Solvent-free method for preparing 1,3-propane sultone

Abstract

The invention discloses a solvent-free method for preparing 11,3-propane sultone. According to the method, propenol and ammonium sulfite are used as reaction raw materials; and deionized water is adopted as medium. The preparation method comprises the following steps: stirring ammonium sulfate and deionized water; at 20-50 DEG C, preparing a mixed solution from acrolein, an initiator and deionizedwater, dropwise adding the mixed solution into a beaker, and carrying out catalytic reaction to generate an aqueous solution of 3-hydroxypropylammonium sulfonate; adding calcium hydroxide to carry out alkalization reaction, after alkalization is completed, adding concentrated sulfuric acid for acidification treatment to obtain 3-hydroxypropanesulfonic acid and solid calcium sulfate, and performing filtration to obtain an aqueous solution of the 3-hydroxypropanesulfonic acid; carrying out concentration and reduced pressure rectification to obtain a target product; adding a certain amount of calcium hydroxide and water into kettle residues, performing hydrolysis to obtain an aqueous solution of calcium 3-hydroxypropanesulfonate, adding concentrated sulfuric acid for acidification treatment,performing filtration to obtain an aqueous solution of 3-hydroxypropanesulfonic acid, and carrying out concentration and reduced pressure rectification to obtain the target product. The method has the advantages of simple process, simple raw materials, no solvent and no waste, and the yield can reach 95%.

Description

technical field [0001] The invention relates to the field of electrolyte additives for lithium-ion batteries, in particular to a solvent-free method for preparing 1,3-propane sultone which can be used as an additive for electrolytes of lithium-ion batteries. Background technique [0002] The structural formula of 1,3-propane sultone is: 1,3-propane sultone is widely used in dyes, medicines, surfactants, lithium batteries and other fields; the preparation method of 1,3-propane sultone has been reported at home and abroad, and the application number is 20081023414. A Chinese patent specification of X discloses a preparation method for synthesizing 1,3-propane sultone. The method uses bisulfite, sulfite and propylene alcohol as raw materials, water as a medium, and crown ether as a catalyst. React at a temperature of 40-100°C to form a reaction mixture containing hydroxypropanesulfonate, then add hydrochloric acid to the reaction mixture containing hydroxypropanesulfonate for...

AI Technical Summary

Problems solved by technology

[0003] The disadvantage of adopting the above preparation method is that the reaction requires a certain temperature and time, the solvent is flammable and explosive, and the recovered ethanol contains acid, which is easy to corrode the equipment; it needs to use absolute ethanol, and it is difficult to dehydrate the recovered ethanol to anhydrous. There is loss in production, it is difficult to handle in production, and the cost is high. Distillation at high temperature is easy to intermolecular polymerization of 3-hydroxypropanesulfonic acid, which affects the product yield.