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Preparation method of asymmetric type bi-fluoro sulfimide potassium

A bisfluorosulfonimide potassium, asymmetric technology, applied in the field of preparation of asymmetric bisfluorosulfonyl imide potassium, can solve the problems of high toxicity and high equipment requirements, and achieve reasonable cost and high product purity , purification of simple effects

Active Publication Date: 2011-09-14
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The latest report on the synthesis of asymmetric imines and alkali metal salts (Zhou Zhibin et al., CN 101747242 A, 2010; Hong-Bo Han et al. Chem. Lett. 2010, 39, 472) improved the previous methods , using chlorosulfonic acid, sulfamic acid and thionyl chloride as raw materials, asymmetric bis(fluorosulfonyl)imides and alkali metal salts were synthesized by a "one-pot method", but chlorosulfur was still used Although its toxicity is less than that of fluorosulfonic acid, it is still highly toxic, and it is highly corrosive and requires high equipment requirements.

Method used

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  • Preparation method of asymmetric type bi-fluoro sulfimide potassium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) In a 250mL three-necked flask, add 7.48g (25mmol) perfluorobutylsulfonamide and 1.19g (22mmol) sodium methoxide, 10mL methanol, and add 100mL anhydrous ether to dissolve the solid, heat to reflux for 3 hrs and filter, the filtrate After distillation under reduced pressure, the residue was washed with 30 mL of anhydrous ether to remove excess perfluorobutanesulfonamide, and dried in a vacuum to obtain sodium perfluorobutanesulfonamide, weighing 6.58 g, with a conversion rate of 93%;

[0025] 2) Under the protection of nitrogen, in a 250mL three-necked flask, 5g (15.6mmol) perfluorobutylsulfonamide sodium was dissolved in 100mL anhydrous acetonitrile at room temperature, and 25.1g (156mmol) hexamethyldi Silamine (HMDS) was gradually dropped into the above solution, and heated to reflux at 110 °C for 12 hr; the solvent and excess HMDS were removed under reduced pressure to obtain (C 4 f 9 SO 2 )N(Na)Si(CH 3 ) 3 , which is easy to deliquescence and difficult to obtai...

Embodiment 2

[0030] 1) In a 250mL three-necked flask, add 7.48g (25mmol) perfluorobutanesulfonamide and 1.19g (22mmol) sodium methoxide, 10mL methanol, and add 100mL anhydrous ether to dissolve the solid, heat to reflux for 5 hr and filter, the filtrate Distilled under reduced pressure, the residue was washed with 30 mL of anhydrous ether to remove excess perfluorobutanesulfonamide, and dried in vacuum to obtain sodium perfluorobutanesulfonamide with a conversion rate of 94.5%;

[0031] 2) Under nitrogen protection, in a 250mL three-necked flask, dissolve 5g (15.6mmol) sodium perfluorobutanesulfonamide in 100mL anhydrous acetonitrile at room temperature, and gradually drop 37.7g (234mmol) HMDS just distilled into In the above solution, heat and reflux at 110 ° C for 24 hr; remove the solvent and excess HMDS under reduced pressure to obtain (C 4 f 9 SO 2 )N(Na)Si(CH 3 ) 3 , which is easy to deliquescence and difficult to obtain conversion rate;

[0032] 3) Under the protection of nitro...

Embodiment 3

[0036] 1) In a 250mL three-necked flask, add 20g (40mmol) perfluorooctane sulfonamide and 1.74g (32mmol) sodium methoxide, 20mL methanol, and add 150mL anhydrous ether to dissolve the solid, heat and reflux for 4 hrs and filter, and the filtrate is passed through Distilled under reduced pressure, the residue was washed with 50 mL of anhydrous ether to remove unreacted perfluorooctane sulfonamide, and dried in vacuo to obtain sodium perfluorobutane sulfonamide with a conversion rate of 89%;

[0037] 2) Under the protection of nitrogen, in a 250mL three-necked flask, dissolve 8g (15.4mmol) sodium peroctylsulfonamide in 100mL of anhydrous acetonitrile at room temperature, and gradually drop 24.9g (154mmol) of HMDS just distilled into the above solution, heated to reflux for 36 hr; the solvent and excess HMDS were removed under reduced pressure to obtain (C 4 f 9 SO 2 )N(Na)Si(CH 3 ) 3 , which is easy to deliquescence and difficult to obtain conversion rate;

[0038] 3) Under...

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Abstract

The invention discloses a preparation method of asymmetric type bi-fluoro sulfimide potassium, which includes the following steps: dissolving sulfonamide and sodium methoxide in methanol and ether, reflowing and filtering; decompressing and concentrating filtrate, and vacuum drying to obtain sodium amide sulfonylurea; conducting backflow reaction of newly distilled hexamethyldisilazane and the sodium amide sulfonylurea, decompressing and distilling to obtain trimethylsilane sodium bis[(perfluoroalkyl)sulfonyl]imides; slowly dripping sulfonyl chloride in trimethylsilane sodium bis[(perfluoroalkyl)sulfonyl]imides solution; dissolving by using the ether after backflow reaction, washing and decompressing, thus obtaining (RfSO2) (ClSO2) NH; and adding KF in (RfSO2) (ClSO2) NH solution, conducting reflux reaction, filtering, decompressing, distilling and recrystallizing by using CH-2 Cl2, thus obtaining the asymmetric type bi-fluoro sulfimide potassium. The preparation method has the advantages of easy product separation, little toxicity and corrosivity of raw materials, low requirement on equipment and moderate cost.

Description

technical field [0001] The invention relates to the technical field of electrolyte salt production for lithium secondary batteries, in particular to a method for preparing an asymmetric potassium bisfluorosulfonyl imide. Background technique [0002] Electrolyte salt is an important part of the electrolyte of lithium-ion batteries, and its performance largely determines the performance of lithium-ion batteries in all aspects. Currently the most used electrolyte salt is LiPF 6 , due to its comprehensive advantages of good electrical conductivity, stable electrochemical performance and less environmental pollution, it has been widely used in the market at present. However, its thermal stability is poor, and it will decompose at a certain temperature to produce LiF and PF. 5 , PF 5 When it meets water, it will be hydrolyzed to produce highly corrosive HF, which will have a great negative impact on the positive electrode material of the lithium battery and the cycle charge an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/48C07C303/40H01M10/0568
CPCY02E60/12Y02E60/10
Inventor 詹晓力胡锋波张庆华陈丰秋
Owner ZHEJIANG UNIV
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