Method for preparing imidodisulfuryl fluoride lithium

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 risk, high difficulty in operation, corrosion of equipment, etc., and achieve high product quality , The effect of low raw material price and easy removal

Inactive Publication Date: 2018-02-06
JIANGSU LEE & MAN CHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese patent CN103524387A has reported that bischlorosulfonimide (HClSI) reacts with lithium chloride in thionyl chloride to generate bischlorosulfonimide lithium (LiClSI), and then utilizes metal fluoride (KF, ZnF 2 etc.) the fluorinating agent reacts with LiClSI to obtain LiFSI, and the introduction of the second step metal salt in this reaction route will cause difficulties in separation from the final product, thereby failing to obtain high-purity LiFSI
[0005] Chinese patent CN101747242 discloses potassium bisfluorosulfonimide (KFSI) to obtain LiFSI after carrying out ion exchange reaction with lithium perchlorate in solvent, but the product that this reaction route obtains can always remain a small amount of perchlorate (ClO 4- ) and potassium ions (K + )

Method used

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  • Method for preparing imidodisulfuryl fluoride lithium
  • Method for preparing imidodisulfuryl fluoride lithium
  • Method for preparing imidodisulfuryl fluoride lithium

Examples

Experimental program
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Effect test

Example Embodiment

[0041] Example 1

[0042] Under the protection of nitrogen, add 214g of bischlorosulfonimide into a 500ml reactor, and then add 161g of antimony trifluoride in batches. The process temperature is controlled at 20-25°C and reacted for 20 hours, and then continuous vacuum distillation twice to obtain 162g The bisfluorosulfonimide has a yield of 90% and a purity of 99.5%.

Example Embodiment

[0043] Example 2

[0044] Under the protection of flowing nitrogen, add 200ml of anhydrous methanol to a 500ml reactor, then add 1.4g of lithium metal, control the temperature below 40℃, stir and react for 3 hours, then concentrate under reduced pressure to dryness to obtain 7.6g of lithium methoxide, yield 100%.

Example Embodiment

[0045] Example 3

[0046] Under the protection of flowing nitrogen, add 200ml of absolute ethanol into the 500ml reactor, then add 1.4g of lithium metal, the process temperature is controlled at 40-50℃, the reaction is stirred for 3 hours, and then concentrated under reduced pressure to dryness to obtain 10.3g of lithium ethoxide. The rate is 99%.

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Abstract

The invention provides a method for preparing imidodisulfuryl fluoride lithium. The method comprises the following steps: (1) reacting imidodisulfuryl fluoride with antimony trifluoride under a solvent free condition, and distilling to obtain imidodisulfuryl fluoride lithium intermediate; (2) reacting metal lithium with anhydrate low alcohol, and concentrating and drying to obtain anhydrate low alcohol lithium; and (3) reacting the imidodisulfuryl fluoride lithium with lithium alkoxide, concentrating, pulping, filtering and drying to obtain a high-purity imidodisulfuryl fluoride lithium product. The method for preparing the imidodisulfuryl fluoride lithium has the characteristics of low cost, high purity and simple operation, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a lithium battery electrolyte additive, in particular to a preparation method of lithium bisfluorosulfonyl imide. Background technique [0002] Lithium bisfluorosulfonyl imide (Li[N(SO 2 F) 2 ], hereinafter 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 a wide range of LiPF6, it has many excellent properties, and is a better choice for lithium battery electrolytes. [0003] In the prior art, the preparation methods of lithium bisfluorosulfonyl imide mainly contain the following types: [0004] Chinese patent CN103524387A has reported that bischlorosulfonimide (HClSI) reacts with lithium chloride in thionyl chloride to generate bischlorosulfonimide lithium (LiClSI), and then utilizes metal fluoride (KF, ZnF 2 etc....

Claims

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Application Information

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IPC IPC(8): C01B21/086
CPCC01B21/086C01P2002/86C01P2006/80
Inventor 黎星术谢家伟王波谢文健辛伟贤陈新滋
Owner JIANGSU LEE & MAN CHEM
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