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A kind of method that magnesium-aluminum-lanthanum composite oxide catalyzes synthetic ethyl methyl carbonate

A technology of ethyl methyl carbonate and composite oxides, applied in chemical instruments and methods, organic carbonate preparation, physical/chemical process catalysts, etc., can solve problems such as difficult large-scale application, complicated preparation process, and high price, and achieve Easy separation, good selectivity and low cost

Active Publication Date: 2019-11-08
SHAOYANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although MgO / NC-2 and magnesium aluminate spinel used in the prior art can promote the reaction to reach an equilibrium state in a short period of time, their preparation process is complicated and expensive, making it difficult to achieve large-scale application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Catalyst preparation: 0.3 mol magnesium chloride, 0.12 mol aluminum chloride and 0.03 mol lanthanum chloride were prepared into 300 mL of aqueous solution A; 0.75 mol of sodium hydroxide and 0.23 mol of sodium carbonate were prepared into 300 mL of aqueous solution B; at a constant temperature of 40 Under the condition of constant stirring, add solution A and solution B into 100 mL water at the same speed, keep the pH of the mixed solution = 9-11, react for 0.5 h, crystallize at 90 °C for 15 h; filter, wash and dry , after pulverization, the magnesium aluminum lanthanum hydrotalcite Mg 2 + 2 / 3 Al 3+ 4 / 15 La 3+ 1 / 15 (OH) 2 (CO 3 2- ) 1 / 6 4H 2 O; The resulting magnesium-aluminum-lanthanum hydrotalcites were calcined at 400°C for 6 h to obtain magnesium-aluminum-lanthanum composite oxides.

Embodiment 2

[0022] Catalyst preparation: 0.4 mol magnesium nitrate, 0.05 mol aluminum nitrate and 0.05 mol lanthanum nitrate were prepared into 800 mL aqueous solution A; 0.9 mol sodium hydroxide and 0.12 mol sodium carbonate were prepared into 800 mL aqueous solution B; And under the condition of continuous stirring, add solution A and solution B into 100mL water at the same speed, keep the mixed solution pH=9~11, react for 2 hours, and crystallize at 120°C for 8 hours; after filtering, washing, drying and crushing , to obtain magnesium aluminum lanthanum hydrotalcite Mg 2+ 0.8 Al 3 + 0.1 La 3+ 0.1 (OH) 2 (CO 3 2- ) 0.1 ·8H 2 O; The resulting hydrocalumite was calcined at 500°C for 4 h to obtain the magnesium-aluminum-lanthanum composite oxide.

Embodiment 3

[0024] Catalyst preparation: Prepare 200 mL of aqueous solution A with 0.2 mol of magnesium sulfate, 0.18 mol of aluminum sulfate and 0.02 mol of lanthanum sulfate; prepare 200 mL of aqueous solution B with 0.56 mol of sodium hydroxide and 0.18 mol of sodium carbonate; Under the condition of continuous stirring, add solution A and solution B into 100 mL water at the same speed, keep the pH of the mixed solution at 9~11, react for 2 h, and crystallize at 150°C for 4 h; filter, wash, dry, After pulverization, magnesium aluminum lanthanum hydrotalcite Mg is obtained 2+ 0.5 Al 3+ 0.45 La 3+ 0.05 (OH) 2 (CO 3 2- ) 0.252H 2 O; The resulting hydrocalumite was calcined at 600°C for 2 h to obtain the magnesium-aluminum-lanthanum composite oxide.

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Abstract

The invention relates to a method for synthesizing ethyl methyl carbonate under the catalysis of magnesium-aluminum-lanthanum composite oxide. The method comprises the following steps: adopting dimethyl carbonate and diethyl carbonate as raw materials to be synthesized into ethyl methyl carbonate under the catalytic effect of the magnesium-aluminum-lanthanum composite oxide. The method is characterized in that the magnesium-aluminum-lanthanum composite oxide is a product obtained by roasting magnesium-aluminum-lanthanum hydrotalcite for 2 to 8 hours at 400 to 600 DEG C, wherein a structural general formula of the magnesium-aluminum-lanthanum hydrotalcite is as follows: Mg2+1-x-yAl3+xLa3+y(OH)2(CO32-)(x+y) / 2.mH2O, wherein (x+y) is greater than or equal to 0.2 and less than or equal to 0.5, x / y is greater than or equal to 1 and less than or equal to 9, m is a number of crystal water, and m is greater than or equal to 1 and less than or equal to 8. The method provided by the invention has the following advantages that: the catalyst preparation process is simple, the production cost is low, the yield of products is high, the catalyst is easy to separate, and the repeatability is good.

Description

technical field [0001] The invention relates to a method for catalytically synthesizing ethyl methyl carbonate, in particular to a method for catalytically synthesizing ethyl methyl carbonate with a magnesium-aluminum-lanthanum composite oxide. Background technique [0002] Ethyl methyl carbonate is an environmentally friendly asymmetric organic carbonate, which is mainly used as an organic synthesis intermediate and solvent, especially as a solvent for electrolytes in lithium-ion batteries. Compared with traditional lithium-ion battery electrolyte solvents, the advantages of ethyl methyl carbonate are that it can increase the energy density and discharge capacity of the battery, improve safety performance, prolong service life, and have good low-temperature performance. [0003] According to the different raw materials used, the synthetic route of EMC mainly contains the following three: (1), methyl chloroformate and ethanol transesterification method; (2), dimethyl carbona...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C68/06C07C69/96B01J27/236
CPCB01J27/236C07C68/06C07C69/96
Inventor 周喜张超
Owner SHAOYANG UNIV
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