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Method for purifying 1,3-propanesultone

A technology of propane sultone and purification method, applied in directions such as organic chemistry, can solve problems such as low purity, long time consumption, loss of purification method, etc., and achieve the effects of high purity, short time consumption and wide application value

Inactive Publication Date: 2018-03-23
HUIZHOU CAPCHEM CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved in the application of the present invention is to provide a kind of 1,3-propane sultone product purification method for the shortcomings of serious loss, long time consumption and low purity in the prior art. Purification method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] This example is used to illustrate the purification method of 1,3-propane sultone disclosed in the present invention. At room temperature, 18.0Kg of 1,3-propane sultone crude product was injected into a 20L static melting crystallizer similar to a tube heat exchanger through N2, and the main content of the product was detected by gas chromatography to be 93.52%. Set the initial cooling point to 34°C, turn on the heat exchange medium circulation switch, and cool down by 1°C every 1 hour until the temperature drops to 29°C, crystallization begins to appear on the tube wall, continue to cool down to 26°C, most of the crystals have precipitated, and the crystal form is Small blocks of tetrahedrons are regularly distributed, stay at this temperature for 2 hours, there is still a small amount of unsolidified low-concentration raffinate, and the color is darker, released, weighing 3.2Kg, gas chromatography shows that 1,3-propanesulfonic acid in the raffinate The lactone conten...

Embodiment 2

[0023] This example is used to illustrate the purification method of 1,3-propane sultone disclosed in the present invention. At room temperature, put 24.7Kg of the crude product of 1,3-propane sultone in a 20L static melting crystallizer, set the initial cooling point to 32°C, turn on the heat exchange medium circulation switch, drop the temperature by 1°C every 1h, and drop the temperature to At 25°C, the tube wall began to crystallize, and continued to cool down to 21°C, most of the crystals were precipitated, and the crystals were regularly distributed in the shape of small tetrahedrons. After staying at this temperature for 2 hours, there was still a small amount of unsolidified low-concentration raffinate, and The color is darker, released, weighing 4.3Kg, gas chromatography shows that the content of 1,3-propane sultone in the raffinate is 77.24%.

[0024] The temperature of the crystal starts to rise slowly, and the temperature is increased by 1°C every 1h, and the melti...

Embodiment 3

[0026] This example is used to illustrate the purification method of 1,3-propane sultone disclosed in the present invention. At room temperature, 22.5Kg of 1,3-propane sultone crude product was injected into a 20L static melting crystallizer similar to a tube heat exchanger through N2, and the main content of the product was detected by gas chromatography to be 93.46%. Set the initial cooling point to 31°C, turn on the heat exchange medium circulation switch, and cool down by 0.5°C every 1 hour until the temperature drops to 25.5°C, crystallization begins to appear on the tube wall, continue to cool down to 21°C, most of the crystals have precipitated, and the crystal form is Small blocks of tetrahedrons are regularly distributed, stay at this temperature for 2 hours, there is still a small amount of unsolidified low-concentration raffinate, and the color is darker, released, weighing 4.1Kg, gas chromatography shows that 1,3-propanesulfonic acid in the raffinate The content of...

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Abstract

The invention provides a method for purifying 1,3-propanesultone. The method comprises the following steps: S1, providing crude 1,3-propanesultone; and 2, purifying the crude 1,3-propanesultone: cooling and crystallizing the crude 1,3-propanesultone to obtain crystals and a raffinate, separating out the crystals, heating the crystals, and separating the obtained solid substance to obtain the finished 1,3-propanesultone. The method for purifying the 1,3-propanesultone has the advantages of short time, high purity and wide application values.

Description

technical field [0001] The application of the present invention relates to a method for purifying 1,3-propane sultone, which belongs to the technical field of chemical industry. Background technique [0002] 1,3-Propane sultone is a chemical substance with the chemical formula C3H6O3S, a sulfonating agent, widely used in pharmaceutical and chemical industries, photosensitive materials, lithium batteries, biochemistry, textiles, lubrication, wastewater treatment, surface treatment and other industries. It is a widely used lithium-ion battery electrolyte additive. Contribute to the formation of SEI film, can improve the cycle performance of lithium-ion batteries and enhance the safety of batteries. During the first charging and discharging process of the liquid lithium-ion battery, the electrode material and the electrolyte react at the solid-liquid phase interface to form a passivation layer covering the surface of the electrode material. The formed passivation film can eff...

Claims

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Application Information

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IPC IPC(8): C07D327/04
Inventor 曹英杰王帮应乔兴民陈群周建新
Owner HUIZHOU CAPCHEM CHEM CO LTD
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