Method for preparing high-purity annular sulfuric acid ester

A cyclic sulfate, high-purity technology, used in organic chemistry and other directions, can solve problems such as high acidity, difficult to remove cleanly, and inability to react

Active Publication Date: 2009-06-17
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Abstract
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Problems solved by technology

[0007] The industrial production method of cyclic sulfuric acid ester is usually prepared by oxidation of sodium hypochlorite with cyclic sulfite in the presence of ruthenium trichloride catalyst, and this preparation method usually cannot react completely, and because cyclic sulfurous acid The boiling point

Method used

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Embodiment Construction

[0011] The following is a detailed description of the invention. As a solvent for dissolving the crude cyclic sulfate ester, polar solvents, aromatic compound solvents, or at least one of them can be used as solvents, and these solvents are ideal alone or in combination of two or more. The so-called dissolving in the present invention refers to dissolving the crude cyclic sulfate in the above solution, including the state of emulsion or suspension.

[0012] The concrete example of the polar solvent that adopts among the present invention has ketones such as acetone, butanone, methyl propyl ketone; Methyl formate, ethyl formate, propyl formate, butyl formate, methyl acetate, ethyl acetate, Propyl acetate, butyl acetate and other carboxylic acid esters; Acetonitrile, propionitrile, butyronitrile and other nitriles; Methylene chloride, chloroform, tetrachloromethane, dichloroethane and other halogenated hydrocarbons; Dimethyl carbonate , diethyl carbonate, methyl ethyl carbonate...

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Abstract

The invention discloses a method for preparing a high-purity cyclic sulfuric ester. The method comprises the following steps: adopting a method of removing residual raw materials by reaction, namely dissolving the prepared cyclic sulfuric ester crude product in a proper solvent, then adding certain amount of water into the solution, adding a proper amount of potassium permanganate solid in batch under stirring, reducing the generated manganese dioxide and excessive potassium permanganate by using a reducing agent such as sodium bisulfite, and finally treating an organic layer by the steps of water washing, alkali washing, water washing, drying, decompressing to remove the solvent and the like to obtain the high-purity cyclic sulfuric ester. The purified cyclic sulfuric ester is suitable to be used as an electrolyte additive of a lithium secondary battery to improve cycle performance, high-temperature performance and the like of the lithium secondary battery.

Description

technical field [0001] The present invention relates to the purification of high-purity cyclic sulfuric acid ester and the method for preparing high-purity products. In detail, the crude cyclic sulfate is dissolved in a suitable amount of solvent, and in the presence of water, the residual raw material is oxidized with potassium permanganate, and then the manganese dioxide generated is reduced with a reducing agent such as sodium bisulfite and excess potassium permanganate, and the organic layer is washed with water, neutralized, washed with water, dried, and desolvated under reduced pressure to obtain a high-purity cyclic sulfuric acid ester. The cyclic sulfate can be used as an additive to the electrolyte of a lithium secondary battery to improve the cycle performance and high temperature performance of the lithium secondary battery. Background technique [0002] Since the lithium-ion battery produced by Sony Corporation of Japan was launched in early 1991, the lithium-io...

Claims

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Application Information

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IPC IPC(8): C07D327/10
Inventor 吴茂祥
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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