Preparation method of electronic grade 1,3-propane sultone

Abstract

The invention discloses a preparation method of electronic grade 1,3-propane sultone. The preparation method comprises the steps of carrying out recrystallization on industrial-grade 1,3-propane sultone by virtue of an anhydrous organic solvent, separating crystals, rectifying the crystals, and separating moisture and impurities at a total reflux state, so as to obtain electronic grade 1,3-propanesultone. According to the preparation method, electronic grade 1,3-propane sultone is prepared through the combination of recrystallization and rectification, free acids and impurities in industrial-grade 1,3-propane sultone are removed by virtue of the anhydrous organic solvent, trace solvents and moisture in the crystals are removed through rectification, the whole operation process is simple,stable and controllable, and the preparation method is low in equipment requirement and suitable for industrial production; and compared with a traditional method, only the moisture, low-boiling-pointsolvents and the impurities are separated in the rectification process, and the finished product does not need to be condensed and collected after being distilled, so that the three wastes are few, the energy consumption is saved, and the production capacity and the production yield are increased.

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...

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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

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