CN117265575A - Method for preparing electrolytic water catalyst - Google Patents

Method for preparing electrolytic water catalyst Download PDF

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Publication number
CN117265575A
CN117265575A CN202310824668.7A CN202310824668A CN117265575A CN 117265575 A CN117265575 A CN 117265575A CN 202310824668 A CN202310824668 A CN 202310824668A CN 117265575 A CN117265575 A CN 117265575A
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solution
electrolyzed water
salt solution
preparing
water catalyst
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CN202310824668.7A
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Inventor
陆文雅
蒋涛
李丹
龚鸣
吴建翔
卞铁铮
贾飞
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Jiangsu Tianheyuan Hydrogen Technology Co ltd
Fudan University
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Jiangsu Tianheyuan Hydrogen Technology Co ltd
Fudan University
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Priority to CN202310824668.7A priority Critical patent/CN117265575A/en
Publication of CN117265575A publication Critical patent/CN117265575A/en
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • 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
    • C25B11/054—Electrodes comprising electrocatalysts supported on a carrier
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Catalysts (AREA)

Abstract

The embodiment of the disclosure provides a preparation method of an electrolytic water catalyst, which comprises the steps of mixing a nickel salt solution, a chromium salt solution and a salt solution of a third element to obtain a precursor solution, wherein the third element is non-noble metal, coating the precursor solution on an electrode plate, and drying and calcining. The embodiment of the disclosure provides a novel preparation method of a catalyst containing non-noble metal, which combines a coating and calcining process, has stable catalyst loading capacity and uniform distribution, realizes low-cost preparation of an electrolyzed water catalyst, and further realizes large-scale development of a electrolyzed water hydrogen production technology.

Description

Method for preparing electrolytic water catalyst
Technical Field
The disclosure relates to the technical field of electrolyzed water, in particular to a preparation method of an electrolyzed water catalyst.
Background
With the transition exploitation and utilization of fossil energy and the increasing emphasis of global environmental problems, the technical development and large-scale application of novel clean energy are getting more and more attention, such as solar energy, wind energy, tidal energy and the like. Wherein, hydrogen can be prepared by water, and the source is wide. Meanwhile, the combustion heat value of the hydrogen is high, and the combustion products are pollution-free. Therefore, the hydrogen energy source has wide development prospect.
In the related art, the electrolytic water hydrogen production is a common hydrogen production technology, and the basic principle is that under the action of direct current, water molecules are dissociated into hydrogen and oxygen through an electrochemical process, and the hydrogen and the oxygen are separated out at the cathode and the anode respectively.
How to realize large-scale hydrogen production by water electrolysis with lower cost is a subject considered in the industry.
Disclosure of Invention
In view of the above drawbacks of the related art, an object of the present disclosure is to provide a method for preparing an electrolytic water catalyst, so as to solve the technical problem of high cost of producing hydrogen by water electrolysis in the related art.
A first aspect of the present disclosure provides a method for preparing an electrolyzed water catalyst, comprising:
mixing a nickel salt solution, a chromium salt solution and a salt solution of a third element to obtain a precursor solution, wherein the third element is non-noble metal;
and coating the precursor solution on the electrode plate, and drying and calcining.
In some embodiments, the third element comprises at least one of the following non-noble metals:
molybdenum, manganese, cobalt, cadmium, magnesium, lithium, copper, barium, titanium, iron, tin, and calcium.
In some embodiments, the nickel salt solution is obtained by dissolving 1-100mg of the metallic nickel salt in 1-200ml of solvent.
In some embodiments, the chromium salt solution is obtained by dissolving 1-40mg of the metal chromium salt in 1-200ml of solvent.
In some embodiments, the third element solution is obtained by dissolving 1-20mg of the substance comprising the third element in 1-200ml of solvent.
In some embodiments, the at least one salt of a nickel salt and a chromium salt comprises one or more of a nitrate, chloride, oxalate, acetate, citrate, acetylacetonate, and triethanolamine salt.
In some embodiments, mixing the nickel salt solution, the chromium salt solution, and the salt solution of the third element to obtain a precursor solution includes:
mixing a nickel salt solution, a chromium salt solution and a third element solution, heating and stirring to obtain a precursor solution, wherein the heating temperature is 60-250 ℃ and the heating time is 3-6 hours.
In some embodiments, the heating temperature is 80 to 150 ℃.
In some embodiments, the calcination environment during calcination includes one or more of hydrogen, argon, nitrogen, ammonia.
In some embodiments, the calcination temperature during calcination is 300 to 400 ℃.
As described above, the embodiment of the disclosure provides a method for preparing an electrolytic water catalyst, which includes mixing a nickel salt solution, a chromium salt solution, and a salt solution of a third element to obtain a precursor solution, wherein the third element is a non-noble metal, coating the precursor solution on an electrode sheet, and drying and calcining the electrode sheet. The embodiment of the disclosure provides a novel preparation method of a catalyst containing non-noble metal, which combines a coating and calcining process, has stable catalyst loading capacity and uniform distribution, realizes low-cost preparation of an electrolyzed water catalyst, and further realizes large-scale development of a electrolyzed water hydrogen production technology.
Drawings
Fig. 1 shows a flowchart of a method for preparing an electrolyzed water catalyst provided in an embodiment of the present disclosure.
Fig. 2 is one of the scanning electron microscope images of the surface of the electrode sheet coated with the electrolytic water catalyst prepared using the embodiment of the present disclosure.
Fig. 3 is a second scanning electron microscope image of a surface of an electrode sheet coated with an electrolyzed water catalyst prepared using an embodiment of the present disclosure.
Fig. 4 is a graph of oxygen evolution performance of an electrode with an electrolyzed water catalyst made in accordance with the related art and examples of the present disclosure.
Detailed Description
Other advantages and effects of the present disclosure will be readily apparent to those skilled in the art from the following description of the embodiments of the disclosure by means of specific examples. The disclosure may be practiced or carried out in other embodiments or applications, and details of the disclosure may be modified or changed from various points of view and applications without departing from the spirit of the disclosure. It should be noted that, without conflict, the embodiments of the present disclosure and features of the embodiments may be combined with each other.
The embodiments of the present disclosure will be described in detail below with reference to the attached drawings so that those skilled in the art to which the present disclosure pertains can easily implement the same. The present disclosure may be embodied in many different forms and is not limited to the embodiments described herein.
In the description of the present disclosure, references to the terms "one embodiment," "some embodiments," "examples," "particular examples," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. Furthermore, the particular features, structures, materials, or characteristics may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples, as well as features of various embodiments or examples, presented in this disclosure may be combined and combined by those skilled in the art without contradiction.
Although not differently defined, including technical and scientific terms used herein, all terms have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs. The term append defined in commonly used dictionaries is interpreted as having a meaning that is consistent with the meaning of the relevant technical literature and the currently prompted message, and is not excessively interpreted as an ideal or very formulaic meaning, so long as no definition is made.
In the technology of hydrogen production by water electrolysis, a catalyst is used for catalyzing oxidation-reduction reaction in the water electrolysis process. In the related art, the platinum catalyst is a common catalyst for producing hydrogen by electrolyzing water, but the platinum belongs to noble metal, has higher cost and limits the development of the technology for producing hydrogen by electrolyzing water.
The use of non-noble metals to prepare electrolyzed water catalysts can reduce production costs, but how to prepare catalysts comprising non-noble metals is a problem to be solved in the industry.
Fig. 1 shows a flowchart of a method for preparing an electrolytic water hydrogen production catalyst according to an embodiment of the present disclosure, and as shown in fig. 1, the method for preparing an electrolytic water hydrogen production catalyst includes, but is not limited to, the following steps:
step 110: mixing a nickel salt solution, a chromium salt solution and a salt solution of a third element to obtain a precursor solution, wherein the third element is non-noble metal;
step 120: and coating the precursor solution on the electrode plate, and drying and calcining.
The embodiment of the disclosure provides a novel preparation method of a catalyst containing non-noble metal, which combines a coating and calcining process, has stable catalyst loading capacity and uniform distribution, realizes low-cost preparation of an electrolyzed water catalyst, and further realizes large-scale development of a electrolyzed water hydrogen production technology.
Embodiments of the present disclosure use non-noble metals to reduce catalyst costs, wherein the third element comprises at least one of the following non-noble metals:
molybdenum, manganese, cobalt, cadmium, magnesium, lithium, copper, barium, titanium, iron, tin, and calcium.
In practice, suitable non-noble metals may be selected as desired.
In the disclosed embodiments, the nickel salt solution is obtained by dissolving 1-100mg of metallic nickel salt in 1-200ml of solvent. In the corresponding embodiment, the method can be selected in the range according to specific hydrogen production requirements of water electrolysis, and higher catalytic efficiency can be obtained. In further embodiments, the above parameter ranges may be exceeded, as well, with the feasibility ensured.
In an alternative embodiment of the present disclosure, the chromium salt solution is obtained by dissolving 1-40mg of the metal chromium salt in 1-200ml of solvent. In the corresponding embodiment, the method can be selected in the range according to specific hydrogen production requirements of water electrolysis, and higher catalytic efficiency can be obtained. In further embodiments, the above parameter ranges may be exceeded, as well, with the feasibility ensured.
In an alternative embodiment, the third element solution is obtained by dissolving 1-20mg of the substance containing the third element in 1-200ml of the solvent. In the corresponding embodiment, the hydrogen production can be selected in the above range according to the specific water electrolysis hydrogen production requirement, and higher catalytic efficiency can be obtained under the condition of ensuring low cost. In further embodiments, the above parameter ranges may be exceeded, as well, with the feasibility ensured.
In an alternative embodiment, the nickel salt solution, the chromium salt solution and the third element solution are mixed to obtain a precursor solution, which specifically may include:
according to the required metering ratio, 1-100mg of metal nickel salt is dissolved in 1-200mL of solvent to obtain solution A, 1-40mg of chromium salt is dissolved in 1-200mL of solvent to obtain solution B, 1-20mg of substance containing a third element is dissolved in 1-200mL of solvent to obtain solution C, and the three solutions are mixed to obtain the precursor solution.
In an alternative embodiment of the present disclosure, the at least one salt of the nickel salt, the chromium salt, and the salt solution of the third element includes one or more of a nitrate, a chloride, an oxalate, an acetate, a citrate, an acetylacetonate, and a triethanolamine salt.
In practice, suitable non-noble metals may be selected as desired.
In an embodiment of the present disclosure, mixing a nickel salt solution, a chromium salt solution, and a salt solution of a third element to obtain a precursor solution, including:
mixing a nickel salt solution, a chromium salt solution and a third element solution, heating and stirring to obtain a precursor solution, wherein the heating temperature is 60-250 ℃ and the heating time is 3-6 hours.
The three solutions can be fully mixed by heating, and the three solutions are uniformly mixed by stirring. The heating temperature and heating time may be selected within the above-mentioned parameter ranges including the end points, such as 60 c, 250 c, 3 hours, 6 hours, and more uniformly mixed precursor solutions may be obtained.
In a corresponding embodiment, the heating temperature may be set to 80-150 ℃.
In embodiments of the present disclosure, the calcination environment during calcination includes one or more of hydrogen, argon, nitrogen, ammonia. The gases introduced into the calcination environment can carry away water vapor or gaseous products.
In embodiments of the present disclosure, the calcination temperature during calcination is 300 to 400 ℃.
In embodiments of the present disclosure, the electrolyzed water catalyst has a specific microstructure, and at least 70% of the catalyst has a particle size between 0.01 μm and 0.2 μm, optionally in the range of 0.05 μm to 0.1 μm. Wherein the particle size of the metallic nickel is between 100 and 300nm, and the average particle size of the metallic nickel particles is more than twice that of other particles.
In the embodiment of the disclosure, the contact ratio between the metallic nickel and the chromium-containing compound is 20-60 wt%, the contact ratio between the metallic nickel and the third element-containing compound is 10-30 wt%, and the contact ratio between the chromium-containing compound and the third element-containing compound is 5-15 wt%.
In the embodiment of the disclosure, the thickness of the prepared electrolyzed water catalyst is 0.5-3 mu m, and the load is 200-700 mg/cm 2 The preferable range is 300-400 mg/cm 2 The coverage is more than 95%.
In the embodiment of the disclosure, the density of the electrolyzed water catalyst is between 0.90 and 0.99.
In the embodiment of the disclosure, the electrode plate can be made of a non-noble metal conductive material or other conductive materials, so that the noble metal conductive material is used as a substrate, and other non-noble metal elements are loaded to form the stable, conductive, safe and high-specific-surface-area hydrogen evolution catalyst.
In one embodiment, the electrode sheet may be used as a negative electrode sheet or a positive electrode sheet, which is not limited herein.
The method for preparing the electrolyzed water catalyst according to the embodiments of the present disclosure is further described below with reference to the corresponding examples.
Example 1
60mg of nickel nitrate hexahydrate, 18mg of chromium nitrate and 6mg of copper nitrate trihydrate are dissolved in 100 ml of N, N-dimethylformamide, and the precursor solution is obtained by heating and stirring uniformly at 200 ℃ for 4 hours;
coating the precursor solution on a 120 mesh 304 stainless steel mesh of a conductive carrier, drying, calcining at 400 ℃ under the calcining environment H 2 /N 2 (5/95) gas, and maintaining vacuum to obtain electrode sheet NiCr carrying catalyst 2 O 3 CuO-1。
Fig. 2 shows a scanning electron microscope image of the electrode sheet, and it can be seen that the catalyst particles are uniformly distributed on the conductive carrier. The catalyst prepared in example 1 was tested for the catalytic activity and stability of electrolyzed water using a carbon rod as a counter electrode and silver/silver chloride as a reference electrode, and the prepared catalyst was a working electrode and a 1M KOH solution was an electrolytic solution. Linear volt-ampere scanning is carried out at a scanning speed of 5mv/s within the range of-0.6V-0.2V vs RHE voltage, so that the polarization curve of the catalyst for electrocatalytic hydrogen evolution can be obtained, as shown in figure 3, 100mA/cm under the environment of 1M KOH alkaline solution at normal temperature 2 The overpotential is only 150mV when tested at a current of (c).
Example 2
60mg of nickel nitrate hexahydrate, 18mg of chromium nitrate and 6mg of cobalt nitrate hexahydrate are dissolved in 100 ml of N, N-dimethylformamide, and the precursor solution is obtained by heating and stirring uniformly at 200 ℃ for 4 hours;
the precursor solution is coated on a stainless steel mesh with a mesh number 304 of a conductive carrier 120,calcining after drying, wherein the calcining temperature is 400 ℃ and the calcining environment is H 2 /N 2 (5/95) gas, and maintaining vacuum to obtain electrode sheet NiCr carrying catalyst 2 O 3 CoO。
Referring to the scanning electron microscope image shown in fig. 4, it can be seen that the catalyst particles are uniformly distributed on the conductive support. As shown in FIG. 3, 100mA/cm in an alkaline solution of 1M KOH at room temperature 2 The overpotential was measured to be only 155mV at the current of (c).
Example 3
60mg of nickel chloride hexahydrate, 18mg of chromium chloride and 6mg of copper chloride dihydrate are dissolved in 100 ml of N, N-dimethylformamide, and the precursor solution is obtained by heating and stirring uniformly at 200 ℃ for 4 hours;
coating the precursor solution on a 120 mesh 304 stainless steel mesh of a conductive carrier, drying, calcining at 400 ℃ under the calcining environment H 2 /N 2 (5/95) gas, and maintaining vacuum to obtain electrode sheet NiCr carrying catalyst 2 O 3 CuO-2。
As shown in FIG. 3, 100mA/cm in an alkaline solution of 1M KOH at room temperature 2 The overpotential was measured at a current of only 160mV.
Example 4
60mg of nickel nitrate hexahydrate, 18mg of chromium nitrate and 6mg of copper nitrate trihydrate are dissolved in 100 ml of water and ethanol mixed solution, and the mixed solution is heated and stirred uniformly at 200 ℃ to obtain a precursor solution, wherein the heating time is 4 hours;
coating the precursor solution on a 120 mesh 304 stainless steel mesh of a conductive carrier, drying, calcining at 400 ℃ under H2/N2 (5/95) gas, and vacuum maintaining to obtain the electrode plate NiCr carrying the catalyst 2 O 3 CuO-3. As shown in FIG. 3, 100mA/cm in an alkaline solution of 1M KOH at room temperature 2 The overpotential was measured to be only 190mV at the current of (c).
The above embodiments are merely illustrative of the principles of the present disclosure and its efficacy, and are not intended to limit the disclosure. Modifications and variations may be made to the above-described embodiments by those of ordinary skill in the art without departing from the spirit and scope of the present disclosure. Accordingly, it is intended that all equivalent modifications and variations which a person having ordinary skill in the art would accomplish without departing from the spirit and technical spirit of the present disclosure be covered by the claims of the present disclosure.

Claims (10)

1. A method for preparing an electrolyzed water catalyst, comprising:
mixing a nickel salt solution, a chromium salt solution and a salt solution of a third element to obtain a precursor solution, wherein the third element is non-noble metal;
and coating the precursor solution on an electrode plate, and drying and calcining.
2. The method for preparing an electrolyzed water catalyst according to claim 1, wherein the third element comprises at least one non-noble metal selected from the group consisting of:
molybdenum, manganese, cobalt, cadmium, magnesium, lithium, copper, barium, titanium, iron, tin, and calcium.
3. The method for preparing an electrolyzed water catalyst according to claim 1, wherein the nickel salt solution is obtained by dissolving 1 to 100mg of a metallic nickel salt in 1 to 200ml of a solvent.
4. The method for preparing an electrolyzed water catalyst according to claim 1, wherein the chromium salt solution is obtained by dissolving 1 to 40mg of a metal chromium salt in 1 to 200ml of a solvent.
5. The method for producing an electrolyzed water catalyst according to claim 1, wherein the third element solution is obtained by dissolving 1 to 20mg of a substance containing a third element in 1 to 200ml of a solvent.
6. The method for preparing an electrolyzed water catalyst according to claim 1, wherein the at least one salt of nickel salt and chromium salt comprises one or more of nitrate, chloride salt, oxalate, acetate, citrate, acetylacetonate and triethanolamine salt.
7. The method for preparing the electrolyzed water catalyst according to claim 1, wherein the step of mixing the nickel salt solution, the chromium salt solution and the salt solution of the third element to obtain the precursor solution comprises the steps of:
mixing a nickel salt solution, a chromium salt solution and a third element solution, heating and stirring to obtain the precursor solution, wherein the heating temperature is 60-250 ℃ and the heating time is 3-6 hours.
8. The method for preparing an electrolyzed water catalyst according to claim 7, wherein the heating temperature is 80 to 150 ℃.
9. The method for preparing an electrolyzed water catalyst according to claim 1, wherein the calcination environment in the calcination process comprises one or more of hydrogen, argon, nitrogen, and ammonia.
10. The method for preparing an electrolyzed water catalyst according to claim 1, wherein the calcination temperature during the calcination is 300 to 400 ℃.
CN202310824668.7A 2023-07-06 2023-07-06 Method for preparing electrolytic water catalyst Pending CN117265575A (en)

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