Method for synthesizing ethyl methyl carbonate through ester exchange

A technology for methyl ethyl carbonate and dimethyl carbonate, which is applied in the field of transesterification synthesis of methyl ethyl carbonate, can solve the problems of complex preparation process of heterogeneous catalyst, difficult catalyst recycling, easy precipitation and scaling, etc., and achieves low cost catalyst. , easy to control, good stability

Active Publication Date: 2014-01-01
HEBEI UNIV OF TECH
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  • Abstract
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  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve problems such as poor solubility, easy precipitation and fouling, blockage of pipelines, etc. in homogeneous catalysts such as alkoxides in the current technology, as well as difficulties in recycling and utilization of catalysts, etc., and the preparation process of heterogeneous catalysts is relatively complicated. Insufficient, provide a kind of method that raw material is easy to get, technique is simple, cost is low, catalyst is easy to recycle synthetic ethyl methyl carbonate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Load 6.0g of K-ZSM-5 molecular sieve catalyst into the fixed bed reactor (the catalyst is obtained by exchanging twice the concentration of 1g molecular sieve per 10mL solution with 0.1mol / L KCl), and raise the temperature to 180°C under nitrogen Purge for 2 hours, then lower the temperature to 130°C as the reaction temperature, pump dimethyl carbonate and ethanol into the reactor at a molar ratio of 1:2, and the space velocity is 8h -1 , Reaction under normal pressure, samples were collected at feed 30min, 1h, 2h, 4h, 8h respectively, after chromatographic analysis, the conversion rate of dimethyl carbonate was 33.2%, and the selectivity of ethyl methyl carbonate was 91.8%.

Embodiment 2

[0021] Fill 6.0g of the molecular sieve catalyst of Example 1 into a fixed-bed reactor, raise the temperature to 180°C for nitrogen purging for 2 hours, then cool down to 130°C, and mix dimethyl carbonate and ethanol at a molar ratio of 1:2 Pump into the reactor with a space velocity of 4h -1 , reacted under normal pressure, collected samples at 30min, 1h, 2h, 4h, and 8h of feeding, and analyzed by chromatography, the conversion rate of dimethyl carbonate was 62.5%, and the selectivity of ethyl methyl carbonate was 90.6%.

Embodiment 3

[0023] Fill 6.0g of the molecular sieve catalyst of Example 1 into a fixed-bed reactor, raise the temperature to 180°C for nitrogen purging for 2 hours, then cool down to 130°C, and mix dimethyl carbonate and ethanol at a molar ratio of 2:1 Pump into the reactor with a space velocity of 4h -1 , Reaction under normal pressure, samples were collected at feed 30min, 1h, 2h, 4h, 8h respectively, after chromatographic analysis, the conversion rate of dimethyl carbonate was 44.8%, and the selectivity of ethyl methyl carbonate was 93.6%.

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Abstract

The invention relates to a method for synthesizing ethyl methyl carbonate through ester exchange. The method comprises the following steps: filling a fixed bed reactor with catalysts, pumping dimethyl carbonate and ethyl alcohol into the fixed bed reactor according to the molar ratio of 0.5-2:1 after nitrogen purging is carried out, reacting at the air speed of 0.5-15h-1, the temperature of 100-240DEG C and the reaction operation pressure of 0-1MPa, and finally the ethyl methyl carbonate is obtained. The catalysts are modified molecular sieve based catalysts. The method is simple in technology condition, easy to control, capable of achieving continuous production due to the gas-solid phase reaction and low in cost of the adopted catalysts. The selectivity of the ethyl methyl carbonate can be higher than 90%, and the yield can be higher than 55%.

Description

technical field [0001] The invention relates to a method for synthesizing ethyl methyl carbonate by using dimethyl carbonate and ethanol as raw materials and using modified molecular sieves as catalysts for transesterification. Background technique [0002] Ethyl methyl carbonate is a widely used asymmetric organic carbonate, which contains active reactive groups such as methyl, ethyl and carbonyl, and is widely used as a fine synthesis intermediate and solvent. Because of its strong solubility to lithium salt, safety and stability, it can not only improve the energy density and discharge capacity of the battery, but also has the characteristics of long cycle life, good safety performance, no memory effect, and good low-temperature performance. It has been widely used in mobile phones Among the batteries used in high-end electrical appliances such as portable audio-visual equipment and notebook computers, this is currently the most promising small secondary battery. [0003...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/96C07C68/06
CPCC07C68/06C07C69/96
Inventor 王延吉贾爱忠赵新强李芳
Owner HEBEI UNIV OF TECH
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