Preparation method of vinylene carbonate for lithium ion-cell

The technology of vinylene carbonate and ethylene carbonate is applied in the field of preparation of vinylene carbonate for lithium ion batteries, which can solve the problems of many by-products, complicated operation and high chloride content, and avoid the generation of peroxide, The effect of avoiding decomposition reaction and low operating temperature

Inactive Publication Date: 2008-04-16
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Its disadvantages are: the chlorination reaction raw materials are highly toxic, the operation is complicated, and the conversion rate is low. The hydrogen chloride elimination reaction is carried out in an ether organic solvent, and the flash point is low and it is easy to form peroxides during storage, resulting in hidden dangers; and carbonic acid The melting point of vinyl ester is as high as 37°C, and it is not easy to separate EC and VC in the later stage
The purification process adopts multiple rectification, the product is easy to decompose, the by-products are many, the yield is low, and the chloride content is high, which affects the use effect in lithium-ion batteries

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Synthesis of chloroethylene carbonate:

[0028] Dissolve 2g of azobisisobutyronitrile in 20ml of 1,2-dichloroethane, fully dissolve and set aside. 600 grams of ethylene carbonate was melted in an oven at 60°C and then added to the reactor. The reactor is heated with a jacket, and the heat source comes from 80°C hot water in a constant temperature water bath. When the material temperature in the reactor reaches 75°C, the azobisisobutyronitrile solution is added, and sulfuryl chloride is dropped in at the same time. Take 15ml of the previously prepared azobisisobutyronitrile solution and add it in three times, each time 5ml. A total of 700ml of sulfuryl chloride was added, which was divided into three additions, 250ml, 250ml and 200ml respectively. Both are added after azobisisobutyronitrile, which is continuous dropwise addition, and the time for each addition is 30 minutes. After adding all the sulfuryl chloride, take 5ml of the previously prepared azobisisobuty...

Embodiment 2

[0034] (1) Synthesis of chloroethylene carbonate:

[0035] Dissolve 2g of azobisisobutyronitrile in 20ml of 1,2-dichloroethane, fully dissolve and set aside. 600 grams of ethylene carbonate was melted in an oven at 60°C and then added to the reactor. The reactor is heated with a jacket, and the heat source comes from 80°C hot water in a constant temperature water bath. When the material temperature in the reactor reaches 75°C, the azobisisobutyronitrile solution is added, and sulfuryl chloride is dropped in at the same time. Take 15ml of the previously prepared azobisisobutyronitrile solution and add it in three times, each time 5ml. A total of 700ml of sulfuryl chloride was added, which was divided into three additions, 250ml, 250ml and 200ml respectively. Both are added after azobisisobutyronitrile, which is continuous dropwise addition, and the time for each addition is 30 minutes. After adding all the sulfuryl chloride, take 5ml of the previously prepared azobisisobuty...

Embodiment 3

[0041] The preparation method of chloroethylene carbonate and the synthetic method of vinylene carbonate are the same as embodiment 1, and the vinylene carbonate of 512 grams of 95.2% is carried out rectifying and purifying once, and the theoretical plate number of rectifying tower is 20, and vacuum degree It is -0.098MPa, obtains 460 grams of 98% vinylene carbonate, recrystallizes in 500 grams of toluene, the recrystallization temperature is 5 ° C, and obtains 335 grams of vinylene carbonate with a purity of 99.89%, and the chlorine content is 62ppm.

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Abstract

A preparation method for vinylene carbonate used for lithium ion battery, which is characterized in that Vinylene carbonate and Sulphuryl chloride are adopted as raw materials to prepare chloro-substited ethylene carbonate under the function of an initiator, and the chloro-substituted ethylene carbonate and triethylamine undergo a reaction to eliminate hydrogen chloride, in order to produce vinylene carbonate, the synthesized crude vinylene carbonate undergoes multiple purifications and extractions such as decompressed distillation, fine distillation, and recrystallization to obtain vinylene carbonate used for battery.

Description

technical field [0001] The invention relates to lithium-ion battery technology, in particular to a preparation method of vinylene carbonate for lithium-ion batteries. Background technique [0002] Vinylene carbonate (VC for short) is currently the most ideal organic film-forming additive in lithium-ion secondary batteries. VC can undergo free radical polymerization on the surface of the carbon negative electrode to generate polyalkylcarbonate compounds, thereby effectively It can effectively inhibit the co-intercalation reaction of solvent molecules, effectively improve the charge-discharge efficiency and cycle characteristics of lithium-ion secondary batteries, and improve the battery's storage resistance and other performances. It is an important electrolyte additive for lithium-ion batteries. . [0003] The traditional method for preparing vinylene carbonate mainly comprises the following steps: [0004] (1) Taking ethylene carbonate as raw material, introducing chlorin...

Claims

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Application Information

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IPC IPC(8): C07D307/40
Inventor 张健宋晓莉赵洪李晓磊
Owner CHINA NAT OFFSHORE OIL CORP
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