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Preparation method of imidodisulfuryl fluoride lithium salt

A technology of bisfluorosulfonimide lithium salt and bisfluorosulfonimide, which is applied in the field of preparation of bisfluorosulfonimide lithium salt, can solve the problems of hydrochloride separation and low product purity, and meet the conditions Mild, high reaction conversion rate, simple operation effect

Active Publication Date: 2017-09-29
SUZHOU HUAYI NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the yield of the reaction is high, the hydrochloride is not separated during the preparation process, and the final product is low in purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] This embodiment provides a preparation method of bisfluorosulfonimide, the preparation method is as follows:

[0032] Under the protection of dry nitrogen or argon, add 214 g (1 mol) of dichlorosulfonic acid imide (HCSI), 113 g (0.7 mol) of triethylamine trihydrogen fluoride and dimethyl carbonate into a four-necked flask equipped with a reflux tube (DMC) 110ml, add 168g (1.33mol) of triethylamine dropwise under stirring at room temperature, drop it over in 0.5 hours, keep warm for 4 hours, filter and separate triethylamine hydrochloride, and the filtrate undergoes decompression precipitation to obtain difluorosulfonyl The crude amine was then rectified under reduced pressure to obtain 178 g of bisfluorosulfonimide product with a purity of 97.52% (GC).

Embodiment 2

[0034] This embodiment provides a preparation method of bisfluorosulfonimide, the preparation method is as follows:

[0035] Under the protection of dry nitrogen or argon, add 428 g (2 mol) of dichlorosulfonate imide (HCSI), triethylamine trihydrogen fluoride (Et 3 N.3HF) 220g (1.37mol) and dimethyl carbonate (DMC) 500ml, add 275g (2.72mol) of triethylamine dropwise under stirring at room temperature, finish dropping within 1 hour, keep warm for 4 hours, filter and separate the triethylamine salt , the filtrate was precipitated under reduced pressure to obtain a crude product of bisfluorosulfonimide, and then subjected to vacuum distillation to obtain 345 g of a bisfluorosulfonimide product with a purity of 99.75% (GC).

Embodiment 3

[0037] This embodiment provides a preparation method of lithium bisfluorosulfonyl imide, the preparation method is as follows:

[0038] Under nitrogen protection, in a three-necked flask with a reflux device, take 90.5 g (0.5 mol) of bisfluorosulfonimide (HFSI) obtained in Example 2, and slowly add lithium hydroxide (LiOH.H 2 (0) 21g (0.5mol), warming up to 90-110°C, stirring for 2 hours, dehydrating under reduced pressure, adding 100ml of dimethyl carbonate into the three-necked flask after cooling, filtering under reduced pressure to remove insoluble substances, then concentrating and filtering the filtrate under reduced pressure , washing, and vacuum drying to obtain 91.5 g of lithium bisfluorosulfonyl imide, 99.65% (HPLC).

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Abstract

The invention relates to a preparation method of imidodisulfuryl fluoride lithium salt. The preparation method comprises the following steps: (1) performing a fluorination reaction of imidodisulfuryl chloride by taking a hydrogen fluoride complex salt as a fluorinating agent in the presence of a solvent, the fluorinating agent and an initiator, performing filter pressing separation at the end of the reaction, distilling filtrate under a reduced pressure to remove the solvent, and rectifying under a reduced pressure to obtain imidodisulfuryl fluoride; (2) reacting the imidodisulfuryl fluoride with a lithium compound at the temperature of 80 to 110 DEG C to obtain a crude imidodisulfuryl fluoride lithium salt. The preparation method provided by the invention has the advantages of easiness in operation of a fluorinating process route, mild conditions, high operability and easiness in implementation of industrial production; the prepared imidodisulfuryl fluoride lithium salt is 99 percent or more in purity, and is suitable for lithium batteries.

Description

technical field [0001] The invention relates to a preparation method of bisfluorosulfonimide lithium salt. Background technique [0002] Bisfluorosulfonimide is a versatile organic intermediate, and its lithium bisfluorosulfonimide lithium is an effective lithium-ion secondary battery electrolyte, used as an ionic liquid electrolyte for dye-sensitized solar cells to obtain photoelectricity Efficient and thermally stable devices with power conversion efficiency of 7.5%, avoiding the use of ionic liquid electrolytes containing TCB anions. Due to the characteristics of molecular structure, bisfluorosulfonimide and its lithium salt have strong chemical electrophilicity, strong acidity and excellent solid surface characteristics. They are used in many fields, especially in high-performance electrolytes, Ionic liquids and catalysts are widely used in fields such as. [0003] Wherein, the structural formula of bisfluorosulfonimide is: [0004] The structural formula of lithium...

Claims

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Application Information

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IPC IPC(8): C01B21/086H01M10/0563H01M10/052
CPCC01B21/086C01P2006/80H01M10/052H01M10/0563Y02E60/10
Inventor 汪许诚王小龙王振一顾乃刚周龙
Owner SUZHOU HUAYI NEW ENERGY TECH CO LTD
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