CN110639488A - Application of biomass-based carbon material in electrochemical reduction of carbon dioxide - Google Patents
Application of biomass-based carbon material in electrochemical reduction of carbon dioxide Download PDFInfo
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- CN110639488A CN110639488A CN201910816056.7A CN201910816056A CN110639488A CN 110639488 A CN110639488 A CN 110639488A CN 201910816056 A CN201910816056 A CN 201910816056A CN 110639488 A CN110639488 A CN 110639488A
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 49
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 49
- 239000002028 Biomass Substances 0.000 title claims abstract description 35
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 26
- 239000003054 catalyst Substances 0.000 claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000009792 diffusion process Methods 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 229920000557 Nafion® Polymers 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 23
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- 230000007935 neutral effect Effects 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000003763 carbonization Methods 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 238000010000 carbonizing Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 241000219823 Medicago Species 0.000 claims description 2
- 235000017587 Medicago sativa ssp. sativa Nutrition 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims description 2
- 229910021397 glassy carbon Inorganic materials 0.000 claims description 2
- 238000006722 reduction reaction Methods 0.000 abstract description 38
- 239000011148 porous material Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 7
- 238000010531 catalytic reduction reaction Methods 0.000 abstract description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 6
- 238000002484 cyclic voltammetry Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000004502 linear sweep voltammetry Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000001075 voltammogram Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B01J35/33—
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- B01J35/61—
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/20—Processes
- C25B3/25—Reduction
Abstract
The invention discloses an application of a biomass-based carbon material of a catalyst for electrochemical reduction of carbon dioxide in the electrochemical reduction of carbon dioxide, which comprises the following steps: dispersing a biomass-based carbon material serving as a catalyst for electrochemical reduction of carbon dioxide into ethanol, adding a Nafion solution, and stirring and ultrasonically treating to obtain a mixed solution; then coating the mixed solution on a gas diffusion electrode body, drying to obtain a gas diffusion electrode loaded with a biomass-based carbon material, wherein the gas diffusion electrode is used for electrochemical reduction of carbon dioxide, and performing efficient electrochemical reduction conversion on the carbon dioxide to obtain an organic product with a high added value; compared with the conventional catalyst, the biomass-based carbon material catalyst has the advantages of low preparation cost, simple process and mild reaction conditions, and the prepared product has a rich pore structure, large specific surface area and stable performance, and the reduction potential required by the catalytic reduction of carbon dioxide is low and the generated current density is high.
Description
The technical field is as follows:
the invention relates to application of a biomass-based carbon material in electrochemical reduction of carbon dioxide.
Background art:
carbon dioxide is a main greenhouse gas causing problems of global warming, environmental pollution and the like as a large amount of carbon dioxide is discharged into the atmosphere along with the rapid consumption of non-renewable traditional fossil fuels such as coal, petroleum, natural gas and the like, and is a carbon resource which is abundant in reserves, renewable, cheap and easy to obtain. Carbon dioxide is regarded as an inexhaustible resource, and the purpose of changing waste into valuable and converting the waste into chemical products with high added value is achieved. But the carbon dioxide has stable chemical property and is not easy to be converted and utilized. At present, the resource utilization technology of carbon dioxide comprises methods such as thermochemical reduction, photochemical reduction, photoelectrocatalysis reduction, electrochemical reduction and the like. Although many reduction and conversion processes are theoretically possible, the reduction of carbon dioxide into high value-added organic matters with the lowest possible energy consumption is one of the research difficulties and hotspots, and the electrochemical reduction method is expected to be an effective means for solving the problem of the difficulty. The electrochemical reduction method has the advantages that: (1) the reaction condition is mild, and clean energy is used in the reaction process; (2) the conversion efficiency is high, and the unit reaction is simple; (3) the reaction process and the target product can be regulated and controlled by controlling the electrolysis condition; (4) realizing the cyclic conversion and utilization of carbon dioxide and synthesizing fine chemicals.
The catalyst is a key for improving the electrochemical reduction efficiency of carbon dioxide, and at present, the research on the catalyst mostly focuses on noble metals or transition metals, so that the catalyst is expensive, scarce and pollutes the environment, and meanwhile, the problems of poor stability, low current efficiency, low selectivity of target products and the like exist. Therefore, the preparation of the efficient, stable and cheap carbon dioxide electrochemical reduction catalyst has great research significance.
The invention content is as follows:
the invention aims to provide application of biomass-based carbon materials in electrochemical reduction of carbon dioxide, biomass is used as a raw material to synthesize a catalyst biomass-based carbon material for electrochemical reduction of carbon dioxide, and efficient electrochemical reduction conversion is carried out on carbon dioxide to obtain organic products with high added values.
The invention is realized by the following technical scheme:
the application of the biomass-based carbon material in the electrochemical reduction of carbon dioxide comprises the following steps: dispersing a biomass-based carbon material used as a carbon dioxide electrochemical reduction catalyst into ethanol, adding a Nafion solution, and stirring and ultrasonically treating to obtain a mixed solution; then coating the mixed solution on a gas diffusion electrode body, drying to obtain a gas diffusion electrode loaded with a biomass-based carbon material, wherein the gas diffusion electrode is used for electrochemical reduction of carbon dioxide, and performing efficient electrochemical reduction conversion on the carbon dioxide to obtain an organic product with a high added value; the preparation method of the biomass-based carbon material of the catalyst for electrochemical reduction of carbon dioxide comprises the following steps: using C, O, N-rich biomass as a raw material, performing hydrothermal reaction at 160-200 ℃ for 18-24 h, cooling, alternately cleaning with ethanol and water until the solution is neutral, drying at 80-105 ℃, carbonizing the obtained solid at 700-1000 ℃ for 2h under the protection of inert gas, cooling, washing with water until the solid is neutral, drying at 100-110 ℃, and grinding to 100-150 meshes to obtain the target product.
More preferably, the method for preparing a biomass-based carbon material of the catalyst for electrochemical reduction of carbon dioxide comprises the steps of:
using C, O, N-rich biomass as a raw material, performing hydrothermal reaction at 160-200 ℃ for 18-24 h, cooling, alternately cleaning with ethanol and water until the solution is neutral, drying at 80-105 ℃, carbonizing the obtained solid at 700-1000 ℃ for 2h under the protection of inert gas, washing with water to be neutral after cooling, drying at 100-110 ℃, grinding to 100-150 meshes, adding the obtained solid into 5-10 mol/L strong acid solution, stirring at room temperature for 12-24h, filtering, washing with water to adjust the pH value to be neutral, and drying at 100-110 ℃ to obtain a target product; the mass ratio of the strong acid to the biochar is 3: 1.
Particularly, the using amount of the biomass-based carbon material is 10-30 mg.
The dosage of the ethanol is 800-1200 mu L.
The dosage of the Nafion solution is 10-30 mu L.
The gas diffusion electrode body is a glass carbon sheet, carbon paper, carbon cloth or carbon felt.
The C, O, N-enriched biomass is preferably cheap biomass such as moss, alfalfa and the like.
More preferably, the hydrothermal reaction temperature is 180 ℃.
The carbonization temperature is preferably 900 ℃.
The invention also provides a gas diffusion electrode, and the preparation method comprises the following steps: dispersing the biomass-based carbon material of the catalyst for electrochemical reduction of carbon dioxide into ethanol, adding a Nafion solution, and stirring and ultrasonically treating to obtain a mixed solution; and then coating the mixed solution on a gas diffusion electrode body, and drying to obtain the target gas diffusion electrode.
The invention also protects the application of the gas diffusion electrode in the electrochemical reduction of carbon dioxide.
The invention has the following beneficial effects: the biomass-based carbon material obtained by the invention is used as a catalyst for electrochemical reduction of carbon dioxide, compared with a conventional catalyst, the preparation cost is lower, the process is simple, the reaction condition is mild, the prepared product has rich pore structure, large specific surface area and stable performance, the reduction potential required by catalytic reduction of carbon dioxide is low, and the generated current density is large.
Description of the drawings:
FIG. 1 is SEM spectra of biochar obtained in examples 1, 2 and 3 under different hydrothermal temperature conditions; wherein a, b and c represent hydrothermal temperatures of 160 ℃, 180 ℃ and 200 ℃, respectively.
FIG. 2 is SEM spectra of biochar obtained in examples 2, 4, 5 and 6 under different carbonization temperature conditions; wherein a, b, c and d respectively represent pyrolysis temperatures of 700 ℃, 800 ℃, 900 ℃ and 1000 ℃.
FIG. 3 is a linear sweep voltammogram of example 9;
FIG. 4 is a cyclic voltammogram of example 10.
The specific implementation mode is as follows:
the following is a further description of the invention and is not intended to be limiting.
Example 1: preparation of biomass-based carbon material for catalyst for electrochemical reduction of carbon dioxide
20g of biomass material moss is placed in a 150mL hydrothermal reaction kettle, hydrothermal reaction is carried out for 24h at 160 ℃, cooling is carried out, ethanol and water are alternately cleaned until the solution is neutral, and drying is carried out for 12h at 80-105 ℃. And carbonizing the obtained solid for 2h at 900 ℃ in a tubular furnace with nitrogen as protective gas, cooling, washing with water to adjust the pH value to be neutral, drying for 12h at 100-110 ℃ to obtain the biochar which is named as a TX-C-160-one-catalyst 900 catalyst and carrying out SEM characterization. As shown in fig. 1 a. TX-C-160-900 has a certain pore structure, but is irregular.
Example 2
The specific preparation process is as shown in example 1, and the biochar named as TX-C-180-900 catalyst can be obtained by changing the hydrothermal temperature to 180 ℃ and is subjected to SEM characterization. As shown in fig. 1b, 2 c. TX-C-180-900 is a regular lamellar structure with abundant pores.
Example 3
The specific preparation process is shown in example 1, the hydrothermal temperature is changed to 200 ℃, and the biochar named as TX-C-200-900 catalyst can be obtained in the same way, and is subjected to SEM characterization, as shown in FIG. 1C, the biochar has a porous structure similar to that of example 2, but the reaction energy consumption is high.
Example 4
The specific preparation process is shown in example 2, and the biochar named as TX-C-180-700 catalyst is obtained by changing the carbonization temperature to 700 ℃ and is subjected to SEM characterization, as shown in FIG. 2 a. TX-C-180-700 is irregular with a small number of pore structures.
Example 5
The specific preparation process is shown in example 2, and the biochar named as TX-C-180-800-catalyst is obtained by changing the carbonization temperature to 800 ℃ and is subjected to SEM characterization, as shown in FIG. 2 b. More pores and regular arrangement.
Example 6
The specific preparation process is shown in example 2, and the biochar named as TX-C-180-1000 catalyst is obtained by changing the carbonization temperature to 1000 ℃ and is subjected to SEM characterization, as shown in FIG. 2 d. Part of the pore structure collapses and has a certain pore structure.
Example 7
Adding the biochar prepared in the example 2 into 6mol/L HCl (the mass ratio of the HCl to the biochar is 3:1), stirring for 12h at room temperature, filtering, washing with water to adjust the pH value to be neutral, drying and grinding at the temperature of 100-.
Example 8: preparation of gas diffusion electrode loaded with carbon dioxide electrochemical reduction catalyst
20mg of the biomass-based carbon material of the catalyst for electrochemical reduction of carbon dioxide prepared in examples 2 and 7 was dispersed in 1000. mu.L of absolute ethanol, 20. mu.L of an Afion solution was added, and ultrasonic dispersion was performed for 30min to obtain a mixed solution, and 10. mu.L of the mixed solution was applied to a glassy carbon electrode and dried to obtain a gas diffusion electrode loaded with the catalyst for electrochemical reduction of carbon dioxide.
Example 9: carbon dioxide electrochemical reduction performance test experiment:
the gas diffusion electrode prepared in example 8 was subjected to linear sweep voltammetry tests under argon saturation and carbon dioxide saturation conditions, respectively, with a sweep range of 0 to-1.8V and a sweep frequency of 10mV/s, to obtain corresponding linear sweep voltammetry curves, as shown in fig. 3. The comparative catalyst found that the biochar of example 7, which was acid washed, was stronger than the biochar of example 2, which was not acid washedElectrochemical activity, reduction potential of-0.8V vs. Ag/AgCl, and maximum current density of 50mA cm-2。
The biochar after acid washing in the example 7 is found to have a better pore structure and a larger specific surface area than the biochar without acid washing in the example 2.
Example 10
The gas diffusion electrode prepared in example 8 was subjected to cyclic voltammetry sweep tests under the conditions of argon saturation and carbon dioxide saturation, respectively, with a sweep range of 0 to-1.8V and a sweep frequency of 10mV/s, to obtain corresponding cyclic voltammetry sweep curves, as shown in fig. 4. Analysis shows that the cyclic voltammetry curve measured in the carbon dioxide saturation state is located below the cyclic voltammetry curve measured in the argon saturation state, which indicates that the current density of the gas diffusion electrode made of the biochar material in example 7 is higher when the carbon dioxide is saturated at the same potential, that is, the gas diffusion electrode has the carbon dioxide electrochemical reduction performance, and the analysis result is consistent with the analysis result in fig. 3.
Claims (10)
1. The application of the biomass-based carbon material in the electrochemical reduction of carbon dioxide is characterized by comprising the following steps: dispersing a biomass-based carbon material used as a carbon dioxide electrochemical reduction catalyst into ethanol, adding a Nafion solution, and stirring and ultrasonically treating to obtain a mixed solution; then coating the mixed solution on a gas diffusion electrode body, drying to obtain a gas diffusion electrode loaded with a biomass-based carbon material, wherein the gas diffusion electrode is used for electrochemical reduction of carbon dioxide, and performing efficient electrochemical reduction conversion on the carbon dioxide to obtain an organic product with a high added value; the preparation method of the biomass-based carbon material of the catalyst for electrochemical reduction of carbon dioxide comprises the following steps: using C, O, N-rich biomass as a raw material, performing hydrothermal reaction at 160-200 ℃ for 18-24 h, cooling, alternately cleaning with ethanol and water until the solution is neutral, drying at 80-105 ℃, carbonizing the obtained solid at 700-1000 ℃ for 2h under the protection of inert gas, cooling, washing with water until the solid is neutral, drying at 100-110 ℃, and grinding to 100-150 meshes to obtain the target product.
2. Use according to claim 1, characterized in that the preparation process of the biomass-based carbon material of the catalyst for electrochemical reduction of carbon dioxide comprises the following steps: using C, O, N-rich biomass as a raw material, performing hydrothermal reaction at 160-200 ℃ for 18-24 h, cooling, alternately cleaning with ethanol and water until the solution is neutral, drying at 80-105 ℃, carbonizing the obtained solid at 700-1000 ℃ for 2h under the protection of inert gas, washing with water to be neutral after cooling, drying at 100-110 ℃, grinding to 100-150 meshes, adding the obtained solid into 5-10 mol/L strong acid solution, stirring at room temperature for 12-24h, filtering, washing with water to adjust the pH value to be neutral, and drying at 100-110 ℃ to obtain a target product; the mass ratio of the strong acid to the biochar is 3: 1.
3. The use according to claim 1 or 2, wherein the biomass-based carbon material is used in an amount of 10 to 30 mg.
4. Use according to claim 1 or 2, wherein the ethanol is used in an amount of 800 μ L to 1200 μ L.
5. Use according to claim 1 or 2, wherein the Nafion solution is used in an amount of 10 μ L to 30 μ L.
6. Use according to claim 1 or 2, wherein the gas diffusion electrode body is a sheet of glassy carbon, carbon paper, carbon cloth or carbon felt.
7. The use according to claim 1 or 2, wherein said C, O, N-enriched biomass is moss, alfalfa.
8. Use according to claim 1 or 2, wherein the hydrothermal reaction temperature is 180 ℃; the carbonization temperature is 900 ℃.
9. A gas diffusion electrode is characterized in that the preparation method is as follows: dispersing the biomass-based carbon material of the catalyst for electrochemical reduction of carbon dioxide as claimed in claim 1 or 2 into ethanol, adding a Nafion solution, and stirring and ultrasonically treating to obtain a mixed solution; and then coating the mixed solution on a gas diffusion electrode body, and drying to obtain the target gas diffusion electrode.
10. Use of a gas diffusion electrode according to claim 9 for electrochemical reduction of carbon dioxide.
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| CN113697793A (en) * | 2021-08-31 | 2021-11-26 | 江苏筑原生物科技研究院有限公司 | Preparation of bone-based biochar and application of bone-based biochar in carbon dioxide reduction |
| CN114934284A (en) * | 2022-06-16 | 2022-08-23 | 河南大学 | Novel phthalocyanine nickel modified pericarp carbon framework catalyst for electrocatalytic reduction of carbon dioxide and preparation method and application thereof |
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