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Method for preparing oxalic acid by electrochemically reducing CO2 in aromatic ester ionic liquid system

An ionic liquid and electrochemical technology, applied in the field of CO2 resource utilization, can solve the problem of low current density and other issues

Active Publication Date: 2020-10-27
郑州中科新兴产业技术研究院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention proposes a method for electrochemically reducing CO in an aromatic ester ionic liquid system 2 The method for producing oxalic acid overcomes the existing electrochemical reduction of CO 2 Oxalic acid production technology has low current density, slow oxalic acid generation rate, and the need to add auxiliary electrolytes and catalysts at the same time. For the first time, the electrochemical reduction of CO in aromatic ester ionic liquid complex systems was proposed. 2 The method for producing oxalic acid, ionic liquid can simultaneously activate and catalyze CO 2 This method can effectively increase the current density and increase the rate of oxalic acid generation

Method used

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  • Method for preparing oxalic acid by electrochemically reducing CO2 in aromatic ester ionic liquid system
  • Method for preparing oxalic acid by electrochemically reducing CO2 in aromatic ester ionic liquid system
  • Method for preparing oxalic acid by electrochemically reducing CO2 in aromatic ester ionic liquid system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] An electrochemical reduction of CO in an aromatic ester ionic liquid system 2 The method for making oxalic acid, its condition is as follows:

[0029] (1) Synthesis of 4-(methoxycarbonyl)tetraethylammonium phenolate ([TEA][4-MF-PhO])

[0030]The ionic liquid is synthesized by reacting methyl p-hydroxybenzoate and tetraethylammonium hydroxide in a molar ratio of 1:1. The synthesis temperature is 25 °C, stirring under normal pressure conditions, and the reaction time is 10 h. After the reaction, the ethanol and water were removed by rotary evaporation, the temperature was 65°C, the time was 0.5 h; the time was 75°C, the time was 2 h. Finally, it was dried in a vacuum oven at 75 °C for 24 h.

[0031] The synthesis route of [TEA][4-MF-PhO] ionic liquid is as follows:

[0032]

[0033] (2) Electrochemical reduction of CO in [TEA][4-MF-PhO] ionic liquid system 2 Oxalic acid

[0034] Take 0.8442 g [TEA][4-MF-PhO] and dissolve it in acetonitrile to make 30 mL, the solu...

Embodiment 2

[0036] An electrochemical reduction of CO in an aromatic ester ionic liquid system 2 The method for making oxalic acid, its condition is as follows:

[0037] (1) Preparation of 4-(methoxycarbonyl)tetrabutylammonium phenolate ([TBA][4-MF-PhO])

[0038] Methyl p-hydroxybenzoate and tetrabutylammonium hydroxide were synthesized by reacting at a molar ratio of 1:1. The synthesis temperature is 30° C., stirring under normal pressure conditions, and the reaction time is 11 h. After the reaction, the ethanol and water were removed by rotary evaporation, the temperature was 65°C, the time was 0.5 h; the time was 75°C, the time was 2 h. Finally, it was dried in a vacuum oven at 75 °C for 24 h.

[0039] (2) Electrochemical reduction of CO in [TBA][4-MF-PhO] ionic liquid system 2 Oxalic acid

[0040] Take 1.1809 g [TBA][4-MF-PhO] and dissolve it in acetonitrile to make 30 mL, the solution with a concentration of 0.1 mol / L is used as the catholyte, and prepare 0.1 mol / L H 2 SO 4 Th...

Embodiment 3

[0042] An electrochemical reduction of CO in an aromatic ester ionic liquid system 2 The method for making oxalic acid, its condition is as follows:

[0043] (1) Preparation of 4-(methoxycarbonyl)phenol tetraethylphosphonium ([TEP][4-MF-PhO])

[0044] Methyl p-hydroxybenzoate and tetraethylphosphorus hydroxide are synthesized by reacting in a molar ratio of 1:1. The synthesis temperature is 30 °C, stirring under normal pressure conditions, and the reaction time is 12 h. After the reaction, the ethanol and water were removed by rotary evaporation, the temperature was 65°C, the time was 0.5 h; the time was 75°C, the time was 2 h. Finally, it was dried in a vacuum oven at 75 °C for 24 h.

[0045] (2) Electrochemical reduction of CO in [TEP][4-MF-PhO] ionic liquid system 2 Oxalic acid

[0046] Take 4.476 g [TEP][4-MF-PhO] dissolved in dimethyl sulfoxide to make 30 mL, the concentration is 0.5 mol / L solution as catholyte, prepare 0.1 mol / L H 2 SO 4 The dilute solution is use...

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Abstract

The invention provides a method for electrochemically reducing CO in an aromatic ester ionic liquid system 2 The method for producing oxalic acid is the aromatic ester ionic liquid synthesized with methyl p-hydroxybenzoate and tetraethylammonium hydroxide, tetrabutylammonium hydroxide, tetraethylphosphorus hydroxide and tetradecyltrihexylphosphorus hydroxide respectively as Electrolyte and catalyst, Pb as working electrode, Pt as counter electrode, Ag / Ag + As a reference electrode, the electrochemical reduction of CO is carried out in an H-type electrolytic cell 2 Oxalic acid. This method has the advantages of high current density and fast oxalic acid generation rate.

Description

technical field [0001] The present invention relates to CO 2 The technical field of resource utilization, specifically relates to a method for electrochemically reducing CO in an aromatic ester ionic liquid system 2 The method of making oxalic acid. Background technique [0002] In recent years, carbon dioxide (CO 2 ) As the main greenhouse gas, its emission and concentration are increasing with the massive combustion of fossil fuels, which has a huge impact on the climate and the environment. CO 2 Emission reduction has attracted widespread international attention. In addition, CO 2 It is also considered to be a natural, abundant, renewable and cheap carbon source. Therefore, for CO 2 for capture and conversion, especially CO 2 Reduction conversion into CO, formic acid, methanol and other fuels and other high value-added chemicals is a hot spot of international research. Currently CO 2 Reduction methods mainly include thermal reduction, photocatalytic reduction, el...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/04C25B3/25
CPCC25B3/25
Inventor 张香平杨英梁高红帅聂毅白银鸽袁磊胡延杰贾永高
Owner 郑州中科新兴产业技术研究院
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