CN115974014A - Preparation method of potassium bis (fluorosulfonyl) imide - Google Patents
Preparation method of potassium bis (fluorosulfonyl) imide Download PDFInfo
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- CN115974014A CN115974014A CN202211689035.1A CN202211689035A CN115974014A CN 115974014 A CN115974014 A CN 115974014A CN 202211689035 A CN202211689035 A CN 202211689035A CN 115974014 A CN115974014 A CN 115974014A
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Abstract
The invention discloses a preparation method of potassium bis (fluorosulfonyl) imide, which comprises the following steps: (1) Reacting chlorosulfonic acid, sulfamic acid and thionyl chloride under the protection of nitrogen to obtain dichlorosulfimide; (2) Reacting dichlorosulfonimide with potassium chloride in a solvent under the action of a catalyst to obtain dichlorosulfonimide potassium; (3) Reacting the potassium bis (chlorosulfonyl) imide with potassium fluoride under the action of a catalyst to obtain the potassium bis (fluorosulfonyl) imide. The method has the advantages of simple process, milder reaction conditions, easier process control, high environmental protection property, no hydrogen fluoride generation, low risk coefficient and high yield, and is more suitable for industrial application.
Description
Technical Field
The invention relates to a preparation method of potassium bis (fluorosulfonyl) imide, belonging to the technical field of fluorine chemical industry and chemical synthesis.
Background
Lithium hexafluorophosphate is a commonly used electrolyte lithium salt at present, but the thermal stability and the chemical stability of the lithium hexafluorophosphate are poor, so that the application prospect of the lithium hexafluorophosphate is hindered. The lithium bis (fluorosulfonyl) imide has the advantages of high conductivity, high thermal stability, excellent low-temperature resistance, good hydrolytic stability and the like, and is the optimal choice for replacing lithium hexafluorophosphate at present. The potassium bifluorosulfonyl imide is an important raw material for preparing the lithium bifluorosulfonyl imide, so that the development of a preparation method of the potassium bifluorosulfonyl imide has important social significance and economic value.
Roesky et al, inorganic Chemistry (1969), 8 (8), 1733-5, reported that fluorination of bis (chlorosulfonyl) imide using arsenic trifluoride as a fluorinating agent, in which arsenic trifluoride as a fluorinating agent has a great toxicity and a great risk in practical operation, and hydrogen fluoride is generated in the reaction, which is highly corrosive, environmentally unfriendly and uncompetitive.
PCT patent application WO2011065502 reports a process for the preparation of potassium bis (fluorosulfonyl) imide by reacting bis (chlorosulfonyl) imide with zinc fluoride as a fluorinating agent. The method needs to use ammonia water to separate the product, the used fluorination reagent zinc fluoride is not easy to obtain industrially, the cost is high, a large amount of zinc-containing wastewater is generated, the industrial production is not facilitated, and hydrogen fluoride is generated in the reaction, so that the method has strong corrosivity, is not environment-friendly and has no competitive advantage.
Japanese Cao Da Kabushiki Kaisha CN103391896A firstly, chlorosulfonyl isocyanate reacts with chlorosulfonic acid to obtain bis-chlorosulfonyl imide, then the bis-chlorosulfonyl imide reacts with ammonium fluoride to obtain bis-fluorosulfonyl imide ammonium salt, and the bis-fluorosulfonyl imide potassium salt is obtained after the reaction with potassium hydroxide solution. The method has low yield of the intermediate bischlorosulfonimide, leads to high cost of industrial production of products, generates hydrogen fluoride in the reaction, has strong corrosivity, is not environment-friendly and has no competitive advantage.
Patent CN106006586a firstly reacts chlorosulfonic acid and chlorosulfonyl isocyanate in the presence of a catalyst to obtain bis-chlorosulfonyl imide, then reacts with hydrogen fluoride in the presence of a catalyst to obtain bis-fluorosulfonyl imide, and finally reacts with alkaline potassium compound to obtain bis-fluorosulfonyl imide potassium salt. The method has low yield of the intermediate bischlorosulfonimide, leads to higher industrial cost of the product, uses hydrogen fluoride, has higher danger coefficient, has more complex process and has no competitive advantage.
Therefore, the development of the preparation method of the potassium bis (fluorosulfonyl) imide with high yield, simple process, high environmental protection and low risk coefficient has more important social significance and higher economic value.
Disclosure of Invention
In view of the defects of the prior art, the invention provides the preparation method of the potassium bis (fluorosulfonyl) imide, which has the advantages of simple process, high environmental friendliness, no use of hydrogen fluoride, no generation of hydrogen fluoride, low risk coefficient and high yield, and is more suitable for industrial application.
The specific technical scheme of the invention is as follows:
a preparation method of potassium bis (fluorosulfonyl) imide comprises the following steps:
(1) Under the protection of gas, mixing sulfamic acid and thionyl chloride, heating to the reaction temperature, dropwise adding chlorosulfonic acid, and continuing the heat preservation reaction after the chlorosulfonic acid is dropwise added to obtain dichlorosulfimide;
(2) Under the protection of gas, uniformly mixing potassium chloride, a catalyst and an organic solvent I, then heating to the reaction temperature, dropwise adding a mixed solution of bischlorosulfonimide and the organic solvent I, and continuing a heat preservation reaction after dropwise adding to obtain bischlorosulfonimide potassium;
(3) Under the protection of gas, mixing the potassium bis (chlorosulfonyl) imide, the potassium fluoride, a catalyst and an organic solvent II, and then heating to react to obtain the potassium bis (fluorosulfonyl) imide.
Further, the reaction equation in the step (1) is as follows:
further, the reaction equation in the step (2) is as follows:
further, the reaction equation in the step (3) is as follows:
further, in the step (1), the molar ratio of chlorosulfonic acid, sulfamic acid and thionyl chloride is 1:1:2 to 5, such as 1:2, 1:3, 1:4, 1:5.
Further, in the step (1), sulfamic acid and thionyl chloride are mixed at 50-100 ℃ until complete mixing, and the mixing time is generally 1-3 hours.
Further, in the step (1), the dropping time of the chlorosulfonic acid is 5 to 6 hours, and the heat preservation reaction is continued for 10 to 30 hours after the dropping is finished.
Further, in the step (1), the temperature of dropping chlorosulfonic acid is 80 to 150 ℃, for example, 80 ℃, 90 ℃, 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃.
Further, in the step (1), after the reaction is carried out while maintaining the temperature, the bischlorosulfonimide is distilled under reduced pressure, wherein the pressure during distillation is controlled to be 1 to 5kPa, and the temperature is controlled to be 100 to 120 ℃.
Furthermore, in the step (1), the tail gas generated by the reaction is absorbed by two stages of water and one stage of alkali liquor, so that the pollution of the tail gas to the environment is avoided.
Further, in the step (2), the catalyst is selected from one of N-chlorosuccinimide, dioctyldimethylammonium chloride and N-dichloromethyleneaniline. The molar ratio of the catalyst to the bischlorosulfonimide is 1 to 10, for example, 1.
Further, in the step (2), the molar ratio of potassium chloride to bis (chlorosulfonyl) imide is 1:1.
further, in the step (2), the organic solvent one is one or a combination of two or more selected from the group consisting of nitromethane, nitroethane, dichloromethane, dichloroethane and trifluorotrichloroethane.
Further, in the step (2), the bischlorosulfonimide and the organic solvent I are mixed according to the volume ratio of 1:1-5, and the potassium chloride and the organic solvent I are mixed according to the mass ratio of 1:1-20.
Further, in the step (2), the first mixing and dissolving temperature of the potassium chloride and the organic solvent is controlled to be 80-100 ℃, and the time is controlled to be 30-90 min.
Further, in the step (2), the dropping temperature of the mixed solution of the bis-chlorosulfonyl imide and the first organic solvent is 100 to 150 ℃, for example, 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃ and 150 ℃, the dropping time is 8 to 10 hours, and the reaction is continued to be carried out for 4 to 5 hours at the temperature after the dropping.
Further, after the reaction in the step (2) is finished, filtering is carried out, and the obtained filter cake is the potassium bischlorosulfonimide.
Further, in the step (3), the catalyst is one of a calcium-based catalyst, an aluminum-based catalyst, a magnesium-based catalyst, and a chromium-based catalyst. The calcium-based catalyst may be CaO and the aluminum-based catalyst may be Al 2 O 3 The magnesium-based catalyst may be MgO, and the chromium-based catalyst may be Cr 2 O 3 . The molar ratio of the catalyst to potassium bis (chlorosulfonyl) imide is 1 to 100, such as 1.
Further, in the step (3), the molar ratio of the potassium bischlorosulfonimide to the potassium fluoride is 1:2 to 3.
Further, in the step (3), the reaction temperature of the product of the step (2) and potassium fluoride is controlled to be 100 to 150 ℃, for example, 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃ and 150 ℃, and the reaction time is controlled to be 10 to 15 hours.
Further, in the step (3), the organic solvent II is one or a combination of two or more selected from ethyl acetate, butyl acetate, ethyl formate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, acetonitrile and butyronitrile. The mass ratio of the potassium bischlorosulfonimide to the organic solvent II is 1:1-5.
Further, in the step (3), when the pH value of the reaction solution is neutral, the reaction is finished, and the reaction solution is cooled to room temperature and filtered. And distilling the obtained filtrate under reduced pressure, distilling off the organic solvent II, adding the organic solvent I when the organic solvent II is pasty, cooling to room temperature, and filtering to obtain a white solid. And drying the obtained white solid under reduced pressure to obtain the potassium bis (fluorosulfonyl) imide. The pressure of reduced pressure distillation is controlled to be 2-5 kPa, and the temperature is controlled to be 120-150 ℃. The drying pressure of the solid is controlled to be 5-10 kPa, and the temperature is controlled to be 60-80 ℃.
The invention has the following beneficial effects:
1. the method comprises the steps of firstly reacting potassium chloride with bischlorosulfonimide under the action of a catalyst to obtain potassium bischlorosulfonimide, and then reacting potassium fluoride with the potassium bischlorosulfonimide in the presence of the catalyst to obtain potassium bisfluorosulfonimide. Compared with the one-step reaction in CN111483986A, CN114436226A, the two-step reaction enables the reaction conditions to be milder, and particularly, the corresponding catalyst is added in the key synthesis steps of the potassium bis (chlorosulfonyl) imide and the potassium bis (fluorosulfonyl) imide, so that the synthesis process is easier to control, and the purity and the yield of the finally obtained potassium bis (fluorosulfonyl) imide are higher.
2. The method does not adopt raw materials such as zinc fluoride and hydrogen fluoride, does not generate a large amount of zinc-containing wastewater, does not generate hydrogen fluoride, adopts sylvite, has low risk coefficient in the whole production process, can purify and recycle the potassium chloride generated by the fluorination reaction, reduces the discharge of waste salt, has stronger environmental protection property, and is more beneficial to industrial production.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the invention to these embodiments.
Example 1
Step one, preparation of bis (chlorosulfonyl) imide
Under the protection of nitrogen, sulfamic acid and thionyl chloride (molar ratio is 1:3) are added into a dry synthesis kettle in sequence, stirred and heated, the temperature is controlled to be 60 ℃, and stirring is carried out under heat preservation for 2.5 hours, so that the sulfamic acid and the thionyl chloride are completely mixed and dissolved. Subsequently, the temperature was gradually increased to 100 ℃ and chlorosulfonic acid was added dropwise in an amount equimolar to sulfamic acid for 6 hours. After the chlorosulfonic acid is added dropwise, the reaction is carried out for 24 hours under the condition of heat preservation. Finally, vacuumizing to 4.5kPa, heating to 120 ℃ and distilling to obtain the bis-chlorosulfonyl imine, wherein the yield is 95.0 percent calculated by sulfamic acid, and the purity (HPLC) is 99.95 percent; the tail gas is absorbed by two stages of water and one stage of alkali liquor.
Step two, preparation of potassium bis (chlorosulfonyl) imide
Adding dichloromethane with the volume of 2 times of that of the bischlorosulfimide obtained in the step (1), uniformly mixing, and then hermetically placing for later use. Adding potassium chloride with the same molar ratio as the bischlorosulfonyl imide and N-chlorosuccinimide with the molar weight of the bischlorosulfonyl imide being 5 percent into a synthesis kettle, and then adding dichloromethane with the mass 5 times that of the potassium chloride. The temperature is raised to 80 ℃ and stirred for 40min. Then heating to 120 ℃, dropwise adding the prepared mixed solution of the bischlorosulfonimide and the dichloromethane, and dropwise adding for 10 hours. After the completion of the dropwise addition, the reaction was continued for 4 hours. Cooling to 40 ℃ and filtering, dissolving the obtained filter cake with acetonitrile with 2 times of mass, controlling the dissolving temperature at 40 ℃, and filtering to obtain the solution of the dichlorosulfonimide potassium in acetonitrile, wherein the yield is 95.6 percent calculated by the dichlorosulfonimide, and the purity (HPLC) is 99.90 percent.
Step three, preparation of potassium bis (fluorosulfonyl) imide
Adding the solution of the potassium bischlorosulfonyl imide into a synthesis kettle after nitrogen replacement, adding dry potassium fluoride and a calcium-based catalyst CaO, wherein the molar quantity of the potassium fluoride is 2 times that of the potassium bischlorosulfonyl imide, the molar quantity of the calcium-based catalyst is 5 percent of that of the potassium bischlorosulfonyl imide, heating to 150 ℃, and reacting for 10 hours under stirring. And dipping the reaction solution by using a pH test paper, wherein the reaction is finished when the pH is neutral. Cooled to room temperature and filtered. Decompressing the obtained filtrate to 2kPa, controlling the temperature to be 120 ℃, distilling out acetonitrile, adding dichloromethane when the filtrate is pasty, cooling to 60 ℃, and filtering to obtain white solid. And finally, drying the obtained white solid under reduced pressure at 60 ℃ in an environment of 5kPa to obtain a finished product of potassium bis (fluorosulfonyl) imide, wherein the finished product of potassium bis (fluorosulfonyl) imide is a white crystal, the yield is 95.1% by the potassium bis (chlorosulfonyl) imide, and the purity (HPLC) is 99.95%.
Example 2
Step one, preparation of bis (chlorosulfonyl) imide
Under the protection of nitrogen, sulfamic acid and thionyl chloride (molar ratio is 1:5) are sequentially added into a dry synthesis kettle, stirred and heated, the temperature is controlled to be 100 ℃, and the mixture is stirred for 1.5 hours under heat preservation, so that the sulfamic acid and the thionyl chloride are completely mixed and dissolved. Subsequently, the temperature was gradually increased to 150 ℃ and chlorosulfonic acid was added dropwise in an amount equimolar to sulfamic acid for 5 hours. After the chlorosulfonic acid is added dropwise, the reaction is carried out for 20 hours under the condition of heat preservation. Finally, vacuumizing to 5kPa, heating to 100 ℃ and distilling to obtain the dichlorosulfonimide, wherein the yield is 95.5 percent calculated by sulfamic acid, and the purity (HPLC) is 99.93 percent; the tail gas is absorbed by two stages of water and one stage of alkali liquor.
Step two, preparation of potassium bis (chlorosulfonyl) imide
Adding dichloroethane with the volume 5 times that of the dichlorosulfimide obtained in the step (1), uniformly mixing, and then hermetically placing for later use. Adding potassium chloride with the same molar ratio as the bischlorosulfonimide and dioctyldimethylammonium chloride with the molar quantity of 5 percent of the bischlorosulfonimide into a synthesis kettle, and then adding dichloroethane with the mass 10 times that of the potassium chloride. The temperature is raised to 100 ℃ and stirred for 80min. Then the temperature is raised to 150 ℃, and the prepared mixed solution of the bischlorosulfonimide and dichloroethane is dripped for 8 hours. After the completion of the dropwise addition, the reaction was continued for 5 hours. Cooling to 50 ℃ and filtering, dissolving the obtained filter cake with 5 times of diethyl carbonate by mass, controlling the dissolving temperature at 50 ℃, and filtering to obtain a solution of the dichlorosulfonimide potassium in the diethyl carbonate, wherein the yield is 96.1 percent calculated by the dichlorosulfonimide, and the purity (HPLC) is 99.92 percent.
Step three, preparation of potassium bis (fluorosulfonyl) imide
Adding the solution of potassium dichlorosulfonimide into a synthesis kettle after nitrogen replacement, and adding dry potassium fluoride and a chromium-based catalyst Cr 2 O 3 The molar quantity of the potassium fluoride is 2 times of that of the potassium bischlorosulfonyl imide, the molar quantity of the chromium-based catalyst is 5 percent of that of the potassium bischlorosulfonyl imide, the temperature is raised to 120 ℃, and the reaction is carried out for 15 hours under the stirring condition. Dipping the reaction solution by using a pH test paper, wherein the reaction is finished when the pH is neutral. Cooled to room temperature and filtered. Decompressing the obtained filtrate to 5kPa, controlling the temperature to be 150 ℃, distilling diethyl carbonate out, adding dichloroethane when the mixture is pasty, cooling to 80 ℃, and filtering to obtain white solid. Finally, the obtained white solid is dried under reduced pressure at 80 ℃ and under the environment of 10kPa to obtain the finished product of the potassium bis (fluorosulfonyl) imide, which is whiteColored crystals, 96.3% yield based on potassium bischlorosulfonimide and 99.93% purity (HPLC).
Example 3
The method comprises the following steps: preparation of bischlorosulfonimide example 2 was repeated.
Step two: preparation of potassium bis (chlorosulfonyl) imide, same as example 2, except that: the catalyst used is N-dichloromethyleneaniline. The yield of the obtained potassium bischlorosulfonimide based on bischlorosulfonimide was 96.2%, and the purity (HPLC) was 99.98%.
Step three: preparation of potassium bis-fluorosulfonylimide, same as in example 2, except that: the catalyst is aluminum-based catalyst Al 2 O 3 . The yield of the obtained potassium difluorosulfonimide was 95.9% in terms of potassium dichlorosulfonimide, and the purity (HPLC) was 99.92%.
Example 4
The method comprises the following steps: preparation of bischlorosulfonimide example 2 was repeated.
Step two: potassium bischlorosulfonimide was prepared as in example 2.
Step three: preparation of potassium bis-fluorosulfonylimide, same as in example 2, except that: the catalyst is magnesium-based catalyst MgO. The yield of the obtained potassium difluorosulfonimide was 96.0% in terms of potassium dichlorosulfonimide, and the purity (HPLC) was 99.95%.
Comparative example 1
Potassium bischlorosulfonimide was prepared as in example 2, except that: no catalyst dioctyldimethylammonium chloride was added. The yield of the obtained potassium bischlorosulfonimide based on bischlorosulfonimide was 90.2%, and the purity (HPLC) was 99.50%.
Comparative example 2
Potassium bis-fluorosulfonylimide was prepared according to the method of example 2, except that: no addition of Cr catalyst 2 O 3 . The yield of the obtained potassium difluorosulfonimide was 90.5% in terms of potassium dichlorosulfonimide, and the purity (HPLC) was 99.40%.
Comparative example 3
The method comprises the following steps: preparation of bischlorosulfonimide example 2 was repeated.
Step two: preparation of potassium bis (fluorosulfonyl) imide
216g of potassium fluoride (3.7 mol) and 704g of dichloroethane (7.1 mol) are put into a 2L four-mouth bottle, the temperature is raised to 80 ℃, the bis-chlorosulfonylimide reaction liquid in the first step is dripped for 3h (gas is released by violent reaction at the end of dripping, the temperature is controlled well), and the temperature is kept for 15h after dripping.
And washing the filter cake obtained by filtering with 590g of dichloroethane (5.9 mol) at room temperature for 2 hours, filtering, and drying the filter cake in vacuum at 120 ℃ to obtain a mixture of the crude potassium bis (fluorosulfonyl) imide and KF and KCl.
The dried product obtained above was dissolved in 996g of ethyl acetate (11.3 mol), and filtered. The solid is KF and KCl, and the filtrate is decompressed and concentrated at the temperature of less than 60 ℃ to obtain white solid which is crude product of potassium bis-fluoro-sulfonimide.
And (3) stirring the crude product with 520g of dichloromethane (6.1 mol) at room temperature for 15h for refining, filtering to obtain a filter cake, and vacuum-drying the filter cake at 30 ℃ for 24h to obtain the potassium bis (fluorosulfonyl) imide product. The yield was 85.5% based on bischlorosulfimide and the purity (HPLC) was 98.92%.
Claims (10)
1. A preparation method of potassium bis (fluorosulfonyl) imide is characterized by comprising the following steps:
(1) Under the protection of gas, mixing sulfamic acid and thionyl chloride, heating to the reaction temperature, dropwise adding chlorosulfonic acid, and continuing the heat preservation reaction after the dropping to obtain dichlorosulfimide;
(2) Under the protection of gas, uniformly mixing potassium chloride, a catalyst and an organic solvent I, then heating to the reaction temperature, dropwise adding a mixed solution of bischlorosulfonimide and the organic solvent I, and continuing a heat preservation reaction after dropwise adding to obtain bischlorosulfonimide potassium;
(3) Under the protection of gas, mixing the potassium bis (chlorosulfonyl) imide, the potassium fluoride, a catalyst and an organic solvent II, and then heating to react to obtain the potassium bis (fluorosulfonyl) imide.
2. The method of claim 1, wherein: in the step (1), the molar ratio of chlorosulfonic acid, sulfamic acid and thionyl chloride is 1:1:2 to 5.
3. The method for preparing a polycarbonate according to claim 1 or 2, wherein: in the step (1), the dropping time of the chlorosulfonic acid is 5 to 6 hours, the dropping temperature of the chlorosulfonic acid is 80 to 150 ℃, and the temperature is kept for reaction for 10 to 30 hours after the dropping is finished.
4. The method of claim 1, wherein: in the step (2), the catalyst is N-chlorosuccinimide, dioctyldimethylammonium chloride or N-dichloromethyleneaniline.
5. The method for preparing a polycarbonate resin composition according to claim 1 or 4, wherein: in the step (2), the molar ratio of the potassium chloride to the bischlorosulfonimide is 1:1, the molar ratio of the catalyst to the bischlorosulfonimide is 1-10.
6. The method of claim 1, 4 or 5, wherein: in the step (2), the dropping temperature of the mixed solution of the bischlorosulfonimide and the organic solvent I is 100-150 ℃, the dropping time is 8-10 hours, and the reaction is continued to be carried out for 4-5 hours under the temperature after the dropping.
7. The method for preparing a polycarbonate resin composition according to claim 1, wherein: in the step (3), the catalyst is a calcium-based catalyst, an aluminum-based catalyst, a magnesium-based catalyst or a chromium-based catalyst, the calcium-based catalyst is CaO, and the aluminum-based catalyst is Al 2 O 3 The magnesium-based catalyst is MgO, and the chromium-based catalyst is Cr 2 O 3 。
8. The method according to claim 1 or 7, wherein: in the step (3), the molar ratio of the potassium bischlorosulfonimide to the potassium fluoride is 1:2 to 3; the molar ratio of the catalyst to the potassium bischlorosulfonimide is 1-10.
9. The method of claim 1, wherein: in the step (2), the organic solvent I is at least one of nitromethane, nitroethane, dichloromethane, dichloroethane and trifluorotrichloroethane; in the step (3), the organic solvent II is at least one of ethyl acetate, butyl acetate, ethyl formate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, acetonitrile and butyronitrile; in the step (2), mixing potassium chloride with an organic solvent I according to a mass ratio of 1:1-20, and mixing dichlorosulfimide with the organic solvent I according to a volume ratio of 1:1-5; in the step (3), the mass ratio of the potassium bis (chlorosulfonyl) imide to the organic solvent II is 1:1-5.
10. The method of claim 1, 7 or 8, wherein: in the step (3), the reaction temperature is 100-150 ℃ and the reaction time is 10-15 hours.
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