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Synthesis method for converting glyoxal into glyoxylic acid through photoelectrocatalytic oxidation

A technology of photoelectric catalysis and synthesis method, which is applied in the direction of electrodes, electrolysis process, electrolysis components, etc., to achieve the effects of mild reaction conditions, environmental friendliness and simple equipment

Active Publication Date: 2021-12-14
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no research report on the application of photoelectrocatalytic technology in the synthesis of glyoxylic acid by catalytic oxidation of glyoxal at home and abroad.

Method used

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  • Synthesis method for converting glyoxal into glyoxylic acid through photoelectrocatalytic oxidation
  • Synthesis method for converting glyoxal into glyoxylic acid through photoelectrocatalytic oxidation
  • Synthesis method for converting glyoxal into glyoxylic acid through photoelectrocatalytic oxidation

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Experimental program
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Effect test

Embodiment 1

[0032] Embodiment 1: Using WO with nanosheet (NPs) array structure 3 Materials as photoanodes for photocatalytic oxidation of glyoxal to glyoxylic acid

[0033] (1) Preparation of WO by hydrothermal method 3 NPs photoanode

[0034] Take FTO conductive glass (2*15*50mm) as the carrier, soak in 25mL aqueous solution containing sodium tungstate and citric acid (the molar ratio of sodium tungstate and citric acid is 19:37, the concentration of sodium tungstate is 0.018mol / L) In the solution, the pH value of the solution was adjusted to 7 with 9.5% hydrochloric acid. The hydrothermal reaction was carried out at 120°C for 12h, then filtered, washed, and fired at 450°C for 2h, and the WO with nanosheet structure array was obtained on the FTO conductive glass substrate. 3 Photoanode (denoted as FTO / WO 3 NPs).

[0035] figure 1 (a), (b) are the prepared FTO / WO 3 Scanning electron microscope image of NPs, it can be seen that its microscopic morphology is WO with high-density verti...

Embodiment 2

[0041] Embodiment 2: Using TiO with nanorod (NBs) structure array 2 Materials as photoanodes for photocatalytic oxidation of glyoxal to glyoxylic acid

[0042] (1) Preparation of TiO by hydrothermal method 2 NBs photoanode

[0043] Using FTO conductive glass as a carrier, soak it in 24.35mL aqueous hydrochloric acid solution containing tetrabutyl titanate (the molar ratio of tetrabutyl titanate to HCl is 1:340.32, and the concentration of tetrabutyl titanate is 0.04mol / L). Perform hydrothermal reaction at 150°C for 6 hours, then filter, wash with absolute ethanol, and burn in air at 450°C for 3 hours to obtain TiO on the FTO conductive glass substrate 2 NBs photoanode (denoted as FTO / TiO 2 NBs).

[0044] Figure 5 For the prepared FTO / TiO 2 Scanning electron microscope image of NBs, it can be seen that its microscopic morphology is vertical nanorod TiO on FTO substrate 2 Arrange evenly.

[0045] (2) with TiO 2 NBs material as photoanode for photocatalytic oxidation of...

Embodiment 3

[0048] Embodiment 3: Using BiVO with nanosheet structure 4 Materials as photoanodes for photocatalytic oxidation of glyoxal to glyoxylic acid

[0049] (1) Preparation of BiVO by precipitation method 4 Photoanode:

[0050] Take FTO conductive glass as the carrier, soak in 70mL ethanol aqueous solution containing potassium iodide, bismuth nitrate pentahydrate and p-benzoquinone (the volume ratio of ethanol: water is 2:5, the concentration ratio of potassium iodide, bismuth nitrate pentahydrate and p-benzoquinone is 4: 4:23, potassium iodide concentration 0.04mol / L), apply a voltage of -0.1V vs Ag / AgCl, take it out after 5 minutes of electrodeposition, rinse and dry; The concentration ratio of vanadyl acetonate and dimethyl sulfoxide is 1:35, the concentration of vanadyl acetylacetonate is 0.4mol / L) dropwise on the surface of the material, and then burnt by air at 450°C for 2h, stirred and soaked in 1mol / L NaOH solution for 0.5h, washed , after drying, BiVO was obtained on the...

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Abstract

The invention discloses a synthesis method for converting glyoxal into glyoxylic acid through photoelectrocatalytic oxidation. According to the method, a cathode and anode electrolytic bath is adopted, a cathode and an anode are separated by a cationic membrane, a WO3, TiO2 or BiVO4 semiconductor material is used as the anode, a graphite carbon material is used as the cathode, and under the conditions of optical radiation and bias voltage application, photoelectrocatalytic oxidation is carried out on an inorganic acid solution containing glyoxal to finally synthesize glyoxylic acid. The WO3, TiO2 or BiVO4 semiconductor material is used as the photo-anode, so that the use of noble metals and harmful materials is avoided, the reaction condition is mild, the process is simple and easy to control, and the cost is low; and the method has excellent glyoxal catalytic oxidation performance, the highest glyoxylic acid yield reaches 239 mmol / m<2>. H, the selectivity reaches 95%, and compared with a chemical oxidation method and an electrochemical oxidation method, the method is environmentally friendly and has wide application prospects.

Description

technical field [0001] The invention relates to a method for synthesizing glyoxylic acid, in particular to a method for oxidizing glyoxal into glyoxylic acid by photoelectric catalysis using semiconductor photoanode materials. Background technique [0002] Glyoxylic acid, also known as formaldehyde formic acid or diglycolic acid, is the simplest aldehyde acid in organic matter. It has the properties of both aldehyde and carboxylic acid, and its chemical properties are lively. Glyoxylic acid is the starting material for the synthesis of many high value-added fine chemicals, and is widely used in the synthesis of perfume and cosmetic industrial products. [0003] Currently, the methods for synthesizing glyoxylic acid mainly use chemical oxidation and electrochemical oxidation. The chemical oxidation method usually needs to be carried out under high temperature and high pressure conditions, and the reaction time is long; at the same time, high-concentration sulfuric acid, nitr...

Claims

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Application Information

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IPC IPC(8): C25B3/21C25B3/23C25B3/07C25B11/049C25B11/047
CPCC25B3/21C25B3/23C25B3/07C25B11/049C25B11/047
Inventor 赵浙菲石红梅郑华均
Owner ZHEJIANG UNIV OF TECH
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