CN116374966A - Preparation method of potassium bis (fluorosulfonyl) imide - Google Patents

Preparation method of potassium bis (fluorosulfonyl) imide Download PDF

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CN116374966A
CN116374966A CN202310335808.4A CN202310335808A CN116374966A CN 116374966 A CN116374966 A CN 116374966A CN 202310335808 A CN202310335808 A CN 202310335808A CN 116374966 A CN116374966 A CN 116374966A
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potassium
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difluorosulfimide
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崔毅鑫
徐鹏飞
张涛
马帅
杜二星
胡泽慧
王超
陈寅镐
张先满
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Zhejiang Zhongxin Fluorine Materials Co ltd
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    • C—CHEMISTRY; METALLURGY
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    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
    • C01B21/093—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more sulfur atoms
    • C01B21/096—Amidosulfonic acid; Salts thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/086—Compounds containing nitrogen and non-metals and optionally metals containing one or more sulfur atoms
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Abstract

The invention discloses a preparation method of potassium bis (fluorosulfonyl) imide, which belongs to the technical field of chemical synthesis and is characterized by comprising the following steps: in aqueous solution or polar organic solvent, organic ammonium salt of difluoro sulfonimide is as reaction raw material, directly react with potassium reagent through double decomposition, get difluoro sulfonimide potassium, this reaction has the advantage that the procedure is easy to operate, and the reaction product purity is good, the reaction yield is high, safe, environmental protection and high-efficient etc.; the method for preparing the difluoro sulfonimide potassium salt disclosed by the invention does not need to use strong corrosive gas reaction raw materials such as hydrofluoric acid and the like, is suitable for industrial production, and the generated difluoro sulfonimide potassium salt can be further used for chemical reactions with different purposes.

Description

Preparation method of potassium bis (fluorosulfonyl) imide
Technical Field
The invention relates to a preparation method of potassium bis (fluorosulfonyl) imide, belonging to the technical field of chemical synthesis.
Background
The lithium ion battery has the advantages of high energy density, high working voltage, wider working temperature, high recycling times and the like, and has wide application in the fields of electronic products, electric automobiles, aerospace, military products, storage of renewable energy sources and the like. However, we have to face the objective reality that the lithium resource reserves on earth are relatively scarce, the abundance of the lithium resource reserves in the crust is only 0.0065%, the lithium resource reserves on earth can only be maintained for about 65 years according to the current development speed of consuming the lithium resource (J.—Y. Hwang, S.—T.Myung, Y.— K.Sun, chem.Soc.Rev.2017,46, 3529-3614.), and meanwhile, the natural distribution of the lithium resource on the crust is also very uneven, so that the limited lithium resource can prevent the sustainable development pace of the lithium ion battery with new energy in the future. On the other hand, the distribution of potassium resources in the crust is relatively uniform, the abundance of the potassium resources is about 380 times of the abundance of the corresponding lithium resources, and the potassium resources are easier to extract than the corresponding lithium resources, so the production cost price of the potassium resources is far cheaper than that of the lithium resources. Since the theoretical capacity (theoretical capacity) of the potassium ion battery is closest to the theoretical capacity (B.Wang, et.al.Chem.Eur.J.2021,27,512) of the lithium ion battery, in order to ensure the safety, independence and sustainability of the development of new energy strategies, no matter in university research institutions or enterprises in the past decade, the steps of theoretical research and product development of potassium ion battery technology without resource limitation have been accelerated.
The electrolyte performance is one of key factors for determining the performance of all the ion batteries, and directly influences the storage capacity, electrochemical performance, safety and environmental protection of the ion batteriesPerformance and other important indexes. Considering the comprehensive factors such as the cost, the electrochemistry and the safety performance of the ion battery, the potassium hexafluorophosphate (KPF) 6 ) Is the electrolyte which is most widely adopted in the preparation of the potassium ion battery at present and plays a role in transporting charges. However, because hexafluorophosphate has poor thermal and chemical stability, poor low-temperature cycle efficiency, and is easy to be decomposed into highly corrosive Hydrogen Fluoride (HF) gas by trace water, and the like, the instability of hexafluorophosphate not only can cause electrolyte loss in the charge and discharge process, but also can damage the chemical structures of electrolyte and electrodes, thereby influencing the normal operation of the battery, leading to rapid attenuation of the battery capacity and bringing potential safety hazards, and bringing great challenges to practical production and application. Therefore, developing an electrolyte that is safer, more efficient, and suitable for use in harsh conditions such as low and high temperatures would be the most economical and efficient method of improving the chemical properties of potassium ion batteries. Bis (fluorosulfonyl) imide salt (M) + bisfluorosulfonylimide,M + FSI - ) The electrolyte has better comprehensive electrochemical properties such as conductivity, stability to heat and trace water, low-temperature circulation efficiency and the like than corresponding hexafluorophosphate, is considered to be the next generation novel ion battery electrolyte for replacing hexafluorophosphate electrolyte by the domestic and foreign industry professionals, and is the ideal electrolyte with the industrialization prospect at present. In addition, the potassium difluorosulfimide salt has application prospect in the fields of ionic liquid, catalysts and the like.
The preparation of the metal salt of the difluoro-sulfonyl imide is firstly to synthesize the difluoro-sulfonyl imide or the anion intermediate product of the difluoro-sulfonyl imide through reaction. Since the N-H bond of the bisfluorosulfonyl imide links two strongly electron withdrawing groups (FSO) 2 (-) its pKa value (1.28) is low, indicating that it is a very strong organic acid, which in organic solvents is very acidic close to sulfuric acid. The prior publications (J.K.Ruff, M.Lustig, inorg.Synth.1968,11,138; J.K.Ruff, inorg.Chem.1965,4,1446 and M.Beran, et al, polyhedron,2006,25,1292-1298) and the published patent (Zhou Zhibin, et al, CN 102786451A) report that a solution of difluorosulfimide can be directly reacted with potassium salts such as potassium carbonate or potassium perchlorate to give a potassium difluorosulfimide salt, and interestingly the resulting difluorosulfimide salt is obtained by the reactionThe potassium imide salt product is insensitive to water. Potassium bis-fluorosulfonyl imide can also be prepared by reacting bis-chlorosulfonyl imide with excess anhydrous potassium fluoride (M.Beran, J.Prihoda, Z.Anorg.Allg.Chem.2005, 631,55. And m.cernik, et al us Patent 7253317B 2). However, the raw materials for preparing the potassium difluorosulfonyl sulfite product by the method are not easy to obtain, the product purity is not high, and the method is not suitable for large-scale industrial production.
Disclosure of Invention
The invention aims to solve the defects in the existing production process of the potassium difluorosulfimide, and provides a safe, environment-friendly and efficient preparation method of the potassium difluorosulfimide, which has high product yield.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the potassium bis-fluorosulfonyl imide is characterized by comprising the following steps: in aqueous solution or polar organic solvent, the organic ammonium salt of the difluoro-sulfonyl imide is used as a reaction raw material, and directly reacts with a potassium reagent through double decomposition reaction to obtain the difluoro-sulfonyl imide potassium.
The reaction equation involved in the present invention is as follows:
Figure SMS_1
the further arrangement is that:
the polar organic solvent is selected from: acetonitrile, alcohols such as methanol and ethanol, acetone, esters such as dimethyl carbonate, diethyl carbonate, ethyl acetate and the like, ethers such as tetrahydrofuran, methyl tert-butyl ether, ethylene glycol dimethyl ether and the like, is preferably acetonitrile.
The potassium reagent is one of potassium hydroxide, potassium fluoride, potassium chloride, potassium bromide, potassium iodide, potassium perchlorate, potassium carbonate, potassium bicarbonate, potassium sulfate, potassium bisulfate, potassium oxalate, potassium acetate, potassium alkoxide and other potassium reagents.
The molar ratio of the organic ammonium salt of the difluoro-sulfonyl imide to the potassium reagent is 1:0.5-10, preferably 1:1.0-1.1.
The reaction temperature is 0 to 100 ℃, preferably 10 to 50 ℃.
After the reaction is finished, the reaction solvent is distilled off under reduced pressure to obtain a solid reactant, namely the potassium bis-fluorosulfonyl imide product.
The difluoro sulfimide organic ammonium salt is prepared by the following method:
the difluoro sulfinyl imine organic ammonium salt is obtained by taking sulfuryl fluoride and ammonium salt as reaction raw materials and reacting under the action of an aprotic polar solvent and an organic alkaline acid binding agent.
Figure SMS_2
The ammonium salt is selected from any one of the following ammonium salts: ammonium fluoride, ammonium chloride, ammonium bromide, ammonium bisulfate, ammonium bicarbonate, ammonium bisulfate.
The aprotic solvent is: acetonitrile, acetone, esters such as dimethyl carbonate, diethyl carbonate, ethyl acetate, etc., ethers such as tetrahydrofuran, methyl tert-butyl ether, ethylene glycol dimethyl ether, etc., and acetonitrile is preferred.
The organic alkaline acid binding agent is as follows: any one of trimethylamine, triethylamine, N-diisopropylethylamine, tri-N-propylamine, tri-N-butylamine, pyridine and the like, preferably triethylamine.
As a preferred embodiment: the prepared organic ammonium salt of the difluoro-sulfonyl imide can be directly used for preparing potassium difluoro-sulfonyl imide without purification, and is concretely as follows:
the preparation and production method of the potassium bis-fluorosulfonyl imide is characterized by comprising the following steps:
(1) The sulfuryl fluoride and ammonium salt are used as reaction raw materials, the reaction is carried out under the action of an aprotic polar solvent and an organic alkaline acid binding agent, the reaction solvent is removed by reduced pressure distillation, and the obtained reaction liquid is directly used for the chemical reaction for preparing the potassium difluorosulfimide without further purification;
(2) And (3) directly carrying out double decomposition reaction on the reaction solution prepared in the step (1) and a potassium reagent in an aqueous solution or a polar organic solvent to obtain a potassium bis (fluorosulfonyl) imide reaction solution.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a preparation method of potassium bis (fluorosulfonyl) imide, which has the advantages of easily available reaction raw materials, safety, easy operation, good product purity and high yield, and is suitable for large-scale industrial production.
2. The invention avoids the step of generating the difluoro sulfonamide strong acid intermediate by acidification, does not use strong materials such as sulfuric acid, has the advantages of high reaction safety, easy operation, low equipment requirement, suitability for industrial production and the like.
3. The invention has the advantages that the raw materials are easy to obtain, the ammonium salt serving as the main reaction raw material can be added into a reaction system in a simple powder solid or solution mode with accurate concentration, the simultaneous use of various gas raw materials is avoided, and the reaction control difficulty and the reaction risk are effectively reduced.
4. The prepared potassium bis (fluorosulfonyl) imide can be used for preparing other chemical reactions, such as lithium bis (fluorosulfonyl) imide, without purification.
Drawings
FIG. 1 is a diagram of a bis-fluorosulfonyl imide triethylammonium prepared according to the present invention 1 HNMR spectra.
FIG. 2 is a schematic representation of potassium bis-fluorosulfonyl imide prepared according to the present invention 19 F NMR spectrum.
Detailed Description
In the following examples, bis-fluorosulfonyl imide organoammonium salts were prepared as follows:
under the nitrogen atmosphere, 9.3g of ammonium fluoride is added into a 250mL high-pressure reaction kettle, the temperature is controlled to 10 ℃, 75.5g of triethylamine and 60.0g of acetonitrile are sequentially pumped in, the mixture is stirred for 0.5 hour, 51.0g of sulfuryl fluoride gas is slowly introduced at the temperature of 10 ℃ and is continuously kept at the temperature of 10 ℃ for 4 hours, and the reaction is finished. The reaction solution is distilled under reduced pressure to recover the reaction solvent, the concentrated solution is washed with water to obtain 65.0g of organic phase, the yield is 95 percent, and the product is obtained 1 The HNMR spectrum is shown in fig. 1: bis-fluorosulfonyl imide triethylammonium.
According to the method, triethylamine is replaced by trimethylamine, tri-n-butylamine and tripropylamine, and the dipotassium ammonium bis-fluorosulfonyl imide, tri-n-butylamine bis-fluorosulfonyl imide and tripropylamine are prepared respectively.
Example 1
In a 250mL three-port reaction flask, 55.0 g of triethylammonium bifluoride and 60.0g of acetonitrile were added under nitrogen atmosphere, followed by 26.0 g of anhydrous potassium carbonate, and stirring and heating reflux were carried out until no carbon dioxide gas was generated. Insoluble inorganic matters were removed by filtration, and the reaction solvent was recovered by distillation under the reduced pressure to give 39.6g of a white solid in a yield of 95%.
Product confirmation:
LC/MS test shows that the molecular weight (m/e) of the negative ion is 180, which is consistent with the chemical structure (II) of the difluoro sulfimide negative ion,
Figure SMS_3
the reaction product was further tested by anion chromatography, and the retention time and peak type of the ion peak of the obtained product are consistent with those of standard difluoro sulfonimide salt.
Of the reaction products 19 The F NMR spectrum is shown in FIG. 1, and only one resonance absorption peak of 51.90ppm fluorine is contained, which is consistent with the chemical structure of potassium difluorosulfonyl fluoride.
Example 2
55.0 g of triethylammonium bifluoride and 60 g of acetone were added to a 250mL three-port reaction flask under a nitrogen atmosphere, followed by addition of 31.0 g of anhydrous potassium bicarbonate, stirring and heating reflux until no carbon dioxide gas was generated. Insoluble inorganic matters were filtered, and the reaction solvent was recovered by distillation under reduced pressure to give 37.5g of a white solid in 90% yield.
Example 3
50.0 g of tripotassium ammonium bis-fluorosulfonyl imide and 60.0g of water were added to a 250mL three-port reaction flask under nitrogen atmosphere, followed by 19.0 g of potassium methoxide, and stirring and refluxing under heating until no carbon dioxide gas was generated. Insoluble inorganic matters were filtered, and the reaction solvent was recovered by distillation under reduced pressure to give 42.2g of a white solid in 92% yield.
Example 4
50 g of trimethylammonium bis-fluorosulfonyl imide and 60 g of water were added to a 250mL three-port reaction flask under nitrogen atmosphere, followed by 16 g of potassium hydroxide, and stirred and heated under reflux until no carbon dioxide gas was generated. Insoluble inorganic matters were filtered, and the reaction solvent was recovered by distillation under reduced pressure to give 41g of a white solid in 89% yield.
Example 5
60 g of tri-n-butyl ammonium bis-fluorosulfonyl imide and 60 g of tetrahydrofuran were added to a 250mL three-port reaction flask under nitrogen atmosphere, followed by 23 g of anhydrous potassium carbonate, and stirring and heating reflux were performed until no carbon dioxide gas was generated. Insoluble inorganic matters were filtered, and the reaction solvent was recovered by distillation under reduced pressure to give 33g of a white solid in 91% yield.
Example 6
60 g of tri-n-butyl ammonium bis-fluorosulfonyl imide and 60 g of ethylene glycol dimethyl ether were added to a 250mL three-port reaction flask under nitrogen atmosphere, followed by 13 g of potassium hydroxide, and stirring and heating reflux were performed until no carbon dioxide gas was generated. Insoluble inorganic matters were filtered, and the reaction solvent was recovered by distillation under reduced pressure to give 34g of a white solid in 93% yield.
Example 7
Under nitrogen atmosphere, 60 g of tripropylammonium difluorosulfonimide and 60 g of dimethyl carbonate were added to a 250mL three-port reaction flask, followed by 30 g of potassium bicarbonate, and stirred and heated under reflux until no carbon dioxide gas was generated. Insoluble inorganic matters were filtered, and the reaction solvent was recovered by distillation under reduced pressure to give 38g of a white solid in 94% yield.
Example 8
Under nitrogen atmosphere, 60 g of tripropylammonium difluorosulfonimide and 60 g of diethyl carbonate were added to a 250mL three-port reaction flask, followed by 23 g of potassium ethoxide, and stirred and heated under reflux until no carbon dioxide gas was generated. Insoluble inorganic matters were filtered, and the reaction solvent was recovered by distillation under reduced pressure to give 38g of a white solid in 93% yield.
The above examples illustrate only some embodiments of the invention and it should be clear to a person skilled in the art that the above examples do not limit the scope of the present application, which is defined by the claims.

Claims (10)

1. The preparation method of the potassium bis-fluorosulfonyl imide is characterized by comprising the following steps: in aqueous solution or polar organic solvent, using organic ammonium salt of difluoro-sulfonyl imide as reaction raw material, directly making double decomposition reaction with potassium reagent so as to obtain the invented product.
2. The method for preparing the potassium difluorosulfimide according to claim 1, wherein the method comprises the following steps: the polar organic solvent is selected from: any one or more of acetonitrile, methanol, ethanol, acetone, dimethyl carbonate, diethyl carbonate, ethyl acetate, tetrahydrofuran, methyl tertiary butyl ether and ethylene glycol dimethyl ether.
3. The method for preparing the potassium difluorosulfimide according to claim 1, wherein the method comprises the following steps: the potassium reagent is selected from any one of potassium hydroxide, potassium fluoride, potassium chloride, potassium bromide, potassium iodide, potassium perchlorate, potassium carbonate, potassium bicarbonate, potassium sulfate, potassium bisulfate, potassium oxalate, potassium acetate and potassium alkoxide.
4. The method for preparing the potassium difluorosulfimide according to claim 1, wherein the method comprises the following steps: the molar ratio of the organic ammonium salt of the difluoro-sulfonyl imide to the potassium reagent is 1:0.5-10.
5. The method for preparing the potassium difluorosulfimide according to claim 1, wherein the method comprises the following steps: the temperature of the reaction is 0-100 ℃.
6. The method for preparing the potassium difluorosulfimide according to claim 1, wherein the method comprises the following steps: the difluoro sulfimide organic ammonium salt is prepared by the following method: the difluoro sulfinyl imine organic ammonium salt is obtained by taking sulfuryl fluoride and ammonium salt as reaction raw materials and reacting under the action of an aprotic polar solvent and an organic alkaline acid binding agent.
7. The method for preparing the potassium difluorosulfimide according to claim 6, wherein the method comprises the following steps: the ammonium salt is selected from any one of the following: ammonium fluoride, ammonium chloride, ammonium bromide, ammonium bisulfate, ammonium bicarbonate, ammonium bisulfate.
8. The method for preparing the potassium difluorosulfimide according to claim 6, wherein the method comprises the following steps: the aprotic solvent is: acetonitrile, acetone, dimethyl carbonate, diethyl carbonate, ethyl acetate, tetrahydrofuran, methyl tert-butyl ether, and ethylene glycol dimethyl ether.
9. The method for preparing the potassium difluorosulfimide according to claim 6, wherein the method comprises the following steps: the organic alkaline acid binding agent is as follows: trimethylamine, triethylamine, N-diisopropylethylamine, tri-N-propylamine, tri-N-butylamine, pyridine.
10. The method for preparing potassium difluorosulfimide according to claim 6, comprising the steps of:
(1) The sulfuryl fluoride and ammonium salt are used as reaction raw materials, the reaction is carried out under the action of an aprotic polar solvent and an organic alkaline acid binding agent, the reaction solvent is removed by reduced pressure distillation, and the obtained reaction liquid is directly used for the chemical reaction for preparing the potassium difluorosulfimide without further purification;
(2) And (3) directly carrying out double decomposition reaction on the reaction solution prepared in the step (1) and a potassium reagent in an aqueous solution or a polar organic solvent to obtain a potassium bis (fluorosulfonyl) imide reaction solution.
CN202310335808.4A 2023-03-31 2023-03-31 Preparation method of potassium bis (fluorosulfonyl) imide Pending CN116374966A (en)

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