CN114540831A - Nickel-iron bimetal coordination polymer catalyst for water electrolysis and preparation method thereof - Google Patents
Nickel-iron bimetal coordination polymer catalyst for water electrolysis and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nickel-iron bimetal coordination polymer catalyst for electrolyzing water and a preparation method thereof. The chemical composition formula of the catalyst is NixFe1‑x(L‑)yWherein, 0<x<1,0<y is less than or equal to 1. The preparation method comprises the following steps: the nickel-iron bimetal coordination polymer catalyst is characterized in that a solution containing iron ions, nickel ions, nitrate ions and rigid aromatic polycarboxylic acid ligands is used as a working electrolyte, a three-electrode system is adopted for electrochemical deposition, and a working electrode obtained by electrochemical deposition is washed, oxidized and dried to obtain the nickel-iron bimetal coordination polymer catalyst; it still maintains high catalytic activity after multiple CV cycles; meanwhile, the effect of constant current water electrolysis also shows that the invention is applied toThe obtained catalyst has extremely high catalytic stability and catalytic activity.
Description
Technical Field
The invention relates to a preparation method of a nickel-iron bimetal coordination polymer catalyst for water electrolysis, belonging to the technical field of catalytic materials.
Background
With the progress of science and technology, renewable energy represented by solar energy and wind energy is greatly developed, and the proportion of the renewable energy in the total amount of the global energy power generation and installation machine is increased continuously. However, since the emerging renewable energy sources have time period fluctuation in the power supply, a reliable energy storage method must be found to adjust the energy difference between the peak and the trough of the power generation. Among the many currently proposed energy storage solutions, electrolyzed water is considered the most potential energy storage means. The scheme generally refers to that hydrogen and oxygen are prepared by electrolyzing water by utilizing electric energy when the power generation wave crest is generated, and the electric energy is stored in chemical energy; and the electric energy is released by the reaction of hydrogen and oxygen in the trough period of power generation, so that the carbon emission problem is not involved in the circulation process, and the energy storage method is a real green energy storage mode. In addition, the generated hydrogen and oxygen can be used in other industrial production processes. At present, a great deal of research shows that catalysts containing noble metal elements, such as platinum, ruthenium and other noble metal catalysts, show very excellent performance in electrolyzed water, but the noble metals are expensive due to scarcity on the earth, and the cost of the process of storing energy in the electrolyzed water is seriously influenced. Therefore, a catalyst material with low cost, good catalytic effect and extremely high stability is sought, and the catalyst material plays a vital role in realizing industrial application of the electrolyzed water.
Current nickel-based catalysts are found in large laboratories by virtue of their non-noble metal properties and high performance catalytic effect. With continued research, researchers have found that the catalytic performance of nickel-based catalysts is greatly improved by incorporating iron into the catalysts. This may be due to the fact that the iron element is added to play a role in regulating the electronic structure of nickel, but the research on the mechanism of the regulation is still in debate. The electron transport and the proton transport in the electrolytic water catalysis process respectively represent the thermodynamic and kinetic characteristics of the reaction, and the two characteristics basically determine the rate problem of the electrolytic water. The thermodynamic property of the nickel-based catalyst is solved by doping iron element into the nickel-based catalyst, and the improvement of the kinetic property relates to the restructuring of a novel catalyst framework structure.
Disclosure of Invention
The technical problem solved by the invention is as follows: how to further improve the catalytic performance of the iron-doped nickel-based catalyst so as to realize the technical problem of industrial application of low-cost electrolyzed water energy storage.
In order to solve the technical problem, the invention provides a nickel-iron bimetal coordination polymer catalyst for electrolyzing water, the chemical composition formula of which is NixFe1-x(L-)yWherein, 0<x<1,0<y is less than or equal to 1, Ni is + 2-valent nickel and + 3-valent nickel, and Fe is + 3-valent iron; l is a rigid aromatic polycarboxylic acid ligand, the carboxyl group of which is represented by carboxylate COOH and carboxylate ion COO-Is present in the form of L-The valence of (c) includes at least one of-1, -2, and-3.
Preferably, 0< y.ltoreq.0.6.
Preferably, the rigid aromatic polycarboxylic acid ligand is selected from at least one of the following compounds:
preferably, the nickel-iron bimetallic coordination polymer catalyst is prepared by taking ferric nitrate and/or hydrate thereof, nickel nitrate and/or hydrate thereof and rigid aromatic polycarboxylic acid ligand as raw materials and performing electrochemical deposition on a conductive substrate.
More preferably, the rigid aromatic polycarboxylic acid ligand is selected from at least one of pyromellitic acid, trimesic acid and terephthalic acid.
More preferably, the conductive substrate is nickel foam.
The invention also provides a preparation method of the nickel-iron bimetal coordination polymer catalyst for electrolyzing water, which comprises the following steps:
step 1, preparing Fe-containing3+、Ni2+、NO3 -And a rigid aromatic polycarboxylic acid ligandLiquid;
step 2, adopting a three-electrode system consisting of a working electrode, a reference electrode and a counter electrode to carry out electrochemical deposition in the electrolyte solution prepared in the step 1;
and step 3: and after the electrochemical deposition is finished, taking out the working electrode, washing, oxidizing and drying to obtain the nickel-iron bimetal coordination polymer catalyst.
Preferably, in step 1, the iron salt used for preparing the electrolyte solution is ferric nitrate and/or hydrate thereof, the nickel salt used for preparing the electrolyte solution is nickel nitrate and/or hydrate thereof, and the solvent used for preparing the electrolyte solution is dimethylformamide and deionized water.
Wherein, the solvent is a polar organic solvent capable of dissolving iron salt, nickel salt and rigid aromatic polycarboxylic acid ligand, and DMF can be replaced by polar organic solvents such as DMSO, methanol and the like.
Preferably, the molar ratio of iron ions, nickel ions and pyromellitic acid in the electrolyte solution prepared in the step 1 is 0.01-1: 0.01-1: 0.01 to 1; the molar concentration of the iron ions is 0.01-0.1 mol/L.
Preferably, the three-electrode system in step 2 uses a Pt electrode as a counter electrode, an Ag/AgCl electrode as a reference electrode, and the processed nickel foam as a working electrode.
The working electrode is not limited to be made of nickel foam, and can be any conductive electrode, such as any one of graphite paper, carbon felt, carbon cloth and conductive glass.
Preferably, the treatment mode of the foamed nickel is as follows: and (3) performing ultrasonic treatment on dilute hydrochloric acid for more than 5 minutes, respectively washing with deionized water and ethanol, performing ultrasonic treatment on the mixture in ethanol for more than 5 minutes, and finally drying.
Preferably, the electrochemical deposition conditions in step 2 are: -3mA/cm2 5s+0mA/cm2And (5) constant current deposition is carried out for 500-700 times under the condition of 10 s.
The electrochemical deposition method is not limited to constant current deposition, and constant voltage deposition or other electrochemical deposition methods can also be adopted.
Preferably, the washing in step 3 is: washing with ethanol.
More preferably, the volume ratio of the dimethylformamide to the deionized water is 10: 0.2-1.
More preferably, the concentration of the dilute hydrochloric acid is 0.5-2 mol/L; and the drying is realized by adopting nitrogen for drying.
The invention also provides the nickel-iron bimetal coordination polymer catalyst prepared by the preparation method, which has excellent electrocatalytic performance and good stability.
Compared with the prior art, the invention has the following beneficial effects:
1. the structure of the nickel-iron bimetal coordination polymer catalyst prepared by the invention is a metal organic complex, and the adopted materials are all low-cost materials, so that the high-efficiency catalysis efficiency and the extremely stable catalysis stability are realized;
2. compared with the traditional catalyst synthesis condition, the catalyst synthesis condition adopted by the invention is a method of electrodeposition at normal temperature, the method has the characteristic of mild reaction condition, and meanwhile, the synthesis method adopting low current is a method of synthesizing and preparing the catalyst with low consumption, so that the cost in the process of preparing the catalyst is further reduced;
3. the catalyst obtained by the invention has extremely high catalytic stability, and still maintains high catalytic activity after the voltammetry is carried out for multiple cycles; meanwhile, the effect of constant current water electrolysis also shows that the catalyst has extremely high catalytic stability and catalytic activity.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention;
FIG. 2 is a LSV curve of the metal coordination polymers prepared in examples 1 to 5 and comparative examples 1 to 2;
FIG. 3 shows Ni catalyst prepared in example 10.7Fe0.3-infrared (a) and raman (b) spectra of PMA before and after electrochemical reaction;
FIG. 4 shows Ni catalyst prepared in example 10.7Fe0.3LSV display of PMA (a), Tafel slope plot (b) and stability test results for catalytic performance(c、d);
FIG. 5 shows Ni catalyst prepared in example 10.7Fe0.3TEM image (a), spectroscopy region (b) and spectral scans (c-g) of PMA.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
Nickel-iron bimetallic coordination polymer catalyst (Ni)0.7Fe0.3Preparation of PMA):
152mg (namely 0.6mmol) of pyromellitic acid, 121.2mg (namely 0.3mmol) of ferric nitrate nonahydrate and 203.55mg (namely 0.7mmol) of nickel nitrate hexahydrate are weighed and placed in an electrolytic cell. Then 10mL of DMF solution and 0.6mL of deionized water were added. Sealing the electrolytic cell with graphite paper, and then placing the electrolytic cell in an ultrasonic machine for ultrasonic treatment until pyromellitic acid, ferric nitrate and nickel nitrate in the solution are completely dissolved. For the preparation of nickel foam, a thickness of 2 mm was used, cut to a size of 1cm by 2.5 cm. Then placing the mixture into 1mol/L hydrochloric acid solution, carrying out ultrasonic treatment for 5 minutes, taking out the mixture, and then washing the mixture for five times again by using deionized water. And then ethanol is used for washing twice again, and then the obtained product is placed into an ethanol solution for 5 minutes of ultrasonic treatment, and after the ultrasonic treatment is finished, the obtained product is taken out and dried by nitrogen. And then performing an electrochemical deposition experiment by taking Ag/AgCl as a reference electrode, a platinum mesh electrode as a counter electrode, the processed foamed nickel as a working electrode and the prepared solution as electrolyte. The condition of electrochemical deposition is-3 mA/cm2 5s+0mA/cm2Repeat 600 times for 10 s. After the deposition is finished, the working electrode is taken out, washed by ethanol and then placed in the air for drying and oxidation treatment. The preparation process is shown in figure 1. According to different molar proportions of different NiFe, different examples of NiFe-PMA catalysts are prepared. Note that different NiFe ratios merely changed the amount of iron nitrate and nickel nitrate incorporation.
Example 2
Preparation of Ni-Fe bimetal coordination polymer catalyst0.9Fe0.1-PMA):
The preparation process is the same as example 1, except that 152mg (i.e., 0.6mmol) of pyromellitic acid, 40.4mg (i.e., 0.1mmol) of iron nitrate nonahydrate and 261.7mg (i.e., 0.9mmol) of nickel nitrate hexahydrate are weighed and prepared.
Example 3
Preparation of Ni-Fe bimetal coordination polymer catalyst0.5Fe0.5-PMA):
The preparation process is the same as example 1, except that 152mg (i.e., 0.6mmol) of pyromellitic acid, 202mg (i.e., 0.5mmol) of iron nitrate nonahydrate and 145.4mg (i.e., 0.5mmol) of nickel nitrate hexahydrate are weighed and prepared.
Example 4
Preparation of nickel-iron bimetallic coordination polymer catalyst (Ni)0.3Fe0.7-PMA):
The preparation process is the same as example 1, except that 152mg (i.e., 0.6mmol) of pyromellitic acid, 282.8mg (i.e., 0.7mmol) of iron nitrate nonahydrate and 87.2mg (i.e., 0.3mmol) of nickel nitrate hexahydrate are weighed and prepared.
Example 5
Preparation of nickel-iron bimetallic coordination polymer catalyst (Ni)0.1Fe0.9-PMA):
The preparation process is the same as example 1, except that 152mg (i.e., 0.6mmol) of pyromellitic acid, 363.6mg (i.e., 0.9mmol) of iron nitrate nonahydrate and 29.1mg (i.e., 0.1mmol) of nickel nitrate hexahydrate are weighed and prepared.
Comparative example 1
Preparation of nickel metal coordination polymer catalyst (Ni-PMA):
the preparation process is the same as example 1, except that 152mg (i.e., 0.6mmol) of pyromellitic acid and 290.8mg (i.e., 1mmol) of nickel nitrate hexahydrate are weighed and prepared.
Comparative example 2
Preparation of iron Metal coordination Polymer catalyst (Fe-PMA):
the preparation method is the same as example 1, except that 152mg (i.e. 0.6mmol) of pyromellitic acid and 404mg (i.e. 1mmol) of ferric nitrate nonahydrate are weighed and prepared.
Comparative example 3
Preparation of NiFe-LDH (nickel iron double hydroxide):
0.05mmol of ferric nitrate nonahydrate and 0.05mmol of nickel nitrate hexahydrate are added into 10mL of water, and then electrodeposition is carried out for 300s at a constant voltage of-1V to obtain NiFe-LDH.
Test:
1. testing of LSV curves
LSV curve tests were conducted on the metal coordination polymer catalysts prepared in examples 1 to 5 and comparative examples 1 to 2 using a three-electrode system in which a platinum electrode was used as a counter electrode, the catalyst was used as a working electrode, and the reference electrode was a Hg/HgO electrode inserted in an electrolytic cell in such a manner as to be inserted transversely in the electrolytic cell and as close as possible to one end of the working electrode containing a NiFe-PMA catalyst. The test environment was an electrochemical test performed in 1M KOH electrolyte at room temperature using the electrochemical workstation Bio-Logic VMP3 FlexP 0160. The scan rates were all 5 mV/s. The voltage scanned ranged from 0V to 0.65V (V vs. Hg/HgO). The results are shown in FIG. 2. from FIG. 2, it can be seen that the catalyst Ni prepared in example 10.7Fe0.3PMA has a lower potential, so the optimal proportion of nickel and iron in the catalyst is Ni: fe-7: 3. Based on the conclusions drawn from this experiment, a catalyst with a NiFe ratio of 7:3 was therefore considered as the optimal catalyst, and subsequent testing and analysis were performed.
2. Infrared and Raman Spectroscopy testing
The infrared spectrum and raman spectrum of the catalyst sample prepared in example 1 and the sample after the electrochemical reaction were measured, and the results are shown in fig. 3. It can be observed from FIG. 3 that the prepared bimetallic complex polymer catalyst contains Carboxylate (COOH) and carboxylate ion (COO)-)。
3. Test for catalytic Performance
The catalytic performance and stability of the catalyst were tested in comparison with NiFe-LDH and Nickel foam (Nickel foam) prepared in comparative example, and the results are shown in FIG. 4. from FIG. 4a, it can be seen that NiFe-PMA has more excellent electrolytic water catalytic ability than conventional NiFe-LDH. The Tafel slope of FIG. 4b further illustrates the very outstanding performance of NiFe-PMA in electron transport rate. The stability tests of FIGS. 4c and 4d confirm the stable performance of NiFe-PMA during electrocatalysis.
4. Transmission Electron Microscopy (TEM) testing
The transmission electron micrograph was taken with a JEOL JEM-2100Plus apparatus. As shown in FIG. 5, it can be seen from FIG. 5a that the NiFe-PMA microstructure contains a large number of particles and a large number of carbon structures around the particles, which proves that the PMA forms coordination polymer with the Ni-Fe element, and the interplanar spacing of 0.25nm can also be seen in FIG. 5 a; the EDS scans in FIGS. 5C-g show the distribution of Ni, Fe, C, and O elements.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A nickel-iron bimetal coordination polymer catalyst for electrolyzing water is characterized in that the chemical composition formula is NixFe1-x(L-)yWherein, 0<x<1,0<y is less than or equal to 1, Ni is + 2-valent nickel and + 3-valent nickel, Fe is + 3-valent iron, L is a rigid aromatic polycarboxylic acid ligand, and carboxyl in the rigid aromatic polycarboxylic acid ligand is carboxylic acid radical COOH and carboxylic acid radical ion COO-Is present in the form of L-The valence of (c) includes at least one of-1, -2, and-3.
3. the method for preparing a nickel-iron bimetallic coordination polymer catalyst for electrolyzing water according to claim 1 or 2, characterized by comprising the steps of:
step 1, preparing Fe-containing3+、Ni2+、NO3 -And a rigid aromatic polycarboxylic acid ligand;
step 2, adopting a three-electrode system consisting of a working electrode, a reference electrode and a counter electrode to carry out electrochemical deposition in the electrolyte solution prepared in the step 1;
and step 3: and after the electrochemical deposition is finished, taking out the working electrode, washing, oxidizing and drying to obtain the nickel-iron bimetal coordination polymer catalyst.
4. The method for preparing a nickel-iron bimetal coordination polymer catalyst for electrolyzing water as claimed in claim 3, wherein in the step 1, the iron salt used for preparing the electrolyte solution is ferric nitrate and/or hydrate thereof, the nickel salt used for preparing the electrolyte solution is nickel nitrate and/or hydrate thereof, and the solvent used for preparing the electrolyte solution is dimethylformamide and deionized water.
5. The method for preparing a nickel-iron bimetal coordination polymer catalyst for electrolyzing water as claimed in claim 3, wherein the molar ratio of iron ions, nickel ions and pyromellitic acid in the electrolyte solution prepared in the step 1 is 0.01-1: 0.01-1: 0.01 to 1; the molar concentration of the iron ions is 0.01-0.1 mol/L.
6. The method for preparing a nickel-iron bimetal coordination polymer catalyst for electrolyzing water as claimed in claim 3, wherein the three-electrode system of step 2 uses Pt electrode as counter electrode, Ag/AgCl electrode as reference electrode, and processed foamed nickel as working electrode.
7. The method for preparing a nickel-iron bimetal coordination polymer catalyst for electrolyzing water as claimed in claim 6, wherein the treatment mode of the foamed nickel is as follows: and (3) performing ultrasonic treatment on dilute hydrochloric acid for more than 5 minutes, respectively washing with deionized water and ethanol, performing ultrasonic treatment on the mixture in ethanol for more than 5 minutes, and finally drying.
8. The method for preparing a nickel-iron bimetallic coordination polymer catalyst for electrolyzing water as claimed in claim 3, wherein the electrochemical deposition conditions in step 2 are: -3mA/cm2 5s+0mA/cm2And (5) constant current deposition is carried out for 500-700 times under the condition of 10 s.
9. The method for preparing a nickel-iron bimetal complex polymer catalyst for electrolyzing water as claimed in claim 3, wherein the washing in the step 3 is: washing with ethanol.
10. The method for preparing a nickel-iron bimetallic coordination polymer catalyst for electrolyzing water as claimed in claim 4, wherein the volume ratio of the dimethylformamide to the deionized water is 10:0.2 to 1.
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CN115747875A (en) * | 2022-11-22 | 2023-03-07 | 上海科技大学 | Citric acid-doped ferronickel catalyst, preparation method thereof and application thereof in hydrogen production by electrolyzing water |
CN115786959A (en) * | 2022-12-22 | 2023-03-14 | 大连理工大学 | Electrochemical preparation method of carbon-supported nickel-iron double-metal hydroxide catalyst for synthesizing ammonia by electro-reduction of nitrate |
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CN115747875B (en) * | 2022-11-22 | 2024-03-29 | 上海科技大学 | Citric acid doped ferronickel catalyst, preparation method thereof and application thereof in hydrogen production by water electrolysis |
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CN115746323B (en) * | 2022-11-24 | 2023-08-01 | 四川顺应动力电池材料有限公司 | Preparation method and electrocatalytic application of Fe-based metal organic framework material |
CN115786959A (en) * | 2022-12-22 | 2023-03-14 | 大连理工大学 | Electrochemical preparation method of carbon-supported nickel-iron double-metal hydroxide catalyst for synthesizing ammonia by electro-reduction of nitrate |
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