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Method used for preparing high-purity ethyl methyl carbonate

A technology of ethyl methyl carbonate and diethyl carbonate, which is applied in the field of synthesis of ethyl methyl carbonate, can solve the problems of long reaction time, high requirements for catalyst raw materials, unsatisfactory conversion rate, etc., and achieve short reaction time and high selectivity , highly active effect

Inactive Publication Date: 2015-07-15
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In summary, the catalysts mentioned above have problems such as high requirements on raw materials, long reaction time, unsatisfactory conversion rate, and difficulty in product separation and purification.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Solid super base Na-NaOH / γ-Al 2 o 3 Preparation: Add 100 grams of γ-Al to the reactor 2 o 3 , under the conditions of strong stirring and nitrogen purging, heating to 200°C to remove water adsorbed on the surface of the carrier. The temperature was raised to 300°C, and 25 g of NaOH was added under vigorous stirring and nitrogen purging, and kept for 3 h. Afterwards, 8 g of metallic sodium were quickly added and stirring was continued for 3 hours. Cool to get solid super base Na-NaOH / γ-Al 2 o 3 catalyst.

[0023]Synthesis of EMC by transesterification of DMC and DEC: 152 grams of DMC and 100 grams of DEC (DMC and DEC molar ratio 2:1) were added to the reactor, and 5 grams of the super-strong base catalyst prepared above. Slowly raise the temperature to 90°C and react for 1h. The catalyst and liquid product were separated by filtration. The liquid product was analyzed by chromatography and EMC was found to be the only product with a yield of 45%. Filter and sepa...

Embodiment 2

[0026] Solid super base Na-KOH / γ-Al 2 o 3 Preparation: Add 100 grams of γ-Al to the reactor 2 o 3 , under the conditions of strong stirring and nitrogen purging, heating to 200°C to remove water adsorbed on the surface of the carrier. The temperature was raised to 300°C, and 30 g of KOH was added under vigorous stirring and nitrogen purging, and kept for 3 h. After that, 8 g of sodium metal was added quickly, and stirring was continued for 3 h. Cool to get solid super base Na-KOH / γ-Al 2 o 3 catalyst.

[0027] Synthesis of EMC by transesterification of DMC and DEC: 229 grams of DMC and 100 grams of DEC (3:1 molar ratio of DMC and DEC) were added to the reactor, and 5 grams of the super-strong base catalyst prepared above. Slowly raise the temperature to 90°C and react for 1h. The catalyst and liquid product were separated by filtration. The liquid product was analyzed by chromatography and EMC was found to be the only product with a yield of 48%. Filter and separate t...

Embodiment 3

[0030] Solid super base K-KOH / γ-Al 2 o 3 Preparation: Add 100 grams of γ-Al to the reactor 2 o 3 , under the conditions of strong stirring and nitrogen purging, heating to 200°C to remove water adsorbed on the surface of the carrier. The temperature was raised to 300°C, and 30 g of KOH was added under vigorous stirring and nitrogen purging, and kept for 3 h. After that, 10 g of potassium metal was added quickly, and stirring was continued for 3 h. Cool to get solid super base K-KOH / γ-Al 2 o 3 catalyst.

[0031] Synthesis of EMC by transesterification of DMC and DEC: Add 152 grams of DMC and 100 grams of DEC (the molar ratio of DMC and DEC is 2:1) into the reaction kettle, and 3 grams of the super base catalyst prepared above. Slowly raise the temperature to 100°C and react for 1 hour. The catalyst and liquid product were separated by filtration. The liquid product was analyzed by chromatography and EMC was found to be the only product with a yield of 50%. Filter and ...

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PUM

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Abstract

The invention relates to a synthetic method of ethyl methyl carbonate (EMC), and specifically relates to a method used for catalyzing dimethyl carbonate and diethyl carbonate with a solid super base so as to synthesize ethyl methyl carbonate. According to the method, the solid super base is taken as a catalyst; and high-selectivity catalyzing of dimethyl carbonate and diethyl carbonate is carried out; so that ethyl methyl carbonate is obtained via synthesis; the molar ratio of dimethyl carbonate to diethyl carbonate is 0.25-4:1; reaction temperature is lower than 150 DEG C; reaction is carried out at normal pressure; reaction time ranges from 1 to 3h; and catalyst amount accounts for 1 to 5% of the weight of the raw materials. The solid super base is taken as the catalyst; reaction time is short; selectivity is high; and EMC products with a purity required by lithium ion battery electrolyte can be obtained via simple distillation. Activity of the catalyst is high; and recycling of the catalyst after reaction can be realized.

Description

technical field [0001] The invention relates to a synthesis method of ethyl methyl carbonate, specifically utilizing a solid superbasic catalyst to catalyze the transesterification of dimethyl carbonate and diethyl carbonate to synthesize ethyl methyl carbonate. Background technique [0002] Ethyl Methyl Carbonate (EMC) is a widely used asymmetric carbonate compound, mainly used as a solvent and an intermediate in organic synthesis. It is particularly pointed out that in recent years it has been found that EMC is used as a solvent for lithium-ion battery electrolytes, which can significantly improve the ion conductivity of lithium-ion conduction, improve the energy density and discharge capacity of the battery, improve safety performance and prolong service life, and have Good low temperature performance, etc. However, lithium-ion battery electrolytes have high requirements on purity, and impurities often have a significant impact on electrochemical performance (Industry Fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/06C07C69/96
CPCY02P20/584C07C68/06C07C69/96
Inventor 李学兵李有国李宁郭鹏宋亮
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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