CN112978783A - Cuprous oxide nano material, preparation method and application thereof - Google Patents
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Abstract
The invention provides a Cu2O nano material consisting of a hollow core and Cu coated on the surface of the hollow core2O shell composition, said Cu2The O shell is 1-3 layers and is loose and porous. The present application also provides Cu2The preparation method of the O nano material comprises the following steps: in Cu2SO4Adding 1-3 times of hydrazine hydrate solution into the precursor solution, and curing to obtain Cu2And (4) O nano material. The present application also provides Cu2The application of the O nano catalyst in carbon dioxide electroreduction reaction. Cu provided by the present application2O nano material throughMultilayer Cu2The O shell has mass transfer effect on the CO reaction intermediate and inhibits desorption of the CO reaction intermediate, thereby effectively improving the C-C coupling probability and promoting carbon dioxide electroreduction to C2+ selectivity of the product.
Description
Technical Field
The invention relates to the technical field of energy catalysis, in particular toCu2O nano material, preparation method and application thereof.
Background
The large development and consumption of fossil energy continuously increase the carbon dioxide content in the environment, and the greenhouse effect caused by the carbon dioxide content causes global warming, thereby causing a series of ecological environmental problems. Thus, mitigating the continuing increase in atmospheric carbon dioxide concentration is an important issue that is currently urgently needed to be solved worldwide.
The carbon dioxide electroreduction technology can reduce the content of carbon dioxide in the environment, relieve the greenhouse effect caused by the carbon dioxide electroreduction technology, can convert the carbon dioxide into a chemical product with higher utilization value, and is a technology with important application prospect and research significance. However, in the process of carbon dioxide reduction, the hydrogen evolution reaction in the water phase has a lower reduction potential, so that the selectivity of the product of electrocatalytic carbon dioxide reduction is poor, and the main problem of restricting the practical application of the product is solved; in addition, products of electrocatalytic carbon dioxide reduction are numerous, including carbon monoxide, formic acid, and C, which has high chemical value2+Products (ethylene, ethanol) and the like.
Limited to the adsorption characteristic determined by an electronic structure, the Cu-based catalyst is the only catalyst which can realize high-efficiency C-C coupling to obtain C2+ high value-added chemical material systems. How to improve the p-C simultaneously on the basis of inhibiting the hydrogen evolution reaction2The selectivity of + products is currently the main research target for carbon dioxide electrocatalysts. The common idea of modifying the Cu-based catalyst is to optimize an electronic structure through surface regulation and stabilize the adsorption of a Cu surface to a CO intermediate, thereby promoting C-C coupling and promoting C2+ selectivity of the product. However, the regulation and control thought of limiting the mass transfer process of the CO intermediate to increase the C-C coupling probability by designing the three-dimensional structure of the catalyst is rarely reported.
Disclosure of Invention
The invention aims to provide Cu2O nano material and preparation method thereof, and Cu provided by application2The O nano material is used as a catalyst for carbon dioxide electroreduction, and can improve the carbon dioxide electroreduction pair C2+ selectivity of the product.
In view of the above, the present application provides a Cu2O nano material consisting of a hollow core and Cu coated on the surface of the hollow core2O shell composition, said Cu2The O shell is 1-3 layers and is loose and porous.
Preferably, the Cu2The grain diameter of the O nano material is 200-300 nm.
The application also provides the Cu2The preparation method of the O nano material comprises the following steps:
in Cu2SO4Adding 1-3 times of hydrazine hydrate solution into the precursor solution, and curing to obtain Cu2And (4) O nano material.
Preferably, Cu is obtained2The specific process of the O nano material is as follows:
in Cu2SO4Adding hydrazine hydrate solution into the precursor solution, stirring and curing to obtain Cu2O nanomaterial, Cu of said nanomaterial2The O shell is 1 layer.
Preferably, Cu is obtained2The specific process of the O nano material is as follows:
in Cu2SO4Adding a hydrazine hydrate solution into the precursor solution, stirring and curing the solution, then adding the hydrazine hydrate solution again, stirring and curing the solution again to obtain the Cu2O nanomaterial, Cu of said nanomaterial2The O shell is 2 layers.
Preferably, Cu is obtained2The specific process of the O nano material is as follows:
in Cu2SO4Adding a hydrazine hydrate solution into the precursor solution, stirring, curing, adding the hydrazine hydrate solution again, stirring again, curing, adding the hydrazine hydrate solution for three times, stirring for three times, curing to obtain Cu2O nanomaterial, Cu of said nanomaterial2The O shell is 3 layers.
Preferably, the Cu2SO4The preparation process of the precursor solution comprises the following specific steps:
adding polyvinylpyrrolidone to CuSO at normal temperature4Stirring the solution to obtain Cu2SO4And (3) precursor solution.
Preferably, the CuSO4CuSO in solution4And the molar ratio of polyvinylpyrrolidone to hydrazine hydrate added once is 1: (0.005-0.02): (0.01-0.04).
Preferably, the method further comprises washing treatment and drying treatment after the curing;
the washing treatment specifically comprises the following steps: performing centrifugal separation on a product obtained after stirring, performing ultrasonic washing on the product obtained by centrifugal separation by using a mixed solution of ethanol and water, and then continuously performing centrifugal separation, wherein the ultrasonic washing time is 1-2 min each time, the rotating speed of each centrifugal separation is 7000-8000 rpm, and the time of each centrifugal separation is 3-5 min;
the drying treatment is vacuum drying, the temperature is 50-100 ℃, and the time is 12-24 hours.
The application also provides the Cu2O nano material or Cu prepared by the preparation method2The application of the O nano material in carbon dioxide electroreduction reaction.
The present application provides a Cu2O nano material consisting of a hollow core and Cu coated on the surface of the hollow core2O shell composition, said Cu2The O shell is 1-3 layers and is loose and porous. The present application also provides Cu2A preparation method of O nano material. The present application is through multi-layer Cu2The mass transfer limitation of the O shell to the CO improves the concentration of the CO, so that the desorption balance of CO is shifted to the left, and the desorption of the intermediate CO is inhibited, thereby effectively improving the rate of the C-C coupling agent and improving the carbon dioxide electro-reduction pair C2+ selectivity of the product.
Drawings
FIG. 1 shows Cu obtained in examples 1, 2 and 3 of the present invention2Transmission electron microscope images of the O nano catalyst;
FIG. 2 shows Cu obtained in examples 1, 2 and 3 of the present invention2X-ray electron diffraction images of O nanocatalysts;
FIG. 3 shows Cu obtained in examples 1, 2 and 3 of the present invention2X-ray photoelectron Auger spectrum of O nano catalyst Cu;
FIG. 4 is a drawing showingExamples, examples 2 and 3 electrocatalytic carbon dioxide reduction at different voltages C2+ product with C1The ratio of the products;
fig. 5 is a graph of performance stability of examples 1, 2 and 3 over a constant potential test of 8 h.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
The embodiment of the invention discloses Cu2O nano material consisting of a hollow core and Cu coated on the surface of the hollow core2O shell composition, said Cu2The O shell is 1-3 layers and is loose and porous, in other words, the Cu is2The O nano material is loose and porous Cu with 1-3 layers2And (3) O shell coated hollow nano material. More specifically, the Cu2The O shell can be 1 layer, 2 layers or 3 layers; multiple layers of Cu with increasing number of catalyst layers2The enrichment effect of the O shell on the CO reaction intermediate is gradually increased, and the desorption of the CO reaction intermediate is inhibited, so that the electrocatalytic CO is effectively improved2Reduction reaction pair C2+ selectivity of the product.
In the present application, the Cu2The grain diameter of the O nano material is 200-300 nm. The Cu2If the particle size of the O nano material is too large, mass transfer limitation is too strong, and the performance is poor.
The application also provides the Cu2The preparation method of the O nano material comprises the following steps:
in Cu2SO4Adding 1-3 times of hydrazine hydrate solution into the precursor solution, and curing to obtain Cu2And (4) O nano material.
The method specifically comprises the following steps: firstly, preparing CuSO4Adding a hydrazine hydrate solution for 1-3 times into the precursor solution, and curing to obtain Cu with different layers2O nano catalyst; more specifically, in Cu2SO4Precursor ofAdding hydrazine hydrate solution into the solution, stirring and curing to obtain Cu2O nanomaterial, Cu of said nanomaterial2The O shell is 1 layer;
in Cu2SO4Adding a hydrazine hydrate solution into the precursor solution, stirring and curing the solution, then adding the hydrazine hydrate solution again, stirring and curing the solution again to obtain the Cu2O nanomaterial, Cu of said nanomaterial2The O shell is 2 layers;
in Cu2SO4Adding a hydrazine hydrate solution into the precursor solution, stirring, curing, adding the hydrazine hydrate solution again, stirring again, curing, adding the hydrazine hydrate solution for three times, stirring for three times, curing to obtain Cu2O nanomaterial, Cu of said nanomaterial2The O shell is 3 layers.
In the present application, the Cu2SO4The preparation process of the precursor solution comprises the following specific steps:
adding polyvinylpyrrolidone to CuSO at normal temperature4Stirring the solution to obtain Cu2SO4And (3) precursor solution.
During the last preparation, the CuSO4CuSO in solution4And the molar ratio of polyvinylpyrrolidone to hydrazine hydrate added once is 1: (0.005-0.02): (0.01-0.04), more specifically, CuSO4And the molar ratio of polyvinylpyrrolidone to hydrazine hydrate added once is 1: 0.01: 0.02. the curing time is 30-60 min. In the curing process, the polyvinylpyrrolidone is coated on the surface of the cuprous oxide to limit the growth of the cuprous oxide, so that the purpose of controlling the appearance is achieved; more specifically, in the curing process, the cuprous oxide nanoparticles reduced by hydrazine hydrate are reconstructed in appearance and are initially assembled into loose spherical particles, the spherical particles are divided into an inner layer and an outer layer, the inner sphere is small in size, large in specific surface area and high in surface energy, and therefore the inner sphere is gradually dissolved and deposited to the outer layer, and the outer sphere is shrunk to form a spherical shell under the double effects of thermodynamic driving and surface coating agent guiding. The mechanism of formation of each subsequent curing process is the same.
After each curing, washing and drying the obtained product; the washing treatment specifically comprises the following steps: performing centrifugal separation on a product obtained after stirring, performing ultrasonic washing on the product obtained by centrifugal separation by using a mixed solution of ethanol and water, and then continuously performing centrifugal separation, wherein the ultrasonic washing time is 1-2 min each time, the rotating speed of each centrifugal separation is 7000-8000 rpm, and the time of each centrifugal separation is 3-5 min; the drying treatment is vacuum drying, the temperature is 50-100 ℃, and the time is 12-24 hours.
The cure described herein is an oswald cure, a phenomenon that can be observed in solid or hydrosol, which describes the change in a heterogeneous structure over time: smaller crystals or sol particles in the solute are dissolved and re-deposited onto larger crystals or sol particles; the driving force of the process is the reduction of the surface energy.
The application also provides the Cu2The application of the O nano material in carbon dioxide electroreduction reaction.
Cu obtained by multiple Oswald ripening2The O nano catalyst has mild preparation conditions, simple procedures, low cost and environmental protection, and the obtained Cu is2The O nano catalyst has 1-3 layers of loose porous Cu2And an O shell coated hollow structure. With a single layer of Cu2Compared with the nano catalyst with O shell, the nano catalyst has three layers of Cu2The O-shell nano-catalyst is prepared by performing carbon dioxide electroreduction on the O-shell nano-catalyst in neutral electrolyte at an overpotential of-0.88V2The Faraday efficiency of the + product can reach 77%, single-layer Cu2C of O-shell nano-catalyst2The Faraday efficiency of the + product was 40%, double layer Cu2C of O-shell nano-catalyst2The Faraday efficiency of the + product was 62%, which was shown with Cu2The enrichment effect on CO reaction intermediates is gradually increased by increasing the number of O shells, so that the carbon dioxide electro-reduction pair C is improved2+ selectivity of the product. In addition, after 8h potentiostatic test, three layers of Cu are provided2The performance of the O-shell nano catalyst is not obviously attenuated basically, and the stability of the catalyst prepared by the method is further shown to be good.
For further understanding of the present invention, the following combinations are madeExample of Cu provided by the invention2The O nanocatalyst and its applications are illustrated in detail, and the scope of the present invention is not limited by the following examples.
The various starting materials used in the following examples are all commercially available products known in the art unless otherwise specified.
Example 1
300mg of polyvinylpyrrolidone (PVP) was added to 30mL of 0.01M CuSO at room temperature4In the solution, under the condition of magnetic stirring at 300rpm, the solid is completely dissolved to obtain CuSO4Precursor solution; then to CuSO4Adding 10 mu L of hydrazine hydrate solution with volume fraction of 85% into the precursor solution, and continuing to perform magnetic stirring at normal temperature for 30 min;
and (2) carrying out centrifugal separation on the reaction product, carrying out ultrasonic washing on the product obtained by centrifugal separation by using a mixed solution of ethanol and water, then continuing carrying out centrifugal separation, wherein the ultrasonic washing time is 1min each time, the rotating speed of each centrifugal separation is 7000rpm, the centrifugal separation time is 3min each time, carrying out vacuum drying treatment on the obtained reaction product after carrying out centrifugal washing three times, the vacuum drying temperature is 60 ℃, and the vacuum drying time is 12 h.
After detection, the Cu obtained in this example2The O nano catalyst is single-layer porous Cu2O-coated hollow sphere structure.
Example 2
300mg of polyvinylpyrrolidone (PVP) was added to 30mL of 0.01M CuSO at room temperature4In the solution, under the condition of magnetic stirring at 300rpm, the solid is completely dissolved to obtain CuSO4Precursor solution; then to CuSO4Adding 10 mu L of hydrazine hydrate solution with volume fraction of 85% into the precursor solution, and continuing to carry out magnetic stirring at normal temperature; stirring for 30min, adding 10 μ L of 85% hydrazine hydrate solution, and magnetically stirring at room temperature for 30 min;
and after stirring, centrifugally separating a reaction product, ultrasonically washing the product obtained by centrifugal separation by using a mixed solution of ethanol and water, then continuously carrying out centrifugal separation, wherein the ultrasonic washing time is 1min each time, the rotating speed of each centrifugal separation is 7000rpm, the centrifugal separation time is 3min each time, carrying out vacuum drying treatment on the obtained reaction product after three times of centrifugal washing, and the vacuum drying temperature is 60 ℃ and the vacuum drying time is 12 h.
After detection, the Cu obtained in this example2The O nano catalyst is double-layer porous Cu2O-coated hollow sphere structure.
Example 3
300mg of polyvinylpyrrolidone (PVP) was added to 30mL of 0.01M CuSO at room temperature4In the solution, under the condition of magnetic stirring at 300rpm, the solid is completely dissolved to obtain CuSO4Precursor solution; then to CuSO4And adding 10 mu L of hydrazine hydrate solution with volume fraction of 85% into the precursor solution, and continuing to perform magnetic stirring at the normal temperature. Stirring for 30min, adding 10 μ L of 85% hydrazine hydrate solution, and magnetically stirring at room temperature; stirring for 30min, adding 10 μ L of 85% hydrazine hydrate solution, and magnetically stirring at room temperature for 30 min;
and after stirring, centrifugally separating a reaction product, ultrasonically washing the product obtained by centrifugal separation by using a mixed solution of ethanol and water, then continuously carrying out centrifugal separation, wherein the ultrasonic washing time is 1min each time, the rotating speed of each centrifugal separation is 7000rpm, the centrifugal separation time is 3min each time, carrying out vacuum drying treatment on the obtained reaction product after three times of centrifugal washing, and the vacuum drying temperature is 60 ℃ and the vacuum drying time is 12 h.
After detection, the Cu obtained in this example2The O nano catalyst is three-layer porous Cu2O-coated hollow sphere structure.
From FIG. 1, it can be seen that Cu2The grain size of the O nano catalyst is 200-300 nm.
As can be seen from FIG. 2, Cu obtained by the method2The O nano catalyst has uniform phase formation and is in good correspondence with a standard card.
From the peak position in fig. 3, it can be known that the valence states of Cu in the obtained nano catalyst are all + 1.
Example 4Cu2Catalytic performance test of O nano catalyst
Cu obtained in example 3 of the present invention2Test of catalytic performance of O nano catalyst for carbon dioxide electroreduction reaction
12mg of Cu obtained in example 32Mixing O nanometer catalyst with 10 μ L perfluorosulfonic acid resin and 1mL isopropanol, coating on 2cm × 2cm carbon Gas Diffusion Layer (GDL), drying, cutting out 1cm × 2cm carbon paper as working electrode, and adding 0.5M potassium bicarbonate (KHCO)3) One Cu obtained in example 3 was measured in a flow cell using the solution as an electrolyte2The activity of the O nano catalyst as a carbon dioxide electro-reduction catalyst; CO in the test procedure2The flow rate is kept at 50sccm, and the flow rate of the potassium bicarbonate solution is kept at 50 mL/h; adopting a constant voltage method, and adopting-0.65V, -0.79V, -0.85V, -0.88V and-0.91V as test voltages relative to the reversible hydrogen electrode; and detecting a reaction gas-phase product by gas chromatography, detecting a liquid-phase product by nuclear magnetic resonance hydrogen spectrum, calculating the coulomb amount corresponding to the product concentration, and obtaining data such as selectivity and activity of the catalysis according to the total coulomb amount recorded by an electrochemical workstation.
Referring to FIG. 4, example 1, example 2 and example 3 are shown for electrocatalytic carbon dioxide reduction C at different voltages2+ product with C1Product ratios, as shown in FIG. 4, were measured with porous Cu at each test voltage2Increasing the number of O layers, Cu2C for electrocatalysis of carbon dioxide reduction by O nano catalyst2+ product with C1The ratio of the products is increased, and is shown to be along with Cu2The enrichment effect on CO reaction intermediates is gradually increased by increasing the number of O shells, so that the carbon dioxide electro-reduction pair C is improved2+ selectivity of the product. In addition, with reference to FIG. 5, three layers of Cu were tested for 8h potentiostatic testing2The performance of the O-shell nano catalyst is not obviously attenuated basically, and further shows that the catalyst prepared by the method has good stability and can be recycled after long-time catalytic reaction。
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. Cu2O nano material consisting of a hollow core and Cu coated on the surface of the hollow core2O shell composition, said Cu2The O shell is 1-3 layers and is loose and porous.
2. Cu according to claim 12O nanomaterial characterized in that the Cu2The grain diameter of the O nano material is 200-300 nm.
3. Cu according to claim 12The preparation method of the O nano material comprises the following steps:
in Cu2SO4Adding 1-3 times of hydrazine hydrate solution into the precursor solution, and curing to obtain Cu2And (4) O nano material.
4. The production method according to claim 3, wherein Cu is obtained2The specific process of the O nano material is as follows:
in Cu2SO4Adding hydrazine hydrate solution into the precursor solution, stirring and curing to obtain Cu2O-nanomaterialCu of the nanomaterial2The O shell is 1 layer.
5. The production method according to claim 3, wherein Cu is obtained2The specific process of the O nano material is as follows:
in Cu2SO4Adding a hydrazine hydrate solution into the precursor solution, stirring and curing the solution, then adding the hydrazine hydrate solution again, stirring and curing the solution again to obtain the Cu2O nanomaterial, Cu of said nanomaterial2The O shell is 2 layers.
6. The production method according to claim 3, wherein Cu is obtained2The specific process of the O nano material is as follows:
in Cu2SO4Adding a hydrazine hydrate solution into the precursor solution, stirring, curing, adding the hydrazine hydrate solution again, stirring again, curing, adding the hydrazine hydrate solution for three times, stirring for three times, curing to obtain Cu2O nanomaterial, Cu of said nanomaterial2The O shell is 3 layers.
7. The production method according to any one of claims 4 to 6, wherein the Cu is2SO4The preparation process of the precursor solution comprises the following specific steps:
adding polyvinylpyrrolidone to CuSO at normal temperature4Stirring the solution to obtain Cu2SO4And (3) precursor solution.
8. The method of claim 7, wherein the CuSO is applied to a substrate4CuSO in solution4And the molar ratio of polyvinylpyrrolidone to hydrazine hydrate added once is 1: (0.005-0.02): (0.01-0.04).
9. The method according to claim 3, wherein the aging further comprises a washing treatment and a drying treatment;
the washing treatment specifically comprises the following steps: performing centrifugal separation on a product obtained after stirring, performing ultrasonic washing on the product obtained by centrifugal separation by using a mixed solution of ethanol and water, and then continuously performing centrifugal separation, wherein the ultrasonic washing time is 1-2 min each time, the rotating speed of each centrifugal separation is 7000-8000 rpm, and the time of each centrifugal separation is 3-5 min;
the drying treatment is vacuum drying, the temperature is 50-100 ℃, and the time is 12-24 hours.
10. Cu according to any one of claims 1 to 22O nanomaterial or Cu prepared by the preparation method of any one of claims 3 to 92The application of the O nano material in carbon dioxide electroreduction reaction.
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