Method for preparing cyclic sulphate

Abstract

The invention discloses a method for preparing cyclic sulphate. The method comprises the following steps: in turn, adding cyclic sulphite, a polar solvent and a catalyst into a reaction container, dipping an oxidant water solution to perform catalytic oxidation reaction under a reaction temperature, adjusting the pH value of the reaction system by alkali in the catalytic oxidation reaction process, standing after finishing reaction, separating the water layer, removing the solvent by distilling an organic layer to obtain the cyclic sulphite crude product, and re-crystallizing or performing vacuum refinery distillation on the crude product to obtain the cyclic sulphate. The method has the advantages of mild catalytic oxidation reaction, easy control, easily available raw materials and cheap raw materials, simple process, convenient operation, high purity and yield of the obtained cyclic sulphate, good stability and easy transportation and storage.

Description

technical field [0001] The invention relates to a preparation method of a cyclic sulfate ester. The cyclic sulfate ester prepared by the method can be used as an additive for lithium-ion battery electrolyte, and can also be used as an intermediate for drug synthesis. Background technique [0002] With the enhancement of people's awareness of environmental protection and the advancement of science and technology, people pay more and more attention to new green energy technologies, especially lithium-ion secondary batteries, due to their characteristics such as high working voltage, small size, light weight, high energy density, Due to the advantages of less environmental pollution, less self-discharge, long cycle life, and no memory effect, it has attracted the attention of the battery industry and has been widely used. Cyclic sulfate, as an additive for lithium-ion battery electrolyte, can effectively avoid the decrease of the initial capacity of lithium-ion batteries, incre...

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Problems solved by technology

[0008] The first is to oxidize cyclic sulfite with sodium hypochlorite to obtain the corresponding cyclic sulfate (Wang P., Chun B; Rachakonda S. et al., J. Org. Chem. 2009, 74, 6819-6824), but Sodium hypochlorite has strong oxidizing properties and is extremely unstable. The process cost is high, it is not easy to control, and it is dangerous. On the other hand, there are many chlorinated impurities in the product, which affects the application of the product in the later stage.

[0009] The second is to oxidize cyclic sulfites with sodium periodate to obtain corresponding cyclic sulfates (Paddon-Jones G.C., Mcerulean C.S.P., Hayes P.et al, J.Org.Chem., 2001, 66, 7487- 7695; Shao H., Rueter J.k., Goodman M., J.Org.Chem., 1998, 63, 5240-5244; Zhang L.Luo S., Mi X.etal., Orange & Biomolecular Chemistry, 2009, 74, 6819- 6824), this method is that sodium periodate is extremely expensive on the one hand, and the cost is too high, can only be used as the preparation of reagent in the laboratory, can't realize industrialization; On the other hand, there are many iodo impurities in the product, which affects the later application

[0010] The third is to oxidize cyclic sulfite with potassium permanganate to obtain the corresponding cyclic sulfate (Berridge M.S, Franceschini M.P., Rosenfeld E.et al, J.Org.Chem., 1990,55,1211-1217) , the method has many side reactions, low yield and difficult product purification

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