Preparation method of lithium bis (fluorosulfonyl) imide

A technology of lithium bisfluorosulfonyl imide and bisfluorosulfonyl imide, which is applied in the field of preparation of lithium bisfluorosulfonyl imide, can solve the problems of inability to obtain high-quality products, difficulty in separation of final products, and difficult separation of intermediates and other issues, to achieve the effect of improving the catalytic effect, high quality, and sufficient contact area

Active Publication Date: 2021-06-11
ZHEJIANG SANMEI CHEM IND
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Problems solved by technology

[0003] Most of the existing synthetic methods of bisfluorosulfonimide lithium salt (LiFSI) are to first synthesize bischlorosulfonimide (HClSI), and then react it with a fluorinated metal salt to prepare the corresponding bisfluorosulfonimide Salt intermediate, which is then combined with lithium hydroxide (LiOH) or lithium carbonate (Li 2 CO 3 ) for cation exchange to obtain lithium bisfluorosulfonimide (LiFSI). The disadvantage is that it is difficult to continue after the cation exchange reaches equilibrium, so that the reaction is incomplete, the conversion rate is low, and the unreacted intermediate is difficult to completely react with LiFSI. Separation, so that high-quality products cannot be obtained
[0004] Chinese patent CN103524387A discloses that bischlorosulfonimide (HClSI) reacts with lithium chloride in thionyl chloride to generate bischlorosulfonimide lithium (LiClSI), and then utilizes metal fluorides (such as KF, ZnF 2 ) reacts with LiClSI as a fluorinating agent to obtain LiFSI, and the introduction of metal salts will cause difficulties in separation from the final product, thereby failing to obtain high-purity LiFSI

Method used

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  • Preparation method of lithium bis (fluorosulfonyl) imide
  • Preparation method of lithium bis (fluorosulfonyl) imide
  • Preparation method of lithium bis (fluorosulfonyl) imide

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preparation example Construction

[0035] Such as Figure 1 to Figure 5 Shown, be the preparation method of a kind of bisfluorosulfonimide lithium of the present invention, comprise the steps:

[0036] (a) Condensation reaction: first purify chlorosulfonic acid, the boiling point of chlorosulfonic acid is 151°C, use the principle of atmospheric distillation, use still kettle to distill chlorosulfonic acid, collect the fraction with boiling point at 150~152°C, generally Chlorosulfonic acid sold on the market contains a small amount of HCl, SO 3 , SO 2 , Cl 2 , SO 2 Cl 2 Impurities such as impurities are purified before use, which improves the purity of chlorosulfonic acid and reduces the impact of these impurities on subsequent reactions. Then add chlorosulfonic acid and catalyst into the reaction kettle, stir and heat up to 100-120°C, then add chlorosulfonyl isocyanate dropwise for reaction, the molar ratio of chlorosulfonic acid to chlorosulfonyl isocyanate is 1:0.9-1: 1.1, to obtain dichlorosulfonimide,...

Embodiment 1

[0052] 450g of chlorosulfonic acid and 1.8g of ZnCl 2Add it into the reaction kettle, start stirring, heat up to 100-105°C, add 630g of chlorosulfonyl isocyanate dropwise for reaction, stir for 9 hours, and distill under reduced pressure to obtain 813g of the product dichlorosulfonyl imide; take 680g of dichlorosulfonyl isocyanate Imine, 0.6gSnCl 4 Put it into the reaction tower 1, raise the temperature to 95-100°C, pass 160g of hydrogen fluoride into the reaction tower 1, react for 7 hours, cool down to room temperature naturally, and pass in nitrogen for 6 hours to obtain 561g of the product bisfluorosulfonimide; 500g of acetic acid Methyl ester, 10gLiOH·H 2 Add O into the reactor, lower the temperature to 0-5°C, add 150g of bisfluorosulfonimide under stirring, filter after the reaction, and precipitate the filtrate under reduced pressure to obtain viscous lithium salt of bisfluorosulfonimide , add the above-mentioned bisfluorosulfonyl imide lithium salt into a dissolving ...

Embodiment 2

[0054] 500g of chlorosulfonic acid and 2.0g of MnCl 2 Add it into the reaction kettle, start stirring, heat up to 100-105°C, add 700g of chlorosulfonyl isocyanate dropwise for reaction, stir for 10 hours, and distill under reduced pressure to obtain 946g of the product dichlorosulfonyl imide; take 800g of dichlorosulfonyl isocyanate imine, 1.2g SbCl 5 Put it into the reaction tower 1, raise the temperature to 95-100°C, pass 220g of hydrogen fluoride into the reaction tower 1, react for 8 hours, cool to room temperature naturally, and pass nitrogen for 7 hours to obtain 673g of the product bisfluorosulfonimide; 500g of carbonic acid Dimethyl ester, 34gLi 2 CO 3 Add it into the reactor, lower the temperature to 0-5°C, add 150g of bisfluorosulfonimide under stirring, filter after the reaction, and desolvate the filtrate under reduced pressure to obtain viscous lithium salt of bisfluorosulfonimide. Add the above-mentioned lithium bisfluorosulfonyl imide salt into a dissolving t...

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Abstract

The invention discloses a preparation method of lithium bis (fluorosulfonyl) imide. The preparation method comprises the following steps: (a) condensation reaction; (b) fluorination reaction; and (c) lithiation reaction. The method is short in process route, mild in process condition, simple in reaction system, easy to operate and control and high in reaction conversion rate, ensures high quality, high yield and high purity of the product, is green and environment-friendly, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of lithium ion electrolyte preparation, and in particular relates to a preparation method of lithium bisfluorosulfonyl imide. Background technique [0002] Lithium bisfluorosulfonyl imide (Li[N(SO 2 f) 2 ], referred to as LiFSI), is a very important lithium battery electrolyte additive, which has the advantages of high electrical conductivity, good thermal stability, high electrochemical stability, good cycle performance, and good safety performance. Compared with LiPF6, it has many excellent properties and is a better choice for lithium battery electrolyte. [0003] Most of the existing synthetic methods of bisfluorosulfonimide lithium salt (LiFSI) are to first synthesize bischlorosulfonimide (HClSI), and then react it with a fluorinated metal salt to prepare the corresponding bisfluorosulfonimide Salt intermediate, which is then combined with lithium hydroxide (LiOH) or lithium carbonate (Li 2 CO 3 ) ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/096C01B21/086
CPCC01B21/096C01B21/086C01P2006/80Y02E60/10
Inventor 王晓东胡彬柯泓昊韩达成徐爽
Owner ZHEJIANG SANMEI CHEM IND
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