CN110975907B - Preparation method of foam nickel electrode loaded with iron and basic cobalt carbonate for catalyzing oxidation of water or organic matters - Google Patents
Preparation method of foam nickel electrode loaded with iron and basic cobalt carbonate for catalyzing oxidation of water or organic matters Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 110
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 55
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 33
- 239000006260 foam Substances 0.000 title claims abstract description 31
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 230000003647 oxidation Effects 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- OBWXQDHWLMJOOD-UHFFFAOYSA-H cobalt(2+);dicarbonate;dihydroxide;hydrate Chemical compound O.[OH-].[OH-].[Co+2].[Co+2].[Co+2].[O-]C([O-])=O.[O-]C([O-])=O OBWXQDHWLMJOOD-UHFFFAOYSA-H 0.000 title claims description 29
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002131 composite material Substances 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 150000001868 cobalt Chemical class 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 8
- 238000004070 electrodeposition Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims abstract description 6
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 33
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 11
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical group [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 8
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical group [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 4
- 239000012266 salt solution Substances 0.000 claims 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims 1
- 238000000151 deposition Methods 0.000 abstract description 4
- HIYNGBUQYVBFLA-UHFFFAOYSA-D cobalt(2+);dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Co+2].[Co+2].[Co+2].[Co+2].[Co+2].[O-]C([O-])=O.[O-]C([O-])=O HIYNGBUQYVBFLA-UHFFFAOYSA-D 0.000 abstract description 2
- 229910000001 cobalt(II) carbonate Inorganic materials 0.000 abstract description 2
- 229910021446 cobalt carbonate Inorganic materials 0.000 abstract 1
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 abstract 1
- 238000010335 hydrothermal treatment Methods 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 abstract 1
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 10
- 230000003197 catalytic effect Effects 0.000 description 8
- 239000002070 nanowire Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910001429 cobalt ion Inorganic materials 0.000 description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- -1 however Chemical compound 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- NKCVNYJQLIWBHK-UHFFFAOYSA-N carbonodiperoxoic acid Chemical compound OOC(=O)OO NKCVNYJQLIWBHK-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004502 linear sweep voltammetry Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000001075 voltammogram 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
- B01J27/236—Hydroxy carbonates
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- 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
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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- 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
- C25B3/23—Oxidation
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/20—Electroplating: Baths therefor from solutions of iron
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
A preparation method of a foam nickel electrode loaded with iron and basic cobaltous carbonate for catalyzing the oxidation of water or organic matters belongs to the technical field of composite nano materials. The method comprises the following steps: ultrasonically washing the required foamed nickel by using dilute hydrochloric acid, ethanol and deionized water respectively; then placing the foamed nickel into a hydrothermal reaction kettle, and adding a mixed solution of soluble divalent cobalt salt and urea for hydrothermal reaction; and then depositing iron on the electrode after the hydrothermal treatment in a solution containing ferric salt by adopting an electrochemical deposition method to finally obtain the iron-base cobalt carbonate foamed nickel electrode. The electrode can efficiently catalyze water oxidation and organic substrate oxidation, and has high practical value and popularization value.
Description
Technical Field
The invention belongs to the technical field of nano composite materials, and particularly relates to a preparation method of a foam nickel electrode loaded with iron and basic cobalt carbonate for efficiently catalyzing water oxidation and organic substrate oxidation.
Background
The water oxidation reaction is a bottleneck limiting the whole water decomposition process. Regardless of the water decomposition method, the development of an electrocatalytic water oxidation catalyst with high activity and high stability is a crucial step. Early electrocatalytic water oxidation catalysts that were extensively studied were oxides of ruthenium and iridium, however, ruthenium and iridium are very abundant on earth and are therefore difficult to apply on a large scale. Therefore, the development of transition metal catalysts has received much attention from researchers. The electrocatalytic oxidation process of small organic molecules is a very active research area. Electrocatalytic oxidation of benzyl alcohol is one of the most important reactions. The selective oxidation of alcohols to the corresponding aldehydes is of great importance both academically and in the actual industrialization. Benzaldehyde is an important organic intermediate and can be used in the industries of pesticides, medicines, spices, dyes, foods, agriculture and the like. The chemical synthesis method of benzaldehyde generates a plurality of three wastes and has great environmental pollution. The electrochemical synthesis method utilizes the advantages of electrochemical reaction and belongs to a green synthesis method. In organic electrosynthesis reactions, the choice of electrode material is one of the crucial influencing factors. Many examples of organic electrosynthesis reactions show that different electrode materials can produce different products. The foam nickel has a three-dimensional pore structure and a smooth surface, the structure is favorable for the permeation of electrolyte and the release of oxygen bubbles, basic cobalt carbonate nanowires are loaded on the foam nickel by a hydrothermal method, the specific surface area of the material is increased, more active sites can be exposed, the electron transmission is accelerated, and meanwhile, iron deposited by electrodeposition and the basic cobalt carbonate have a certain synergistic effect and are more favorable for efficiently catalyzing water oxidation and organic substrate oxidation.
Disclosure of Invention
The invention aims to provide a preparation method of a foam nickel electrode loaded with iron and basic cobalt carbonate for efficiently catalyzing water oxidation and organic substrate oxidation, and mainly solves the problems of low water oxidation reaction activity, large overpotential, low organic substrate catalytic oxidation efficiency, poor selectivity and the like in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a foam nickel electrode loaded with iron and basic cobalt carbonate for efficiently catalyzing water oxidation and organic substrate oxidation comprises the following steps:
(S1) the desired base nickel foam is ultrasonically washed with dilute hydrochloric acid, ethanol and deionized water for 15 minutes to remove oxide impurities remaining on the nickel foam.
(S2) putting the nickel foam cleaned in the step (S1) into a hydrothermal reaction kettle, adding a mixed solution of soluble divalent cobalt salt and urea, and carrying out hydrothermal reaction for 5-24h at 80 ℃ to obtain the basic cobalt carbonate-loaded nickel foam electrode.
(S3) loading iron on the surface of the foamed nickel electrode loaded with basic cobalt carbonate obtained in the step (S2) in a solution containing soluble ferric salt by adopting an electrochemical deposition method to obtain the composite material.
(S4) washing the obtained composite material with deionized water, and dialyzing to remove the residual salt on the surface to obtain the required iron and basic cobalt carbonate supported foamed nickel electrode.
Further, the concentration of urea in the step (S2) is 0.05-0.5 mol/L.
Further, the soluble divalent cobalt salt in the step (S2) is cobalt chloride, and the concentration is 0.05-0.5 mol/L.
Specifically, the soluble ferric salt in the step (S3) is ferric nitrate, and the concentration is 5-100 mmol/L.
Compared with the prior art, the invention has the following beneficial effects:
(1) the substrate foamed nickel adopted by the invention has a three-dimensional pore structure and a smooth surface, and the structure is more favorable for the permeation of electrolyte and the release of oxygen bubbles.
(2) According to the invention, foam nickel with a required size is placed in a hydrothermal reaction kettle, and soluble divalent cobalt salt and urea are added simultaneously, so that the urea not only is one of raw materials for preparing the basic cobalt carbonate nanowire, but also provides an alkaline environment for hydrolysis of cobalt ions. Finally, needle-shaped nanowires are grown in situ on smooth foamed nickel, and have larger specific surface area and electrochemical active area, and more active sites are exposed.
(3) The electrode prepared by the invention can electrically deposit iron on the basic cobalt carbonate, and the deposited iron and the basic cobalt carbonate can better contact due to the large specific surface area of the nano wire, thereby being beneficial to enhancing the synergistic catalytic action of cobalt ions and iron ions and being more beneficial to catalyzing water oxidation and organic substrate oxidation.
Drawings
FIG. 1 is a schematic view of the flow structure of the present invention.
Fig. 2 is a scanning electron microscope photograph of the surface of the basic cobalt carbonate-supported nickel foam and the iron and basic cobalt carbonate-supported nickel foam electrode of the present invention.
Fig. 3 shows the catalytic performance and stability of the water oxidation reaction of the foamed nickel electrode loaded with iron and basic cobalt carbonate.
Fig. 4 is a linear sweep voltammogram of a nickel foam electrode loaded with iron and cobalt hydroxycarbonate according to the invention in a catalytic benzyl alcohol oxidation reaction, and the conversion of benzyl alcohol and the selectivity of benzaldehyde over the catalytic time.
Detailed Description
The present invention is further illustrated by the following figures and examples, which include, but are not limited to, the following examples.
A preparation method of a foam nickel electrode loaded with iron and basic cobalt carbonate for efficiently catalyzing water oxidation and organic substrate oxidation comprises the following steps:
(S1) the desired base nickel foam is ultrasonically washed with dilute hydrochloric acid, ethanol and deionized water for 15 minutes to remove oxide impurities remaining on the nickel foam.
(S2) placing the cleaned nickel foam in the step (S1) into a hydrothermal reaction kettle, adding a mixed solution of soluble divalent cobalt salt with the concentration of 0.05-0.5mol/L and urea with the concentration of 0.1-1mol/L, and carrying out hydrothermal reaction for 5-24h at the temperature of 80 ℃ to obtain the basic cobalt carbonate-loaded nickel foam electrode.
(S3) loading iron on the surface of the foamed nickel electrode loaded with basic cobalt carbonate obtained in the step (S2) in a solution containing soluble ferric salt with the concentration of 5-100mmol/L by adopting an electrochemical deposition method to obtain the composite material.
(S4) washing the obtained composite material with deionized water, and dialyzing to remove the residual salt on the surface to obtain the required iron and basic cobalt carbonate supported foamed nickel electrode.
The specific embodiments are as follows:
example 1
Cutting the foamed nickel into 3 x 2cm, respectively ultrasonically washing the foamed nickel for 15 minutes by using dilute hydrochloric acid, ethanol and deionized water, and removing oxide impurities remained on the foamed nickel. And (3) putting the cleaned foamed nickel into a hydrothermal reaction kettle, adding a mixed solution of cobalt chloride with the concentration of 0.15mol/L and urea with the concentration of 0.4mol/L, and carrying out hydrothermal reaction for 12 hours at the temperature of 80 ℃ to obtain the basic cobalt carbonate-loaded foamed nickel electrode. And then, carrying out electrochemical deposition in ferric nitrate with the concentration of 10mmol/L at the deposition voltage of-1.2V for 200s to load iron on the surface of the electrode to obtain the foamed nickel electrode composite material loaded with iron and basic cobalt carbonate. The raw material nickel foam was purchased from a Xinyuan metallic materials plant, and the contact number was 17859675352.
The foam nickel electrode composite material loaded with iron and basic cobaltous carbonate is applied to catalytic water oxidation reaction.
As can be seen from fig. 2 (a, b), the smooth nickel foam surface densely and uniformly grows needle-shaped nanowires on the surface after hydrothermal reaction, and as can be seen from fig. 2 (c, d), the surface of the needle-shaped nanowires becomes rough after iron is electrodeposited, which indicates that iron is deposited on the surface of the basic cobalt carbonate nanowires. As can be seen from FIG. 3, the activity of the iron and basic cobalt carbonate-loaded nickel foam electrode was highest at current densities of up to 100mA/cm2When the catalyst is used, the overpotential is only 255mV, the catalytic stability is high, and the effect is basically kept unchanged after the catalytic water is oxidized for 50 hours.
Example 2
Cutting the foamed nickel into 3 x 2cm, respectively washing with dilute hydrochloric acid, ethanol and deionized water for 15 minutes by ultrasonic waves, and removing oxide impurities remained on the foamed nickel. And (3) putting the cleaned foamed nickel into a hydrothermal reaction kettle, adding a mixed solution of cobalt chloride with the concentration of 0.15mol/L and urea with the concentration of 0.4mol/L, and carrying out hydrothermal reaction for 12 hours at the temperature of 80 ℃ to obtain the basic cobalt carbonate-loaded foamed nickel electrode. And then, carrying out electrochemical deposition in a solution containing ferric nitrate with the concentration of 10mmol/L, wherein the deposition voltage is-1.2V, the deposition time is 200s, and loading iron on the surface of the electrode to obtain the foam nickel electrode composite material loaded with iron and basic cobalt carbonate.
The foam nickel electrode composite material loaded with iron and basic cobalt carbonate is used for catalyzing the benzyl alcohol oxidation reaction. As can be seen from (a) in fig. 4, it can be seen from the linear sweep voltammetry that a large oxidation peak of benzyl alcohol appears when the applied voltage is 0.4V after benzyl alcohol is added into the solution, which indicates that the electrode prepared by us can catalyze the oxidation of the organic benzyl alcohol. Fig. 4 (b) is a graph showing the relationship between the catalytic reaction time, the conversion of benzyl alcohol and the selectivity of benzaldehyde, and it can be seen from the graph that the conversion of benzyl alcohol can reach more than 70% and the selectivity of benzaldehyde is about 60% after two hours.
The above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, but all changes that can be made by applying the principles of the present invention and performing non-inventive work on the basis of the principles shall fall within the scope of the present invention.
Claims (1)
1. The application of the foam nickel electrode loaded with iron and basic cobalt carbonate in catalyzing the oxidation of benzyl alcohol is characterized in that:
the preparation method of the foamed nickel electrode comprises the following steps:
(S1) ultrasonically washing the needed substrate foamed nickel for 15 minutes by respectively using dilute hydrochloric acid, ethanol and deionized water;
(S2) placing the cleaned nickel foam in the step (S1) into a hydrothermal reaction kettle, adding a mixed solution of a soluble divalent cobalt salt solution and urea, and carrying out hydrothermal reaction for 5-24h at 80 ℃ to obtain a basic cobalt carbonate-loaded nickel foam electrode; the concentration of the urea is 0.05-0.5 mol/L; the soluble divalent cobalt salt is cobalt chloride, and the concentration of the soluble divalent cobalt salt solution is 0.05-0.5 mol/L;
(S3) loading iron on the surface of the foamed nickel electrode loaded with basic cobalt carbonate in a solution containing soluble ferric salt by adopting an electrochemical deposition method to obtain a composite material; the soluble ferric iron salt is ferric nitrate, and the concentration is 5-100 mmol/L;
(S4) washing the obtained composite material with deionized water, dialyzing to remove residual salt on the surface, and obtaining a foam nickel electrode loaded with iron and basic cobalt carbonate;
the foamed nickel electrode is applied to catalyzing the oxidation of benzyl alcohol.
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| CN113322477B (en) * | 2021-05-19 | 2023-01-31 | 北京化工大学 | Method for preparing benzaldehyde by oxidizing benzyl alcohol through 3D printing flow electrochemical reactor |
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| CN109174146A (en) * | 2018-07-24 | 2019-01-11 | 安徽师范大学 | One-dimensional basic cobaltous carbonate@dimensional Co Se/NF heterojunction structure composite material and preparation method and application |
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