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Process for preparing methyl ethyl carbonate by ester exchanging reaction

A technology of ethyl methyl carbonate and transesterification reaction, which is applied in the field of preparation of ethyl methyl carbonate by transesterification reaction, and can solve the problem of high energy consumption in the evaporation process

Inactive Publication Date: 2007-01-24
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

Its advantage is that after the reaction is over, the unreacted raw materials and products are evaporated, and the catalyst left in the reactor can still be used; the disadvantage is that the yield of ethyl methyl carbonate is less than 50%, and the evaporation process consumes a lot of energy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Embodiment 1: impregnation method is prepared in binary composite solid base catalyst

[0011] Take 3 grams of potassium carbonate and 2 grams of zinc nitrate, dissolve them in 100ml of deionized water, add 20 grams of 80-100 mesh alumina powder after dissolving, stir, stand still, repeat several times, and put the suspension in an oven after 12 hours , and dry at 70°C. Then transfer to a muffle furnace and bake at 500° C. for 5 hours. got K 2 21.5 grams of solid base catalyst with 5.9% O content and 3.1% ZnO content.

Embodiment 2

[0012] Embodiment 2: Sol-gel method is prepared in binary composite solid base catalyst

[0013] Take 4.2 grams of calcium nitrate, 1.1 grams of copper nitrate, and 47 grams of aluminum nitrate, dissolve them in 200 ml of deionized water, then add 0.5% ammonia water dropwise, until the pH value is 8, white flocculent precipitates are formed, stir for 30 minutes, and set at room temperature Under aging for 16 hours. Filter, wash and dry, transfer to a muffle furnace, and bake at 500°C for 5 hours. Obtained 21.8 grams of solid base catalysts with a CaO content of 6.2% and a CuO content of 2.1%.

Embodiment 3

[0015] In a three-necked flask equipped with a rectifying column, add 90 grams of dimethyl carbonate, 14 grams of ethanol, and 3.5 grams of the catalyst prepared in Example 1, place in a constant temperature bath, heat to 80° C., and react under normal pressure for 8 hours. After chromatographic analysis, the reaction solution contained 40.8 grams of dimethyl carbonate and 29.8 grams of ethyl methyl carbonate. The yield of ethyl methyl carbonate was 94.3%.

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Abstract

The transesterification process for preparing methyl ethyl carbonate features that the materials dimehtyl carbonate and ethanol in the molar ratio of 1-4 to 1 produce transesterification reaction at normal pressure and 50-110 deg.c in the presence of binary heterogeneous solid alkali catalyst for 1-8 hr to prepare methyl ethyl carbonate. The solid alkali catalyst has consumption of 5-25 % of ethanol weight and is prepared through soaking process or sol-gel process, and used catalyst may be separated easy from the reaction product for reuse. The transesterification reaction is completed in a reaction-rectification apparatus and has methyl ethyl carbonate yield up to 90 %.

Description

technical field [0001] The invention relates to a process for preparing ethyl methyl carbonate by taking dimethyl carbonate and ethanol as raw materials and using solid base as a catalyst for transesterification. Background technique [0002] Ethyl methyl carbonate is an asymmetric carbonate, which has a wide range of uses in organic synthesis, medicine, pesticides, solvents, additives, etc. Due to the low viscosity, high dielectric constant and strong solubility of lithium salts, ethyl methyl carbonate can be used in the organic electrolyte of lithium-ion batteries to improve the energy density, discharge capacity and low-temperature performance of the battery. [0003] The synthesis methods of ethyl methyl carbonate mainly include phosgene method, oxidative carbonylation method and transesterification method. The phosgene method involves toxic and harmful substances, causing great danger to the environment and operators, and this method has been gradually eliminated. The...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/06B01J23/06B01J23/04B01J21/04B01J23/835
Inventor 胡望明蒋严军
Owner ZHEJIANG UNIV
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