Synthetic method of cyclosulphate

Abstract

The invention discloses a synthetic method of cyclosulphate. A peroxysulfate solution is pre-synthesized through sulfuric acid and hydrogen peroxide, then under existence of an organic solvent, a metal inorganic compound and a catalyst, the peroxysulfate solution is dropwise added to generate a catalytic oxidation reaction with cyclosulfite, after the reaction is completed, salt residue is filtered out, still standing for layering is conducted, an organic layer is taken to be distilled, concentrated and purified, and a cyclosulphate high-quality product is obtained. According to the syntheticmethod of the cyclosulphate, the cheap sulfuric acid and hydrogen peroxide are used as the raw materials, the peroxysulfate solution is prepared to conduct catalytic oxidation on the cyclosulfite, onthe one hand, the reaction is mild, control is easy, and the reaction conversion rate is high; on the other hand, the evaporation capacity of water is small, energy consumption is low, generated wastewater is less, and a synthetic process is more environmentally friendly; and the prepared cyclosulphate is few in impurity, high in purity and wide in market prospect.

Description

technical field [0001] The invention relates to the technical field of synthesis of new energy materials, in particular to a method for synthesizing cyclic sulfate esters. The cyclic sulfate esters prepared by the method can be used as additives for lithium-ion battery electrolytes, and can also be used as intermediates in drug synthesis. body. 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, The advantages of low environmental pollution, small self-discharge, long cycle life and no memory effect have attracted the attention of the battery industry and been widely used. As an additive for lithium-ion battery electrolyte, cyclic sulfate can effectively avoid the ...

AI Technical Summary

Problems solved by technology

[0008] The first is to oxidize cyclic sulfite with sodium hypochlorite to obtain the corresponding cyclic sulfate (Wang P., ChunB; Rachakonda S. et al., J. Org. Chem. 2009, 74, 6819-6824), although sodium hypochlorite Strong oxidizing property but extremely unstable, especially low active oxygen content, large amount of wastewater, and the by-product sodium chloride is difficult to recycle and can only be treated as solid waste, which increases the pressure on environmental protection and is highly corrosive to equipment; On the other hand, the introduction of chlorine-containing oxidants has the potential risk of increasing impurities, which also increases the difficulty of product purification in the later stage and downstream use

[0009] The second is to oxidize cyclic sulfites with sodium periodate to obtain corresponding cyclic sulfates (Paddon-JonesG.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., MiX.etal., Orange & Biomolecular Chemistry, 2009, 74, 6819 -6824), the method is that sodium periodate is extremely expensive on the one hand, and the cost is too high, and can only be prepared as a reagent in the laboratory, and cannot realize industrialization; on the other hand, there are many iodo impurities in the product, which affects the later stage. 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

[0011] The fourth is to adopt potassium hydrogen persulfate compound salt to oxidize cyclic sulfuric acid ester (CN103012386A, CN104744427A), although this method is mild in reaction, easy to control, but the cost of oxidizing agent is high, and the sulfate amount of by-product is relatively large