Continuous purifying method of crude product of fluoroethylene carbonate

A technology of fluoroethylene carbonate and chloroethylene carbonate, which is applied in the field of continuous purification of fluoroethylene carbonate crude products, can solve the problems of non-continuous process, low production efficiency, unstable product quality and yield, etc. Achieve the effects of reducing energy consumption, ensuring purity, and improving product quality stability

Inactive Publication Date: 2013-01-23
CHINA NAT OFFSHORE OIL CORP +2
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  • Claims
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Problems solved by technology

[0005] The above-mentioned purification process combines a certain treatment method with a rectification process to obtain high-purity fluoroethylene carbonate, but these purification processes are not continuous processes, the production efficiency is low, and the product quality and yield are unstable.
No detailed method for the continuous purification process has been found so far

Method used

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  • Continuous purifying method of crude product of fluoroethylene carbonate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] To process 100 tons / year of high-purity fluoroethylene carbonate, the feed composition is as follows: the content of fluoroethylene carbonate is 23%, the content of solvent is 73%, the content of impurities in light components is 1.5%, and the content of impurities in heavy components is 2.5%.

[0023] Two layers of sodium carbonate adsorption layers and zeolite adsorption layers are alternately installed in the pretreatment tower. The sodium carbonate adsorption layer provides a retention time of 20 minutes, and the zeolite adsorption layer provides a residence time of 30 minutes; The number is 30, the feed is located on the 10th plate (from top to bottom, the same below), the reflux ratio is 5, and the temperature at the top of the tower is controlled at 18 o C; the pressure at the top of the weight-removing rectification tower is 5 mmHg, the number of trays is 30, the feed is located at the 20th plate, the reflux ratio is 10, and the temperature at the top of th...

Embodiment 2

[0025] Processing 500 tons / year of high-purity fluoroethylene carbonate, the feed composition is as follows: the content of fluoroethylene carbonate is 77%, the content of solvent is 20%, the content of impurities in light components is 1.5%, and the content of impurities in heavy components is 1.5%.

[0026] In the pretreatment tower, five layers of potassium hydroxide adsorption layers and five activated carbon adsorption layers are alternately installed. The potassium hydroxide adsorption layer provides a retention time of 60 minutes, and the activated carbon adsorption layer provides a residence time of 80 minutes; the top pressure of the light removal rectification tower is 100 mmHg, The number of trays is 80, the feed is located at the 25th plate, the reflux ratio is 40, and the temperature at the top of the tower is controlled at 34 o C; The pressure at the top of the weight-removing rectification tower is 100 mmHg, the number of trays is 100, the feed is located a...

Embodiment 3

[0028] Processing 350 tons / year of high-purity fluoroethylene carbonate, the feed composition is as follows: the content of fluoroethylene carbonate is 45%, the content of solvent is 53%, the content of impurities in light components is 1.5%, and the content of impurities in heavy components is 0.5%.

[0029] Three layers of calcium bicarbonate adsorption layers and activated clay particle adsorption layers are installed alternately in the pretreatment tower. The calcium bicarbonate adsorption layer provides a retention time of 45 minutes, and the activated clay particle adsorption layer provides a residence time of 55 minutes; The pressure is 50 mmHg, the number of trays is 60, the feed is located at the 20th plate, the reflux ratio is 30, and the temperature at the top of the tower is controlled at 28 o C; The pressure at the top of the weight-removing rectification tower is 60 mmHg, the number of trays is 80, the feed is located at the 65th plate, the reflux ratio is 4...

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Abstract

The invention provides a continuous purifying method of a crude product of fluoroethylene carbonate. The continuous purifying method is characterized by mainly comprising the steps as follows: processing 20-80% of fluoroethylene carbonate crude product (1) generated in the reaction between chloroethylene carbonate and fluorinating agent by virtue of a pre-processing tower (2), so as to obtain colorless decolorized fluoroethylene carbonate (5); carrying out reduced-pressure distillation to the processed crude fluoroethylene carbonate under pressure of 5-100mmHg; and respectively removing light components (7) and heavy components (1) from the top of a light component removing rectifying column (6) and the bottom of a heavy component removing rectifying column (9), so as to obtain fine fluoroethylene carbonate (10).

Description

[0001] technical field [0002] The invention belongs to the technical field of fluoroethylene carbonate production for lithium ion batteries, and in particular relates to a continuous purification method for crude fluoroethylene carbonate products. Background technique [0003] Fluoroethylene carbonate can be used as an additive in the organic electrolyte of a lithium-ion battery. Its addition is small, but it can significantly improve battery performance, such as improving the cycle life of the battery, increasing the safety of the battery, and improving the performance of the battery. low temperature performance. Therefore, fluoroethylene carbonate has been widely used in lithium battery manufacturers such as China, South Korea and Japan. [0004] Fluoroethylene carbonate is usually prepared from chloroethylene carbonate by fluorination. The reaction product contains products, solvents, catalysts and impurities generated by side reactions. If the reaction product is dir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/42
Inventor 吴巍刘红光叶学海郭西凤张洪源周立山
Owner CHINA NAT OFFSHORE OIL CORP
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