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A kind of preparation method of electronic grade 1,3-propane sultone

A propane sultone, electronic-grade technology, applied in the field of organic compound preparation, can solve the problems of affecting product quality, difficult to realize industrialization, complicated process operation, etc., and achieves stable and controllable operation process, low equipment requirements, and operation process. simple effect

Active Publication Date: 2021-02-09
湖北吉和昌化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) In the patent CN200910068035.8, the liquid 1,3-propane sultone raw material is put into a circulating crystallizer, so that the raw material forms a film-like crystal in the crystallization tube, and then heats and dissolves to collect the finished product. However, this method cannot Value and moisture are effectively controlled, which is not suitable for industrial production;
[0005] (2) In the patent CN201710282245.1, electronic grade 1,3-propane sultone is prepared by molecular sieve, nanofiltration membrane and reverse osmosis device; this method can remove the moisture in the product, but there is a pressure difference of 15-20Mpa during the operation , and the process is cumbersome and difficult to realize industrialization;
[0006] (3) In our company's patent CN201510355390.9, the acid value and moisture in 1,3-propane sultone are removed by adding a compound acid and water removal agent to 1,3-propane sultone industrial products, and then pass Electronic grade products are obtained by distillation; however, the yield of this method is low, and adding a compound acid and water removal agent will affect the quality of the product
[0007] It can be seen that the above-mentioned method for preparing electronic grade 1,3-propane sultone all has weak points

Method used

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  • A kind of preparation method of electronic grade 1,3-propane sultone

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preparation example Construction

[0023] This example provides a preparation method of electronic grade 1,3-propane sultone, comprising the following steps: after recrystallizing industrial grade 1,3-propane sultone with anhydrous organic solvent, separating the crystal, The crystal is rectified, and the water and impurities are separated under the state of total reflux to obtain electronic grade 1,3-propane sultone.

[0024] In some preferred embodiments, the recrystallization specifically adopts the following method: add industrial grade 1,3-propane sultone to an enamel reactor with frequency conversion and speed regulation mechanical stirring, and raise the temperature of the reactor to 40-45°C , then drop anhydrous organic solvent into the reaction kettle to dissolve 1,3-propane sultone, keep stirring for 50 to 70 minutes, slow down the stirring speed of the mixed solution, and slowly lower the temperature of the mixed solution, and after the crystals are precipitated, the The solution was centrifuged, and...

Embodiment 1

[0035] Embodiment 1 of the present invention provides a preparation method of electronic grade 1,3-propane sultone, comprising the following steps:

[0036] (1) After adding 300kg of industrial grade 1,3-propane sultone to a 500L enamel reactor with frequency conversion speed regulation mechanical stirring, the temperature of the reactor was raised to 40°C, and then 100kg of Water ethanol, at a stirring speed of 80r / min, after insulated and stirring for 60min, the stirring speed was reduced to 25r / min, and the temperature of the mixed solution was slowly lowered at a cooling speed of 3°C / h until crystals were precipitated. Centrifugal separation, the solvent recovery sleeve is used for the next batch;

[0037] (2) Add the crystals obtained by centrifugation in step (1) into a 200L rectification kettle, heat the temperature in the rectification kettle to 100°C with an electric heating oil bath, and turn on the vacuum unit to reduce the vacuum in the rectification kettle to 100°...

Embodiment 2

[0044] Embodiment 2 of the present invention provides a preparation method of electronic grade 1,3-propane sultone, comprising the following steps:

[0045](1) After adding 250kg of industrial-grade 1,3-propane sultone into a 500L enamel reactor with frequency conversion speed regulating mechanical stirring, the temperature of the reactor was raised to 40°C, and then 100kg of For water methanol, the stirring speed is 85r / min, after 60min of heat preservation and stirring, the stirring speed is reduced to 20r / min, and the temperature of the mixed solution is slowly lowered at a cooling speed of 2°C / h until the crystals are precipitated. Centrifugal separation, the solvent recovery sleeve is used for the next batch;

[0046] (2) Add the crystals obtained by centrifugation in step (1) into a 200L rectification kettle, heat the temperature in the rectification kettle to 110°C with electric heating in an oil bath, and turn on the vacuum unit to reduce the vacuum in the rectificatio...

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Abstract

The invention discloses a preparation method of electronic grade 1,3-propane sultone, which comprises the following steps: after recrystallizing industrial-grade 1,3-propane sultone with anhydrous organic solvent, separating the crystal, and dissolving the The above crystals are rectified, and the water and impurities are separated under the state of total reflux to obtain electronic grade 1,3-propane sultone. The preparation method of the present invention prepares electronic-grade 1,3-propane sultone by combining recrystallization and rectification, and removes free acid in industrial-grade 1,3-propane sultone through recrystallization in anhydrous organic solvent and impurities, the trace solvent and water in the crystal are removed by rectification, the whole operation process is simple, stable and controllable, the requirements for equipment are not high, and it is suitable for industrial production; only water, low boiling point solvent and impurities are separated during the rectification process , The finished product does not need to be condensed and collected after distillation. Compared with the traditional method, it not only has less waste and saves energy consumption, but also improves production capacity and product yield.

Description

technical field [0001] The invention relates to the technical field of organic compound preparation, in particular to a preparation method of electronic grade 1,3-propane sultone. Background technique [0002] 1,3-Propane sultone is an important intermediate in organic synthesis. 1,3-Propane sultone is a white crystal at room temperature with a melting point of 30-33°C. It is widely used in electroplating, medicine, photosensitive materials, lithium battery electrolyte, surfactant and other fields. In recent years, with the development of lithium-ion batteries in the new energy field, high-end lithium-ion battery electrolytes have higher and higher quality requirements for 1,3-propane sultone, especially purity (≥99.9%), moisture (< 50ppm) and acid value (<50ppm) have higher requirements. However, 1,3-propane sultone is a heat-sensitive material, and side reactions such as carbonization, decomposition, and polymerization will occur during the high-temperature process...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 冯庆诚杨威付远波肖忠新宋文华
Owner 湖北吉和昌化工科技有限公司
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