Preparation method of fluorosultone

A fluorosulfonic acid, sultone technology, applied in the direction of organic chemistry, can solve the problems of difficult separation and purification, low synthesis yield, difficult reaction, etc., and achieve the effects of easy purification, short reaction steps and high product purity

Inactive Publication Date: 2017-05-10
宁德市凯欣电池材料有限公司
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Problems solved by technology

[0007] There are very few reports on the preparation of fluorosultone in the prior art. The possible reason is that the reaction of introducing fluorine atoms to fluorosultone is relatively difficult, the synthesis yield is low, and it is difficult to separate and purify

Method used

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  • Preparation method of fluorosultone
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  • Preparation method of fluorosultone

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specific Embodiment approach

[0034] A preparation method of fluorosultone, is characterized in that, comprises the following steps:

[0035] (1), use saturated sodium sulfite aqueous solution and the chlorinated dihydroxyl compound generation substitution reaction with formula (I) structure, generate the dihydroxysulfonic acid sodium salt compound with formula (II) structure,

[0036]

[0037] M in formula (I) and formula (II) is C n h 2n+1 , wherein, n=1~4;

[0038] (2) The dihydroxysulfonic acid sodium salt compound obtained in step (1) is dehydrated with an excess dehydrating agent, the excess dehydrating agent is removed after the reaction, and the reaction product is washed and extracted to remove residual sodium dihydroxysulfonate Salt, then obtain the hydroxy-substituted sultone compound with formula (III) structure through drying and purification

[0039]

[0040] M of formula (III) is C n h 2n+1 , wherein, n=1~4;

[0041] (3) The hydroxy-substituted sultone compound obtained in step (...

Embodiment 1

[0053] 2-fluoro-1,3-propane sultone

[0054] The reaction formula is as follows:

[0055]

[0056] Its preparation method comprises the following steps:

[0057](1), use saturated sodium sulfite aqueous solution and 3-chloro-1,2-propanediol to generate 2,3-dihydroxy-propanesulfonate sodium. Specifically, 33.2g (0.3mol) of 3-chloro-1,2-propanediol was slowly added dropwise to a reactor containing an aqueous solution of sodium sulfite (wherein the quality of sodium sulfite was 45.4g, and the molar weight was 0.36mol), and then Stir under reflux at 110° C. for 4 hours until the system becomes homogeneous, and a solution containing sodium 2,3-dihydroxy-propanesulfonate is obtained. The obtained solution of sodium 2,3-dihydroxy-propanesulfonate was concentrated to obtain a saturated solution, and then crystallized to obtain a solid product (hydrate) of sodium 2,3-dihydroxy-propanesulfonate.

[0058] (2) 2,3-dihydroxy-sodium propanesulfonate obtained in step (1) is subjected t...

Embodiment 2

[0060] Example 2: 3-fluoro-1,4-butane sultone

[0061] The reaction formula is as follows:

[0062]

[0063] Its preparation method comprises the following steps:

[0064] (1), use saturated sodium sulfite aqueous solution and 4-chloro-1,3-butanediol to generate 2,4-dihydroxy-sodium butanesulfonate. Specifically, 37.4g (0.3mol) of 4-chloro-1,3-butanediol was slowly added dropwise to a reactor filled with an aqueous solution of sodium sulfite (wherein the quality of sodium sulfite was 45.4g and the molar weight was 0.36mol), Then reflux and stir at 110° C. for 4 hours until the system became homogeneous, and a solution containing sodium 2,4-dihydroxy-butanesulfonate was obtained. The obtained solution of sodium 2,4-dihydroxy-butanesulfonate was concentrated to obtain a saturated solution, and then crystallized to obtain a solid product (hydrate) of sodium 2,4-dihydroxy-butanesulfonate.

[0065] (2) carrying out dehydration condensation reaction with 2,4-dihydroxy-sodium b...

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Abstract

The invention relates to generation of a sodium dihydroxyl sulfonate compound by a substitution reaction of a saturated aqueous solution of sodium sulfite and a chloro dihydroxy compound; a dehydration reaction is carried out for the sodium dihydroxyl sulfonate compound obtained by the step and excess dehydrating agents, after the reaction, excess dehydrating agents are removed; residual sodium dihydroxyl sulfonate is removed by washing and extracting the reaction products; drying and purification are carried out in order to obtain a hydroxy substituted sultone compound; a fluorination reaction is carried out for the obtained hydroxy substituted sultone compound and a fluorating agent, underpressure distillation and purification are carried out, and the fluorosultone compound is obtained. The method has the advantages of cheap raw material, easy purchase, simple operation steps, mild reaction conditions, short reaction steps, easy purification, and high purity of produced products.

Description

technical field [0001] The invention belongs to the technical field of synthesis methods of organic compounds, in particular to a fluorosulfonic acid internal [0002] Method for the preparation of esters. Background technique [0003] The market for lithium-ion secondary batteries in civilian mobile devices and power batteries has developed rapidly in the last decade. Sultone compounds, as commonly used film-forming additives for lithium-ion battery electrolytes, can significantly improve the life of lithium secondary batteries (Leggesse, E.G. and J.-C. Jiang (2012). "Theoretical Study of the Reductive Decomposition of 1,3-Propane Sultone: SEI Forming Additive in Lithium-ion Batteries."RSC Advances."). In recent years, the application of fluorosultone compounds in the fields of lithium-ion secondary batteries and non-aqueous electrolyte materials has often been reported in domestic and foreign journals. It can be seen that this class of compounds has important applicatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/04C07D327/06
CPCC07D327/04C07D327/06
Inventor 廖帅玲王盛温雄吴良煜
Owner 宁德市凯欣电池材料有限公司
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