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Method for preparing methyl ethyl carbonate

A technology for ethyl methyl carbonate and dimethyl carbonate, applied in the field of preparing ethyl methyl carbonate, can solve the problems of difficulty in meeting raw material requirements, relatively high raw material requirements, and unsatisfactory yields, and achieves no environmental pollution and preparation costs. Low, high yield effect

Inactive Publication Date: 2003-02-05
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] Japanese patent JP10237026 uses titanium oxide as the active component, reacts at 50°C-200°C, pressure 0-10kg / cm 2 under, but in most cases the yield is not ideal
[0011] Japanese patent JP2000281630 uses oxides such as lanthanum, actinium, scandium, and yttrium as the active components of the catalyst. The catalyst is not easy to deactivate, but the requirements for raw materials are relatively high. It is required that the total content of salt in the raw material is less than 10ppm, and the content of inorganic salts is 1ppm. Below, such raw material requirements are difficult to meet

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Measure GaCl 3 Solution (0.64mol / L) 20.7mL, add 8g 60-80 mesh Al 2 o 3 , add ammonia water dropwise until the pH of the solution is 10, stir for 2 hours, dry at 110°C, and then burn at 550°C for 5 hours to obtain Ga 2 o 3 Content (weight) of 13.4% Ga 2 o 3 / Al 2 o 3 .

Embodiment 2

[0022] In the 100mL round bottom flask, add dimethyl carbonate 21.6g, the catalyst Ga prepared by diethyl carbonate 28.3g and embodiment 1 method 2 o 3 / Al 2 o 3 3.2g (Ga 2 o 3 Accounting for 0.9% of the total amount of reaction raw materials), reacted at 100 ° C, the flask was connected with a reflux condenser, and the reaction was carried out under normal pressure. After reacting for 8 hours, the reaction solution was analyzed by gas chromatography, containing: dimethyl carbonate 13.3g , 17.4 g of diethyl carbonate, 19.1 g of ethyl methyl carbonate. The yield of ethyl methyl carbonate was 38.2%.

Embodiment 3

[0024] Experimental apparatus is the same as embodiment 2, and reactant dimethyl carbonate and diethyl carbonate add-on are the same as embodiment 2, add 4.6g catalyst MoO 3 / Al 2 o 3 (MoO 3 The content in the catalyst is 15%, accounting for 1.4% of the total amount of reaction raw materials), the reaction is carried out under normal pressure, the reaction temperature is 104 ° C, after 10 hours of reaction, the reaction solution is analyzed by gas chromatography, containing: dimethyl carbonate 12.1g, 15.8g of diethyl carbonate, 21.7g of ethyl methyl carbonate. The yield of ethyl methyl carbonate was 43.6%.

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Abstract

The preparation method of methylethyl carbonate uses dimethyl carbonate and diethyl carbonate as raw material, in the presence of catalyst makes them implement ester exchange reaction, and is characterized by that the dosage (mass) ratio of raw material dimethyl carbonate and diethyl carbonate is 1:2-2:1, its catalyst is load type metal oxide loaded on alumina, its metal oxide content (wt%) is 2%-30%, and the rest is Al2O3. In the ester exchange reaction the addition quantity of metal oxide is 0.1%-10% of total quantity of raw material, its reaction temp. is 50-200 deg.C, reaction pressure is normal pressure and its reaction time is 2-48 hr.

Description

technical field [0001] The present invention relates to the method for preparing ethyl methyl carbonate. Background technique [0002] Ethyl methyl carbonate is a versatile organic compound that can be used as a solvent and an intermediate in organic synthesis. It is widely used as a solvent for non-water-soluble electrolytes in lithium batteries, which can improve the discharge performance of batteries, such as: increase the energy density of batteries And discharge capacity, improve safety performance and increase service life, etc. [0003] There are three main synthetic routes of ethyl methyl carbonate: [0004] The first synthetic route is to take methyl chloroformate and ethanol as raw materials, in the presence of alkali (pyridine and organic amine), carry out transesterification, as shown in reaction formula (1): <chemistry num="001"> <chem file="02136322_cml001.xml" / > < / chemistry> [0005] The literature of this synthet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/08C07C69/96
Inventor 沈振陆赵卫娟卓广澜姜玄珍
Owner ZHEJIANG UNIV
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