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Synthesis technology of ethylene sulfate

A technology of vinyl sulfate and synthesis process, applied in the direction of organic chemistry, etc., can solve the problems of difficult treatment, large amount of waste water, etc., and achieve the effects of low production cost, less three wastes, and easy availability of raw materials

Inactive Publication Date: 2018-11-16
山东贵邦药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as CN102241662A, CN106187989A, etc., in the oxidation step, a large amount of water is used as a solvent, and metal catalysts (such as iron sulfate, ruthenium chloride, etc.) are used, so the amount of waste water is relatively large and difficult to handle

Method used

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  • Synthesis technology of ethylene sulfate
  • Synthesis technology of ethylene sulfate
  • Synthesis technology of ethylene sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 62g (1mol) of ethylene glycol, 242g (2mol) of dimethylaniline, and 1000mL of chloroform into the reaction flask, cool the temperature to -10°C, add 135g (1mol) of sulfuryl chloride dropwise under stirring, and control the temperature not to exceed 0 ℃. After the dropwise addition was completed, the reaction was incubated for 1 hour. The dimethylaniline hydrochloride produced by filtration, the mother liquor was washed with deionized water to neutrality, after drying with anhydrous sodium sulfate, the solvent was evaporated to dryness to obtain 101 g of a light yellow solid, which was recrystallized with dichloromethane to obtain 94 g of a white product, passed The product was analyzed by liquid chromatography to be vinyl sulfate, and the yield was 75.8%. Melting point: 95-97°C. GC analysis purity: 99.5%.

Embodiment 2

[0029] Add 62g (1mol) of ethylene glycol, 222g (2.2mol) of triethylamine, and 1000mL of dichloromethane into the reaction flask, cool the temperature to -10°C, add 135g (1mol) of sulfuryl chloride dropwise under stirring, and control the temperature not to exceed 0 ℃. After the dropwise addition was completed, the reaction was incubated for 1 hour. The produced triethylamine hydrochloride was filtered, the mother liquor was washed with deionized water until neutral, dried with anhydrous sodium sulfate, and the solvent was evaporated to dryness to obtain 87 g of light yellow solid. Recrystallization with dichloromethane gave 78g of white product. The product was analyzed by liquid chromatography to be vinyl sulfate, and the yield was 63%. Melting point: 95-97°C. GC analysis purity: 99.48%.

Embodiment 3

[0031] Add 62g (1mol) of ethylene glycol, 200g (2.5mol) of pyridine, and 1000mL of dichloroethane into the reaction flask, cool the temperature to -10°C, add 135g (1mol) of sulfuryl chloride dropwise under stirring, and control the temperature not to exceed 0°C . After the dropwise addition was completed, the reaction was incubated for 1 hour. The generated pyridine hydrochloride was filtered, the mother liquor was washed with deionized water until neutral, dried with anhydrous sodium sulfate, and the solvent was evaporated to dryness to obtain 97 g of light yellow solid. Recrystallization with dichloromethane gave 87g of white product. The product was analyzed by liquid chromatography to be vinyl sulfate, and the yield was 70.2%. Melting point: 95-97°C. GC analysis purity: 99.6%.

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Abstract

The invention relates to a synthesis technology of ethylene sulfate. The synthesis technology comprises following steps: reacting glycol with sulfuric chloride under the action of a solvent and an alkaline catalyst, wherein the mole ratio of glycol to sulfuric chloride is 1:0.8-2, the alkaline catalyst is organic amines, the mole ratio of the catalyst to the substrate glycol is 1-4:1, and the reaction temperature is -40 to 50 DEG C; after reactions, filtering to remove salt to obtain a mother liquor, evaporating the mother liquor to obtain a crude product of ethylene sulfate, and finally refining and purifying the crude product to obtain a target product. Compared with the prior art, the synthesis technology has the advantages that glycol and sulfuric chloride are taken as the raw materials to directly synthesize ethylene sulfate under base catalysis; the production steps are few, the production can be easily controlled, the raw materials are easily available, the product is refined only through recrystallization, the production cost is low, and the generation of waste gas, waste solid and waste gas is inhibited.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, in particular to a vinyl sulfate synthesis process. Background technique [0002] With the continuous expansion of the use of lithium-ion batteries, the technology of lithium-ion batteries is also improving. Adding some additives to the electrolyte of lithium-ion batteries can greatly improve and enhance the performance of the battery. Vinyl sulfate, also known as ethylene sulfate (see the structure below), is an excellent SEI film-forming additive, which can inhibit the initial capacity drop of the battery, increase the initial discharge capacity, reduce battery expansion after high temperature storage, and improve battery performance. Charge-discharge performance and cycle times. [0003] [0004] Vinyl sulfate structure [0005] From the literature data of report, the main method of preparing vinyl sulfate has following several kinds: [0006] (1) Direct addition of sulfur trioxid...

Claims

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Application Information

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IPC IPC(8): C07D333/48
CPCC07D333/48
Inventor 向玉联索振贵周海涛
Owner 山东贵邦药业有限公司
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