CN115852417A - Spherical Cu 2 O nanoparticle catalyst and preparation method and application thereof - Google Patents
Spherical Cu 2 O nanoparticle catalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of electrocatalysts, in particular to spherical Cu 2 O nano-particle catalyst, and a preparation method and application thereof. Dissolving copper acetate in ethanol solvent by adopting a solvothermal method to grow Cu in situ 2 O nanospheres, cu nanospheres with different particle sizes can be obtained by adjusting heating time and concentration of copper acetate 2 O nanospheres of Cu 2 The O nanospheres are loaded on commercial conductive carbon paper to obtain a series of Cu with different particle sizes 2 O nanosphere catalyst electrode. Compared with other catalysts, the Cu disclosed by the invention 2 The O nanosphere catalyst is synthesized in liquid phase by adopting a solvothermal method, and has the advantages of simple method, controllable conditions, low raw material price and good catalytic activityThe environment is non-toxic and harmless. The catalyst is applied to electrocatalysis of carbon dioxide reduction to obtain high-value products such as ethylene, ethanol and the like, and the Faraday efficiency is high and the catalytic performance is stable.
Description
Technical Field
The invention relates to the technical field of electrocatalysts, in particular to spherical Cu 2 O nano-particle catalyst, and a preparation method and application thereof.
Background
Recently, with the progress of human science and technology and the development of industry, a large amount of fossil energy has been consumed, and the fossil energy is still the largest energy consumed globally today. However, the rapid consumption of fossil energy is currently accompanied by a large amount of CO 2 Emission of CO 2 As greenhouse gases with the highest content in the atmosphere, global disasters such as global warming, sea level elevation, greenhouse effect, etc. have been caused. Therefore, how to utilize CO while making global efforts to reduce carbon emissions 2 The method for obtaining a series of high-value chemical raw materials from the carbon source is also a powerful means for solving the problems of the current energy crisis and climate environment.
Conventional CO 2 The storage technique cannot solve the problem fundamentally and CO in industrial production 2 The hydrogenation process has extremely high energy consumption due to the reaction conditions of high temperature and high pressure, and the CO is biologically reduced 2 And photocatalytic reduction of CO 2 The yield was low and not yet mature and was yet to be studied further.
Electrocatalytic CO 2 The reduction has the advantages of mild condition, simple and convenient operation, controllable reaction and the like, and more importantly, the electric energy generated by clean energy sources such as solar energy, wind energy, light energy and the like can be directly stored in the chemical energy of the product, namely CO 2 One of the best ways to recover and utilize. CO in aqueous electrolyte 2 The electrochemical reduction of (a) takes place at the cathode, and the hydrogen evolution reaction with the cathode is a competing reaction. Due to CO 2 High stability of molecule, CO 2 The reduction requires higher activation energy, and thereforeThe reaction takes place at a higher potential. With the rise of overpotential, the hydrogen evolution reaction will be more serious due to the influence of mass transfer effect, which is to CO 2 The reduction of (2) is disadvantageous. With CO 2 The reduction to products of ethylene, ethanol, methane and the like is a multi-electron transfer and multi-step process, a plurality of intermediates exist in the process, the reaction mechanism is complex, and the CO is generated 2 The reduction results in a mixture of multi-valent carbon-containing compounds. So how to prepare the catalyst with high efficiency, stability and good product selectivity is electrochemical reduction of CO 2 Is a key factor of (1).
CO of current research 2 The electrochemically reduced metals are mainly concentrated in the transition metal region and can be classified into the following three categories according to product selectivity: (1) formic acid selective metals (e.g., sn, pb, bi, in, etc.) represented by the following transition metals; (2) CO selective metals (e.g., au, ag, pd, zn, etc.) represented by noble metals; (3) can remove CO 2 Metal (Cu) reduced to one-to-many carbon products such as hydrocarbons, alcohols, etc. The Cu-based catalyst is the only current density CO reported to be applicable to industrialization 2 Electrochemical reduction into some high-value chemical raw materials (such as CH) 4 、C 2 H 4 、CH 3 OH、C 2 H 5 OH, etc.). In particular C 2 H 4 As a basic raw material in petrochemical industry, a product with higher value can be obtained by processes such as hydration, polymerization, chlorination and the like. It can be seen that a Cu-based catalyst was developed for CO 2 Solving the problem of the existing CO by electrochemical reduction to obtain a multi-carbon product 2 The method has good method for large discharge amount.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides spherical Cu 2 O nano-particle catalyst, its preparation and application, dissolving copper acetate in alcohol solvent by solvothermal method to grow Cu in situ 2 O nanosphere catalyst for solving CO 2 The electrocatalytic reduction obtains a multi-carbon product.
In order to solve the technical problems, the invention provides the following technical scheme:
in order to achieve the purpose, the technical scheme adopted by the invention is as follows:
it is a first object of the present invention to provide spherical Cu 2 The preparation method of the O nanoparticle catalyst comprises the following steps:
s1, dissolving copper acetate in absolute ethyl alcohol, and mixing and stirring to obtain a catalyst synthesis stock solution;
s2, transferring the catalyst synthesis stock solution obtained in the step S1 into a polytetrafluoroethylene reaction kettle for heating, and naturally cooling to room temperature after heating to obtain a solid-liquid mixture;
s3, centrifuging the solid-liquid mixture obtained in the S2, washing the centrifugally separated solid for 3-5 times by using absolute ethyl alcohol, and drying to obtain spherical Cu 2 An O nanoparticle catalyst.
Further, in S1, the mass-to-volume ratio (g/mL) of the copper acetate to the absolute ethyl alcohol is 1:130-170.
Further, in S1, ultrasonic is used for dissolving for 15-30min.
Further, in S2, the heating is to place the reaction kettle in an oven at 100-120 ℃ for heating for 8-12h.
Furthermore, in S3, the centrifugal speed is 10000-12000rpm, and the time is 2-4min.
Further, in S3, the drying is heating for 1-2h in a vacuum drying oven at 45-55 ℃.
It is a second object of the present invention to provide spherical Cu 2 An O nanoparticle catalyst.
The third object of the present invention is to provide a spherical Cu 2 The application of the O nanoparticle catalyst in electrocatalytic reduction of carbon dioxide.
Further, spherical Cu is loaded 2 Commercial conductive carbon paper of O nanoparticle catalyst is used as a working electrode, a high-purity graphite rod is used as a counter electrode, ag/AgCl is used as a reference electrode, and an electrolyte is 0.5M KHCO 3 Introducing CO into the solution in H-type electrolytic cell at constant voltage of-1.6V 2 And electrolyzing to obtain a multi-carbon product.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts a solvothermal method to synthesize spherical Cu 2 The O nano-particle catalyst has the advantages of simple synthesis method, no toxicity and harm to the environment of raw materials, controllable conditions and low price.
2. The catalyst obtained by the invention has high efficiency, high selectivity and high stability, and particularly, the Faraday efficiency of a multi-carbon product (ethylene and ethanol) can reach 58.6 percent, which is the future CO 2 The industrial production of the electrocatalytic reduction provides the possibility.
3. Spherical Cu 2 The O nano-particle catalyst is prepared by in-situ growth in ethanol liquid, and spherical Cu with specific size is obtained by effectively regulating and controlling the concentration of raw materials in the ethanol solution, the time required by the heating process and other conditions 2 An O nanoparticle catalyst. The catalyst is used for CO 2 In terms of electrochemical reduction performance, the nano-scale particle size enables the catalyst to have a larger active specific surface area and provide abundant catalytic active sites. XRD shows that the prepared spherical Cu 2 The O nano-particles take a (111) crystal face as a main component, and the specific crystal face solves the problem of electrocatalysis of CO 2 The problem of poor selectivity in the process is solved, and the Faraday efficiency of the multi-carbon product in the conversion process is obviously improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 shows spherical Cu prepared in example 1 of the present invention 2 A scanning electron micrograph of the O nanoparticle catalyst;
FIG. 2 shows spherical Cu prepared in example 1 of the present invention 2 An X-ray crystal diffraction pattern of the O nanoparticle catalyst;
FIG. 3 is a linear scanning voltammogram of the electrocatalytic reduction of carbon dioxide in test example 1;
FIG. 4 shows electrocatalytic reduction in test example 1Reduction of CO at different potentials in the presence of carbon dioxide 2 Generating a faraday efficiency map of the multi-carbon product;
FIG. 5 is a graph showing the stability of electrocatalytic reduction of carbon dioxide in test example 2.
Detailed Description
The experimental procedures in the following examples are conventional unless otherwise specified, and the starting materials and reagents used in the present invention are ordinary commercial products and are commercially available.
The technical features and characteristics of the present invention are described in detail by the following embodiments, which are not intended to limit the scope of the present invention.
The technical solution of the present invention is further described in detail with reference to the accompanying drawings (fig. 1-5) and the detailed description.
Example 1: prepared spherical Cu 2 O nanoparticle catalyst
Spherical Cu 2 The preparation of the O nanoparticle catalyst comprises the following steps:
s1, adding 200mg of copper acetate into 30mL of absolute ethyl alcohol, performing ultrasonic treatment for 20min until the copper acetate is completely dissolved to form a blue-green solution, and mixing and stirring to obtain a catalyst synthesis stock solution;
s2, transferring the catalyst synthesis stock solution obtained in the step S1 to a 50mL polytetrafluoroethylene reaction kettle, heating at 110 ℃ for 10h, and naturally cooling to room temperature after heating to obtain a solid-liquid mixture;
s3, mixing the solid-liquid mixture obtained in the S2 at 11000rpm, centrifuging for 3min, washing the centrifugally separated solid for 3 times by using absolute ethyl alcohol, and drying in a vacuum drying oven at 50 ℃ to obtain spherical Cu 2 An O nanoparticle catalyst.
And (3) carrying out morphology characterization on the prepared catalyst, and analyzing the structure. FIG. 1 shows spherical Cu 2 Scanning electron microscopy and elemental analysis plots of O nanoparticle catalysts. As shown in FIG. 1, the catalyst particles have a spherical morphology of about 100nm, and a large number of particles are agglomerated to form a sheet-like structure, which may be CO 2 Provides a high active area. The elemental analysis of FIG. 1 shows that only Cu and O are present in the catalystBoth elements were uniformly distributed, indicating that the phases of the synthesized catalyst were homogeneous.
Prepared spherical Cu 2 And (4) carrying out X-ray crystal diffraction test on the O nanoparticle catalyst, and analyzing the crystal form of the catalyst. FIG. 2 shows spherical Cu 2 X-ray crystal diffraction spectrogram of O nanoparticle catalyst is shown in figure, and the catalyst is cuprite type Cu with (111) crystal face as the main component 2 O is accompanied by the (200) and (110) plane.
Example 2: prepared spherical Cu 2 O nanoparticle catalyst
Spherical Cu 2 The preparation of the O nanoparticle catalyst comprises the following steps:
s1, adding 200mg of copper acetate into 28mL of absolute ethyl alcohol, performing ultrasonic treatment for 30min until the copper acetate is completely dissolved to form a blue-green solution, and mixing and stirring to obtain a catalyst synthesis stock solution;
s2, transferring the catalyst synthesis stock solution obtained in the step S1 to a 45mL polytetrafluoroethylene reaction kettle, heating at 120 ℃ for 12h, and naturally cooling to room temperature after heating to obtain a solid-liquid mixture;
s3, mixing the solid-liquid mixture obtained in the S2 at 10000rpm, centrifuging for 4min, washing the centrifugally separated solid for 4 times by using absolute ethyl alcohol, and drying in a vacuum drying oven at 55 ℃ to obtain spherical Cu 2 An O nanoparticle catalyst.
Example 3: prepared spherical Cu 2 O nanoparticle catalyst
Spherical Cu 2 The preparation of the O nanoparticle catalyst comprises the following steps:
s1, adding 200mg of copper acetate into 32mL of absolute ethyl alcohol, performing ultrasonic treatment for 15min until the copper acetate is completely dissolved to form a blue-green solution, and mixing and stirring to obtain a catalyst synthesis stock solution;
s2, transferring the catalyst synthesis stock solution obtained in the step S1 to a 55mL polytetrafluoroethylene reaction kettle, heating at 100 ℃ for 11h, and naturally cooling to room temperature after heating to obtain a solid-liquid mixture;
s3, mixing the solid-liquid mixture obtained in the S2 at 12000rpm, centrifuging for 2min, washing the centrifugally separated solid for 3 times by using absolute ethyl alcohol, and drying in a vacuum drying oven at 45 ℃ to obtain the productSpherical Cu 2 An O nanoparticle catalyst.
Test example 1: electrocatalytic reduction of carbon dioxide test
5mg of the catalyst obtained in example 1 was dispersed in 5mL of isopropanol, dissolved by sonication, 40. Mu.L of a 5% nafion D520 solution was added thereto until completely dispersed to obtain a catalyst dispersion, and 1mL of the catalyst dispersion was dropped on a 1X 1cm scale 2 And drying the commercial conductive carbon paper by flowing nitrogen to prepare the working electrode for electrocatalytic reduction of carbon dioxide.
In order to test the catalytic performance of the catalyst, a linear sweep voltammetry test is carried out on a working electrode, a high-purity graphite rod is used as a counter electrode, ag/AgCl is used as a reference electrode, and 0.5M KHCO is added 3 The solution is electrolyte, and in H-type electrolytic cell, ar and CO are respectively 2 The test was performed under the conditions. As shown in FIG. 3, the working electrode is at CO at the same potential 2 The current density at the turn-on was significantly greater than that at the turn-on of Ar, indicating that the catalyst had good electrocatalytic CO 2 Performance of reduction.
And assembling the working electrode in an H-shaped electrolytic cell to perform carbon dioxide electroreduction tests at different potentials. The test uses a high-purity graphite rod as a counter electrode, ag/AgCl as a reference electrode and 0.5M KHCO 3 The solution is an electrolyte. 30minCO is introduced before electrolysis 2 Making the electrolyte CO 2 Saturation, followed by electrocatalytic performance tests at-0.80V, -1.00V, -1.20V, -1.40V, -1.60V, -1.80V, -2.00V (both relative to the reversible hydrogen electrode) potentials, yielded polycarbonic products (ethylene, ethanol) with faradaic efficiencies of 27.3%,35.6%,47.8%,52.6%,58.6%,50.0%,43.3%, respectively, with the product distributions at the potentials shown in fig. 4, showing that the maximum value of the faradaic efficiency of the polycarbonic product reached 58.6% at-1.60V.
Test example 2: stability test of electrocatalytic reduction of carbon dioxide
5mg of the catalyst obtained in example 1 was dispersed in 5mL of isopropanol, dissolved by sonication, 40. Mu.L of a 5% nafion D520 solution was added thereto until completely dispersed to obtain a catalyst dispersion, and 1mL of the catalyst dispersion was dropped on a 1X 1cm scale 2 Electrocatalysis prepared by blowing flowing nitrogen on commercial conductive carbon paperA working electrode for reducing carbon dioxide.
And assembling the working electrode in an H-shaped electrolytic cell to perform a carbon dioxide electroreduction stability test. The test uses a high-purity graphite rod as a counter electrode, ag/AgCl as a reference electrode and 0.5M KHCO 3 The solution is an electrolyte. Introducing CO for 30min before electrolysis 2 Making the electrolyte CO 2 Saturation, and then carrying out the electrocatalytic stability performance test of the catalyst for 7h at a potential of-1.60V. As shown in the data of fig. 5, the catalyst-loaded working electrode did not significantly decay for 7h of current density at 25 mA.
While the preferred embodiments of this patent have been described in detail, this patent is not limited to the embodiments described above, and variations and modifications in other forms may occur to those skilled in the art, within the knowledge of the person skilled in the art. This need not be, nor should it be exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (9)
1. Spherical Cu 2 The preparation method of the O nanoparticle catalyst is characterized by comprising the following steps of:
s1, dissolving copper acetate in absolute ethyl alcohol, mixing and stirring to obtain a catalyst synthesis stock solution;
s2, transferring the catalyst synthesis stock solution obtained in the step S1 into a polytetrafluoroethylene reaction kettle for heating, and naturally cooling to room temperature after heating to obtain a solid-liquid mixture;
s3, centrifuging the solid-liquid mixture obtained in the S2, washing the centrifugally separated solid for 3-5 times by using absolute ethyl alcohol, and drying to obtain spherical Cu 2 An O nanoparticle catalyst.
2. The method according to claim 1, wherein in S1, the mass-to-volume ratio (g/mL) of copper acetate to absolute ethyl alcohol is 1:130-170.
3. The method according to claim 1, wherein the dissolving in S1 is performed with ultrasound for 15 to 30min.
4. The preparation method according to claim 1, wherein in S2, the heating is carried out by placing the reaction kettle in an oven at 100-120 ℃ for 8-12h.
5. The method according to claim 1, wherein in S3, the centrifugation is carried out at 10000 to 12000rpm for 2 to 4 minutes.
6. The preparation method according to claim 1, wherein in S3, the drying is heating in a vacuum drying oven at 45-55 ℃ for 1-2h.
7. Spherical Cu produced by the production method according to any one of claims 1 to 6 2 An O nanoparticle catalyst.
8. Spherical Cu produced by the production method according to any one of claims 1 to 6 2 The application of the O nanoparticle catalyst in electrocatalytic reduction of carbon dioxide.
9. Use according to claim 8, characterized in that spherical Cu is loaded 2 Commercial conductive carbon paper of O nanoparticle catalyst is used as a working electrode, a high-purity graphite rod is used as a counter electrode, ag/AgCl is used as a reference electrode, and an electrolyte is 0.5M KHCO 3 Introducing CO into the solution in H-type electrolytic cell at constant voltage of-1.6V 2 And electrolyzing to obtain a multi-carbon product.
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