Preparation method of cyclic sulfate

Abstract

The invention relates to the field of organic synthesis, in particular to a preparation method of cyclic sulfate. The structural formula of cyclic sulfate is shown as formula I. The preparation methodof cyclic sulfate comprises the following step: cyclic sulfate in the formula I is prepared from a compound in formula II and sulfuryl fluoride by reacting in the presence of an acid binding agent and a catalyst. The preparation method of cyclic sulfate adopts short reaction step, cyclic sulfate can be prepared with the one-step reaction, cost of raw and auxiliary materials is low, and expensiveraw materials and oxidizing agent are not used.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of cyclic sulfuric acid ester. Background technique [0002] The diol compound shown in formula II is esterified to obtain the cyclic sulfuric acid ester shown in formula I. This cyclic sulfuric acid ester is a kind of additive that can make the electrolyte solution of lithium-ion batteries more effective. For example, vinyl sulfate (CAS No.: 1072-53-3) added to the lithium-ion battery electrolyte can inhibit the decline in the initial capacity of the battery, increase the initial discharge capacity, reduce the expansion of the battery after being placed at high temperature, and improve the charging capacity of the battery. Discharge performance and cycle times. Propylene sulfate (CAS No.: 1073-05-8) is used as an electrolyte additive for lithium batteries, which can improve the low-temperature performance of the electrolyte and prevent propylene carbonate m...

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Problems solved by technology

[0011] 1. The reaction steps are long, the manufacturing cost is high, and the complexity of the process and the difficulty of post-processing are increased;

[0012] 2. The chloride ion content of the product is relatively high, and the process of removing chloride ion needs to increase the manufacturing cost of the project;

[0013] 3. The quality of the crude product is low and difficult to purify;

[0014] 4. The oxidation reaction uses expensive catalysts such as ruthenium metal oxide or ruthenium salt, which increases the cost of raw and auxiliary materials;

[0015] 5. It is necessary to contact with water during the manufacturing process, and the intermediate vinyl sulfite and the product vinyl sulfate are unstable in aqueous solution, which will easily lead to the reduction of product yield and purity; the current reported processes require strict control of the pH of the system value, the difficulty of industrialized production is increased, which is unfavorable for obtaining high-quality and high-yield products;

[0016] 6. There is a lot of wastewater output, and the cost of wastewater treatment needs to be increased to reduce the pressure on environmental protection

Due to the difficulty in the preparation of the reagent itself, it is not suitable for industrial production

[0019] Australian Journal of Chemistry, 1977, vol.30, p569-578 reported that 1,2-dibromoethane was used as raw material and silver sulfate to prepare vinyl sulfate by reflux reaction in xylene, the reaction yield was low, and two Both ethyl bromide and silver sulfate are expensive

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