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Method for synthesizing methyl ethyl carbonate

A technology of ethyl methyl carbonate and synthesis method, applied in the direction of organic carbonate preparation, chemical instruments and methods, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of low catalyst activity, low activity and difficult reaction To achieve the effect of high activity, short reaction time and easy separation

Active Publication Date: 2010-10-20
QIQIHAR UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction uses a heterogeneous catalyst, and there is no subsequent separation process of the product. The organic base catalyst has a certain activity, but the activity is much lower than that of the inorganic base. Therefore, the inorganic base is still the first choice for its high activity and low cost. Disadvantages It is difficult to carry out the reaction, and the catalytic activity of the reported catalysts is generally low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add NaOH (5.15g) in there-necked flask, NaOH 2 CO 3 (4.7g), H 2 O 100ml, Mg(NO 3 ) 2 ·6H 2 O(5.5g), Al(NO 3 ) 2 9H 2 O (8.3g) was formulated into a mixed solution, which was dropped into a three-necked flask within 2 hours at room temperature, stirred at 50°C for 24 hours, and the pH value was measured to be 9, and then the resulting colloidal precipitate was crystallized, filtered, and washed with water until it was free. For sodium ions, dry the filter cake at 120°C for 12 hours to remove the adsorbed water; roast it at 900°C for 4 hours, and cool to room temperature to form solid particles that are hydrotalcite-like solid catalysts.

[0015] The obtained solid hydrotalcite is pulverized and sieved, and 10 meshes are selected as the catalyst, and the batch tank is used as the reactor, and the amount of the catalyst used is 0.5% of the mass of the substance with the least amount in the reactant. At a reaction temperature of 130°C, the reaction The reaction is c...

Embodiment 2

[0017] Add NaOH (5.15g) in there-necked flask, NaOH 2 CO 3 (4.7g), H 2 O 100ml, Mg(NO 3 ) 2 ·6H 2 O(5.5g), Al(NO 3 ) 2 9H 2 O (8.3g) was formulated into a mixed solution, which was dropped into a three-necked flask within 2 hours at room temperature, stirred at 50°C for 24 hours, and the pH value was measured to be 9, and then the resulting colloidal precipitate was crystallized, filtered, and washed with water until it was free. For sodium ions, dry the filter cake at 120°C for 12 hours to remove the adsorbed water; roast it at 900°C for 4 hours, and cool to room temperature to form solid particles that are hydrotalcite-like solid catalysts.

[0018] The obtained solid hydrotalcite is pulverized and sieved, and 20 mesh is selected as the catalyst, and the batch tank is used as the reactor. The amount of the catalyst used is 3% of the mass of the substance with the least amount in the reactant. At a reaction temperature of 130°C, the reaction The reaction is carried ou...

Embodiment 3

[0020] Add NaOH (5.15g) in there-necked flask, NaOH 2 CO 3 (4.7g), H 2 O 100ml, Mg(NO 3 ) 2 ·6H 2 O(5.5g), Zn(NO 3 ) 2 ·6H 2 O(6.4g), Al(NO 3 ) 2 9H 2 O (8.1g) was formulated into a mixed solution, which was dropped into a three-necked flask within 2 hours at room temperature, stirred at 50°C for 24 hours, and the pH value was measured to be 9, and then the resulting colloidal precipitate was crystallized, filtered, and washed with water until it was free. For sodium ions, dry the filter cake at 120°C for 12 hours to remove the adsorbed water; roast it at 900°C for 4 hours, and cool to room temperature to form solid particles that are hydrotalcite-like solid catalysts.

[0021] The obtained solid hydrotalcite is pulverized and sieved, and 10 meshes are selected as the catalyst, and the batch tank is used as the reactor, and the amount of the catalyst used is 3% of the mass of the substance with the least amount in the reactant. At a reaction temperature of 130°C, the...

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PUM

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Abstract

The invention discloses a preparation method of hydrotalcite-like solid catalyst for synthesizing methyl ethyl carbonate. The invention relates to a preparation method for hydrotalcite-like solid catalyst, which solves the problem that the low activity in present solid base catalyst result in low yield in methyl ethyl carbonate. In the method, dimethyl carbonate and diethyl carbonate are used as raw materials, a batch kettle is used as a reactor, and a catalyst used is a hydrotalcite-like solid catalyst. The preparation method of the catalyst comprises: preparing nitrate mixed solution of copper, zinc, magnesium and aluminum respectively and preparing mixed solution of NaOH and a carbonate or bicarbonate; mixing the two kinds of solution together by dripping and stirring the mixed solution; performing crystallization, filtration, distillation and washing; drying filter cakes; roasting the filter cakes; and cooling the filter cakes. The catalyst has high activity, is easy to separate, can be recycled, and is long in service life and free from pollution; the reaction time is short; and the cost is low. The catalyst is used in the batch reaction kettle for catalyzing the reaction of the dimethyl carbonate and the diethyl carbonate to synthesize the methyl ethyl carbonate; the raw materials and product of the reaction can be used as electrolyte solvents for lithium ion batteries and can be used directly by controlling water content without separation; and a large part of separation and purification cost can be reduced.

Description

technical field [0001] The present invention relates to a kind of synthetic method of ethyl methyl carbonate. Background technique [0002] Ethyl methyl carbonate electrolyte can prolong battery life and improve safety performance, so it has irreplaceable advantages in lithium-ion battery electrolyte. With the rapid development of lithium-ion batteries, the demand for ethyl methyl carbonate is also increasing. Since the quality of domestically synthesized electrolyte solvents cannot meet the standards for use, electrolyte solvents are generally imported from abroad. The existing main production methods of ethyl methyl carbonate include methyl chloroformate and ethanol transesterification, dimethyl carbonate and ethanol transesterification, dimethyl carbonate and diethyl carbonate transesterification and other methods. Among them, in the reaction route of dimethyl carbonate and diethyl carbonate transesterification, both raw materials and products can be used as lithium-ion...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/06B01J23/06B01J21/10
Inventor 荆涛田景芝邓启刚郑永杰任沼琦
Owner QIQIHAR UNIVERSITY
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