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Method for preparing glycol sulfite

A technology of ethylene sulfite and dimethyl sulfite, which is applied in the field of preparation of ethylene sulfite, can solve the problems of high chlorohydrin content, long reaction time, poor safety, etc., and achieve high product purity, The effect of high reaction yield and stable reaction

Active Publication Date: 2006-07-19
福建邵武创鑫新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] (1) prepare ethylene sulfite with the method for oxirane and sulfur dioxide reaction, this method security is relatively poor, very high to equipment and operation requirement;
[0004] (2) prepare ethylene sulfite with the method for ethylene glycol and thionyl chloride reaction, although this method is low in cost, thionyl chloride toxicity is big, and reaction generates a large amount of acid gases, and post-treatment purification is more difficult, usually The content of impurities such as chloroethanol is very high;
[0005] (3) prepare ethylene sulfite with the method for polyethylene glycol sulfite depolymerization, this method is not too practical;
[0006] (4) Ethylene sulfite is prepared by reacting ethylene glycol with dimethyl sulfite. If this method does not have a catalyst, it can be carried out, but the reaction time needs to be very long, and the reaction is not carried out completely.
And this ethylene sulfite is not suitable for use as a solvent or additive for lithium secondary battery electrolyte, they will affect the storage stability of the electrolyte

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 1100g (10mol) dimethyl sulfite, 620g (10mol) ethylene glycol, and 8.6g p-toluenesulfonic acid to a 2000ml three-neck flask equipped with a stirrer, a fractionating column, and a thermometer, and heat to 70°C to start the reaction , through the method of fractional distillation, the methanol generated by the reaction is continuously removed. During the reaction, the temperature of the reaction is gradually increased. When the temperature of the reaction system reaches above 170°C and no methanol is distilled out, it indicates that the reaction has been carried out. completely. Finally, fractionate and purify the obtained product, and extract the fraction at 172-173°C, which is the product ethylene sulfite. Yield 970 g, purity 99% (HPLC).

Embodiment 2

[0016] In a 2000ml three-neck flask equipped with a stirrer, a fractionation device, and a thermometer, add 1100 (10mol) dimethyl sulfite, 682g (11mol) ethylene glycol, and 7.5g p-toluenesulfonic acid, and heat the reaction system to 70°C Start the reaction, and continuously remove the methanol generated by the reaction by means of fractional distillation. During the reaction, gradually increase the reaction temperature. When the temperature of the reaction system reaches above 170°C and no methanol is distilled out, it indicates that the reaction Completed. Finally, fractionate and purify the obtained product, and extract the fraction at 172-173°C, which is the product ethylene sulfite. Yield 965 g, purity 99% (HPLC).

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Abstract

The preparation method for ethylene sulfite comprises: with dimethyl sulfite and glycol as material without ratio limit and 0.01-5wt% p-toluenesulfonic acid as catalyst, heating from 60-70Deg to 160-180Deg gradually while removing continually the generated methanol to promote the reaction tend to completeness; finally, fractionating and purifying to obtain the product. This invention has high yield and purification with no corrosion to device.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of ethylene sulfite. Background technique [0002] Ethylene sulfite is a raw material for organic synthesis and can be used as a solvent or additive for electrolytes of lithium secondary batteries. At present, the method of producing ethylene sulfite mainly contains the following several kinds: [0003] (1) prepare ethylene sulfite with the method for oxirane and sulfur dioxide reaction, this method security is relatively poor, very high to equipment and operation requirement; [0004] (2) Ethylene sulfite is prepared by reacting ethylene glycol with thionyl chloride. Although the method is low in cost, thionyl chloride is highly toxic, and the reaction generates a large amount of acid gas, which is difficult to purify after treatment. Usually The content of impurities such as chloroethanol is very high; [0005] (3) prepare ethylene sulfite with the meth...

Claims

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Application Information

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IPC IPC(8): C07C301/00
Inventor 吴茂祥高冬寿
Owner 福建邵武创鑫新材料有限公司
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