation, carrying out deep cooling on the gas-phase material, and finally carrying out gas-liquid separation and refining on the gas-phase material to obtain the product of the trifluoromethanesulfonyl fluoride gas. The above two purification methods have the following problems: (1) the purification steps are multiple, the required equipment is more, and multiple steps of gas-liquid separation equipment and water removal equipment are required; (2) the safety of the process is high, and the process route is long, and hydrogen is removed in the last step, so that the leakage and explosion accidents of the hydrogen are easy to happen, and the requirement on the sealing performance of all the purification equipment is high; (3) the trifluoromethanesulfonyl fluoride can be hydrolyzed in an alkaline solution, hydrogen fluoride is removed by absorption of a carbonate solution, a part of trifluoromethanesulfonyl fluoride can be absorbed at the same time, loss of a product is caused, and carbon dioxide is generated by reaction of the trifluoromethanesulfonyl fluoride and the carbonate, so that new impurities are brought, and the purity of the product is influenced; (4) the method of introducing water firstly and dehydrating by a dehydrating agent is adopted, and inert gas and electric energy are consumed for activating the dehydrating agent, so that the energy consumption of purification is increased; (5) the product is obtained by simply separating gas and liquid to remove hydrogen, and light component impurities such as carbon tetrafluoride (CF)4) Difluoro Sulfoxide (SOF)2) Carbon dioxide (CO)2) And oxygen difluoride (OF)2) No effective measures are taken to remove the resulting trifluoromethanesulfonyl fluoride, and the final purity of the product trifluoromethanesulfonyl fluoride is not mentioned. Chinese ship group CN201410631152.1 patentThe seventh and eighth research institute of limited company provides that the trifluoromethanesulfonyl fluoride gas generated by electrolysis is purified in a rectifying tower, and the purity of the finally obtained product is high (99.5%), but the purification method is applicable to the case of low production capacity, and more equipment is needed and the efficiency is low in the case of high production capacity.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a device and a method for preparing trifluoromethanesulfonyl fluoride, wherein the device has the advantages of few equipment, simplified process flow, high safety and effectively reduced cost; the method takes cyclohexanone as a solvent, can separate potassium chloride as a byproduct from excessive potassium fluoride as a raw material, can obtain a product with higher purity by simple reflux, effectively improves the reaction efficiency, and is suitable for industrial production.
The purpose of the invention is realized by the following technical scheme.
A device for preparing trifluoromethanesulfonyl fluoride comprises a trifluoromethanesulfonyl chloride storage tank, a reactor, a reflux heat exchanger and a trifluoromethanesulfonyl fluoride storage tank;
the reactor has a stirring function and a heating function, namely the reactor comprises a stirring mechanism and a heating mechanism;
the discharge hole of the trifluoromethanesulfonyl chloride storage tank is connected with the feed inlet at the bottom of the reactor, potassium fluoride and cyclohexanone are filled in the reactor, the gas outlet at the upper part of the reactor is connected with the lower part of the reflux heat exchanger, and the upper part of the reflux heat exchanger is connected with the trifluoromethanesulfonyl fluoride storage tank.
Further, the apparatus further comprises a gas disperser installed at the bottom inside the reactor.
Further, the pore diameter of the gas disperser is preferably 10 μm to 30 μm.
Further, the heat exchange area of the reflux heat exchanger is preferably 1m2～20m2。
Furthermore, the upper part of the reflux heat exchanger is provided with an analysis port.
The method for preparing the trifluoromethanesulfonyl fluoride by adopting the device provided by the invention has the following specific operations:
according to trifluoromethanesulfonyl chloride: potassium fluoride: cyclohexanone 1: (0.4-0.62): (0.65-1), pre-filling potassium fluoride and cyclohexanone into a reactor, allowing trifluoromethanesulfonyl chloride to enter from the bottom of the reactor and react with potassium fluoride at 40-60 ℃, collecting trifluoromethanesulfonyl fluoride generated by the reaction in a trifluoromethanesulfonyl fluoride storage tank at-20-0 ℃ after passing through a reflux heat exchanger at-30-10 ℃, wherein the purity of the collected trifluoromethanesulfonyl fluoride is not less than 99.5 vol%, the moisture content of the collected trifluoromethanesulfonyl fluoride is not more than 0.01 vol%, and the content of cyclohexanone is not more than 0.3 vol%.
Further, the purity of the potassium fluoride is more than or equal to 99 wt%; the purity of the trifluoromethanesulfonyl chloride is more than or equal to 99.5 wt%, and the purity of the cyclohexanone is more than or equal to 99 wt%.
Furthermore, the ratio of the feeding speed of the trifluoromethanesulfonyl chloride to the heat exchange area of the reflux heat exchanger is preferably (2.5-4.5) kg/(h.m)2)。
Has the advantages that:
(1) the device has the advantages of few equipment, simplified process flow, high safety, capability of collecting the trifluoromethanesulfonyl fluoride with higher purity while reacting, great improvement on equipment utilization efficiency and effective reduction of cost; the gas disperser arranged at the bottom of the reactor can not only disperse the trifluoromethanesulfonyl chloride gas entering the reactor, but also play a role in filtering and filtering excessive unreacted potassium fluoride.
(2) The method of the invention selects higher reaction temperature, so that the vaporization of the trifluoromethanesulfonyl chloride at the reaction temperature is beneficial to improving the reaction rate; the method takes cyclohexanone as a solvent, potassium fluoride serving as a raw material is insoluble in the cyclohexanone, and potassium chloride generated by reaction is soluble in the cyclohexanone, so that raw material waste is avoided, excessive unreacted potassium fluoride and the solvent can be conveniently recycled at a later stage, and the reaction rate is prevented from being influenced by products; the method can collect the trifluoromethanesulfonyl fluoride with the purity of more than 99.5 vol% through simple reflux, has high product purity, is free of hydrogen fluoride and other light component impurities, and is suitable for industrial production.
Drawings
FIG. 1 is a schematic view of the structure of the device of the present invention.
Wherein, the device comprises a 1-trifluoromethanesulfonyl chloride storage tank, a 2-reflux heat exchanger, a 3-reactor, a 4-gas disperser, a 5-trifluoromethanesulfonyl fluoride storage tank, an F1-analysis port and a V1-valve.
Detailed Description
The present invention is further illustrated by the following detailed description, wherein the processes are conventional unless otherwise specified, and the starting materials are commercially available from a public source without further specification.
The reagents used in the following examples are detailed in Table 1 and the assay methods are detailed in Table 2.
TABLE 1
| Raw materials | Purity of | Manufacturer of the product |
| Potassium fluoride | ≥99wt％ | Yellow river Fine chemical Co Ltd of New county City |
| CF3SO2Cl | ≥99.5wt％ | Hangzhou Ontai chemical Co Ltd |
| C6H10O | ≥99wt％ | Daqing refining division of China oil and gas resources Co Ltd |
TABLE 2
| Detecting items | Detection method |
| H2O | Electrolytic process for phosphorus pentoxide |
| Gas component | Gas chromatography |
Note: TABLE 2 gas composition means trifluoromethanesulfonyl fluoride (CF)3SO2F) And cyclohexanone.
The device involved in the preparation of trifluoromethanesulfonyl fluoride in the following examples comprises a trifluoromethanesulfonyl chloride storage tank 1, a reactor 3, a gas disperser 4, a reflux heat exchanger 2 and a trifluoromethanesulfonyl fluoride storage tank 5, as shown in fig. 1;
the reactor 3 is internally provided with a stirring paddle, externally provided with a jacket and has stirring and heating functions;
the aperture of the gas disperser 4 is 10-30 μm;
the heat exchange area of the reflux heat exchanger 2 is 1m2～20m2；
The discharge hole of trifluoromethanesulfonyl chloride storage tank 1 is connected with the feed inlet at the bottom of reactor 3, gas disperser 4 is installed at the bottom inside reactor 3, potassium fluoride and cyclohexanone are installed in reactor 3, the gas outlet at the upper part of reactor 3 is connected with the lower part of reflux heat exchanger 2, the upper part of reflux heat exchanger 2 is connected with trifluoromethanesulfonyl fluoride storage tank 5, valve V1 is installed on the connecting pipeline of reflux heat exchanger 2 and trifluoromethanesulfonyl fluoride storage tank 5, and analysis port F1 is arranged between reflux heat exchanger 2 and valve V1.
Example 1
In this example, 25kg of trifluoromethanesulfonyl chloride was added, 21.4kg of trifluoromethanesulfonyl fluoride was collected, and the reaction yield reached 94.9%. The collected trifluoromethanesulfonyl fluoride after refluxing was examined from port F1 and the results are shown in Table 3.
Example 2
In this example, total 16.7kg of trifluoromethanesulfonyl chloride was added finally, and total 14.4kg of trifluoromethanesulfonyl fluoride was collected, whereby the reaction yield reached 95.8%. The collected trifluoromethanesulfonyl fluoride after refluxing was examined from port F1 and the results are shown in Table 3.
Example 3
In this example, 20kg of trifluoromethanesulfonyl chloride was added, and 17.2kg of trifluoromethanesulfonyl fluoride was collected, whereby the reaction yield reached 95.3%. The collected trifluoromethanesulfonyl fluoride after refluxing was examined from port F1 and the results are shown in Table 3.
Example 4
200kg of potassium fluoride and 325kg of cyclohexanone were charged in advance in a 1000L reactor 3, and the heat exchange area was set to 20m2The temperature of the reflux heat exchanger 2 is controlled to be minus 30 ℃ to minus 25 ℃, the reactor 3, the reflux heat exchanger 2, the trifluoromethanesulfonyl fluoride storage tank 5 and pipelines among the same are vacuumized to 500Pa to 1000Pa, the temperature of the reactor 3 is controlled to be 50 ℃ to 55 ℃, and then liquid trifluoromethanesulfonyl Chloride (CF) is added3SO2Cl) is pressed from the bottom of the reactor 3 at the speed of 80kg/h, liquid trifluoromethanesulfonyl chloride enters the reactor 3 and is rapidly vaporized and reacts with potassium fluoride through a gas disperser 4 with the aperture of 10 mu m, trifluoromethanesulfonyl fluoride generated in the reaction passes through a reflux heat exchanger 2 and is collected in a trifluoromethanesulfonyl fluoride storage tank 5 with the temperature of-20 ℃ to-18 ℃.
In this example, 500kg of trifluoromethanesulfonyl chloride was added altogether, and 430.3kg of trifluoromethanesulfonyl fluoride were collected altogether, whereby the reaction yield reached 95.4%. The collected trifluoromethanesulfonyl fluoride after refluxing was examined from port F1 and the results are shown in Table 3.
Example 5
In this example, 333.3kg of trifluoromethanesulfonyl chloride was added altogether, 291.3kg of trifluoromethanesulfonyl fluoride was collected altogether, and the reaction yield reached 96.8%. The collected trifluoromethanesulfonyl fluoride after refluxing was examined from port F1 and the results are shown in Table 3.
Example 6
200kg of potassium fluoride and 350kg of cyclohexanone were charged in advance in a 1000L reactor 3, and the heat exchange area was set to 20m2The temperature of the reflux heat exchanger 2 is controlled to be minus 25 ℃ to minus 20 ℃, the reactor 3, the reflux heat exchanger 2, the trifluoromethanesulfonyl fluoride storage tank 5 and pipelines among the same are vacuumized to 500Pa to 1000Pa, the temperature of the reactor 3 is controlled to be 50 ℃ to 55 ℃, then liquid trifluoromethanesulfonyl chloride is pressed from the bottom of the reactor 3 at the speed of 60kg/h, the liquid trifluoromethanesulfonyl chloride is rapidly vaporized after entering the reactor 3 and reacts with potassium fluoride upwards through a gas disperser 4 with the aperture of 20 mu m, and trifluoromethanesulfonyl fluoride generated by the reaction is collected in the trifluoromethanesulfonyl fluoride storage tank 5 with the temperature of minus 15 ℃ to minus 13 ℃ after passing through the reflux heat exchanger 2.
In this example, 400kg of trifluoromethanesulfonyl chloride was added altogether, and 345.8kg of trifluoromethanesulfonyl fluoride were collected altogether, whereby the reaction yield reached 95.8%. The collected trifluoromethanesulfonyl fluoride after refluxing was examined from port F1 and the results are shown in Table 3.
TABLE 3
| Component name | CF3SO2F | H2O | C6H10O |
| Example 1 content (vol)% | ≥99.5 | 0.0059 | 0.1326 |
| Example 2 content (vol)% | ≥99.5 | 0.0046 | 0.1023 |
| Example 3 content (vol)% | ≥99.5 | 0.0051 | 0.1752 |
| Example 4 content (vol)% | ≥99.5 | 0.0063 | 0.1339 |
| Example 5 content (vol)% | ≥99.5 | 0.0076 | 0.2311 |
| Example 6 content (vol)% | ≥99.5 | 0.0071 | 0.1568 |
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A device for preparing trifluoromethanesulfonyl fluoride is characterized in that: the device comprises a trifluoromethanesulfonyl chloride storage tank, a reactor, a reflux heat exchanger and a trifluoromethanesulfonyl fluoride storage tank;
the reactor is a reaction container containing a stirring mechanism and a heating mechanism;
the discharge hole of the trifluoromethanesulfonyl chloride storage tank is connected with the feed inlet at the bottom of the reactor, potassium fluoride and cyclohexanone are filled in the reactor, the gas outlet at the upper part of the reactor is connected with the lower part of the reflux heat exchanger, and the upper part of the reflux heat exchanger is connected with the trifluoromethanesulfonyl fluoride storage tank.
2. The apparatus for preparing trifluoromethanesulfonyl fluoride according to claim 1, wherein: the apparatus further comprises a gas disperser mounted at the bottom of the interior of the reactor.
3. The apparatus for preparing trifluoromethanesulfonyl fluoride according to claim 2, wherein: the aperture of the gas disperser is 10-30 μm.
4. The apparatus for preparing trifluoromethanesulfonyl fluoride according to claim 1, wherein: the heat exchange area of the reflux heat exchanger is 1m2～20m2。
5. The apparatus for preparing trifluoromethanesulfonyl fluoride according to claim 1, wherein: the upper part of the reflux heat exchanger is provided with an analysis port.
6. A process for preparing trifluoromethanesulfonyl fluoride using the device according to any one of claims 1 to 5, characterized in that: the steps of the method are as follows,
according to trifluoromethanesulfonyl chloride: potassium fluoride: cyclohexanone 1: (0.4-0.62): (0.65-1), pre-filling potassium fluoride and cyclohexanone into a reactor, allowing trifluoromethanesulfonyl chloride to enter from the bottom of the reactor and react with potassium fluoride at 40-60 ℃, collecting trifluoromethanesulfonyl fluoride generated by the reaction in a trifluoromethanesulfonyl fluoride storage tank at-20-0 ℃ after passing through a reflux heat exchanger at-30-10 ℃, wherein the purity of the collected trifluoromethanesulfonyl fluoride is not less than 99.5 vol%, the moisture content of the collected trifluoromethanesulfonyl fluoride is not more than 0.01 vol%, and the content of cyclohexanone is not more than 0.3 vol%.
7. The process for preparing trifluoromethanesulfonyl fluoride according to claim 6, characterized in that: the purity of the potassium fluoride is more than or equal to 99 wt%; the purity of the trifluoromethanesulfonyl chloride is more than or equal to 99.5 wt%, and the purity of the cyclohexanone is more than or equal to 99 wt%.
8. The process for preparing trifluoromethanesulfonyl fluoride according to claim 6, characterized in that: the ratio of the feeding speed of the trifluoromethanesulfonyl chloride to the heat exchange area of the reflux heat exchanger is (2.5-4.5) kg/(h.m)2)。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011475878.2A CN112724047B (en) | 2020-12-15 | 2020-12-15 | Device and method for preparing trifluoro methanesulfonyl fluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011475878.2A CN112724047B (en) | 2020-12-15 | 2020-12-15 | Device and method for preparing trifluoro methanesulfonyl fluoride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112724047A true CN112724047A (en) | 2021-04-30 |
| CN112724047B CN112724047B (en) | 2023-10-17 |
Family
ID=75602213
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011475878.2A Active CN112724047B (en) | 2020-12-15 | 2020-12-15 | Device and method for preparing trifluoro methanesulfonyl fluoride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112724047B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115400714A (en) * | 2022-09-21 | 2022-11-29 | 中船(邯郸)派瑞特种气体股份有限公司 | Production device and method of trifluoromethanesulfonic acid |
| US11680041B1 (en) | 2021-12-07 | 2023-06-20 | Ses Holdings Pte. Ltd. | Processes for producing high-purity N,N-dialkyl perfluoroalkylsulfonamide |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101039922A (en) * | 2004-10-20 | 2007-09-19 | 组合化学工业株式会社 | 3-triazolylphenyl sulfide derivative and insecticide/acaricide/nematici`de containing the same as active ingredient |
| CN101396647A (en) * | 2007-09-29 | 2009-04-01 | 中科合成油技术有限公司 | Gas-liquid-solid three-phase suspended bed reactor for f-t synthesis and use thereof |
| CN201372256Y (en) * | 2009-03-04 | 2009-12-30 | 中国石油天然气股份有限公司 | Kettle-type high-efficiency esterification reactor for synthesizing dicarboxylic acid ester |
| CN101747238A (en) * | 2008-12-11 | 2010-06-23 | 张家港市国泰华荣化工新材料有限公司 | Method for separating and preparing methanesulfonyl fluoride CH3SO2F by material generated after reaction of methylsufonyl chloride and potassium fluoride |
| CN101747237A (en) * | 2008-12-11 | 2010-06-23 | 张家港市国泰华荣化工新材料有限公司 | Method for preparing methanesulfonyl fluoride CH3SO2F by methylsufonyl chloride CH3SO2Cl |
| CN101842348A (en) * | 2007-11-06 | 2010-09-22 | 中央硝子株式会社 | Process for preparation of trifluoromethanesulfonyl fluoride |
| CN203365361U (en) * | 2013-04-29 | 2013-12-25 | 齐齐哈尔大学 | Heat transfer rate measuring device for kettle type reactor |
| CN104140353A (en) * | 2014-07-18 | 2014-11-12 | 江西格美氟化工有限公司 | Method for preparing 1,1,1-halothane through liquid phase one-step fluorination of vinylidene chloride |
| CN104457854A (en) * | 2014-12-11 | 2015-03-25 | 安徽科技学院 | Liquid metal medium forced convection experimental loop |
| FR3043085A1 (en) * | 2015-10-29 | 2017-05-05 | Arkema France | FUNCTIONALIZED FLUORINATED COPOLYMERS |
| CN109824551A (en) * | 2019-04-04 | 2019-05-31 | 武汉大学 | A method of trimethyl fluoride sulfonyl fluorine is prepared by trimethyl fluoride sulfonyl chlorine |
| CN111676063A (en) * | 2020-04-09 | 2020-09-18 | 宁波科元精化有限公司 | Processing technology for improving 5# and 7# white oil |
-
2020
- 2020-12-15 CN CN202011475878.2A patent/CN112724047B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101039922A (en) * | 2004-10-20 | 2007-09-19 | 组合化学工业株式会社 | 3-triazolylphenyl sulfide derivative and insecticide/acaricide/nematici`de containing the same as active ingredient |
| CN101396647A (en) * | 2007-09-29 | 2009-04-01 | 中科合成油技术有限公司 | Gas-liquid-solid three-phase suspended bed reactor for f-t synthesis and use thereof |
| CN101842348A (en) * | 2007-11-06 | 2010-09-22 | 中央硝子株式会社 | Process for preparation of trifluoromethanesulfonyl fluoride |
| CN101747238A (en) * | 2008-12-11 | 2010-06-23 | 张家港市国泰华荣化工新材料有限公司 | Method for separating and preparing methanesulfonyl fluoride CH3SO2F by material generated after reaction of methylsufonyl chloride and potassium fluoride |
| CN101747237A (en) * | 2008-12-11 | 2010-06-23 | 张家港市国泰华荣化工新材料有限公司 | Method for preparing methanesulfonyl fluoride CH3SO2F by methylsufonyl chloride CH3SO2Cl |
| CN201372256Y (en) * | 2009-03-04 | 2009-12-30 | 中国石油天然气股份有限公司 | Kettle-type high-efficiency esterification reactor for synthesizing dicarboxylic acid ester |
| CN203365361U (en) * | 2013-04-29 | 2013-12-25 | 齐齐哈尔大学 | Heat transfer rate measuring device for kettle type reactor |
| CN104140353A (en) * | 2014-07-18 | 2014-11-12 | 江西格美氟化工有限公司 | Method for preparing 1,1,1-halothane through liquid phase one-step fluorination of vinylidene chloride |
| CN104457854A (en) * | 2014-12-11 | 2015-03-25 | 安徽科技学院 | Liquid metal medium forced convection experimental loop |
| FR3043085A1 (en) * | 2015-10-29 | 2017-05-05 | Arkema France | FUNCTIONALIZED FLUORINATED COPOLYMERS |
| CN109824551A (en) * | 2019-04-04 | 2019-05-31 | 武汉大学 | A method of trimethyl fluoride sulfonyl fluorine is prepared by trimethyl fluoride sulfonyl chlorine |
| CN111676063A (en) * | 2020-04-09 | 2020-09-18 | 宁波科元精化有限公司 | Processing technology for improving 5# and 7# white oil |
Non-Patent Citations (2)
| Title |
|---|
| 李风荣等: "采用低温工艺生产液化石油气" * |
| 范春雷等: "三氟甲烷磺酸酐的合成研究" * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11680041B1 (en) | 2021-12-07 | 2023-06-20 | Ses Holdings Pte. Ltd. | Processes for producing high-purity N,N-dialkyl perfluoroalkylsulfonamide |
| CN115400714A (en) * | 2022-09-21 | 2022-11-29 | 中船(邯郸)派瑞特种气体股份有限公司 | Production device and method of trifluoromethanesulfonic acid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112724047B (en) | 2023-10-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2023116462A1 (en) | Synthesis method for hexafluorophosphate | |
| CN104261369B (en) | Preparation method of high purity phosphorus pentafluoride | |
| CN103130197B (en) | Continuous-pressure-changing rectification method and device for preparing medicine-level sulfoxide chloride | |
| CN101298318B (en) | Method and apparatus for preparing high-pure carbon tetrafluoride gas | |
| CN104311383B (en) | A kind of method of the hydrogen chloride production monochloro methane that utilizes by-product in tetrachloro-ethylene production process | |
| CN112724047B (en) | Device and method for preparing trifluoro methanesulfonyl fluoride | |
| CN103435517A (en) | Yield-increasing and energy-saving technology of carbon dioxide stripping urea and equipment of carbon dioxide stripping urea | |
| CN101440015B (en) | Method for producing methane chloride by using dilute hydrochloric acid | |
| CN113247870B (en) | Method and device for preparing high-purity nitrogen trifluoride gas | |
| CN208200379U (en) | A kind of germane production system | |
| CN111099957A (en) | Purification system and method for electronic-grade carbon tetrafluoride | |
| CN219744427U (en) | Device for separating and recovering sulfur dioxide and hydrogen chloride mixed tail gas | |
| CN214654573U (en) | Device for preparing trifluoromethanesulfonyl fluoride | |
| CN115487522B (en) | Hydrogen fluoride purification system and process | |
| CN114570051B (en) | Device and method for purifying trifluoromethanesulfonyl fluoride through continuous rectification | |
| CN114470826B (en) | Purification device and method of bis (trifluoromethanesulfonyl) imide | |
| CN104387300B (en) | A kind of purification process of fluoroform sulfonic acid fluoride | |
| WO2020212299A1 (en) | Process for the production of anhydrous methanesulfonic acid from methane and so3 | |
| CN109353994A (en) | The device and technique of chlorine aether tail gas production chlorosulfuric acid | |
| CN114014743A (en) | Method for continuously producing hexafluorobutadiene | |
| CN212881113U (en) | Gas-phase material recovery device of methyl ethyl carbonate device | |
| CN102603461A (en) | Method for preparing 1,2-dibromotetrafluoroethane from tail gas in production of tetrafluoroethylene | |
| CN101747241A (en) | Method for preparing trifluoromethyl sulfonic acid potassium CF3SO3K by electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F | |
| CN111646916A (en) | Method for co-producing trifluoroacetamide and ammonium bifluoride from hexafluoropropylene oxide by-product | |
| CN109368601B (en) | Device and method for producing chlorosulfonic acid from m/p-phthaloyl chloride tail gas |
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 | ||
| CB02 | Change of applicant information |
Address after: 057550 No. five Weir Road, chemical industry gathering area, Feixiang District, Handan, Hebei, 1 Applicant after: China shipbuilding (Handan) Perry Special Gas Co.,Ltd. Address before: No.1 Weiwu Road, chemical industry gathering area, Feixiang County, Handan City, Hebei Province Applicant before: PERIC SPECIAL GASES Co.,Ltd. |
|
| CB02 | Change of applicant information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |