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

A technology of lithium bisfluorosulfonimide and imidic acid, which is applied in the directions of nitrosyl chloride, nitrogen and non-metallic compounds, can solve the problems of difficult operation, complex product composition and high cost, and achieves high yield and preparation. The effect of low process energy consumption

Inactive Publication Date: 2020-08-04
CHANGSHU XINHUA CHEM
View PDF5 Cites 11 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the existing preparation technologies at home and abroad have a long process route for preparing lithium bisfluorosulfonyl imide, complex product composition, difficult separation of entrained impurities in the product, and high cost, which affects the industrialization of the product.
For example, the invention patent with the publication number CN104495767A discloses a preparation method of lithium bisfluorosulfonyl imide, which needs to use a large amount of LiPF6 as the lithiation reagent. The total yield is only about 50%, and

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of lithium bis (fluorosulfonyl) imide and lithium bis (fluorosulfonyl) imide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: a kind of preparation method of lithium bisfluorosulfonyl imide comprises the following steps:

[0036] S10), using sulfamic acid, chlorosulfonic acid and thionyl chloride with a mass molar ratio of 1:1.2:2.5 as raw materials in an imidic acid reaction kettle to perform a temperature-intensive reflux reaction to obtain an imidic acid reaction solution, and the temperature-intensive reflux reaction The temperature is kept at 50-140°C, and the heat preservation reaction time is 48 hours; the heating reaction is stopped, and the generated HCL and SO 2 Exhaust gas is discharged into the exhaust gas absorption system, respectively for HCL, SO 2 After the tail gas is treated with water and alkali, the by-products hydrochloric acid and sodium sulfite are collected to obtain by-product hydrochloric acid and sodium sulfite, which meets the environmental protection emission requirements, and hydrochloric acid and sodium sulfite are obtained as by-products, which eff...

Embodiment 2

[0040] Embodiment 2: all the other technical solutions of this embodiment 2 are the same as embodiment 1, the difference is that in this embodiment 2, in step S10), the mass molar ratio of sulfamic acid, chlorosulfonic acid and thionyl chloride is 1:1.4:2.8; in step S20) and step S30), the polar solvent all adopts acetonitrile, and the molar ratio of potassium fluoride and imidic acid is 3:1; in step S30), anhydrous lithium chloride The mass molar ratio with acetonitrile is 1:7.5, and the secondary concentration process in Example 1 is replaced by a primary concentration process (disposable evaporation); after testing, the purity of the lithium bisfluorosulfonyl imide in this Example 2 The yield is 99.5%, wherein the free acid content is 80PPM, the moisture content is 50PPM, the chloride ion content is 3PPM, and the yield reaches 65.6%.

Embodiment 3

[0041] Embodiment 3: the remaining technical solutions of this embodiment 2 are the same as embodiment 1, the difference is that in this embodiment 2, in step S10), the mass molar ratio of sulfamic acid, chlorosulfonic acid and thionyl chloride is 1:1.2:3; in step S20), the molar ratio of potassium fluoride to imidic acid is 6:1. After testing, the purity of lithium bisfluorosulfonyl imide in Example 3 is 99.8%, wherein , the free acid content is 30PPM, the water content is 40PPM, the chloride ion content is 40PPM, and the yield reaches 62.5%.

[0042] This example creatively uses thionyl chloride, chlorosulfonic acid, and sulfamic acid as raw materials with low raw material cost and easy availability, and prepares imidic acid under the condition of elevated temperature and reflux reaction, and then uses the same low-cost raw material and easy-to-obtain Potassium fluoride as a raw material reacts with imidic acid to obtain potassium salt, and then reacts potassium fluoride sal...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a preparation method of lithium bis (fluorosulfonyl) imide and the lithium bis (fluorosulfonyl) imide. Thionyl chloride, chlorosulfonic acid and sulfamic acid which are low inraw material cost and easy to obtain are used as raw materials; imidic acid is prepared under the condition of heating reflux reaction, potassium fluoride which is also used as a raw material and is low in cost and easy to obtain is used as a raw material to react with the imidic acid to obtain sylvite, potassium fluoride salt and anhydrous lithium salt react in a solvent to generate the lithium bis (fluorosulfonyl) imide, and the preparation process is low in energy consumption and has operation safety. And meanwhile, purification process treatment is carried out in each step, so that the high-purity and high-yield lithium bis (fluorosulfonyl) imide can be finally obtained, and the method is very suitable for being used as a process route for batch production of the lithium bis (fluorosulfonyl) imide.

Description

technical field [0001] The invention relates to the field of preparation of electrolytes in lithium-ion battery electrolytes, in particular to a method for preparing lithium bisfluorosulfonyl imide, and the invention also relates to lithium bisfluorosulfonyl imide prepared by the preparation method. Background technique [0002] In the current technology, lithium-ion batteries are widely used in electronic products, electric vehicles, and energy storage devices due to their high energy density. Therefore, for lithium-ion battery products, it is usually required to have excellent performances such as high capacity, long life, high rate performance and safety. Specifically, different compositions of electrolytes in lithium-ion batteries will largely lead to differences in the performance of lithium-ion batteries, especially in high and low temperature environments, electrolyte decomposition and side reactions will significantly affect the life of lithium-ion batteries , Self-...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C01B21/086
CPCC01B21/086C01P2006/80C01P2006/82
Inventor 王正元盛晓东
Owner CHANGSHU XINHUA CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap