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Method for producing a hygroscopic alkali metal salt electrolyte solution

A technology of alkali metal salts and non-aqueous electrolytes, which is applied in the field of preparation of low-water-content electrolyte solutions, can solve problems such as time-consuming, environmental hazards, and expensive, and achieve the effects of reducing solvent consumption and increasing yield

Pending Publication Date: 2020-03-06
SYNTHIO CHEM LLC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Removal of these solvents is time consuming, expensive and presents safety concerns due to the potential release of volatile organic compounds into the environment and disposal of flammable solvents as well as environmental hazards

Method used

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  • Method for producing a hygroscopic alkali metal salt electrolyte solution
  • Method for producing a hygroscopic alkali metal salt electrolyte solution
  • Method for producing a hygroscopic alkali metal salt electrolyte solution

Examples

Experimental program
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Effect test

Embodiment 1

[0085] Example 1: A wet solution of LiFSI and diethyl carbonate (DEC) was prepared by mixing 100 g DEC, 54.6 g LiFSI and 1.59 g water. The solution was found to contain 1.0 wt% water from Karl Fischer titration. This solution was placed in a 1 L three-neck round bottom flask with a magnetic stir bar and heating mantle. One flask neck was closed with a ported stopper through which the thermocouple was immersed in the LiFSI / DEC solution. The other neck was fitted with a 125mL pressure equalizing addition funnel filled with 117.5g of DEC which had 130ppm w Water, as measured by Karl Fischer titration. The final neck is equipped with a vacuum port Liebig distillation head. Connect a 1 L round bottom flask to the receiving end of the distillation head. Immerse the flask in an ice bath. The distillation condenser was cooled to -5°C with an external cooler. A diaphragm vacuum pump was connected to the vacuum port of the distillation head, and the pressure was reduced to about 1...

Embodiment 2

[0087] Example 2: A wet solution of LiFSI and ethyl methyl carbonate (EMC) was prepared by mixing 47.2 g LiFSI, 88.6 g EMC and 1.432 g water. The solution was found to contain 1.06 wt% water by Karl Fischer titration. 123.0 g of this solution was placed in a 300 mL three necked round bottom flask with a magnetic stir bar and heating mantle. The flask was connected to the apparatus described in Example 1. The LiFSI / EMC solution was heated to about 42°C under constant power from a heating mantle. Vacuum was applied at about 30 torr and the condenser was cooled to about -6°C. Add dry EMC to the LiFSI / EMC solution from the addition funnel and observe boiling using condensate collection in the receiving funnel. After adding the contents of the addition funnel, measure the water content of the LiFSI / EMC solution by Karl Fischer titration and refill the addition funnel with dry EMC. Table 1 shows the amount of EMC added and the water concentration in the LiFSI / EMC solution after ...

Embodiment 3

[0092] Example 3 : A solution of LiFSI in water was prepared by mixing HFSI with lithium carbonate. In a jacketed flask equipped with a mechanical stirrer, 814 grams of water and 747 grams of lithium carbonate were added. 3700 g of HFSI was added dropwise to the reactor over the course of 3.5 hours while keeping the reactor temperature below 20°C by circulating a coolant through the jacket. After the addition of HFSI was complete, the reactor contents were drained and filtered to obtain an aqueous solution containing 78 mass % LiFSI. This solution was then mixed with DEC and dried using the method of Example 1.

[0093] Process effluent is CO 2 , water and a small stream of solid impurities (typically <1% of LiFSI production rate). To improve efficiency, the HFSI feed was of high purity, as shown in Table 2. The conversion was almost quantitative as yields above 95% were achieved.

[0094] Table 2. HFSI used in Example 3

[0095] illustrate Value (ppmw) ...

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Abstract

The present invention provides a method for producing low-water-content electrolyte solutions. In particular, the present invention provides a method of removing water from a liquid solution comprising a non-aqueous solvent, a hygroscopic metal salt and water. It also provides a method for producing a low-water content electrolyte solution without isolation of the metal salt. The method of the invention is useful in producing low water content electrolyte solutions for batteries such as lithium- or lithium-ion batteries.

Description

[0001] Cross References to Related Applications [0002] This application claims priority to US Provisional Application No. 62 / 451,931, filed January 31, 2017, which is hereby incorporated by reference in its entirety. technical field [0003] The present invention generally relates to the preparation of low water content electrolyte solutions. The invention is particularly useful in the preparation of low water content electrolytes containing alkali (such as lithium, sodium, potassium or combinations thereof) salts and non-aqueous solvents for alkali metal or alkali metal ion (such as lithium or lithium) batteries. Background technique [0004] Electrolytes for Li-ion and Li-ion batteries generally require non-aqueous electrolytes with low water content to obtain acceptable calendar and cycle life. Commercial electrolytes for Li-ion batteries typically specify a water content of no more than 500 parts per million (ppm) by weight, usually no more than 400 ppm, usually no mo...

Claims

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Application Information

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IPC IPC(8): H01M10/0568H01M10/00H01M10/05H01M10/0564H01M10/0566
CPCH01M10/0568H01M10/0569Y02E60/10H01M2300/0028H01M10/0525H01M10/054
Inventor J·C·珀修斯塔J·L·马丁
Owner SYNTHIO CHEM LLC
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