A kind of method that calcium magnesium aluminum composite oxide catalyzes synthesizing ethyl methyl carbonate

A technology of ethyl methyl carbonate and diethyl carbonate, applied in the field of calcium-magnesium-aluminum composite oxide catalytic synthesis of ethyl methyl carbonate, can solve the problems of complex preparation process, high price, difficulty in large-scale application, etc., and achieve good selectivity , low cost, easy to separate effect

Active Publication Date: 2019-10-11
SHAOYANG UNIV
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  • 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: 0.15 mol calcium chloride, 0.15 mol magnesium chloride and 0.15 mol aluminum 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; 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 at 9~11, react for 0.5h, crystallize at 90°C for 15h; filter, wash, dry, After pulverization, calcium magnesium aluminum hydrotalcite Ca 2+ 1 / 3 Mg 2 + 1 / 3 Al 3+ 1 / 3 (OH) 2 (CO 3 2- ) 1 / 6 4H 2 O; Calcium-magnesium-aluminum hydrotalcite obtained by roasting at 400°C for 6 hours to obtain calcium-magnesium-aluminum composite oxide.

Embodiment 2

[0022] Catalyst preparation: Prepare 800 mL of aqueous solution A with 0.08 mol of calcium nitrate, 0.32 mol of magnesium nitrate and 0.1 mol of aluminum nitrate; prepare 800 mL of aqueous solution B with 0.9 mol of sodium hydroxide and 0.12 mol of sodium carbonate; And under the condition of continuous stirring, add solution A and solution B into 100mL water at the same speed, keep the pH of the mixed solution=9~11, react for 2h, and crystallize at 120°C for 8h; after filtering, washing, drying and crushing, Calcium magnesium aluminum hydrotalcite Ca 2+ 0.16 Mg 2+ 0.64 Al 3+ 0.2 (OH) 2 (CO 3 2- ) 0.1 ·8H 2 O; The resulting hydrocalumite was roasted at 500°C for 4 hours to obtain calcium-magnesium-aluminum composite oxides.

Embodiment 3

[0024] Catalyst preparation: 0.16 mol calcium sulfate, 0.04 mol magnesium sulfate and 0.2 mol aluminum sulfate were prepared into 200 mL of aqueous solution A; 0.56 mol of sodium hydroxide and 0.18 mol of sodium carbonate were prepared into 200 mL of aqueous solution B; And under the condition of continuous stirring, add solution A and solution B into 100 mL water at the same speed, keep the mixed solution pH=9~11, react for 2 hours, and crystallize at 150°C for 4 hours; after filtering, washing, drying and crushing , to obtain calcium magnesium aluminum hydrotalcite Ca 2+ 0.4 Mg 2 + 0.1 Al 3+ 0.5 (OH) 2 (CO 3 2- ) 0.25 2H 2 O; The resulting hydrocalumite was roasted at 600°C for 2 hours to obtain calcium-magnesium-aluminum composite oxides.

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Abstract

The invention relates to a method of catalytically synthesizing ethyl methyl carbonate by a calcium magnesium and aluminum composite oxide. The ethyl methyl carbonate is synthesized under a catalytic action of the calcium magnesium and aluminum composite oxide by taking dimethyl carbonate and diethyl carbonate as raw materials. The method is characterized in that the calcium magnesium and aluminum composite oxide is a product obtained by roasting calcium magnesium and aluminum hydrotalcite for 2-8 hours at 400-600 DEG C; the structural formula of the calcium magnesium and aluminum hydrotalcite is Ca<2+>xMg<2+>yAl<3+>1-x-y(OH)2(CO3<2->)(1-x-y) / 2.mH2O, wherein (x+y) is greater than or equal to 0.5 but less than or equal to 0.8; x / y is greater than or equal to 0.25 but less than or equal to 4; m which is the number of crystal water is greater than or equal to 1 but less than or equal to 8. The method provided by the invention has the advantages that the catalyst is simple in preparation process and low in cost, the product is high in yield, and the catalyst is easy to separate and has a good performance for repeated use.

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 calcium-magnesium-aluminum 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 carbonate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C68/06C07C69/96B01J23/02
Inventor 周喜张超
Owner SHAOYANG UNIV
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