Method for refining and purifying methylene methanedisulfonate

A technology for refining and purifying methylene disulfonate, applied in the field of refining and purifying methylene methane disulfonate and a kind of refining and purifying methylene methane disulfonate, can solve the problem of affecting the performance of lithium ion batteries and cannot improve Lithium-ion battery performance and other issues

Inactive Publication Date: 2012-05-23
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The methylene disulfonate synthesized by the above route contains more impurities, and the purity can only reach about 98%. If it is used as a general organic synthesis intermediate, it can also be used, and if it is used as an electrolyte additive for lithium-ion batteries. It cannot be used directly, because the lithium-ion battery electrolyte additive has extremely high requirements on quality, otherwise it will not only fail to improve the performance of the lithium-ion battery, but will have a negative effect and affect the performance of the lithium-ion battery

Method used

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  • Method for refining and purifying methylene methanedisulfonate
  • Method for refining and purifying methylene methanedisulfonate
  • Method for refining and purifying methylene methanedisulfonate

Examples

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Effect test

Embodiment 1

[0029] Dissolve 200g of methylene disulfonate crude product in 400ml of acetone to make a solution, filter to remove insoluble impurities to obtain methylene disulfonate acetone solution, and then slowly add 1000ml of methylene disulfonate to it under constant stirring white deionized water, gradually a white solid substance is precipitated until the precipitation is complete, filtered, the filter cake is washed twice with deionized water, then drained, and finally dried under high vacuum to obtain 155 g of a white solid substance with a purity of 99.62 % (HPLC), residual metal ion (ICP) ppm: Fe: 9.78; Ca: 7.46; K: 19.22; Na: 22.40.

Embodiment 2

[0031] Dissolve 200 g of methylene disulfonate crude product in 500 ml of ethyl acetate to make a solution, filter to remove insoluble impurities, dry the obtained ethyl acetate solution with anhydrous magnesium sulfate, and filter to obtain dried methylene disulfonate Add 2000ml of n-hexane slowly to the methylene acetate ethyl acetate solution under stirring, gradually precipitate white solid matter until the precipitation is complete, filter, wash the filter cake twice with n-hexane, then drain it, and finally put it in Drying under high vacuum yielded 163 g of white solid material with a purity of 99.81% (HPLC), and residual metal ion (ICP) ppm: Fe: 6.23; Ca: 2.14; K: 8.65; Na: 7.69.

Embodiment 3

[0033] Dissolve 100 g of methylene disulfonate in 500 ml of dichloromethane to make a solution, filter to remove insoluble solid impurities, dry the obtained dichloromethane solution with anhydrous magnesium sulfate, and filter to obtain dried methylene disulfonate Add 1000ml of dichloromethane solution to the dichloromethane solution slowly under stirring, gradually precipitate white solid matter until the precipitation is complete, filter, wash the filter cake twice with diethyl ether, then drain it, and finally put it under high vacuum 85 g of white solid substance was obtained, the purity was 99.78% (HPLC), and the residual metal ion (ICP) ppm: Fe: 6.86; Ca: 3.65; K: 6.73; Na: 8.36.

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Abstract

The invention provides a method for refining and purifying methylene methanedisulfonate and relates to the field of refining and purification of chemicals, in particular to method for refining and purifying methylene methanedisulfonate. The method specifically comprises the following steps of: firstly dissolving the methylene methanedisulfonate in a good solvent to form a saturated solution, then adding a poor solvent to the methylene methanedisulfonate to separate out the methylene methanedisulfonate, and obtaining the methylene methanedisulfonate with high purity by filtering, washing, leaching and vacuum drying, thereby achieving the purpose of refining and purification. The methylene methanedisulfonate can be used for synthesizing pharmaceutical preparations for treating leukemia and the like of animals; and the refined and purified methylene methanedisulfonate is particularly suitable for being used as an addition agent of electrolyte of a lithium battery to prolong the service life of the lithium battery.

Description

technical field [0001] The invention provides a method for refining and purifying methylene disulfonate. The invention relates to the field of refining and purifying chemicals, in particular to a method for refining and purifying methylene disulfonate. In detail, methylene disulfonate is first dissolved in a good solvent to form a saturated solution, and then a poor solvent of methane disulfonate is added to separate out methylene disulfonate, by After filtration, washing, suction filtration and vacuum drying, high-purity methylene disulfonate is obtained to achieve the purpose of refining and purifying. Methylene disulfonate can be used to synthesize pharmaceutical preparations for treating leukemia in animals, etc. The refined and purified methylene disulfonate is especially suitable as an electrolyte additive for lithium batteries to improve the cycle life of lithium-ion batteries. Background technique [0002] Methylene disulfonate referred to in the present invention ...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07D327/00H01M10/0567
CPCY02E60/12Y02E60/10
Inventor吴茂祥卢碧强王文国方桂煌
OwnerFUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI