JPWO2019229366A5

JPWO2019229366A5 -

Info

Publication number: JPWO2019229366A5
Application number: JP2020566973A
Authority: JP
Publication date: 2022-06-02
Anticipated expiration: 2039-05-28

Claims

-A composition comprising at least 99.75% by weight of a lithium salt of bis (fluorosulfonyl) imide; and-strictly more than 0 and a mass content of 400 ppm or less of acetic acid.

At least 99.78 % by weight, preferentially at least 99.80%, preferably at least 99.85%, and even more preferably at least 99.90% by weight of bis (fluoro) based on the total weight of the composition. The composition according to claim 1, which comprises a lithium salt of sulfonyl) imide.

At least 99.95%, preferentially at least 99.97%, preferably at least 99.98%, and even more preferably at least 99.99% by weight, bis (fluoro) to the total weight of the composition. The composition according to claim 1 or 2, which comprises a lithium salt of sulfonyl) imide.

From claim 1, the mass content of acetic acid is 350 ppm or less, preferentially 300 ppm or less, preferably 250 ppm or less, and even more preferably 200 ppm or less, for example 150 ppm or less, based on the total weight of the composition. The composition according to any one of 3.

The mass content of acetic acid is 0.1 ppm to 300 ppm, preferably 0.1 ppm to 200 ppm, preferably 0.1 ppm to 150 ppm, and even more preferably 0.1 ppm to 100 ppm, based on the total weight of the composition. The composition according to any one of claims 1 to 4, which is a range.

-Cl ^- ions with a content in the range of 0 to 20 wt ppm, preferably 0 to 15 ppm, 0 to 10 wt ppm with respect to the total weight of the composition; and / or-with respect to the total weight of the composition. F- ^; and / or-with respect to the total weight of the composition, 0 to 200 ppm, preferably 0 to 50 ppm, preferably 0 to 30 wt ppm. H ₂ O; and / or-the total weight of the composition, preferably in the range of 0 to 100 ppm, preferably in the range of 0 to 50 ppm, and even more preferably in the range of 0 to 30 wt ppm. In contrast, ^{SO 4-2} _; and / Or-with respect to the total weight of the composition, the content is in the range of 0 to 200 ppm, preferably in the range of 0 to 100 ppm, preferably in the range of 0 to 50 ppm, and even more preferably in the range of 0 to 20 wt ppm. Na ⁺ ; and / or-with respect to the total weight of the composition, in the range of 0 to 500 ppm, preferably in the range of 0 to 300 ppm, preferably in the range of 0 to 200 ppm, and even more preferably in the range of 0 to 100 ppm. FSO ₃ Li with a content in the range of 0 to 20 wt ppm; and / or-with respect to the total weight of the composition, in the range of 0 to 200 ppm, preferably in the range of 0 to 100 ppm, preferably 0. FSO ₂ NH ₂ with a content in the range of to 50 ppm, and even more preferably in the range of 0 to 20 ppm, especially in the range of 0 to 10 wt ppm.
The composition according to any one of claims 1 to 5, which comprises.

Any one of claims 1 to 6, comprising butyl acetate having a content of 2000 ppm or less, preferably 1500 ppm or less, preferably 1000 ppm or less, preferably 500 ppm or less, and even more preferably 250 ppm or less, for example 150 ppm or less. The composition according to the section.

Any of claims 1 to 7, wherein the total content of acetic acid and butyl acetate is 2200 ppm or less, preferably 1700 ppm or less, preferably 1200 ppm or less, based on the total weight of the composition. The composition according to one item.

Any one of claims 1 to 8, comprising butanol having a content of 500 ppm or less, preferably 300 ppm or less, preferentially 200 ppm or less, preferably 100 ppm or less, particularly 50 ppm or less, based on the total weight of the composition. The composition according to the section.

It is selected from a chlorinated solvent and an aromatic solvent having a content of 1000 ppm or less, preferably 800 ppm or less, preferably 500 ppm or less, preferably 200 ppm or less, particularly 100 ppm or less, based on the total weight of the composition. The composition according to any one of claims 1 to 9, which comprises a crystallization solvent.

Any one of claims 1 to 10, wherein the total content of acetic acid and water is 400 ppm or less, preferably 300 ppm or less, preferably 250 ppm or less, based on the total weight of the composition. The composition according to the section.

A method for preparing the composition according to any one of claims 1 to 11, wherein the following steps:
-A) The composition C1 containing the organic solvent OS1, water and a bis (fluorosulfonyl) imide salt was pre-concentrated, and the following:
A lithium salt of bis (fluorosulfonyl) imide having a content in the range of 35% by weight to 50% by weight, preferably 40% by weight to 45% by weight, based on the total weight of the composition C2;
Water having a mass content of 500 ppm or less, preferably 300 ppm or less, preferably 100 ppm or less, based on the total mass of the composition C2;
In the step of obtaining the composition C2 containing
A step in which the pre-concentration step is carried out at a temperature of 50 ° C. or lower;
-B) Step of concentrating the composition C2;
-C) A method comprising an optional step of crystallizing the composition obtained in step b).

The composition C1 is as follows:
-Mass in the range of 0.1% by weight to 10% by weight, preferentially 1% by weight to 10% by weight, preferably 1.5% by weight to 10% by weight, based on the total weight of the composition C1. Water content; and / or-contains a salt of bis (fluorosulfonyl) imide having a mass content of 5% to 30% by weight, preferably 5% to 20% by weight, based on the total weight of the composition. The method according to claim 12, wherein the method is characterized by the above.

The organic solvent OS1 is selected from the group consisting of esters, nitriles, ethers, chlorinated solvents, aromatic solvents, and mixtures thereof, preferably methyl t-butyl ether, cyclopentyl methyl ether, ethyl acetate, propyl acetate, butyl acetate. , And a mixture thereof, wherein the organic solvent OS2 is preferentially butyl acetate, claim 12 or 13.

The method according to any one of claims 12 to 14, wherein the pre-concentration step a) is carried out under reduced pressure, for example, at a pressure of 50 mbar abs or less, particularly at a pressure of 30 mbar abs or less.

Step b) is based on the following conditions:
-Between 30 ° C and 95 ° C, preferably between 30 ° C and 90 ° C, preferably between 40 ° C and 85 ° C, especially between 60 ° C and 80 ° C.
-10 ^-3 At pressure between mbar abs and 5 mbar abs, especially between 5 × 10 ^-1 and 2 mbar abs,
-With a residence time of 5 minutes or less, preferably 3 minutes or less.
The method according to any one of claims 12 to 15, which is carried out in a short-pass thin film evaporator.