Method for inhibiting discolorment of vinylene carbonate

A vinylene carbonate, temperature range technology, applied in the field of inhibiting the discoloration of vinylene carbonate, can solve the problems of difficult separation, unstable battery electrochemical window, affecting battery cycle stability, etc., and achieves a simple synthesis process route and residual amount. less effect

Active Publication Date: 2010-06-02
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has the following problems: because the chlorine-containing organic impurities generated by chlorine disproportionation in the raw material cannot be completely reacted, and it is difficult to completely separate due to the close boiling point, it is easy to boil with a trace amount of excessive metal ions at high temperature to form a complex, thereby developing color.
Discolored vinylene carbonate is used in lithium battery electrolyte, which will easily cause the electrochemical window of the battery to be unstable, thus affecting the cycle stability of the battery

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] In a three-necked flask containing 500 g of vinylene carbonate (99.99% purity, 5.81 moles) and 250 g (4.31 moles) of acetone, 5 g (0.083 moles) of urea was added under stirring, and refluxed at 60° C. for 5 hours. After cooling and filtering, 715 g of filtrate was obtained. The components of the filtrate were analyzed with a gas chromatograph (GC-2014, purchased from Shimadzu Corporation), and it was found that the filtrate was a mixture of 69.23% by weight of vinylene carbonate and 29.83% by weight of acetone. Carry out rectification under reduced pressure to the filtrate obtained above, collect 60~70 ℃ / 2~5kPa distillate 490g, record with gas chromatograph (GC-2014, purchased from Shimadzu company), the purity of vinylene carbonate in the distillate is 99.9954 weight%. The obtained product was baked at 60° C. for 24 hours, the chromaticity changed to 1 blackness, and the yield of the high-purity non-discoloring vinylene carbonate product was 98.0%.

Embodiment 2

[0015] In a three-necked flask containing 500 g of vinylene carbonate (purity 99.99%, 5.81 moles) and 250 g (4.31 moles) of cyclohexane, 50 g (0.083 moles) of urotropine was added under stirring, and refluxed at 60° C. for 5 hours. Cool and filter to obtain 685 g of filtrate. After analyzing the components of the filtrate with a gas chromatograph (GC-2014, purchased from Shimadzu Company), it was found that the filtrate was a mixture of 68.61% by weight of vinylene carbonate and 28.75% by weight of acetone. Carry out rectification under reduced pressure to the filtrate obtained above, collect 60~70 ℃ / 2~5kPa distillate 462g, record with gas chromatograph (GC-2014, purchased from Shimadzu company), the purity of vinylene carbonate in the distillate is 99.9958 weight%. The obtained product was baked at 60° C. for 24 hours, the chromaticity changed to 2 degrees of blackness, and the yield of the high-purity non-discoloring vinylene carbonate product was 92.3%.

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Abstract

The invention discloses a method for effectively inhibiting the discolorment of vinylene carbonate, comprising the following steps of: carrying out reflow reaction on vinylene carbonate in the presence of solid organic amine with the alkalinity of 7-10 and a solvent with the boiling point of 40-80 DEG C in the temperature range of 40-80 DEG C; then filtering to obtain a mixture containing the vinylene carbonate; and carrying out rectification under vacuum on the mixture and collecting fraction to obtain the required vinylene carbonate. The invention can be widely suitable for inhibiting the discolorment of the vinylene carbonate.

Description

technical field [0001] The invention relates to a method for suppressing discoloration of vinylene carbonate. Background technique [0002] Vinylene carbonate is mainly used in lithium battery electrolyte, which can effectively improve its cycle performance and so on. In the existing research on the synthesis of vinylene carbonate, a method that has been reported is to take ethylene carbonate and chlorination reagents as raw materials to prepare chloroethylene carbonate, and directly generate vinylene carbonate in the presence of triethylamine The mixture was rectified under reduced pressure to collect high-purity vinylene carbonate product. This method has the following problems: because the chlorine-containing organic impurities generated by chlorine disproportionation in the raw material cannot be completely reacted, it is difficult to completely separate due to the close boiling point, and it is easy to boil with a trace amount of excessive metal ions at high temperatur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/40
Inventor 沈锦良张先林杨志勇李伟锋张丽亚
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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