CN114293200A - Porous carbon loaded amorphous/crystalline ruthenium-based high-efficiency hydrogen evolution catalyst and preparation and application thereof - Google Patents
Porous carbon loaded amorphous/crystalline ruthenium-based high-efficiency hydrogen evolution catalyst and preparation and application thereof Download PDFInfo
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Abstract
The invention provides a porous carbon loaded amorphous/crystalline ruthenium-based high-efficiency hydrogen evolution catalyst and preparation and application thereof, and relates to the fields of new energy materials and electrochemical catalysis. The preparation of the catalyst comprises the following steps: 1) preparing porous carbon; 2) uniformly dispersing porous carbon in a dispersion medium by ultrasonic waves to form a suspension, mixing the suspension with a water solution containing ruthenium trichloride and boric acid in a homogeneous phase or a double-solvent phase, and fully stirring to realize uniform assembly of ruthenium borate in a porous carbon carrier; 3) and annealing the porous carbon assembled with the ruthenium borate at high temperature in a protective gas atmosphere to obtain the porous carbon loaded amorphous/crystalline ruthenium-based catalyst. The porous carbon loaded amorphous/crystalline ruthenium-based catalyst obtained by the invention has the catalytic hydrogen evolution performance far higher than that of a commercial platinum-carbon material under an alkaline condition, can be comparable to that of the commercial platinum-carbon catalyst under an acidic condition, and greatly reduces the use amount of noble metals. The porous carbon loaded amorphous/crystalline ruthenium-based catalyst provided by the invention has the advantages of simple preparation process, high yield, excellent performance and low cost, can replace a commercial platinum-based catalyst, and has wide application prospect.
Description
Technical Field
The invention relates to the field of new energy materials and electrochemical catalysis, in particular to preparation of a porous carbon loaded amorphous/crystalline catalyst and application of the catalyst in electrolytic water-out hydrogen.
Background
With the increasing exhaustion of traditional fossil energy such as petroleum and coal and the increasing severity of environmental pollution, hydrogen (H)2) Due to the advantages of portability, high energy efficiency, no carbon emission, no pollution and the like, the energy is considered to be the cleanest renewable energy source and is a potential unlimited resource. However, there are many problems to be solved in developing a hydrogen energy economy, such as hydrogen production. The traditional non-renewable energy sources (such as coal, natural gas, petroleum and the like) for hydrogen production inevitably aggravate greenhouse gas emission and increase environmental burden, and the water electrolysis driven by renewable energy sources such as solar energy, wind energy or tidal energy provides a cleaner, efficient and sustainable hydrogen production strategy.
In view of the current situation, there is an urgent need to explore efficient, low cost catalysts to replace the baseline platinum-based electrocatalysts to promote the slow kinetics of the important hydrogen evolution half-reactions in large scale water electrolysis. It is also noted that the conversion of platinum in the Hydrogen Evolution Reaction (HER) in alkaline medium is 2-3 orders of magnitude lower than in acidic medium. While some non-noble metal electrocatalysts, such as transition metal oxides, hydroxides, sulfides, etc., used in Oxygen Evolution Reactions (OER) and water electrolysis half-reactions are not stable under acidic conditions. Therefore, efficient, stable, low-cost hydrogen evolution catalysts are being developed toward the practical application of large-scale water electrolysis under alkaline and acidic conditions.
Among the hydrogen evolution electrocatalysts reported in recent years, ruthenium-based electrocatalysts have been found to be inexpensive (only about 4% of the price of Pt), have excellent corrosion resistance in both alkaline and acidic media, and react with hydrogen (about 65kcal mol%-1) Have similar bonding strength and are receiving wide attention. Baek et al reported a hydrogen evolution catalyst based on Ru nanoparticles uniformly dispersed on graphene nanoplatelets, which catalyst has superior performance in both acidic and alkaline electrolytes over Pt. The research group of Feng et al developed a novel ruthenium/nitrogen doped graphite foam electrocatalyst that was in alkaline solution compared to some reported electrocatalysts and platinum catalystsExhibits excellent electrocatalytic activity. These studies confirm that Ru is superior to other metals and even Pt catalysts in water dissociation and chemisorption of OH. Although ruthenium-based electrocatalysts show attractive potential in hydrogen evolution, materials that can meet high activity and durability in both basic and acidic media still pose serious challenges to catalyst design.
Disclosure of Invention
The invention provides a porous carbon loaded amorphous/crystalline ruthenium-based high-efficiency hydrogen evolution catalyst and preparation and application thereof.
The invention is mainly realized by adopting the following technical scheme:
a porous carbon loaded amorphous/crystalline ruthenium-based high-efficiency hydrogen evolution catalyst is characterized in that the catalyst is a synergistic effect of porous carbon uniformly loaded amorphous and crystalline catalytic active components.
The porous carbon is polyhedral porous carbon prepared by taking a zinc-based zeolite imidazole ester framework as a precursor.
The amorphous and crystalline catalytic active components are amorphous Rubx and crystalline Ru catalytic active components.
The particle size of the amorphous RuBx and crystalline Ru catalytic active components is 2-10 nm.
A preparation method of a porous carbon loaded amorphous/crystalline ruthenium-based high-efficiency hydrogen evolution catalyst comprises the following steps:
1) preparation of porous carbon: stirring and uniformly mixing zinc acetate and a methanol or ethanol solution of 2-methylimidazole for 10-60 min, standing for 6-24 h for reaction, performing centrifugal separation and drying to obtain a zinc-based zeolite imidazole ester framework, transferring the zinc-based zeolite imidazole ester framework into a tubular furnace, and performing Ar atmosphere or N atmosphere2And pyrolyzing at the temperature of 800 ℃ and 1100 ℃ for 1-4h in the atmosphere to obtain the polyhedral porous carbon PNCH.
2) Homogeneous assembly of ruthenium borate in porous carbon support: dispersing porous carbon in a dispersion medium according to the mass ratio of 1: 1-1: 3, performing ultrasonic treatment at room temperature for 5-30 min to form a turbid liquid, slowly injecting 2mL of aqueous solution containing 10-50mg of ruthenium trichloride or hydrated ruthenium trichloride and 90mg of boric acid into the turbid liquid of the porous carbon under magnetic stirring at room temperature, violently stirring for 1-5 h, and drying at 80 ℃ to obtain black powder.
3) Preparation of ruthenium-based catalyst: and transferring the black powder sample into a tubular furnace, and carrying out annealing treatment for 1-4h at 400-600 ℃ in a protective gas atmosphere to obtain the catalyst with the amorphous ruthenium boride/crystalline ruthenium nanoparticles uniformly loaded on the porous carbon.
Preferably, in the step 2), the dispersion medium is deionized water or ethanol or pentane or n-hexane.
Preferably, in the step 3), the protective gas atmosphere is an inert gas (argon or nitrogen) or a mixed gas atmosphere of an inert gas and hydrogen.
The invention provides application of a porous carbon loaded amorphous/crystalline ruthenium-based catalyst in catalyzing water electrolysis hydrogen evolution in acidic and alkaline solutions.
Drawings
FIG. 1 is a transmission electron micrograph and a high resolution transmission electron micrograph of the porous carbon-supported amorphous/crystalline ruthenium-based hydrogen evolution catalyst prepared in example 1;
FIG. 2 shows the porous carbon supported amorphous/crystalline ruthenium-based hydrogen evolution catalyst prepared in example 1 in 1M KOH and 0.5M H2SO4Polarization curves in solution;
Detailed Description
The following examples are given to illustrate the present invention in more detail, but do not limit the scope of the claims of the present invention.
Example 1
1) Preparation of porous carbon: respectively dissolving 3.3g of zinc acetate dihydrate and 9.85g of 2-methylimidazole in 900mL of ethanol, pouring the ethanol solution of 2-methylimidazole into the ethanol solution of zinc acetate after all the zinc acetate and the 2-methylimidazole are dissolved, standing for 24 hours for reaction, performing centrifugal freeze drying treatment to obtain a zinc-based zeolite imidazolate framework, transferring the zinc-based zeolite imidazolate framework to a tubular furnace, and pyrolyzing the zinc-based zeolite imidazolate framework for 2 hours at 900 ℃ under Ar atmosphere to obtain the nitrogen-doped polyhedral porous carbon.
2) Homogeneous assembly of ruthenium borate in porous carbon support: 50mg of prepared porous carbon is dispersed in 50mL of n-hexane dispersion medium, and the mixture is subjected to ultrasonic treatment at room temperature for 5min to form a suspension. And (3) slowly injecting 2mL of aqueous solution containing 30mg of ruthenium trichloride and 90mg of boric acid which are uniformly mixed by ultrasound into the porous carbon suspension under magnetic stirring, violently stirring for 3 hours, and drying at the temperature of 80 ℃ to obtain black powder.
3) Preparation of ruthenium-based catalyst: transferring a black powder sample into a tube furnace, and annealing at 600 ℃ for 2h in a 5% hydrogen/argon atmosphere to obtain a catalyst with amorphous ruthenium boride/crystalline ruthenium nanoparticles uniformly loaded on polyhedral porous carbon, which is noted as RuB belowx-Ru @ BNPCH. FIG. 1 is a transmission electron micrograph and a high resolution transmission electron micrograph of the prepared porous carbon-supported amorphous/crystalline ruthenium-based hydrogen evolution catalyst.
Example 2
Example 2 differs from example 1 in that in step 2), deionized water is used as the dispersing medium.
Example 3
Example 3 differs from example 1 in that ethanol is used as the dispersion medium in step 2).
Example 4
1) Preparation of porous carbon: respectively dissolving 3.3g of zinc acetate dihydrate and 9.85g of 2-methylimidazole in 900mL of ethanol, pouring the ethanol solution of 2-methylimidazole into the ethanol solution of zinc acetate after all the zinc acetate and the 2-methylimidazole are dissolved, standing for reaction for 12 hours, carrying out centrifugal freeze drying treatment to obtain a zinc-based zeolite imidazolate framework, transferring the zinc-based zeolite imidazolate framework to a tubular furnace, and carrying out pyrolysis at 1000 ℃ for 2 hours in Ar atmosphere to obtain the nitrogen-doped polyhedral porous carbon.
2) Homogeneous assembly of ruthenium borate in porous carbon support: 50mg of prepared porous carbon is dispersed in 50mL of n-hexane dispersion medium, and the mixture is subjected to ultrasonic treatment at room temperature for 5min to form a suspension. And (3) slowly injecting 2mL of aqueous solution containing 30mg of ruthenium trichloride and 90mg of boric acid which are uniformly mixed by ultrasound into the porous carbon suspension under magnetic stirring, violently stirring for 3 hours, and drying at the temperature of 80 ℃ to obtain black powder.
3) Preparation of ruthenium-based catalyst: and transferring the black powder sample into a tubular furnace, and carrying out annealing treatment at 600 ℃ for 2h in an argon atmosphere to obtain the catalyst with the amorphous ruthenium boride/crystalline ruthenium nanoparticles uniformly loaded on the polyhedral porous carbon.
Comparative example 5
1) Preparation of porous carbon: respectively dissolving 3.3g of zinc acetate dihydrate and 9.85g of 2-methylimidazole in 900mL of ethanol, pouring the ethanol solution of 2-methylimidazole into the ethanol solution of zinc acetate after all the zinc acetate and the 2-methylimidazole are dissolved, standing for 24 hours for reaction, performing centrifugal freeze drying treatment to obtain a zinc-based zeolite imidazolate framework, transferring the zinc-based zeolite imidazolate framework to a tubular furnace, and pyrolyzing the zinc-based zeolite imidazolate framework for 2 hours at 900 ℃ under Ar atmosphere to obtain the nitrogen-doped polyhedral porous carbon.
2) Homogeneous assembly of ruthenium in porous carbon support: 50mg of prepared porous carbon is dispersed in 50mL of n-hexane dispersion medium, and the mixture is subjected to ultrasonic treatment at room temperature for 5min to form a suspension. And slowly injecting 2mL of water solution containing 30mg of ruthenium trichloride and uniformly mixed by ultrasound into the porous carbon suspension under magnetic stirring, violently stirring for 3 hours, and drying at the temperature of 80 ℃ to obtain black powder.
3) Preparation of ruthenium-based catalyst: and transferring the black powder sample into a tubular furnace, and carrying out annealing treatment at 600 ℃ for 2h in a 5% hydrogen/argon atmosphere to obtain the catalyst, namely Ru @ NPCH, in which the crystalline ruthenium nanoparticles are uniformly loaded on the polyhedral porous carbon.
RuB prepared in example 1xThe water electrolysis hydrogen evolution catalytic performance test is carried out on the-Ru @ BNPCH and the Ru @ NPCH prepared in the comparative example 5.
Hydrogen evolution catalytic performance test conditions:
the test was performed on a CHI 660D electrochemical test system (shanghai chenghua) using a standard three-electrode system. Graphite rod and Saturated Calomel Electrode (SCE) were used as auxiliary electrode and reference electrode, respectively, glassy carbon electrode (GCE, diameter 3mm) was used as working electrode, and 4 μ L concentration of 5mg mL was used as glassy carbon electrode-1Modified in alkaline and acidic electrolyte (Ar-saturated 1M KOH/0.5M H)2SO4) Solution) and the LSV test sweep rate is 0.5mV s-1. FIG. 2 shows the results of the catalysts prepared in example 1 and comparative example 5 and commercial Pt/C catalysts in 1M KOH and 0.5M H2SO4Polarization curve in solution.
In 1M KOH solution, RuBx-Ru @ BNPCH catalyst is used at 10,50 and 100mAcm-2The time overpotential is eta respectively10＝ 5mV，η5031mV and eta10053mV, much lower than Ru @ NPCH (eta)10＝21mV，η50＝99mV，η100122 mV) and commercial Pt/C (η)10＝35mV，η50＝165mV，η100185 mV). Furthermore, RuBx-Ru @ BNPCH can also provide 300mAcm at an extremely low overpotential of 114mV-2Is important for practical application of water electrolysis. And still maintain its catalytic performance after 40h stability testing. In addition, at 0.5M H2SO4The result of hydrogen evolution test in the solution shows that the overpotential eta of the RuBx-Ru @ BNPCH catalyst1033mV, the catalytic performance is obviously superior to Ru @ NPCH (eta)1073mV) and comparable to commercial Pt/C performance (η)10＝24mV)。
Claims (9)
1. A porous carbon loaded amorphous/crystalline ruthenium-based high-efficiency hydrogen evolution catalyst is characterized in that porous carbon is used as a catalyst carrier, and amorphous and crystalline catalytic active components are uniformly loaded to realize synergistic effect.
2. The ruthenium-based high-efficiency hydrogen evolution catalyst according to claim 1, wherein the porous carbon is polyhedral porous carbon prepared by using a zinc-based zeolite imidazole ester framework as a precursor.
3. The ruthenium-based high-efficiency hydrogen evolution catalyst according to claim 1, wherein the amorphous and crystalline catalytically active components are amorphous RuBx and crystalline Ru catalytically active components.
4. The ruthenium-based high-efficiency hydrogen evolution catalyst according to claim 1, wherein the particle size of the amorphous Rubx and crystalline Ru catalytic active components is 2-10 nm.
5. A porous carbon supported amorphous/crystalline ruthenium-based high-efficiency hydrogen evolution catalyst according to any one of claims 1 to 4, comprising the steps of:
1) preparation of porous carbon: stirring and uniformly mixing zinc acetate and a methanol or ethanol solution of 2-methylimidazole for 10-60 min, standing for 6-24 h for reaction, performing centrifugal separation and drying to obtain a zinc-based zeolite imidazole ester framework, transferring the zinc-based zeolite imidazole ester framework into a tubular furnace, and performing Ar atmosphere or N atmosphere2And pyrolyzing for 1-4h at 800-1100 ℃ in the atmosphere to obtain the nitrogen-doped porous carbon PNCH.
2) Homogeneous assembly of ruthenium borate in porous carbon support: dispersing porous carbon in a dispersion medium according to the mass ratio of 1: 1-1: 3, performing ultrasonic treatment at room temperature for 5-30 min to form turbid liquid, slowly injecting 2mL of aqueous solution containing 10-50mg of ruthenium trichloride or hydrated ruthenium trichloride and 90mg of boric acid into the turbid liquid of the porous carbon under magnetic stirring at room temperature, violently stirring for 1-5 h, and drying at 80 ℃ to obtain black powder.
3) Preparation of ruthenium-based catalyst: and transferring the black powder sample into a tubular furnace, and carrying out annealing treatment for 1-4h at 400-600 ℃ in a protective gas atmosphere to obtain the catalyst with the amorphous ruthenium boride/crystalline ruthenium nanoparticles uniformly loaded on the porous carbon.
6. The preparation method of the porous carbon supported amorphous/crystalline ruthenium-based high-efficiency hydrogen evolution catalyst according to claim 5, characterized in that: in the step 2), the dispersion medium is deionized water or ethanol or pentane or n-hexane.
7. The method for preparing the amorphous/crystalline synergistic ruthenium-based high-efficiency hydrogen evolution catalyst according to claim 5, characterized in that: in the step 3), the protective gas atmosphere is an inert gas (argon or nitrogen) or a mixed gas atmosphere of the inert gas and hydrogen.
8. The application of the porous carbon supported amorphous/crystalline ruthenium-based high-efficiency hydrogen evolution catalyst as claimed in any one of claims 1 to 7 in hydrogen production by water electrolysis.
9. The application of the porous carbon supported amorphous/crystalline ruthenium-based high-efficiency hydrogen evolution catalyst in hydrogen production by water electrolysis according to claim 8 is characterized in that: the catalyst is suitable for use in alkaline and acidic water electrolysis.
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