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Cyclic silyl disulfonate and preparation method thereof

A technology of silyl disulfonate and methylene disulfonic acid, applied in secondary batteries, organic silicon compounds, electrochemical generators, etc. The effect of strong practicability, high product purity and broad market prospects

Active Publication Date: 2018-01-12
CHANGSHU CHANGJI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, there are few reports about the preparation of silicon disulfonate

Method used

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  • Cyclic silyl disulfonate and preparation method thereof
  • Cyclic silyl disulfonate and preparation method thereof
  • Cyclic silyl disulfonate and preparation method thereof

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preparation example Construction

[0037] The preparation method of above-mentioned cyclic disulfonic acid silicon base ester, comprises the steps:

[0038] With methylene disulfonic acid or the methylene disulfonate of general formula (I) and the dihydrocarbyl diactive functional group silane of general formula (II) in solvent, according to methylene disulfonic acid or methylene disulfonic acid The molar ratio of sulfonate and dihydrocarbyl diactive functional group silane to solvent is 1:0.1~10:3~50 to react;

[0039] Or the methylene disulfonic acid or the methylene disulfonate of the general formula (I) and the dihydrocarbyl cyclosiloxane of the general formula (III) in a solvent, according to the methylene disulfonic acid or the methylene disulfonic acid The molar ratio of disulfonate, dihydrocarbyl cyclosiloxane and solvent is 1:0.1~5:3~50 to react;

[0040] Or the dihydrocarbyl ring silazane of methylene disulfonic acid or general formula (I) and general formula (IV) according to methylene disulfonic ac...

Embodiment 1

[0063] Add 1mol sodium methanedisulfonate into a three-neck flask equipped with a thermometer, magnetic stirring, reflux condenser, and constant pressure dropping funnel, heat in an oil bath at about 100°C, and dehydrate under negative pressure for 2 hours under a slight nitrogen flow. Cool down to room temperature, remove the vacuum with a nitrogen bag, quickly add solvents that have been dehydrated to below 5 ppm: 1 mol of fluorobenzene, 1 mol of dichloroethane and 1 mol of dimethylformamide, and dropwise add 1 mol of dimethyldichlorosilane while stirring, After the dropwise addition, continue to stir for 1 hour, then heat to 80-85°C and reflux for 12 hours, cool to about 10°C, press filter, transfer the filtrate to a rotary evaporator to evaporate dichloroethane and dimethyl Formamide, through repeated recrystallization purification and GC-MS analysis, the structural formula is The target product 98g, purity 99.6%.

Embodiment 2

[0065] Add 1 mol of silver methanedisulfonate into a three-neck flask equipped with a thermometer, magnetic stirring, reflux condenser, and constant pressure dropping funnel, heat in an oil bath at about 100°C, and dehydrate under negative pressure for 2 hours under a slight nitrogen flow. Cool down to room temperature, use a nitrogen bag to eliminate the vacuum, quickly add 50 mol of dioxane that has been dehydrated to less than 5 ppm of moisture, and add 5 mol of methylvinyldibromosilane dropwise while stirring. After the dropwise addition, continue to stir for 1 hour, and then heat Reflux at 100-105°C for 25 hours, cool to about 5°C, filter with suction, transfer the filtrate to a rotary evaporator to evaporate dioxane and excess methylvinyldibromosilane under negative pressure, and recrystallize several times Purification and GC-MS analysis, the structural formula is The target product 116g, purity 99.3%.

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Abstract

The invention discloses cyclic silyl disulfonate. The cyclic silyl disulfonate has a structural formula as follows: the formula is shown in the description. A preparation method comprises the following steps: enabling methanedisulphonic acid or methanedisulphonate shown as a general formula (I), a dialkyl silane containing two active functional groups and shown as a general formula (II), dialkyl cyclosiloxane shown as a general formula (III) or dialkyl cyclo-silazane shown as a general formula (IV) to react in a solvent according to a certain ratio; controlling temperature and time of reaction; after finishing the reaction, separating to remove the solvent and a byproduct, so as to obtain the cyclic silyl disulfonate. According to the cyclic silyl disulfonate and the preparation method, the cyclic silyl disulfonate with different substituent groups is innovatively prepared through selecting special raw materials and designing a synthesis technology; room-temperature and high-temperature circulating performance and high-temprature storage performance of a lithium secondary battery can be effectively improved and the thickness swelling of the battery in a high-temprature storage process is reduced; the preparation method of the cyclic silyl disulfonate has simple technological steps and strong enablement; the obtained product has high purity, the chromatographic purity reaches 99percent or more and the product has a wide market prospect.

Description

technical field [0001] The invention relates to the technical field of preparation of electrolyte additives for lithium batteries, in particular to a cyclic silicon disulfonate and a preparation method thereof. Background technique [0002] Sulfonyl compounds, especially sulfonate ester compounds, as an important pharmaceutical intermediate, have been widely developed and synthesized in the 1940s. With the increasing popularity of small electronic devices, such as smartphones, laptops and tablet computers, the development and use of lithium batteries have entered a stage of vigorous development; while pursuing their battery life, lightweight (portability), environmental protection (Circularity) and security (stability) are also getting more and more attention. At the same time, due to factors such as the depletion of petrochemical energy and its non-renewability, lithium batteries as energy carriers are widely used in small vehicles, such as electric mopeds and electric veh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08H01M10/0567
CPCC07F7/08H01M10/0567Y02E60/10
Inventor 傅人俊范伟贞
Owner CHANGSHU CHANGJI CHEM
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