CN114517308A - Bi-MOF material electrode with catalytic selectivity and preparation method thereof - Google Patents
Bi-MOF material electrode with catalytic selectivity and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an electrode material, and belongs to the field of electrochemistry. A preparation method of a Bi-MOF material electrode with catalytic selectivity comprises the steps of firstly, preparing a solution of ellagic acid and bismuth acetate; adjusting the pH value of the reaction solution to be 2-4 by using glacial acetic acid, centrifuging and purifying after the reaction is finished to obtain a Bi-MOF material, mixing the Bi-MOF material with carbon black, and coating the mixture on the surface of an electrode to obtain the Bi-MOF material electrode for preparing formic acid by carbon dioxide electrocatalysis. The Bi-MOF material prepared by the technical scheme of the invention has uniform appearance, stable structure, acid and alkali resistance (pH is more than 2 and less than or equal to 14) and high temperature resistance (decomposition temperature is as high as about 300 ℃), the prepared Bi-MOF material electrode can realize high-efficiency conversion and utilization of carbon dioxide, and the structure of the Bi-MOF material is not obviously changed after multiple electrocatalysis cycles after the reaction.
Description
Technical Field
The invention relates to processing of an electrode material, in particular to a Bi-MOF material electrode with catalytic selectivity and a preparation method thereof.
Background
The electrocatalytic carbon dioxide reduction reaction, which can convert carbon dioxide into additional-value chemicals and fuels by using renewable electric energy, is considered as a potential energy storage and conversion mode, and thus has received extensive attention of researchers. Formic acid is used as an important industrial raw material, has important application in pharmacy, leather and papermaking, and can be used as a hydrogen carrier for a direct formic acid fuel cell.
At present, CO2Although higher faradaic efficiency can be obtained by electrocatalytic reduction of formic acid, its high faradaic efficiency can usually only be achieved at lower activity, and changes in potential or current will significantly affect its faradaic efficiency, which makes it difficult to increase the rate of formic acid production of industrial concern. Currently, Bi-MOF materials are catalysts capable of converting carbon dioxide to formic acid with high economic efficiency. However, in the electrocatalytic carbon dioxide reduction process, the Bi-MOF is easy to have the problems of structural transformation and the like, and the industrial value of the method for preparing formic acid by electrocatalytic reduction of carbon dioxide by the Bi-MOF is greatly reduced.
Therefore, the development of effective methods and strategies for preparing novel Bi-MOF materials with stable structures is urgently needed to provide theoretical and technical support for reasonable design of catalysts and research on catalytic mechanisms.
Disclosure of Invention
The invention aims to solve the technical problem of providing a Bi-MOF material electrode with catalytic selectivity and a preparation method thereof, and the Bi-MOF material electrode with a stable structure is prepared, so that the aim of preparing formic acid through carbon dioxide electrocatalytic reduction is fulfilled on the premise of higher catalytic activity and catalytic selectivity.
Technical scheme
A preparation method of a Bi-MOF material electrode with catalytic selectivity comprises the following steps,
step I, preparing a solution of ellagic acid and bismuth acetate;
step II, adjusting the pH value to be 2-4 by glacial acetic acid, and centrifuging and purifying after reaction to obtain a Bi-MOF material;
and step III, mixing the Bi-MOF material with carbon black, and coating the mixture on the surface of an electrode to obtain the Bi-MOF material electrode for preparing formic acid by carbon dioxide electrocatalysis.
Further, the mass ratio of ellagic acid to bismuth acetate in step I is 1: 2 to 3.
Further, the mass concentration ratio of the ellagic acid to the bismuth acetate in the step I is 1: 2 to 3.
Further, in the step I, the reaction temperature of the ellagic acid and the bismuth acetate is 25-80 ℃, and the reaction time is 24-72 hours.
Further, the purification treatment step in step II includes vacuum or freeze drying of the centrifuged solid to finally obtain the nanorod-like microstructure.
Further, stirring should be continued during the step II reaction.
And step III, mixing the Bi-MOF material and carbon black, and coating the mixture on the surface of the electrode, wherein the step III comprises the specific steps of uniformly dispersing the Bi-MOF material and the carbon black in a mixed solution of isopropanol and naphthol, uniformly coating the mixed solution on a gas diffusion electrode, and finally drying the prepared working electrode at normal temperature and normal pressure overnight to obtain the Bi-MOF material electrode.
Further, the mass ratio of the Bi-MOF material to the carbon black in step III is 1: 0.9 to 1.1.
Further, the volume ratio of isopropanol to naphthol in the mixed solution of isopropanol and naphthol is 18-20: 1.
further, the coating concentration of the Bi-MOF material on the surface of the electrode is 0.5-1.5 mg/cm2。
Advantageous effects
The Bi-MOF material electrode prepared by the invention has the following outstanding beneficial effects:
1. according to the experimental result analysis of the embodiment, the Bi-MOF material prepared by the technical scheme provided by the invention is represented as a uniform rod-shaped nanometer material with stable appearance on a microscopic level, and the length is about 100-500 nm. After being treated by acid-base solution, the Bi-MOF material prepared by the technical scheme of the invention has strong acid and base resistance 2-14 of which the pH is less than or equal to the pH; according to the thermogravimetric spectrum, the thermal weight loss of the Bi-MOF material prepared by the technical scheme of the invention is not more than 10% below 300 ℃, and the thermal weight loss is not more than 4% below 100 ℃ under the common electrocatalytic limit temperature. Therefore, the Bi-MOF material prepared by the technical scheme of the invention has uniform appearance, stable structure, acid and alkali resistance (pH is more than 2 and less than or equal to 14) and high temperature resistance (decomposition temperature is as high as about 300 ℃), can realize high-efficiency conversion and utilization of carbon dioxide, and the structure of the Bi-MOF material is not obviously changed after reaction.
2. According to data implemented by electrocatalysis reduction, the Bi-MOF material prepared by the invention is applied to the reaction of reducing carbon dioxide by an electrode, and after a plurality of electrocatalysis circulations, the crystal structure is not obviously changed.
3. According to the embodiment of electro-catalytic reduction and experimental results, the Bi-MOF material prepared by the invention is applied to the reaction of reducing carbon dioxide by an electrode, the ratio of the formic acid product prepared by catalysis is high, the Faraday efficiency of formic acid can reach about 94 percent, and the Faraday efficiency is far higher than that of similar products in the prior art, so that the technical scheme has a high application prospect in the field of electro-catalytic reduction of carbon dioxide.
Drawings
FIG. 1 is a scanning electron micrograph of a Bi-MOF material according to the invention;
FIG. 2 is an X-ray diffraction pattern of a Bi-MOF material of the invention after being treated in solutions with different pH values;
FIG. 3 is a thermogravimetric analysis plot of a Bi-MOF material of the present invention;
FIG. 4 is a graph of the performance of the Bi-MOF material electrode of the present invention in a carbon dioxide electroreduction reaction;
FIG. 5 is an XRD pattern of the electrode of the Bi-MOF material of the invention after carbon dioxide electro-reduction reaction.
Detailed Description
The invention will be further elucidated with reference to the following specific examples and figures 1 to 5.
Example 1-1Bi-MOF material preparation:
(1) ellagic acid and bismuth acetate were dissolved in water: 0.15g of ellagic acid and 0.38g of bismuth acetate were weighed out, added to a 40mL brown glass vial, and dissolved by adding 30mL of deionized water.
(2) Adding glacial acetic acid, and controlling the pH value of the solution, the reaction temperature and the reaction time: 1mL of glacial acetic acid (pH. apprxeq.2.3) was added and stirred at room temperature for 48 h.
(3) Obtaining a target product after centrifugal separation and drying treatment: centrifuging the suspension at 8000rpm for 10 min, washing with water and ethanol for three times, centrifuging, and freeze drying to obtain target product with microscopic morphology as shown in FIGS. 1 and 2 and thermogravimetric analysis curve as shown in FIG. 3.
Example 1-2Bi-MOF material preparation:
(1) ellagic acid and bismuth acetate were dissolved in water: 0.15g of ellagic acid and 0.4g of bismuth acetate were weighed out, added to a 40mL brown glass vial, and dissolved by adding 30mL of deionized water.
(2) Adding glacial acetic acid, and controlling the pH value of the solution, the reaction temperature and the reaction time: glacial acetic acid (pH. apprxeq.2.5) was added and stirred at 45 ℃ for 48 h.
(3) Obtaining a target product after centrifugal separation and drying treatment: and centrifuging the suspension at 8000rpm for 10 minutes, washing with water and ethanol for three times, centrifuging, and freeze-drying to obtain the target product.
Examples 1-3Bi-MOF material preparation:
(1) ellagic acid and bismuth acetate were dissolved in water: 0.15g of ellagic acid and 0.42g of bismuth acetate were weighed out, added to a 40mL brown glass vial, and dissolved by adding 30mL of deionized water.
(2) Adding glacial acetic acid, and controlling the pH value of the solution, the reaction temperature and the reaction time: glacial acetic acid (pH. apprxeq.2.7) was added and stirred at 50 ℃ for 48 h.
(3) Obtaining a target product after centrifugal separation and drying treatment: and centrifuging the suspension at 8000rpm for 10 minutes, washing with water and ethanol for three times, centrifuging, and freeze-drying to obtain the target product.
Examples 1-4Bi-MOF material preparation:
(1) ellagic acid and bismuth acetate were dissolved in water: 0.15g of ellagic acid and 0.42g of bismuth acetate were weighed out, added to a 40mL brown glass vial, and dissolved by adding 30mL of deionized water.
(2) Adding glacial acetic acid, and controlling the pH value of the solution, the reaction temperature and the reaction time: glacial acetic acid (pH. apprxeq.2.9) was added and stirred at 55 ℃ for 40 h.
(3) Obtaining a target product after centrifugal separation and drying treatment: and centrifuging the suspension at 8000rpm for 10 minutes, washing with water and ethanol for three times, centrifuging, and freeze-drying to obtain the target product.
Examples 1-5Bi-MOF Material preparation:
(1) ellagic acid and bismuth acetate were dissolved in water: 0.15g of ellagic acid and 0.45g of bismuth acetate were weighed into a 40mL brown glass vial and dissolved by adding 30mL of deionized water.
(2) Adding glacial acetic acid, and controlling the pH value of the solution, the reaction temperature and the reaction time: glacial acetic acid (pH. apprxeq.3) was added and stirred at 60 ℃ for 36 h.
(3) Obtaining a target product after centrifugal separation and drying treatment: and centrifuging the suspension at 8000rpm for 10 minutes, washing with water and ethanol for three times, centrifuging, and freeze-drying to obtain the target product.
Examples 1-6Bi-MOF material preparation:
(1) ellagic acid and bismuth acetate were dissolved in water: 0.15g of ellagic acid and 0.45g of bismuth acetate were weighed out, added to a 40mL brown glass vial, and dissolved by adding 30mL of deionized water.
(2) Adding glacial acetic acid, and controlling the pH value of the solution, the reaction temperature and the reaction time: glacial acetic acid (pH. apprxeq.3.5) was added and stirred at 80 ℃ for 24 h.
(3) Obtaining a target product after centrifugal separation and drying treatment: and centrifuging the suspension at 8000rpm for 10 minutes, washing with water and ethanol for three times, centrifuging, and freeze-drying to obtain the target product.
Examples 1-7Bi-MOF material preparation:
(1) ellagic acid and bismuth acetate were dissolved in water: 0.15g of ellagic acid and 0.45g of bismuth acetate were weighed out, added to a 40mL brown glass vial, and dissolved by adding 30mL of deionized water.
(2) Adding glacial acetic acid, and controlling the pH value, the reaction temperature and the reaction time of the solution: glacial acetic acid (pH. apprxeq.4) was added and stirred at room temperature for 48 h.
(3) Obtaining a target product after centrifugal separation and drying treatment: and (3) centrifuging the suspension at 8000rpm for 10 minutes, washing with water and ethanol for three times, centrifuging, and freeze-drying to obtain the target product.
Example 2 electrode preparation of Bi-MOF material:
uniformly dispersing a certain amount of catalyst products and carbon black in a mixed solution of isopropanol and naphthol, uniformly coating the mixed solution on a gas diffusion electrode, and finally drying the prepared working electrode at normal temperature and normal pressure overnight.
Example 3Bi-MOF Material electrode in CO2Application of electroreduction:
the electrochemical tests of this example were carried out in a three-electrode system, separated by a cation-exchange membrane, in a sealed two-compartment H-cell. Wherein the gas diffusion layer is used as a working electrode, the platinum sheet is used as a counter electrode, and Ag/AgCl (saturated KCl) is used as a reference electrode. Controlling CO using mass flow meters2A flow rate; the electrolyte is KHCO3An aqueous solution; the scanning rate range of the cyclic voltammetry curve is 10-100 mV s-1(ii) a The gas and liquid phase products were quantitatively analyzed by gas chromatography and nuclear magnetic resonance, respectively. The electrochemical curve of the reduction reaction is shown in figure 4, and the XRD detection pattern of the electrode after electrochemical catalysis test is shown in figure 5.
Conclusion analysis:
as can be seen from the attached drawings 1 and 2, the Bi-MOF material prepared by the technical scheme provided by the invention is represented as a uniform rod-shaped nanometer material with stable appearance on a microscopic level, and the length of the rod-shaped nanometer material is about 100-500 nm. After being treated by acid-base solution, the Bi-MOF material is shown in figure 3, and the acid resistance and the alkali resistance of the Bi-MOF material prepared by the technical scheme of the invention are stronger than 2 and less than or equal to 14; as can be seen from the thermogravimetric graph 3, the thermal weight loss of the Bi-MOF material prepared by the technical scheme of the invention is not more than 10% below 300 ℃, and the thermal weight loss is not more than 4% at the common electrocatalytic limit temperature below 100 ℃. Therefore, the Bi-MOF material prepared by the technical scheme of the invention has the advantages of uniform and stable appearance, excellent thermal stability and higher thermal weight loss temperature.
According to the comparison graph of the attached figures 2 and 5, the Bi-MOF material prepared by the invention is applied to the reaction of reducing carbon dioxide by an electrode, the crystal structure is not obviously changed, and compared with similar materials in the prior art, the Bi-MOF material has obvious electrocatalytic structural stability and is suitable for industrial application of catalyzing carbon dioxide to be reduced into formic acid by being used as electrode catalysis.
According to the embodiment of electrocatalysis reduction and the attached figure 4, the Bi-MOF material prepared by the invention is applied to the reaction of reducing carbon dioxide by an electrode, the percentage of the formic acid product prepared by catalysis is high, the Faraday efficiency of formic acid can reach about 94 percent, and the Faraday efficiency is far higher than that of the similar products in the prior art, so that the technical scheme has a higher application prospect in the field of electrocatalysis reduction of carbon dioxide.
Claims (10)
1. A preparation method of a Bi-MOF material electrode with catalytic selectivity is characterized by comprising the steps of I, preparing a solution of ellagic acid and bismuth acetate;
II, regulating the pH value to be 2-4 by using glacial acetic acid, and centrifuging and purifying after reaction to obtain a Bi-MOF material;
and III, mixing the Bi-MOF material with carbon black, and coating the mixture on the surface of an electrode to obtain the Bi-MOF material electrode for preparing formic acid by electrocatalysis of carbon dioxide.
2. The method for preparing a Bi-MOF material electrode having catalytic selectivity according to claim 1, wherein the mass ratio of ellagic acid to bismuth acetate in step I is 1: 2 to 3.
3. The method for preparing a Bi-MOF material electrode having catalytic selectivity according to claim 1, wherein the mass ratio of ellagic acid to bismuth acetate in step I is 1: 2 to 3.
4. The method for preparing a Bi-MOF material electrode with catalytic selectivity according to claim 1, wherein in the step I, the reaction temperature of ellagic acid and bismuth acetate is 25-80 ℃, and the reaction time is 24-72 hours.
5. The method for preparing a Bi-MOF material electrode having catalytic selectivity according to claim 1, wherein the purification treatment step in step II comprises vacuum or freeze drying the centrifugally obtained solid to finally obtain the nanorod microstructure.
6. The method for preparing the Bi-MOF material electrode having catalytic selectivity according to claim 1, wherein the stirring is continued during the step II reaction.
7. The preparation method of the Bi-MOF material electrode with catalytic selectivity according to claim 1, wherein the specific step of the step III comprises the steps of uniformly dispersing the Bi-MOF material and carbon black in a mixed solution of isopropanol and naphthol, coating the mixture on a gas diffusion electrode, and drying to obtain the Bi-MOF material electrode.
8. The method for preparing the Bi-MOF material electrode having catalytic selectivity according to claim 7, wherein the mass ratio of the Bi-MOF material to the carbon black in step III is 1: 0.9 to 1.1.
9. The preparation method of the Bi-MOF material electrode with catalytic selectivity of claim 7, wherein the volume ratio of isopropanol to naphthol in the mixed solution of isopropanol and naphthol is 18-20: 1.
10. the method for preparing the Bi-MOF material electrode with catalytic selectivity of claim 7, wherein the coating concentration of the Bi-MOF material on the surface of the electrode is 0.5-1.5 mg/cm2。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115536860A (en) * | 2022-12-01 | 2022-12-30 | 广东工业大学 | Biological MOF material for electrocatalysis and photocatalysis, and preparation method and application thereof |
| CN116284820A (en) * | 2023-03-06 | 2023-06-23 | 天津大学 | Bismuth-based metal organic framework material and preparation method and application thereof |
| CN116676615A (en) * | 2023-07-21 | 2023-09-01 | 深圳先进技术研究院 | For electrocatalytic CO 2 Gas-phase diffusion electrode for reducing formic acid, preparation method and application |
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| CN111041517A (en) * | 2019-12-24 | 2020-04-21 | 中国科学院福建物质结构研究所 | Preparation method and application of two-dimensional bismuth alkene nanosheet |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115536860A (en) * | 2022-12-01 | 2022-12-30 | 广东工业大学 | Biological MOF material for electrocatalysis and photocatalysis, and preparation method and application thereof |
| CN116284820A (en) * | 2023-03-06 | 2023-06-23 | 天津大学 | Bismuth-based metal organic framework material and preparation method and application thereof |
| CN116676615A (en) * | 2023-07-21 | 2023-09-01 | 深圳先进技术研究院 | For electrocatalytic CO 2 Gas-phase diffusion electrode for reducing formic acid, preparation method and application |
| CN116676615B (en) * | 2023-07-21 | 2024-05-17 | 深圳先进技术研究院 | For electrocatalytic CO2Gas-phase diffusion electrode for reducing formic acid, preparation method and application |
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