CN115959638A - Preparation method of bis (fluorosulfonyl) imide and alkali metal salt thereof - Google Patents
Preparation method of bis (fluorosulfonyl) imide and alkali metal salt thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of bis (fluorosulfonyl) imide and alkali metal salt thereof. Firstly, adopting a one-step method to synthesize the bis-fluorosulfonyl imide, mixing chlorosulfonyl isocyanate and fluorosulfonic acid, continuously introducing anhydrous hydrogen fluoride gas while stirring, and reacting at 25-130 ℃ for 4-30 hours under the action of a catalyst to synthesize the bis-fluorosulfonyl imide. The method improves the production efficiency, reduces the energy consumption, and avoids the synthesis of the dichlorinated sulfonimide (HClSI) which is sensitive to moisture and is easy to decompose to generate byproducts in the conventional route. Then under the protection of inert atmosphere, mixing a compound containing alkali metal cations with an organic solvent, reacting with the bis (fluorosulfonyl) imide at 15-120 ℃ to neutrality to obtain a bis (fluorosulfonyl) imide alkali metal salt solution, and carrying out post-treatment on the reacted material to obtain the corresponding bis (fluorosulfonyl) imide salt.
Description
Technical Field
The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of bis (fluorosulfonyl) imide and alkali metal salt thereof.
Background
The bifluorosulfonyl imide salt (MFSI for short) is a key raw material forming an electrolyte in important energy storage equipment such as a metal ion secondary battery, a super capacitor and the like, and has the characteristics of good electrochemical stability, good hydrolysis resistance, high conductivity and the like, for example, bifluorosulfonyl imide potassium salt (KFSI for short) is used as an additive of the super capacitor, bifluorosulfonyl imide lithium salt (LiFSI for short) is used as electrolyte lithium salt of a lithium ion battery, and bifluorosulfonyl imide sodium salt (NaFSI for short) is used as electrolyte lithium salt of a sodium ion battery. Especially in power batteries, the safety of the power batteries can be effectively improved, the cycle performance and the rate capability of the power batteries are improved, and the power batteries have excellent application prospects.
For the synthesis method of the bis-fluorosulfonyl imide salt (MFSI for short), HClSI is generally prepared first, then fluorinated to bis-fluorosulfonyl imide (HFSI), and finally salified to obtain MFSI. As for the production of bis (fluorosulfonyl) imide (HFSI), there have been studies on the use of urea [ CO (NH) which is available as a raw material and is inexpensive 2 ) 2 ]And fluorosulfonic acid (FSO) 3 H) By reacting, HFSI formed and FSO added in excess 3 H can be recovered by distillation under reduced pressure (e.g. US8337797, US5916475, etc.). However, the yield of HFSI products disclosed in patent US8337797 is only about 40%, and the conditions in the preparation process and the post-treatment of the products are harsh, the energy consumption is large, and the large-scale production is not facilitated.
Therefore, most domestic and overseas use the synthesis method of firstly synthesizing the bis-chlorosulfonyl imide (HClSI) by using chlorosulfonic acid, sulfamic acid and thionyl chloride as raw materials, and then fluorinating the HClSI by using different fluorinating reagents to prepare the bis-fluorosulfonyl imide (HFSI) (such as CA2527802A1, CN106219503A and the like). However, the methods reported in these patents have the disadvantages of complicated process steps, low production efficiency, sensitivity of HClSI to water, rapid decomposition of pre-water, heat release and even explosion hazard. And the fluorination process produces HCl and SO 2 The by-products are difficult to treat, the safety risk is high, the complexing solvent is easy to react with HFSI, and the like, so that the high yield and purity of the products cannot be ensured, and the wide application of LiFSI in lithium batteries is limited. By sulfuryl fluoride (SO) 2 F 2 ) The synthesis of LiFSI from raw materials is also a relatively common synthesis route, for example, SO is used in patent WO2010113835A1 2 F 2 ，NH 3 And triethylamine (Et) 3 N) the bis (fluorosulfonyl) imide triethylamine salt is synthesized from cheap raw materials, has excellent ion exchange capacity, and can be used for efficiently preparing the bis (fluorosulfonyl) imide metal salt. However, excess Et in the reaction 3 N will promote SO 2 F 2 The fluorosulfonic acid, triethylamine salt and other by-products are generated by hydrolysis, so the method for preparing LiFSI is purified and processed into LiFSI in the later stageThe method is high, and large-scale production is difficult to realize.
Chinese patent document CN 112320772A (202011332936.6) discloses a method for preparing bis (fluorosulfonyl) imide, which comprises preparing bis (chlorosulfonyl) imide from chlorosulfonyl isocyanate and chlorosulfonic acid, reacting with anhydrous hydrogen fluoride under the action of a catalyst, and purifying under the environment of inert gas to obtain bis (fluorosulfonyl) imide. However, the patent still adopts a two-step reaction method, and has the disadvantages of complex process, high temperature, long reaction time and low yield. Chinese patent document CN 114604832A (202210275612.6) discloses a preparation method of bis (fluorosulfonyl) imide, wherein bis (fluorosulfonyl) imide can be obtained by reacting fluorosulfonyl isocyanate with fluorosulfonic acid at the reaction temperature of 80-150 ℃, and the yield is 73-76%. However, the fluorosulfonic acid isocyanate used in the method is high in price, so that the product cost is high, the requirement on equipment is high, and the method is not suitable for industrial production.
Disclosure of Invention
The invention aims to overcome the difficulties of complex production process, low product yield and the like in the existing preparation of the bis (fluorosulfonyl) imide and provide a preparation method of the bis (fluorosulfonyl) imide and an alkali metal salt thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a one-step method for synthesizing bis (fluorosulfonyl) imide comprises the following steps:
mixing chlorosulfonyl isocyanate and fluorosulfonic acid, stirring, continuously introducing anhydrous hydrogen fluoride gas, and reacting at 25-130 deg.C for 4-30 hr under the action of catalyst to synthesize the invented bis-fluorosulfonyl imide.
Wherein the molar ratio of chlorosulfonyl isocyanate, fluorosulfonic acid and hydrogen fluoride is 1:1.0 to 3..0: 1.0-6.0, wherein the molar ratio of chlorosulfonyl isocyanate to the catalyst is 1:0.1 per mill to 2 percent. The above reaction equation is as follows:
in a preferred embodiment of the present invention, in the one-step synthesis of bis-fluorosulfonyl imide, the molar ratio of chlorosulfonyl isocyanate to catalyst is 1:1 per mill to 0.5 percent. More preferably 1:0.1 to 0.2 percent.
In a preferred embodiment of the present invention, in the one-step synthesis of bis-fluorosulfonylimide, the molar ratio of chlorosulfonyl isocyanate to fluorosulfonic acid is 1:1.0 to 2. More preferably 1.1 to 1.2.
In a preferred embodiment of the present invention, in the one-step synthesis of bis-fluorosulfonyl imide, the molar ratio of chlorosulfonyl isocyanate to hydrogen fluoride is 1:1.0 to 4.0. More preferably 1.5 to 3.
In the preferred embodiment of the invention, the reaction temperature in the one-step synthesis of the bis-fluorosulfonyl imide is 65-85 ℃. More preferably from 65 to 75 ℃.
In a preferred embodiment of the invention, in the one-step synthesis of bis-fluorosulfonyl imide, the reaction time is 6 to 12 hours. More preferably 8 to 10 hours.
And cooling, crystallizing and distilling the reaction liquid to obtain the bis-fluorosulfonyl imide.
In a preferred embodiment of the invention, the catalyst is a lewis acid-based catalyst; a further preferred catalyst is SbCl 5 、SnCl 4 、MoCl 5 One kind of (1).
The preparation method of the bis-fluorosulfonyl imide provided by the invention at least has the following beneficial effects:
(1) The method adopts a one-step reaction to synthesize the bis-fluorosulfonyl imide, improves the production efficiency, reduces the energy consumption, and avoids the synthesis of the bis-fluorosulfonyl imide (HClSI) which is sensitive to water and is easy to decompose to generate a byproduct in the conventional route.
(2) The method adopts hydrogen fluoride as a fluorination reagent, effectively fluorinates the raw materials under the action of a small amount of catalyst, has high yield, and can obtain the high-purity bis (fluorosulfonyl) imide through cooling crystallization and reduced pressure distillation after the reaction is finished.
(3) The hydrogen chloride and the carbon dioxide generated in the reaction process are easy to separate, and the method has the advantages of less three wastes, low treatment cost, suitability for large-scale application and the like.
The invention also aims to provide a preparation method of the alkali metal salt of the bis-fluorosulfonylimide. The technical scheme is as follows:
a preparation method of bis (fluorosulfonyl) imide metal salt comprises the following steps:
under the protection of inert atmosphere, a compound containing alkali metal cations is mixed with an organic solvent, the obtained bis-fluorosulfonyl imide (HFSI) reacts at 15-120 ℃ to neutrality (pH is approximately equal to 7) to obtain a bis-fluorosulfonyl imide alkali metal salt solution, and the reacted material is subjected to post-treatment to obtain the corresponding bis-fluorosulfonyl imide salt.
Wherein the molar ratio of the bis-fluorosulfonyl imide to the compound containing an alkali metal cation is 1.0 to 5.0.
In a preferred embodiment of the present invention, the molar ratio of the bis-fluorosulfonylimide to the compound containing an alkali metal cation is 1.0 to 2.0; more preferably 1.0 to 1.6.
In a preferred embodiment of the invention, the temperature of the reaction is between 15 and 35 ℃, preferably between 20 and 25 ℃. The reaction time is 0.1 to 10 hours.
In a preferred embodiment of the present invention, the organic solvent is an organic aprotic solvent, and is one or a mixture of two or more of ethyl acetate, dimethyl carbonate, dichloromethane, toluene, petroleum ether, and acetonitrile.
Preferably, the compound containing an alkali metal cation is mixed with the organic solvent and the temperature is reduced to 5 to 10 ℃. The post-treatment refers to solid-liquid separation, recrystallization and drying.
The compound containing an alkali metal cation includes an alkali metal hydroxide, an alkali metal carbonate or an alkali metal hydrogencarbonate. The alkali metal is Li, na and K. Preferably Li 2 CO 3 、LiOH、Na 2 CO 3 、KOH、NaOH、K 2 CO 3 . The alkali metal bicarbonate includes lithium bicarbonate, sodium bicarbonate, and potassium bicarbonate.
The recrystallization method comprises the following steps: and concentrating the solution after reaction to be viscous under the reduced pressure, adding toluene or dichloromethane, and crystallizing to separate out a solid.
The bis-fluorosulfonyl imide metal salt prepared by the method has high yield, low content of chloride ions and metal ions, particularly extremely low water content which can be lower than 10ppm, is beneficial to application of the bis-fluorosulfonyl imide metal salt in the field of new energy, and can effectively improve the product life and quality stability of new energy equipment; the preparation method of the bis-fluorosulfonyl imide alkali metal salt can obtain bis-fluorosulfonyl imide salts (MFSI) of different metal types, and is favorable for promoting large-scale application of the bis-fluorosulfonyl imide alkali metal salt in lithium ion batteries and supercapacitors.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto. The experimental procedures without specifying specific conditions in the following examples were carried out according to the conventional methods and conditions, or according to the instructions of commercial products.
Example 1
A preparation method of bis (fluorosulfonyl) imide comprises the following steps:
to a 1000ml polytetrafluoroethylene reaction vessel were added 566g of chlorosulfonyl isocyanate and 440g of fluorosulfonic acid, followed by thoroughly stirring, and 1.20g of SbCl 5 120g of anhydrous hydrogen fluoride gas is uniformly introduced at 65 ℃, the reaction temperature is maintained, the reaction is carried out for 8 hours, and the reaction is stopped. The reaction product is cooled, crystallized and distilled under reduced pressure to obtain 632.8g of colorless transparent liquid bis (fluorosulfonyl) imide, the yield is 87.4%, and the purity is 99.9%.
Example 2
A preparation method of bis (fluorosulfonyl) imide comprises the following steps:
to a 1000ml polytetrafluoroethylene reaction vessel were added 566g of chlorosulfonyl isocyanate and 440g of fluorosulfonic acid, followed by thoroughly stirring, and 1.20g of SbCl 5 120g of anhydrous hydrogen fluoride gas was uniformly introduced at 75 ℃ and the reaction was stopped after maintaining the reaction temperature and reacting for 10 hours. Reaction products are subjected to temperature reduction crystallization and reduced pressure distillation to obtain 650.9g of colorless transparent liquid bis (fluorosulfonyl) imide, the yield is 89.9%, and the purity is 99.8%.
Example 3
A preparation method of bis (fluorosulfonyl) imide comprises the following steps:
a1000 ml polytetrafluoroethylene reaction vessel was charged with 566g of chlorosulfonyl isocyanate and 480g of fluorosulfonic acid, sufficiently stirred, and 2.40g of SbCl was added 5 240g of anhydrous hydrogen fluoride gas was uniformly introduced at 75 ℃ and the reaction was stopped after maintaining the reaction temperature and reacting for 8 hours. Cooling, crystallizing and distilling the reaction product under reduced pressure to obtain 665.4g of colorless transparent liquid bifluorosulfonyl imide, wherein the yield is 91.9 percent and the purity is 99.9 percent.
Example 4
A preparation method of bis (fluorosulfonyl) imide comprises the following steps:
adding 566g of chlorosulfonyl isocyanate and 480g of fluorosulfonic acid into a 1000ml polytetrafluoroethylene reaction vessel, stirring thoroughly, adding 2.08g of SnCl 4 240g of anhydrous hydrogen fluoride gas was uniformly introduced at 75 ℃ and the reaction was stopped after maintaining the reaction temperature and reacting for 8 hours. The reaction product is cooled, crystallized and distilled under reduced pressure to obtain 659.6g of colorless transparent liquid bis (fluorosulfonyl) imide, the yield is 91.1%, and the purity is 99.8%.
The preparation method of the lithium bis (fluorosulfonyl) imide comprises the following steps:
inert atmosphere N 2 Under the protection of (2), 73.89g of Li was charged in a 1000ml reaction vessel 2 CO 3 And 650ml of anhydrous ethyl acetate, stirring was started and the temperature was reduced to 10 ℃. 181g of difluoride sulfimide (HFSI) is weighed, added into a reaction system drop by drop, heated to 25 ℃, reacted until the pH value is neutral, and filtered by a filter membrane to obtain an ethyl acetate solution of the difluoride sulfimide lithium. And concentrating the solution to be viscous under the reduced pressure, adding dichloromethane, crystallizing to separate out a solid, and finally performing vacuum drying for 12 hours to obtain 164.4g of lithium bis (fluorosulfonyl) imide, wherein the yield is 87.9 percent and the purity is 99.8 percent.
The total yield of lithium bis (fluorosulfonyl) imide prepared in two steps is 80.1%. The water content of the obtained lithium bis (fluorosulfonyl) imide is less than 10ppm, the content of impurity metal ions is less than 10ppm, and the content of chloride ions is less than 5ppm.
Example 5
A preparation method of bis (fluorosulfonyl) imide comprises the following steps:
to a 1000ml polytetrafluoroethylene reaction vessel were added 566g of chlorosulfonyl isocyanate and 440g of fluorosulfonic acid, followed by thoroughly stirring, and 1.10g of MoCl 5 120g of anhydrous hydrogen fluoride gas is uniformly introduced at 65 ℃, the reaction temperature is maintained, the reaction is carried out for 8 hours, and the reaction is stopped. The reaction product is subjected to temperature reduction crystallization and reduced pressure distillation to obtain 641.5g of colorless transparent liquid difluo-sulfimide, the yield is 88.6 percent, and the purity is 99.9 percent.
The preparation method of the lithium bis (fluorosulfonyl) imide comprises the following steps:
inert atmosphere N 2 Under the protection of (1), 35.9g of LiOH and 500ml of anhydrous ethyl acetate are added to a 1000ml reaction vessel, stirring is started and the temperature is reduced to 10 ℃. 181g of difluoride sulfimide (HFSI) is weighed, added into a reaction system drop by drop, heated to 25 ℃, reacted until the pH value is neutral, and filtered by a filter membrane to obtain the dimethyl carbonate solution of difluoride sulfimide lithium. And concentrating the solution to be viscous under the reduced pressure, adding dichloromethane, crystallizing to separate out a solid, and finally performing vacuum drying for 12 hours to obtain 168.5g of lithium bis (fluorosulfonyl) imide, wherein the yield is 90.1% and the purity is 99.9%.
The total yield of lithium bis (fluorosulfonyl) imide prepared in two steps was 79.8%. The water content of the obtained lithium bis (fluorosulfonyl) imide is less than 10ppm, the content of impurity metal ions is less than 10ppm, and the content of chloride ions is less than 5ppm.
Example 6
A preparation method of bis (fluorosulfonyl) imide comprises the following steps:
to a 1000ml polytetrafluoroethylene reaction vessel were added 566g of chlorosulfonyl isocyanate and 440g of fluorosulfonic acid, followed by thoroughly stirring, and 1.10g of MoCl 5 120g of anhydrous hydrogen fluoride gas was uniformly introduced at 75 ℃ and the reaction was stopped after maintaining the reaction temperature and reacting for 10 hours. The reaction product is cooled, crystallized and distilled under reduced pressure to obtain 657.4g of colorless transparent liquid bis (fluorosulfonyl) imide, the yield is 90.8%, and the purity is 99.8%.
The preparation method of the sodium bis (fluorosulfonyl) imide comprises the following steps:
inert atmosphere N 2 Under the protection of (2), 105.99g of Na was added to a 1000ml reaction vessel 2 CO 3 And 550ml of anhydrous carbonic acidAnd (4) starting stirring the dimethyl ester, and cooling to 5 ℃. 181g of difluoride sulfimide (HFSI) is weighed, is added into a reaction system drop by drop, is heated to 20 ℃, reacts until the pH value is neutral, and is filtered by a filter membrane to obtain dimethyl carbonate solution of difluoride sulfimide sodium. And concentrating the solution to be viscous under the reduced pressure, adding toluene, crystallizing to separate out a solid, and finally performing vacuum drying for 12 hours to obtain 180.9g of sodium bis (fluorosulfonyl) imide, wherein the yield is 89.1% and the purity is 99.9%.
The total yield of lithium bis (fluorosulfonyl) imide prepared in two steps was 80.9%. The content of the obtained sodium bis (fluorosulfonyl) imide water is less than 10ppm, the content of impurity metal ions is less than 10ppm, and the content of chloride ions is less than 5ppm.
Example 7
A preparation method of bis (fluorosulfonyl) imide comprises the following steps:
adding 566g of chlorosulfonyl isocyanate and 480g of fluorosulfonic acid to a 1000ml polytetrafluoroethylene reaction vessel, stirring thoroughly, adding 3.3g of MoCl 5 240g of anhydrous hydrogen fluoride gas is uniformly introduced at 75 ℃, the reaction temperature is maintained, the reaction is carried out for 10 hours, and the reaction is stopped. Reaction products are subjected to temperature reduction crystallization and reduced pressure distillation to obtain 674.1g of colorless transparent liquid bifluoro sulfimide, the yield is 93.1%, and the purity is 99.9%.
The preparation method of the potassium bis (fluorosulfonyl) imide comprises the following steps:
inert atmosphere N 2 Under the protection of (2), 87.2g of KOH and 500ml of anhydrous acetonitrile are added to a 1000ml reaction vessel, the stirring is switched on and the temperature is reduced to 5 ℃. 181g of difluoride sulfimide (HFSI) is weighed, is added into a reaction system drop by drop, is heated to 25 ℃, reacts until the pH value is neutral, and is filtered by a filter membrane to obtain acetonitrile solution of difluoride sulfimide potassium. And concentrating the solution to be viscous under the reduced pressure, adding dichloromethane, crystallizing to separate out a solid, and finally performing vacuum drying for 12 hours to obtain 198.4g of potassium bis (fluorosulfonyl) imide, wherein the yield is 90.6% and the purity is 99.8%.
The overall yield of lithium bis (fluorosulfonyl) imide prepared in two steps is 84.3%. The water content of the obtained potassium bis (fluorosulfonyl) imide is less than 10ppm, the content of impurity metal ions is less than 10ppm, and the content of chloride ions is less than 5ppm.
Comparative example 1:
the same as example 1, the main difference is that fluorosulfonic acid is replaced by chlorosulfonic acid, and the specific preparation method of bis-fluorosulfonimide is as follows:
a1000 ml polytetrafluoroethylene reaction vessel was charged with 566g of chlorosulfonyl isocyanate and 512.7g of chlorosulfonic acid, sufficiently stirred, and 1.20g of SbCl was added 5 120g of anhydrous hydrogen fluoride gas is uniformly introduced at 65 ℃, the reaction temperature is maintained, the reaction is carried out for 8 hours, and the reaction is stopped. The reaction product is cooled, crystallized and distilled under reduced pressure to obtain 435.1g of colorless transparent liquid bifluorosulfonyl imide, the yield is 60.1%, and the purity is 99.3%.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. 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 (10)
1. The preparation method of the bis-fluorosulfonyl imide is characterized by comprising the following steps:
mixing chlorosulfonyl isocyanate and fluorosulfonic acid, stirring, continuously introducing anhydrous hydrogen fluoride gas, and reacting at 25-130 deg.C for 4-30 hr under the action of catalyst to synthesize the invented bis-fluorosulfonyl imide.
2. The method according to claim 1, wherein the molar ratio of chlorosulfonyl isocyanate, fluorosulfonic acid and hydrogen fluoride is 1: 1.0-3.0: 1.0-6.0, wherein the molar ratio of chlorosulfonyl isocyanate to the catalyst is 1:0.1 per mill-2 percent.
3. The method according to claim 1, wherein the molar ratio of chlorosulfonyl isocyanate to the catalyst is 1:1 per mill to 0.5 percent.
4. The method according to claim 1, wherein the molar ratio of chlorosulfonyl isocyanate to fluorosulfonic acid is 1:1.0 to 2; the molar ratio of chlorosulfonyl isocyanate to hydrogen fluoride is 1:1.0 to 4.0.
5. The method of claim 1, wherein the reaction temperature is 65 to 85 ℃; the reaction time is 6 to 12 hours.
6. The production method according to claim 1, wherein the catalyst is a Lewis acid-based catalyst; a preferred catalyst is SbCl 5 、SnCl 4 、MoCl 5 One kind of (1).
7. A preparation method of bis (fluorosulfonyl) imide metal salt is characterized by comprising the following steps:
under the protection of inert atmosphere, a compound containing alkali metal cations is mixed with an organic solvent, the mixture reacts with the bis (fluorosulfonyl) imide at the temperature of 15-120 ℃ to be neutral to obtain a bis (fluorosulfonyl) imide alkali metal salt solution, and the reacted material is subjected to post-treatment to obtain the corresponding bis (fluorosulfonyl) imide salt.
8. The method according to claim 7, wherein the molar ratio of the bis-fluorosulfonylimide to the compound containing an alkali metal cation is 1. Preferably, the molar ratio of the bis-fluorosulfonyl imide to the compound containing an alkali metal cation is 1.
9. The method according to claim 7, wherein the reaction temperature is 15 to 35 ℃; the organic solvent is an organic aprotic solvent, and is preferably one or a mixture of more than two of ethyl acetate, dimethyl carbonate, dichloromethane, toluene, petroleum ether and acetonitrile.
10. The production method according to claim 7, wherein the compound containing an alkali metal cation comprises an alkali metal hydroxide, an alkali metal carbonate or an alkali metal hydrogencarbonate; preferably, the alkali metal is Li, na, K; further preferablyLi 2 CO 3 、LiOH、Na 2 CO 3 、KOH、NaOH、K 2 CO 3 One or more of them.
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