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Catalytic ester exchange synthetic method of propylene sulfite and purification method

A technology of propylene sulfite and purification method, applied in organic chemistry and other directions, can solve the problems of multiple impurities, increase equipment investment, and high safety protection requirements, and achieve the effects of high reaction yield, easy reaction and simple operation.

Inactive Publication Date: 2010-06-23
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Due to the high toxicity of thionyl chloride, the safety protection requirements in the production process are relatively high; a large amount of corrosive gas hydrogen chloride is produced in the production process, which seriously corrodes the production equipment, and an additional hydrogen chloride gas absorption device is also required, which increases the equipment Investment; the direct cyclization reaction is not complete, the yield is only about 50%, there are many impurities in the product, it is difficult to purify, and it is even more difficult to obtain high-quality products. To be used as an electrolyte additive for lithium-ion batteries, the quality must be reach battery level
Therefore, the propylene sulfite product obtained by the traditional direct cyclization method is difficult to be applied in lithium batteries

Method used

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  • Catalytic ester exchange synthetic method of propylene sulfite and purification method
  • Catalytic ester exchange synthetic method of propylene sulfite and purification method
  • Catalytic ester exchange synthetic method of propylene sulfite and purification method

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Add 380g propylene glycol, 600g dimethyl sulfite, and 10g concentrated hydrochloric acid to a 1000ml three-necked flask equipped with an electric stirrer, distillation column and thermometer. Heat and stir the reaction. When the internal temperature reaches 70℃, there will be Methanol is distilled out from the rectifying column. As the reaction progresses, the internal temperature continues to rise. Keep the reaction temperature below 130°C until no more methanol is distilled out of the rectifying column, indicating that the reaction has been completed. Reaction time For 5 hours. 620 g of product was obtained. The reaction product was analyzed by gas chromatography. The composition of the product was 91.5% of propylene sulfite, 1.5% of propylene glycol, 1.8% of dimethyl sulfite, and 1.5% of methanol.

Embodiment 2

[0034] In a 1500 ml three-necked flask equipped with an electric stirrer, distillation column and thermometer, add 380g propylene glycol, 760g diethyl sulfite, 8g concentrated hydrochloric acid, heat and stir the reaction, when the internal temperature reaches 85 ℃, there will be Ethanol is distilled out from the rectifying column. As the reaction progresses, the internal temperature continues to increase. Keep the reaction temperature below 130°C until no more ethanol is distilled out of the rectifying column, indicating that the reaction has been completed. Reaction time Is 5.5 hours. 630 g of product was obtained. The reaction product was analyzed by gas chromatography. The product composition was: propylene sulfite 90.3%, propylene glycol 2.2%, diethyl sulfite 3.5%, and ethanol 2.1%.

Embodiment 3

[0036] Add 380g propylene glycol, 630g dimethyl sulfite, and 7.5g p-toluenesulfonic acid into a 1000ml three-necked flask equipped with an electric stirrer, distillation column and thermometer. Heat and stir the reaction. When the internal temperature reaches 70℃ , There is methanol distilled out from the rectifying column. As the reaction progresses, the internal temperature keeps increasing. Keep the reaction temperature below 130°C until no more methanol distills out of the rectifying column, indicating that the reaction has been completed , The reaction time is 4.5 hours. 625 g of product was obtained. The reaction product was analyzed by gas chromatography. The composition of the product was 92.3% propylene sulfite, 1.0% propylene glycol, 2.0% dimethyl sulfite, and 1.8% methanol.

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Abstract

The invention relates to the filed of chemical synthesis and purification, in particular to a catalytic ester exchange synthetic method of propylene sulfite and a purification method. Under the action of a catalyst, propanediol and dialkyl sulfite take the ester exchange reaction, a fractionation reaction method is adopted for producing the propylene sulfite and byproducts of alkylol, then, the coarse products of the propylene sulfite are refined and purified by methods of crude distillation, water washing, neutralization, water washing, drying and fine distillation.

Description

【Technical Field】 [0001] The invention relates to the field of chemical synthesis and purification, in particular to the synthesis method and purification method of propylene sulfite. Propylene sulfite can be used as a raw material for organic synthesis or as an electrolyte additive for lithium-ion batteries. 【Background technique】 [0002] The propylene sulfite referred to in the present invention is a compound having the following structure. [0003] [0004] Propylene sulfite is a raw material for organic synthesis. In organic synthesis, hydroxypropyl groups can be introduced, followed by a series of reactions on the hydroxyl active groups. Another important role is to act as an additive for lithium ion secondary battery electrolyte. Studies have shown that adding 5% (volume fraction) of propylene sulfite to 1mol / L LiClO4 / PC can effectively prevent PC molecules from intercalating into the graphite electrode. At the same time, the low temperature performance of the electrolyte ...

Claims

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Application Information

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IPC IPC(8): C07D327/10
Inventor 吴茂祥方桂煌潘荧王文国黄剑莹
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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