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Preparation method of lithium bis(fluorosulfonyl)amide

A technology of lithium bisfluorosulfonyl imide and bisfluorosulfonyl imide, which is applied in the field of preparation of lithium bisfluorosulfonyl imide, can solve problems such as high price, affecting product application performance, and high price of fluorosulfonic acid

Active Publication Date: 2015-04-08
湖南福邦新材料有限公司
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Problems solved by technology

[0005] In the above method, the second type of synthetic method route is violently exothermic during the reaction process, and solid salt is formed, it is difficult to quickly transfer the heat out, the reaction process is difficult to control, and all the reactants are gaseous, and the reaction needs to be carried out under high pressure. High risk of reaction, large investment in equipment and other defects
The third type of synthetic method is that fluorosulfonic acid is expensive on the one hand, and fluorosulfonic acid is very corrosive to equipment on the other hand, and the yield of this method is not high, resulting in very high cost
First, high-purity LiClO 4 and LiBF 4 The current price is relatively high, exceeding 100,000 yuan / ton; secondly, the residual ClO in the product 4 Ion and BF 4 The ions are not easily removed and may affect the application performance of the product

Method used

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

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preparation example Construction

[0033] The invention provides a kind of preparation method of lithium bisfluorosulfonyl imide, comprising the following steps:

[0034] A) sulfuryl chloride and ammonia are reacted in the presence of an organic base to obtain an organic base salt of dichlorosulfonimide;

[0035] B) mixing the organic base salt of bischlorosulfonimide obtained in step A) with HF, and performing a fluorination reaction to obtain the organic base salt of bisfluorosulfonimide;

[0036] C) mixing the organic alkali salt of bisfluorosulfonimide obtained in step B) with an alkaline substance, and performing a neutralization reaction to obtain a crude alkali metal salt of bisfluorosulfonimide;

[0037] D) purifying the crude bisfluorosulfonimide alkali metal salt obtained in the step C) to obtain the bisfluorosulfonimide alkali metal salt;

[0038] E) mixing the alkali metal bisfluorosulfonyl imide obtained in the step D) with a lithiation reagent, and performing a displacement reaction to obtain lithi...

Embodiment 1

[0092] Under nitrogen protection conditions, 200g of ethyl acetate and 166.7g (1.65mol) of triethylamine were added to a 1L reactor, then the reactor was cooled to 5°C, and then 135g (1.0mol) of sulfuryl chloride was added to the reactor , and then slowly introduce 8.5 g (0.5 mol) of anhydrous ammonia gas into the reactor within 1 h under the control of the flow meter. After the introduction of ammonia gas is completed, the reaction is continued at 5° C. for 0.5 h. Then the cooling was stopped, and the reaction solution was allowed to warm up to room temperature naturally, and the reaction was continued for 48 h. After the reaction, the reaction solution was filtered to remove the triethylamine hydrochloride generated during the reaction to obtain the ethyl acetate filtrate of dichlorosulfonimide triethylamine salt.

[0093] Under the protection of nitrogen, the ethyl acetate filtrate of the above dichlorosulfonimide triethylamine salt was added to a 1L reaction kettle, cooled...

Embodiment 2

[0106] Under nitrogen protection, 200g ethyl acetate and 130.35g (1.65mol) pyridine were added to a 1L reactor, then the reactor was cooled to 5°C, then 135g (1.0mol) of sulfuryl chloride was added to the reactor, and then Under the control of the flow meter, 8.5 g (0.5 mol) of anhydrous ammonia gas was slowly introduced into the reactor within 1 hour. After the introduction of the ammonia gas was completed, the reaction was continued at 5° C. for 0.5 hour. Then stop cooling, allow the reaction solution to naturally warm up to room temperature, and continue the reaction for 48 hours. After the reaction, the reaction solution is filtered to filter out the pyridine hydrochloride generated during the reaction to obtain ethyl acetate of bischlorosulfonimide pyridine salt. ester filtrate.

[0107] Under nitrogen conditions, the ethyl acetate filtrate of the obtained bischlorosulfonimide pyridinium salt was added to a 1L reactor, cooled to 0°C, and 30g of HF was introduced therein u...

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Abstract

The present invention provides a preparation method of lithium bis(fluorosulfonyl)amide. The method comprises the following steps: A) reacting chlorosulfuric acid with ammonia in the presence of an organic base to obtain organic alkali salt of bis(fluorosulfonyl)amide; B) mixing the bis(fluorosulfonyl)amide obtained in the step A) with HF for a fluorinated reaction to obtain an organic alkali salt of bis(fluorosulfonyl)amide; C) mixing the organic alkali salt of bis(fluorosulfonyl)amide obtained in the step B) with an alkaline substance for a neutralization reaction to obtain a bis(fluorosulfonyl)amid metal salt crude product; D) purifying the bis(fluorosulfonyl)amid metal salt crude product obtained in the step C) to obtain bis(fluorosulfonyl)amid metal salt; and E) mixing the bis(fluorosulfonyl)amid metal salt obtained in the step D) with a lithium reagent for a replacement reaction, so as to obtain lithium bis(fluorosulfonyl)amide. The preparation method provided by the invention has the characteristics of low raw material cost, low impurity content in the product and high yield of lithium bis(fluorosulfonyl)amide.

Description

technical field [0001] The invention belongs to the technical field of lithium ion battery electrolytes, in particular to a preparation method of lithium bisfluorosulfonyl imide. Background technique [0002] Since the concept of lithium-ion batteries was proposed and its commercial application was realized in the early 1990s, the basic research and application of lithium-ion batteries have rapidly become one of the hot spots in international electrochemical research. Electrolyte is an important element of lithium-ion batteries. By optimizing the electrolyte system, the composition and battery performance of the SEI film (solid electrolyte interphase) at the electrode interface can be improved, the reversible capacity of the electrode can be increased, and the cycle life can be extended. , improve the charge and discharge performance of the electrode. Therefore, the development of an electrolyte with superior performance has great practical significance for improving the ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086
Inventor 王刚周济苍
Owner 湖南福邦新材料有限公司
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