CN117026281A - Porous material catalyst for electrolytic hydrogen production of seawater system - Google Patents
Porous material catalyst for electrolytic hydrogen production of seawater system Download PDFInfo
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- CN117026281A CN117026281A CN202310677414.7A CN202310677414A CN117026281A CN 117026281 A CN117026281 A CN 117026281A CN 202310677414 A CN202310677414 A CN 202310677414A CN 117026281 A CN117026281 A CN 117026281A
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 42
- 239000001257 hydrogen Substances 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 37
- 239000011148 porous material Substances 0.000 title claims abstract description 29
- 239000013535 sea water Substances 0.000 title claims abstract description 27
- 239000003054 catalyst Substances 0.000 title claims abstract description 24
- 229910000765 intermetallic Inorganic materials 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 229910006639 Si—Mn Inorganic materials 0.000 claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910018098 Ni-Si Inorganic materials 0.000 claims abstract description 12
- 229910018529 Ni—Si Inorganic materials 0.000 claims abstract description 12
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 36
- 239000000843 powder Substances 0.000 claims description 7
- 238000005868 electrolysis reaction Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- -1 polyethylene butanol Polymers 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 229910005883 NiSi Inorganic materials 0.000 claims description 2
- 229910005881 NiSi 2 Inorganic materials 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- 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
- C25B11/089—Alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Catalysts (AREA)
Abstract
The invention relates to a porous material catalyst for electrolytic hydrogen production of a seawater system. The porous material of the invention is porous Ni-Si intermetallic compound, and the preparation steps are as follows: ni, si and Mn are used as raw materials, the raw materials are respectively mixed according to a certain mass percentage, a vacuum sintering method is adopted for sintering to obtain a porous Ni-Si-Mn material, then the porous Ni-Si-Mn material is soaked in hydrochloric acid solutions with different concentrations for dealloying treatment, and finally the porous Ni-Si intermetallic compound with rich pores is obtained. The porous Ni-Si intermetallic compound has the advantages of synergistic effect between Ni and Si elements, optimized electronic structure of the intermetallic compound and increased pore structure of the material after dealloying treatment, so that the material as a catalyst shows excellent catalytic activity in electrolytic hydrogen production of a seawater system, realizes efficient and stable hydrogen production effect, and has wide application prospect.
Description
Technical Field
The invention relates to a porous material catalyst for electrolytic hydrogen production of a seawater system, belonging to the field of inorganic porous materials and the field of clean sustainable energy preparation application.
Background
The combustion of fossil fuels causes the diffusion of a large amount of pollutants into the air and the increasing consumption of non-renewable energy sources, which have serious influence on the environment and human life, and the development of clean renewable energy sources has become the focus of research in China. As a substitute for fossil fuels, hydrogen is considered as one of the most promising clean energy sources, and is also an option for reducing fuel consumption, and research on the development and conversion of hydrogen energy sources will help to improve the energy structure in China. In various hydrogen production technologies, the electrolytic water hydrogen production has the advantages of high purity, simple process, green and recyclable property, easy storage and the like, and is considered as an optimal hydrogen production path. However, the problems of high catalyst cost, insufficient activity and the like of the electrolytic water hydrogen production are often faced, which severely limits the large-scale application of the electrolytic water hydrogen production, so that the development of a cheap and efficient non-noble metal catalyst is important to the electrolytic hydrogen production process.
The electrolytic hydrogen production in alkaline systems such as seawater and the like involves multi-process water separation, the reaction rate is far lower than that in acidic systems, and the hydrogen production efficiency is lower even with noble metal catalysts. Since the electronic structure of transition metal Ni is close to that of noble metal, it is often used as hydrogen evolution catalyst in alkaline systems such as seawater. Compared with metal simple substance and disordered solid solution alloy, the intermetallic compound consists of metal elements and nonmetal elements in specific proportion, so that the electronic structure of the material can be further optimized, the adsorption and release of ions in the electrolytic hydrogen production process are promoted, and H in the seawater system electrolyte is reduced 2 The dissociation energy barrier of O improves the hydrogen production efficiency of the catalyst in a seawater system, and shows good catalytic activity and stability. The Ni-Si intermetallic compound is a promising electrode material because of low density, good conductivity, excellent oxidation resistance and corrosion resistance, and has wide application prospect in the field of seawater electrolysis hydrogen production.
At present, a plurality of intermetallic compound preparation methods exist, wherein the element powder reaction synthesis method has the advantages of low energy consumption, simple and easily controlled process, short production period, low cost and the like in the preparation process of the element powder reaction synthesis method, and is often used for preparing the intermetallic compound, however, the porous intermetallic compound prepared by the method often has the problems of low porosity and small specific surface area, thereby causing few active sites and the like. In order to solve the problems, elements which are more active than matrix elements can be added in the preparation process of the porous intermetallic compound, and then the elements are completely corroded through dealloying treatment without influencing the composition of the matrix elements, so that the pore structure of the material is improved, the specific surface area of the material is increased, and the material has extremely high intrinsic hydrogen evolution catalytic activity. At present, the research report of preparing porous intermetallic compounds as catalysts by dealloying in the electrolytic hydrogen production under the seawater environment is less, so that the development of a porous material catalyst for the electrolytic hydrogen production of a seawater system has great research significance.
Disclosure of Invention
The invention aims to solve the defects of low hydrogen production efficiency, poor stability and the like of the conventional catalyst in a seawater system, and provides a porous material catalyst for hydrogen production by electrolysis of the seawater system.
The invention relates to a porous material catalyst for preparing hydrogen by seawater system electrolysis, wherein the porous material catalyst is porous Ni-Si intermetallic compound, and the phase composition is Ni 3 Si、Ni 31 Si 12 、Ni 2 Si、NiSi、NiSi 2 Combinations of one or more of the following
The preparation of the porous material specifically comprises the following steps:
(1) Ni, si and Mn are used as raw materials, polyethylene butanol accounting for 3-5% of the mass of the powder is added for granulation, sieving and pressing by a press machine to obtain a green body.
(2) And (3) placing the green body prepared in the step (1) into a vacuum sintering furnace for sintering to obtain the porous Ni-Si-Mn material with the regular size.
(3) Soaking the material prepared in the step (2) in hydrochloric acid solution with the concentration of 0.2-1.5 mol/L for 30-100 min to perform dealloying treatment, thus obtaining the porous Ni-Si intermetallic compound.
Wherein the average grain diameter of the raw materials is 3-6 mu m, and the mass percentages of Ni, si and Mn element ingredients are respectively 70-85%, 10-15% and 5-15%.
Wherein the pressure of the press is 50-150 MPa, and the thickness of the porous Ni-Si-Mn material is 400-600 mu m.
Wherein the vacuum degree is maintained at 2.0X10 during vacuum sintering -2 ～1.0×10 -3 Pa, the sintering process is as follows: firstly, raising the temperature from room temperature to 100-150 ℃ at a heating rate of 5-10 ℃/min, and preserving the temperature for 20-60 min; then heating to 450-560 ℃ at a heating rate of 2-5 ℃/min, and preserving heat for 200-300 min; heating to 580-650 ℃ at a heating rate of 1-5 ℃/min, and preserving heat for 200-300 min; then heating to 950-1100 ℃ at a heating rate of 2-5 ℃/min, and preserving heat for 150-210 min; finally cooling along with the furnace to obtain the porous Ni-Si-Mn material.
The porous material catalyst for the electrolytic hydrogen production of the seawater system is prepared by adopting the method to obtain the porous Ni-Si intermetallic compound, and is applied to the field of electrolytic hydrogen production of the seawater system.
Compared with the prior art, the invention has the advantages that:
(1) The porous Ni-Si intermetallic compound is prepared by combining the methods of once vacuum sintering and acid corrosion dealloying, the preparation process has low energy consumption, simple and easily controlled process, short production period and low cost, and is suitable for large-scale industrial production.
(2) According to the invention, the intermetallic compound is formed by Ni and Si elements, so that the electronic structure of the material can be effectively improved, and the synergistic effect between the two elements is combined, so that the adsorption and release of ions in the electrolytic hydrogen production process are promoted, the catalytic material has good oxidation resistance and stability, and excellent conductivity and corrosion resistance, and has the advantages of excellent stability and activity.
(3) The porous Ni-Si intermetallic compound prepared based on the dealloying method has richer pore structure and larger specific surface area than the common porous material, thereby providing more active sites for HER reaction, improving the electrolytic hydrogen production efficiency of the material in a seawater system and realizing the efficient hydrogen production effect.
Drawings
FIG. 1 is porous Ni prepared in example 1 3 Microscopic surface morphology of Si intermetallic compounds.
FIG. 2 is porous Ni prepared in example 1 3 Cathode polarization curve of Si intermetallic compound in sea water system electrolytic hydrogen production.
Detailed Description
The invention will be further illustrated with reference to specific examples, but the invention is not limited to these examples.
Example 1
The porous material catalyst for electrolytic hydrogen production of a seawater system according to the embodiment is porous Ni 3 The Si intermetallic compound is prepared with Ni, si and Mn elements as material and through the steps of pelletizing with average grain size of 5 microns and element compounding weight percentage of 78%,12% and 10% separately, adding 4% concentration polyvinyl butanol, sieving, pressing in a press with pressure of 100MPa and vacuum sintering in vacuum degree of 1.0×10 -3 Pa, the sintering process is as follows: firstly, raising the temperature from room temperature to 120 ℃ at a heating rate of 5 ℃/min, and preserving the temperature for 30min; then heating to 510 ℃ at a heating rate of 3 ℃/min, and preserving heat for 240min; heating to 600 ℃ at a heating rate of 2 ℃/min, and preserving heat for 240min; then heating to 1000 ℃ at a heating rate of 2 ℃/min, and preserving heat for 180min; finally cooling along with the furnace to obtain the porous Ni-Si-Mn material with the thickness of 500 mu m.
Soaking the sintered porous Ni-Si-Mn material in hydrochloric acid solution with the concentration of 0.8mol/L for dealloying treatment for 60min to obtain porous Ni 3 Si intermetallic compound.
Porous Ni prepared in this example 3 The microscopic surface morphology of the Si intermetallic compound is shown in fig. 1, and the cathodic polarization curve is shown in fig. 2, and can be given by: porous Ni 3 The Si intermetallic compound has rich pore structure and higher specific surface area, which provides more active sites for electrolytic hydrogen production and is the reason for increasing the hydrogen evolution activityAnd firstly, the electrode can be used as an electrode to show excellent hydrogen evolution performance in seawater.
Example 2
The porous material catalyst for electrolytic hydrogen production of seawater system is prepared from three elements of Ni, si and Mn as raw materials, wherein the average particle size is 6 μm, the mass percentages of the element ingredients are 72.9%,13.5% and 13.6%, and polyethylene butanol accounting for 3% of the mass of the powder is added for granulating, sieving, pressing by a press machine, the pressure is 70MPa, and the vacuum degree is kept at 5.0x10 during vacuum sintering - 2 Pa, the sintering process is as follows: firstly, raising the temperature from room temperature to 150 ℃ at a heating rate of 7 ℃/min, and preserving the heat for 40min; then heating to 560 ℃ at a heating rate of 4 ℃/min, and preserving heat for 200min; heating to 650 ℃ at a heating rate of 4 ℃/min, and preserving heat for 250min; then heating to 1050 ℃ at a heating rate of 3 ℃/min, and preserving heat for 200min; finally cooling along with the furnace to obtain the porous Ni-Si-Mn material with the thickness of 600 mu m.
Soaking the sintered porous Ni-Si-Mn material in hydrochloric acid solution with the concentration of 1.2mol/L for dealloying treatment for 80min to obtain porous Ni 31 Si 12 Intermetallic compounds.
Example 3
The porous material catalyst for electrolytic hydrogen production of seawater system is prepared from three elements of Ni, si and Mn as raw materials, wherein the average particle size is 4 μm, the mass percentages of the element ingredients are 74%,18.5% and 7.5%, respectively, polyethylene butanol accounting for 5% of the mass of the powder is added for granulating and sieving, a press is used for pressing, the pressure is 120MPa, and the vacuum degree is kept at 8.0x10 during vacuum sintering -2 Pa, the sintering process is as follows: firstly, raising the temperature from room temperature to 110 ℃ at a heating rate of 6 ℃/min, and preserving the heat for 60min; then heating to 540 ℃ at a heating rate of 5 ℃/min, and preserving heat for 250min; heating to 640 ℃ at a heating rate of 3 ℃/min, and preserving heat for 210min; then heating to 980 ℃ at a heating rate of 5 ℃/min, and preserving heat for 210min; finally cooling along with the furnace to obtain the porous Ni-Si-Mn material with the thickness400 μm.
Soaking the sintered porous Ni-Si-Mn material in hydrochloric acid solution with the concentration of 0.5mol/L for dealloying treatment for 50min to obtain porous Ni 2 Si intermetallic compound.
The above is only a preferred example of the present invention, and experimental parameters are actually used: the mass percentage of Ni, si and Mn elements and the particle size of the powder can be properly adjusted, and the concentration and the treatment time of the acid used in the dealloying method can be properly adjusted. Any variation, identical or similar to the present invention, is within the scope of the present invention.
Claims (6)
1. A porous material catalyst for preparing hydrogen by electrolysis of seawater system is characterized in that the porous material catalyst is porous Ni-Si intermetallic compound, and the phase composition is Ni 3 Si、Ni 31 Si 12 、Ni 2 Si、NiSi、NiSi 2 One or more combinations thereof.
2. A porous material catalyst for the electrolytic hydrogen production of a seawater system as claimed in claim 1, wherein the preparation of the porous material comprises the steps of:
(1) Ni, si and Mn are used as raw materials, polyethylene butanol accounting for 3-5% of the mass of the powder is added for granulation, sieving and pressing by a press machine to obtain a green body.
(2) And (3) placing the green body prepared in the step (1) into a vacuum sintering furnace for sintering to obtain the porous Ni-Si-Mn material with the regular size.
(3) Soaking the material prepared in the step (2) in hydrochloric acid solution with the concentration of 0.2-1.5 mol/L for 30-100 min to perform dealloying treatment, thus obtaining the porous Ni-Si intermetallic compound.
3. The preparation method of the porous material according to claim 2, wherein the average particle size of the raw materials is 3-6 μm, and the mass percentages of the ingredients of Ni, si and Mn are 70-85%, 10-15% and 5-15%, respectively.
4. The method for producing a porous material according to claim 2, wherein the pressure during pressing by a press is 50 to 150MPa and the thickness of the porous Ni-Si-Mn material is 400 to 600 μm.
5. The method for preparing a porous material according to claim 2, wherein the sintering process is as follows: vacuum degree is maintained at 2.0X10 -2 ～1.0×10 -3 Pa, then heating from room temperature to 100-150 ℃ at a heating rate of 5-10 ℃/min, and preserving heat for 20-60 min; then heating to 450-560 ℃ at a heating rate of 2-5 ℃/min, and preserving heat for 200-300 min; heating to 580-650 ℃ at a heating rate of 1-5 ℃/min, and preserving heat for 200-300 min; then heating to 950-1100 ℃ at a heating rate of 2-5 ℃/min, and preserving heat for 150-210 min; finally cooling along with the furnace to obtain the porous Ni-Si-Mn material.
6. A porous material catalyst for seawater system electrolysis hydrogen production, which is characterized in that the porous Ni-Si intermetallic compound prepared by the method of any one of claims 1-5 is applied to the field of seawater system electrolysis hydrogen production.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117886404A (en) * | 2024-03-14 | 2024-04-16 | 四川思达能环保科技有限公司 | Water treatment method and water treatment system |
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| CN117886404A (en) * | 2024-03-14 | 2024-04-16 | 四川思达能环保科技有限公司 | Water treatment method and water treatment system |
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