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Method for preparing methyl ethyl carbonate

A technology of ethyl methyl carbonate and dimethyl carbonate, applied in the field of preparation of ethyl methyl carbonate, can solve problems such as many side reactions and low yields

Inactive Publication Date: 2008-10-22
BYD CO LTD
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  • Abstract
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  • Application Information

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Problems solved by technology

[0003] Patent CN1597113A discloses a method for preparing ethyl methyl carbonate by transesterification reaction of dimethyl carbonate and ethanol in the presence of a catalyst. The product has more side reactions and lower yield

Method used

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  • Method for preparing methyl ethyl carbonate

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preparation example Construction

[0021] Preparation of absolute ethanol

[0022] Add 200 grams of 5A molecular sieves to 1000 ml of commercially available ethanol (Guangzhou Chemical Reagent Factory, analytically pure); after sealing and standing for 24 hours, take the supernatant to obtain absolute ethanol. Tested by Swiss Metrohm KF831 moisture tester, the moisture content of the absolute ethanol is 0.02%.

Embodiment 1

[0024] In a 500ml round-bottomed three-necked bottle, add 270 grams (3.0 moles) of dimethyl carbonate, 69 grams (1.5 moles) of absolute ethanol after dehydration treatment, 10 grams (0.25 moles) of catalyst sodium hydroxide, and put In the water bath, heat while stirring, control the temperature rise rate to 5°C / hour, when the reaction temperature rises to 50°C, stop the temperature rise, maintain this temperature, and react for about 2 hours. After the reaction, stop stirring, and cool the reaction solution to 25°C, release the product in the kettle, filter, take the filtrate for atmospheric distillation, collect and separate the solvent dimethyl carbonate in sections, collect 108-110°C fractions, and obtain 122.0g Colorless liquid, product yield 78.2%, carry out gas chromatography-mass spectrometry (GC-MS) to product and carry out qualitative analysis, then carry out quantitative analysis with gas chromatography (GC), record product purity and be 99.9% methyl carbonate Ethyl...

Embodiment 2

[0026] In a 500ml round-bottomed three-necked bottle, add 360 grams (4.0 moles) of dimethyl carbonate, 46 grams (1.0 moles) of dehydrated ethanol after dehydration treatment, and 8 grams (0.2 moles) of catalyst sodium hydroxide, and put into a constant temperature In the water bath, start stirring. Then heat, the temperature of the reaction mixture is raised, and the temperature rise rate is controlled at 7°C / hour. When the reaction temperature rises to 55°C, the temperature rise is stopped and the temperature is maintained for about 3 hours. After the reaction is over, stop stirring and cool to 25°C, release the product in the kettle, filter, take the filtrate and carry out atmospheric distillation, collect and separate the solvent dimethyl carbonate in sections, and then collect 108~110°C fractions to obtain 83.5g colorless liquid Product yield 80.3%, ethyl methyl carbonate purity testing method is the same as embodiment 1.

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Abstract

The invention relates to a preparation method of methyl ethyl carbonate, which takes methyl carbonate and ethanol as raw material and carries on transesterification with the existence of the catalyst with the reaction temperature of 50 DEG C to 60 DEG C. The temperature of the reaction materials rises from room temperature with a heating rate of five to ten DEG C per hour. The method also includes a water removing treatment to the ethanol so that the water content of the ethanol is less than or equal to 0.1 percent of the gross weight of the ethanol. By adopting the preparation method of the invention, the purity of the methyl ethyl carbonate is as high as 99.8 percent and the yield is higher than 70 percent. The method has the advantages of mild reaction condition, simple separation and purification of reaction products and low cost.

Description

technical field [0001] The invention relates to a preparation method of ethyl methyl carbonate, in particular to a method for preparing ethyl methyl carbonate by transesterification reaction of dimethyl carbonate and ethanol in the presence of a catalyst. Background technique [0002] Ethyl methyl carbonate (EMC for short) is a colorless transparent liquid with a melting point of -55°C and a boiling point of 108-109°C. Ethyl methyl carbonate (EMC) is a high value-added fine chemical product that has emerged in recent years and can be used as a solvent for lithium-ion battery electrolytes. At the same time, ethyl methyl carbonate has both methyl and ethyl groups, and has the characteristics of dimethyl carbonate and diethyl carbonate. It is also a solvent for special spices and pharmaceutical intermediates, and has broad application prospects. [0003] Patent CN1597113A discloses a method for preparing ethyl methyl carbonate by transesterification of dimethyl carbonate and e...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/06
Inventor 周刚周天承
Owner BYD CO LTD
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