Preparation method of hydrocarbyl fluoroalkyl asymmetric chain carbonate

A technology of hydrocarbyl fluoroalkyl, chain carbonate, applied in the preparation of organic carbonate, electrochemical generator, organic chemistry, etc., can solve the problems of low yield, complicated synthesis steps, high toxicity of raw materials, etc. The effect of high rate, safe and easy-to-obtain raw materials, and simple process

Inactive Publication Date: 2019-04-05
CHANGSHU CHANGJI CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The main technical problem to be solved by the present invention is to provide a preparation method of hydrocarbyl fluoroalkyl asymmetric chain carbonates, which can solve the problems of high toxicity of raw materials and difficulty in obtaining catalysts in the preparation process of existing chain fluorine-containing carbonates. , cumbersome synthesis steps and low yields

Method used

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  • Preparation method of hydrocarbyl fluoroalkyl asymmetric chain carbonate
  • Preparation method of hydrocarbyl fluoroalkyl asymmetric chain carbonate
  • Preparation method of hydrocarbyl fluoroalkyl asymmetric chain carbonate

Examples

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Embodiment 1

[0034] Add 1980g of 2,2,3,3-tetrafluoropropanol, 2282g of phenyl-p-methylphenyl carbonate, and 250g of sodium carbonate into the reaction kettle, stir and raise the temperature to 68℃, react for 3h, then add 320g of methanol and continue to keep warm After 12h, after the heat preservation is completed, it is transferred to the distillation kettle for atmospheric distillation to obtain 1615 g of methyl tetrafluoropropyl carbonate with a yield of 85.1%. After testing, the purity of the obtained methyl tetrafluoropropyl carbonate is 99.91%, and the moisture content is 56 ppm.

example 2

[0036] Put 3680 g of anhydrous ethanol, 3042 g of bis(o-chlorophenyl) carbonate, and 600 g of solid sodium ethoxide into the reaction kettle, stir and raise the temperature to 78° C., react for 2 hours, and then add 2562 g of 4.4.4-trifluorobutanol. After the dripping is completed, the temperature is kept for 8 hours. After the temperature is completed, it is transferred to the rectification kettle for atmospheric distillation to obtain 1621 g of ethyl tetrafluorobutyl carbonate with a yield of 81.0%. After testing, the purity of the obtained ethyl tetrafluorobutyl carbonate is 99.94%, and the moisture content is 30 ppm.

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Abstract

The invention discloses a preparation method of hydrocarbyl fluoroalkyl asymmetric chain carbonate. The preparation method includes adopting a one-pot method, taking aryl carbonate as an ester exchange matrix, and adding fluoroalkane ester under the action of a basic catalyst to carry out a reaction to obtain fluoroalkyl aryl carbonate, adding hydrocarbyl alcohol for reaction, and performing rectification to obtain the hydrocarbyl fluoroalkyl asymmetric chain carbonate. The preparation method has the advantages of simple technological process, easiness in raw material acquisition, high yield and the like; the purity of the obtained hydrocarbyl fluoroalkyl asymmetric chain carbonate is higher than or equal to 99.9%, the moisture thereof is less than or equal to 100ppm, and the yield thereofis higher than or equal to 80%, so that the application requirements of lithium-ion battery electrolyte additives can be met.

Description

Technical field [0001] The invention relates to the field of lithium ion electrolytes, in particular to a method for preparing a hydrocarbyl fluoroalkyl asymmetric chain carbonate as an additive for lithium battery electrolytes. Background technique [0002] The current commercial lithium battery electrolyte is generally composed of cyclic carbonate. Such cyclic carbonate has a relatively high dielectric constant and can form solvated molecules with lithium ions, which can improve the low-temperature performance of the battery. However, the general cyclic carbonate has a higher freezing point and a lower boiling point, and safety and thermal stability are restricted. [0003] Fluorinated carbonate has the characteristics of high flash point or even no flash point. Studies have shown that adding an appropriate amount of chain fluorocarbonate to the traditional organic electrolyte can achieve a flame-retardant effect, inhibit the burning and explosion of the battery, and reduce the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/06C07C69/96H01M10/0567
CPCH01M10/0525H01M10/0567C07C68/06C07C69/96Y02E60/10
Inventor 傅人俊林晓文丁继华郑翔徐伟文
Owner CHANGSHU CHANGJI CHEM
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