Method for reducing moisture content of 1,3-propane sultone

A technology of propane sultone and content, applied in the direction of organic chemistry and the like, can solve problems such as reduction and low moisture content, and achieve the effects of high efficiency, simple steps and convenient operation

Active Publication Date: 2014-07-23
BLUE OCEAN & BLACK STONE TECH CO LTD FUJIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention aims to solve the problem that in the existing 1,3-propane sultone production process, it is difficult to obtain 1,3-propane sultone with low moisture content, low acidity and high purity, which cannot meet the needs of industrial applications And propose a kind of step is simple, easy to operate, can obtain the 1,3-propanesulfonic acid that moisture content is low, acidity is high and the reduction 1, the method for 3-propane sultone moisture content

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0013] The preparation method of special-purpose 1,3-propane sultone of the present invention is used to prepare 1,3-propane sultone that can be applied to lithium ion secondary batteries, and it comprises the following steps:

[0014] S001. Weigh the crude product of 1,3-propane sultone, then add the water remover and water into the crude product of 1,3-propane sultone according to a certain mass ratio and place them in the reaction kettle together. Airtight and heated for more than half an hour;

[0015] S002. Place the crude 1,3-propane sultone obtained in the above step S001 in a rectification tower for vacuum distillation, that is, when the pressure is lower than 10mmHg, the temperature of the reactor is controlled at 140-160°C, and the temperature at the top of the tower is Perform vacuum distillation at 100-120°C to obtain 1,3-propane sultone with a moisture content of less than 100ppm, an acidity of less than 100ppm, and a purity of more than 99.98%;

[0016] Wherein,...

Embodiment 1

[0019] S011. Put the 1,3-propane sultone raw material with a weight of 497.69g and a moisture value of 524.07ppm and 1.565g of sodium methoxide into a 1L glass reactor, raise the temperature to 60°C, and keep it sealed for 5 Hour;

[0020] S012. Place the 1,3-propane sultone treated in the above step S011 in a rectification tower for vacuum rectification, that is, control the air pressure within 10mmHg, and start receiving after the heating temperature is 160°C and the reflux is stable for 1 hour fraction to give 1,3-propane sultone as a colorless liquid;

[0021] Wherein, the moisture value of 1,3-propane sultone after step S011 treatment in Example 1 of the present invention is 350.92 ppm; the moisture value of 1,3-propane sultone obtained after step S012 treatment The value is 76.17ppm, the acidity is 57.8ppm, the purity is greater than 99.98%, and all indicators meet the requirements.

Embodiment 2

[0023] S021. Put the 1,3-propane sultone raw material with a weight of 498.08g and a moisture value of 667.66ppm and 1.33g of sodium oxide into a 1L glass reactor, raise the temperature to 50°C, and keep it sealed for 6 hours. ;

[0024] S022, placing the 1,3-propane sultone treated in the above step S021 in a rectification tower for vacuum rectification, that is, the pressure is controlled within 10mmHg, and the fraction is received after reflux at a heating temperature of 155° C. for 1 hour, to obtain Colorless liquid 1,3-propane sultone;

[0025] Wherein, the moisture value of the propane sultone treated in step S021 in Example 2 of the present invention is 420.65ppm; the moisture value of the propane sultone treated in step S022 is 82.37ppm, and the acid value is 67.7 ppm, the purity is greater than 99.98%, and all indicators meet the requirements.

[0026] The invention has simple steps and convenient operation, and the obtained product has low moisture content and high...

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Abstract

The invention relates to a method for reducing the moisture content of 1,3-propane sultone. The method comprises the following steps: preparing1,3-propane sultone which can be applied to a lithium ion secondary battery, weighing a crude 1,3-propane sultone product, subsequently adding a dewatering agent and water into the crude 1,3-propane sultone according to a certain mass ratio and putting into a reaction kettle together, and sealing and heating for more than half an hour at normal pressure; (2) putting the crude 1,3-propane sultone product obtained in the step (1) into a rectifying tower for reduced pressure rectification, namely, performing reduced pressure rectification when the pressure is lower than 10mmHg, the temperature of the reaction kettle is controlled to be 140-160 DEG C and the temperature of the tower top is 100-120 DEG C, thereby obtaining the 1,3-propane sultone of which the moisture content is within 100ppm, the acidity is lower than 100ppm and the purity is greater than 99.98%. The method provided by the invention is simple and convenient to operate, low-temperature heating is kept in the operation process, a product and a raw material are effectively prevented from being carbonized and deteriorated, and moreover an obtained product is low in moisture content and high in purity.

Description

technical field [0001] The invention relates to a water removal method for compound additives, in particular to a method for reducing the water content of 1,3-propane sultone. Background technique [0002] 1,3-Propane sultone (PS) is a colorless or light yellow transparent liquid (above 31°C) or colorless transparent crystal (below 31°C). It can be applied to lithium ion secondary batteries in industry. 1,3-propane sultone with high purity (above 99.98%), low moisture (within 100ppm) and low acid value (within 100ppm) can be used as lithium ion secondary battery The additive of the battery electrolyte can enhance the cycle times of the lithium-ion secondary battery, prolong the service life, and prevent flatulence. In recent years, the use of 1,3-propane sultone has become more and more extensive, and the market demand has also increased year by year. At present, the 1,3-propane sultone produced by most manufacturers has high yield and purity, but ignores the problems of m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 李晓峰郭洪杜夕彦罗贺斌
Owner BLUE OCEAN & BLACK STONE TECH CO LTD FUJIAN
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