Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for preparing oxalic acid through CO2 electrochemical reductionf in aromatic ester type 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 achieve the effects of increasing current density, increasing the rate of oxalic acid generation, and enhancing mass transfer.

Active Publication Date: 2019-09-24
郑州中科新兴产业技术研究院 +1
View PDF4 Cites 1 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing oxalic acid through CO2 electrochemical reductionf in aromatic ester type ionic liquid system
  • Method for preparing oxalic acid through CO2 electrochemical reductionf in aromatic ester type ionic liquid system
  • Method for preparing oxalic acid through CO2 electrochemical reductionf in aromatic ester type 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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a method for preparing oxalic acid through CO2 electrochemical reduction in an aromatic ester type ionic liquid system. According to the method, aromatic ester type ionic liquids prepared from methyl parahydroxybenzoats and tetraethylammonium hydroxide, tetrabutyl ammonium hydroxide, tetraethyl phosphonium hydroxide and tetradecyl trihexyl phosphonium hydroxide through synthesis are adopted as electrolytes and catalysts, Pb is adopted as a working electrode, Pt is adopted as a counter electrode, and Ag / Ag<+> is adopted as a reference electrode, CO2 electrochemical reduction is implemented in an H-shaped electrolytic tank, and thus oxalic acid is prepared. The method has the advantages of being large in current density, rapid in oxalic acid generation velocity, and the like.

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(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