CN115595623A - Electrocatalyst and preparation method and application thereof - Google Patents
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- CN115595623A CN115595623A CN202211609076.5A CN202211609076A CN115595623A CN 115595623 A CN115595623 A CN 115595623A CN 202211609076 A CN202211609076 A CN 202211609076A CN 115595623 A CN115595623 A CN 115595623A
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Abstract
The invention discloses an electrocatalyst, a preparation method and application thereof, belonging to the field of catalysts, wherein the preparation method comprises the following steps: (1) preparing a spherical silicon dioxide template; (2) preparing a Co/NC precursor; (3) Co/Co 9 S 8 And (3) preparing an electrocatalyst. Meanwhile, the invention discloses Co/Co prepared by the preparation method 9 S 8 An electrocatalyst and its application in electrocatalytic cracking of alkaline solution and alkaline seawater for hydrogen production. Co/Co prepared by the invention 9 S 8 The electrocatalyst combines hydrogen protons in alkaline solution and alkaline seawater into hydrogen gas, has fast reaction kinetics, and both can be kept stable for a long time. In addition, the present inventionThe preparation method of the electrocatalyst is simple, short in time consumption and high in repeatability.
Description
Technical Field
The invention relates to the field of catalysts, in particular to Co/Co 9 S 8 An electrocatalyst, a preparation method and an application thereof.
Background
The use of fossil energy brings a series of problems such as energy shortage and environmental pollution, and a clean and continuous renewable energy source is urgently needed to replace the traditional fossil energy source. Among them, hydrogen energy is a clean, efficient and sustainable green energy, and attracts attention due to a series of advantages of high weight energy density, zero carbon emission, large abundance of earth elements, and the like. The water electrolysis can realize an important way of green hydrogen production. However, the shortage of fresh water resources leads the water electrolysis attention to be changed to seawater resources, the seawater resources are rich and account for 97 percent of the total water resources in the world, the ion conductivity is high, and the low-cost large-scale hydrogen production and the production of high-purity hydrogen are favorably realized. However, the current electro-catalyst shows poor performance in seawater, i.e. high overpotential and poor stability compared with ultrapure water as electrolyte, which brings great challenge to the preparation of hydrogen from seawater.
Transition metal-based catalysts have attracted considerable attention because of their high earth abundance, low cost, and high activity, and have been studied intensively in recent years as low-cost substitutes for noble metal-based catalysts. Among them, cobalt-based sulfides are attractive as potential electrode materials due to their good electrochemical activity, high thermal conductivity, and low cost compared to other metal sulfides. But still has the problems of lacking active sites and weak mass transfer capability. The mass transfer capacity of an electrocatalyst depends mainly on its specific surface area and porous structure.
Therefore, how to provide an electrocatalyst with many active sites and strong mass transfer capability is a technical problem that needs to be solved urgently by those skilled in the art.
Disclosure of Invention
The invention aims to provide Co/Co 9 S 8 An electrocatalyst, a preparation method and an application thereof, which are used for solving the problems existing in the prior art.
In order to achieve the purpose, the invention provides the following scheme:
a preparation method of an electrocatalyst of which the chemical composition comprises Co 9 S 8 The preparation method comprises the following steps:
(1) Tetraethyl orthosilicate, ammonia water, ethanol and deionized water are mixed and then stirred for reaction, and then the mixture is centrifuged, washed and dried to obtain a spherical silicon dioxide template;
(2) Putting the spherical silicon dioxide template and cobalt nitrate hexahydrate into methanol for reaction to obtain solid powder;
(3) Dispersing the solid powder and dimethyl imidazole in methanol for continuous reaction, then stirring, heating, drying, heating for ablation, and cooling to obtain a Co/NC precursor;
(4) Dispersing the Co/NC precursor and sodium sulfide in water, and obtaining Co/Co through hydrothermal reaction 9 S 8 An electrocatalyst.
Has the advantages that: the spherical structure of the silicon dioxide template in the invention is Co/Co 9 S 8 The electrocatalyst provides excellent specific surface area, increases the load of catalyst particles, provides rich active sites, is favorable for adsorbing water molecules in alkaline solution and alkaline seawater, and accelerates the transfer and mass transfer of electrons.
Preferably, the volume ratio of the tetraethyl orthosilicate, the ammonia water, the deionized water and the ethanol in the step (1) is 3.
Has the advantages that: the concentration of ammonia water and tetraethyl orthosilicate is controlled, so that silicon dioxide nano-spheres with proper particle size can be synthesized conveniently, and the particle size of the nanospheres is 100-200nm.
Preferably, the stirring reaction temperature in the step (1) is 10-30 ℃, the stirring speed is 300-520rpm, and the time is 5h;
the washing is that deionized water and ethanol are respectively washed for 1-3 times;
the drying is vacuum drying, the temperature of the vacuum drying is 5-100 ℃, the time is 8-72 h, and the vacuum degree is 133-267 Pa.
Has the advantages that: removing impurities on the surface of the nano-spheres to obtain pure silicon dioxide nano-particles.
Preferably, the mass ratio of the spherical silica template to the cobalt nitrate hexahydrate to the methanol is 1;
the reaction temperature is 10-30 ℃, and the reaction time is 2-3 h.
Preferably, the ratio of the solid powder, the dimethyl imidazole and the methanol added in the step (3) is 1;
in the stirring and heating process, the stirring speed is 220 rpm, the heating temperature is 70 ℃, and the stirring and heating time is 45 min;
the drying is vacuum drying, the temperature of the vacuum drying is 5-100 ℃, the time is 8-72 h, and the vacuum degree is 133-267 Pa.
The heating ablation is as follows: heating to 750 ℃ at the speed of 5 ℃/min and ablating for 4h.
Has the beneficial effects that: the above conditions can enhance the acid and alkali corrosion resistance of the precursor, and obtain the carbonized product.
Preferably, the mass ratio of the Co/NC precursor, the sodium sulfide and the water in the step (4) is 1 (20-30) to 15.
Has the advantages that: according to the invention, the precursor is vulcanized under the conditions to obtain a vulcanized product.
Preferably, the hydrothermal reaction temperature in the step (4) is 120 ℃ and the time is 15 h.
Has the advantages that: the invention selects mild reaction conditions to obtain the vulcanization product.
Co/Co prepared by preparation method of electrocatalyst 9 S 8 An electrocatalyst.
Co/Co 9 S 8 The application of the electrocatalyst in electrocatalytic cracking of alkaline solution and alkaline seawater hydrogen production. The seawater hydrogen production performance of the target catalyst can be obtained.
Preferably, the working electrode is said Co/Co 9 S 8 The electro-catalyst, the reference electrode is a mercury/mercury oxide electrode, the counter electrode is a platinum sheet electrode, and the electrolyte is alkaline solution and/or alkaline seawater;
the pH value of the electrolyte is 10-14.
The test system for producing hydrogen from seawater is assembled by the components.
The invention discloses an electrocatalyst and a preparation method and application thereofPreparing a precursor in a high-temperature ablation mode, then preparing a target catalyst in a high-temperature hydrothermal mode by taking sodium sulfide as a sulfur source, and applying the target catalyst to the field of hydrogen production by electrolyzing alkaline solution and alkaline seawater. Co/Co prepared by the invention 9 S 8 The electrocatalyst has excellent catalytic performance, combines hydrogen protons into hydrogen in alkaline solution and alkaline seawater, has fast reaction kinetics, and both can keep long-term stability. In addition, co/Co in the present invention 9 S 8 The preparation method of the electrocatalyst is simple, short in time consumption and high in repeatability, and provides good technical basis and material guarantee for further popularization and application.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 shows the Co/Co prepared in example 1 9 S 8 Scanning electron microscopy of the electrocatalyst;
FIG. 2 shows Co/Co prepared in example 1 9 S 8 An X-ray diffraction pattern of the electrocatalyst;
FIG. 3 is the Co/Co ratio prepared in example 1 9 S 8 The electro-catalyst is used for cracking the seawater hydrogen production performance diagram in the alkaline seawater;
FIG. 4 shows Co/Co prepared in example 1 9 S 8 Electrocatalyst stability performance diagram.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
The starting materials used in the examples of the present invention were obtained from commercial sources.
The term "room temperature" as used in the examples of the present invention means 25. + -. 2 ℃.
Example 1
A method of preparing an electrocatalyst, comprising the steps of:
1) Dispersing tetraethyl orthosilicate and ammonia water into ethanol and deionized water, wherein the volume ratio of tetraethyl orthosilicate to ammonia water to ethanol is 3;
2) Dispersing 1g of the spherical silicon dioxide template obtained in the step 1) and 1g of cobalt nitrate hexahydrate in 15g of methanol, carrying out vacuum drying to obtain pink powder, then dispersing 1g of the pink powder and 1g of dimethyl imidazole in 15g of methanol together, carrying out stirring reaction for 45min at the temperature of 70 ℃ until a solvent is evaporated, and carrying out vacuum drying on the obtained solid to obtain a ZIF-67 precursor;
3) Placing the ZIF-67 precursor obtained in the step 2) into a tube furnace, heating to 750 ℃ at a heating rate of 5 ℃/min, keeping the temperature constant for 4h for ablation, taking out the precursor after ablation, and cooling to room temperature under natural conditions to obtain a Co/NC precursor;
4) Mixing and dispersing the Co/NC precursor obtained in the step 3) and sodium sulfide into deionized water, wherein the mass ratio of the Co/NC precursor to the sodium sulfide is 1 9 S 8 An electrocatalyst.
Obtained Co/Co 9 S 8 The scanning electron micrograph of the electrocatalyst is shown in fig. 1, and it can be seen that: synthesis ofThe catalyst has a spherical shell-shaped hollow structure;
Co/Co 9 S 8 the X-ray diffraction spectrum of the electrocatalyst is shown in FIG. 2, and it can be seen that: the target product components of the synthesis are Co and Co 9 S 8 ；
Co/Co 9 S 8 The hydrogen production performance of the electrocatalyst for seawater cracking in alkaline seawater is shown in fig. 3, and can be seen: at 10mAcm -2 At current densities of (c), the resulting electrocatalyst requires an earth overpotential of 136.2mV, similar to that in alkaline KOH;
Co/Co 9 S 8 the electrocatalyst stability performance graph is shown in fig. 4, where it can be seen that: obtained Co/Co 9 S 8 The electrocatalyst remained stable over 24 h.
Example 2
A method of preparing an electrocatalyst, comprising the steps of:
1) Dispersing tetraethyl orthosilicate and ammonia water into ethanol and deionized water, wherein the volume ratio of tetraethyl orthosilicate to ammonia water to ethanol is 3;
2) Dispersing 1g of the spherical silicon dioxide template obtained in the step 1) and 1g of cobalt nitrate hexahydrate in 15g of methanol, carrying out vacuum drying to obtain pink powder, then dispersing 1g of the pink powder and 1g of dimethyl imidazole in 15g of methanol together, stirring for 45min at 70 ℃ until a solvent is evaporated, and then carrying out vacuum drying on the obtained solid to obtain a ZIF-67 precursor;
3) Placing the ZIF-67 precursor obtained in the step 2) into a tube furnace, heating to 750 ℃ at a heating rate of 5 ℃/min, keeping the temperature constant for 4h for ablation, taking out the precursor after ablation, and cooling to room temperature under natural conditions to obtain a Co/NC precursor;
4) Mixing and dispersing the Co/NC precursor obtained in the step 3) and sodium sulfide into deionized water, wherein the mass ratio of the Co/NC precursor to the sodium sulfide is 1Cooling to room temperature after the reaction is finished, centrifuging, washing and vacuum drying to obtain solid powder which is Co/Co 9 S 8 An electrocatalyst.
Example 3
A method of preparing an electrocatalyst, comprising the steps of:
1) Dispersing tetraethyl orthosilicate and ammonia water into ethanol and deionized water, wherein the volume ratio of tetraethyl orthosilicate to ammonia water to ethanol is 3;
2) Dispersing 1g of the spherical silicon dioxide template obtained in the step 1) and 1g of cobalt nitrate hexahydrate in 15g of methanol, performing vacuum drying to obtain pink powder, then dispersing 1g of the pink powder and 1g of dimethyl imidazole in 15g of methanol together, stirring for 45min at 70 ℃ until a solvent is evaporated, and performing vacuum drying on the obtained solid to obtain a ZIF-67 precursor;
3) Placing the ZIF-67 precursor obtained in the step 2) into a tube furnace, heating to 750 ℃ at a heating rate of 5 ℃/min, keeping the temperature constant for 4h for ablation, taking out after ablation, and naturally cooling to room temperature to obtain a Co/NC precursor;
4) Mixing and dispersing the Co/NC precursor obtained in the step 3) and sodium sulfide into deionized water, wherein the mass ratio of the Co/NC precursor to the sodium sulfide is 1 9 S 8 An electrocatalyst.
Example 4
A method of preparing an electrocatalyst, comprising the steps of:
1) Dispersing tetraethyl orthosilicate and ammonia water into ethanol and deionized water, wherein the volume ratio of tetraethyl orthosilicate to ammonia water to ethanol is 3;
2) Dispersing 1g of the spherical silicon dioxide template obtained in the step 1) and 1g of cobalt nitrate hexahydrate in 15g of methanol, carrying out vacuum drying to obtain pink powder, then dispersing 1g of the pink powder and 1g of dimethyl imidazole in 15g of methanol together, stirring and reacting for 45min at 70 ℃ until a solvent is evaporated, and carrying out vacuum drying on the obtained solid to obtain a ZIF-67 precursor;
3) Placing the ZIF-67 precursor obtained in the step 2) into a tube furnace, heating to 750 ℃ at a heating rate of 5 ℃/min, keeping the temperature constant for 4h for ablation, taking out the precursor after ablation, and cooling to room temperature under natural conditions to obtain a Co/NC precursor;
4) Mixing and dispersing the Co/NC precursor obtained in the step 3) and sodium sulfide into deionized water, wherein the mass ratio of the Co/NC precursor to the sodium sulfide is 1 9 S 8 An electrocatalyst.
Example 5
A method of preparing an electrocatalyst, comprising the steps of:
1) Dispersing tetraethyl orthosilicate and ammonia water into ethanol and deionized water, wherein the volume ratio of tetraethyl orthosilicate to ammonia water to ethanol is 3;
2) Dispersing 1g of the spherical silicon dioxide template obtained in the step 1) and 1g of cobalt nitrate hexahydrate in 15g of methanol, carrying out vacuum drying to obtain pink powder, then dispersing 1g of the pink powder and 1g of dimethyl imidazole in 15g of methanol together, stirring and reacting for 45min at 70 ℃ until a solvent is evaporated, and carrying out vacuum drying on the obtained solid to obtain a ZIF-67 precursor;
3) Placing the ZIF-67 precursor obtained in the step 2) into a tube furnace, heating to 750 ℃ at a heating rate of 5 ℃/min, keeping the temperature constant for 4h for ablation, taking out the precursor after ablation, and cooling to room temperature under natural conditions to obtain a Co/NC precursor;
4) Mixing and dispersing the Co/NC precursor obtained in the step 3) and sodium sulfide into deionized water, wherein the mass ratio of the Co/NC precursor to the sodium sulfide is 1 9 S 8 An electrocatalyst.
Comparative example 1
The preparation method of the electrocatalyst specifically comprises the following steps:
1) Dispersing tetraethyl orthosilicate and ammonia water into ethanol and deionized water, wherein the volume ratio of tetraethyl orthosilicate to ammonia water to ethanol is 3;
2) Dispersing 1g of the spherical silicon dioxide template obtained in the step 1) and 1g of cobalt nitrate hexahydrate in 15g of methanol, performing vacuum drying to obtain pink powder, then dispersing 1g of the pink powder and 1g of dimethyl imidazole in 15g of methanol together, stirring for 45min at 70 ℃ until a solvent is evaporated, and performing vacuum drying on the obtained solid to obtain a ZIF-67 precursor;
3) Placing the ZIF-67 precursor obtained in the step 2) into a tube furnace, heating to 750 ℃ at a heating rate of 5 ℃/min, keeping the temperature constant for 4h for ablation, taking out after ablation, and naturally cooling to room temperature to obtain a Co/NC precursor;
4) Mixing and dispersing the Co/NC precursor obtained in the step 3) and sodium sulfide into deionized water, wherein the mass ratio of the Co/NC precursor to the sodium sulfide is 1 9 S 8 ElectrocatalysisAn oxidizing agent.
Comparative example 2
The preparation method of the electrocatalyst specifically comprises the following steps:
1) Dispersing tetraethyl orthosilicate and ammonia water into ethanol and deionized water, wherein the volume ratio of tetraethyl orthosilicate to ammonia water to ethanol is (3);
2) Dispersing 1g of the silicon dioxide template obtained in the step 1) and 1g of cobalt nitrate hexahydrate in 15g of methanol, carrying out vacuum drying to obtain pink powder, then dispersing 1g of the pink powder and 1g of dimethyl imidazole in the methanol together, stirring for 45min at the temperature of 70 ℃ until a solvent is evaporated, and carrying out vacuum drying on the obtained solid to obtain a ZIF-67 precursor;
3) Mixing the ZIF-67 precursor obtained in the step 2) with sodium sulfide, dispersing the mixture into deionized water, wherein the mass ratio of the ZIF-67 precursor to the sodium sulfide is 1 9 S 8 An electrocatalyst.
Test example 1
Co/Co prepared in examples 1-3 and comparative examples 1-2 9 S 8 The application of the electrocatalyst to the hydrogen production by cracking seawater specifically comprises the following steps: mixing Co with Co 9 S 8 The electrocatalyst is directly used as a working electrode, the mercury/mercury oxide electrode is used as a reference electrode, the platinum sheet electrode is used as a counter electrode, and the electrolyte is KOH with the concentration of 1.0M and alkaline seawater (KOH + real seawater, wherein the real seawater is taken from yellow sea in China, and the concentration of KOH is 1.0 mol/L). The test results are shown in table 1.
TABLE 1 Co/Co 9 S 8 Electrocatalytic performance of electrocatalyst
As can be seen from Table 1, when the stirring rate of the synthetic silica is 350rpm and the mass ratio of the Co/NC precursor to the sodium sulfide is 1 9 S 8 The electrocatalyst has excellent electrocatalytic cracking hydrogen production performance.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (10)
1. The preparation method of the electrocatalyst is characterized in that the chemical component of the electrocatalyst comprises Co 9 S 8 The preparation method comprises the following steps:
(1) Tetraethyl orthosilicate, ammonia water, ethanol and deionized water are mixed and then stirred for reaction, and then the mixture is centrifuged, washed and dried to obtain a spherical silicon dioxide template;
(2) Putting the spherical silicon dioxide template and cobalt nitrate hexahydrate into methanol for reaction to obtain solid powder;
(3) Dispersing the solid powder and dimethyl imidazole in methanol for continuous reaction, then stirring, heating, drying, heating for ablation, and cooling to obtain a Co/NC precursor;
(4) Dispersing the Co/NC precursor and sodium sulfide in water, and obtaining Co/Co through hydrothermal reaction 9 S 8 An electrocatalyst.
2. The preparation method of the electrocatalyst according to claim 1, wherein the volume ratio of the tetraethyl orthosilicate, the ammonia water, the deionized water and the ethanol in step (1) is 3.
3. The method for preparing the electrocatalyst according to claim 1, wherein the stirring temperature in step (1) is 10 to 30 ℃, the stirring speed is 350 to 520rpm, and the time is 5 hours;
the washing is respectively washing with deionized water and ethanol for 1-3 times;
the drying is vacuum drying, the temperature of the vacuum drying is 5-100 ℃, the time is 8-72 h, and the vacuum degree is 133-267 Pa.
4. The method for preparing an electrocatalyst according to claim 1, wherein the mass ratio of the spherical silica template, cobalt nitrate hexahydrate and methanol in step (2) is 1;
the reaction temperature is 10-30 ℃, and the reaction time is 2-3 h.
5. The method for preparing an electrocatalyst according to claim 1, wherein the ratio of the addition amounts of the solid powder, dimethylimidazole and methanol in step (3) is 1;
in the stirring and heating process, the stirring speed is 220 rpm, the heating temperature is 70 ℃, and the stirring and heating time is 45 min;
the drying is vacuum drying, the temperature of the vacuum drying is 5-100 ℃, the time is 8-72 h, and the vacuum degree is 133-267 Pa;
the heating ablation is as follows: heating to 750 ℃ at the heating rate of 5 ℃/min and ablating for 4h.
6. The preparation method of the electrocatalyst according to claim 1, wherein the mass ratio of the Co/NC precursor, the sodium sulfide and the water in the step (4) is 1 (20-30): 15.
7. the method for preparing the electrocatalyst according to claim 1, wherein the hydrothermal reaction in step (4) is performed at 120 ℃ for 15 hours.
8. Co/Co prepared by the method for preparing an electrocatalyst according to any one of claims 1 to 7 9 S 8 An electrocatalyst.
9. Use of an electrocatalyst according to claim 8 for electrocatalytic cracking of alkaline solutions and alkaline seawater for hydrogen production.
10. Use according to claim 9, wherein the working electrode is said Co/Co 9 S 8 The electro-catalyst, the reference electrode is a mercury/mercury oxide electrode, the counter electrode is a platinum sheet electrode, and the electrolyte is alkaline solution and/or alkaline seawater;
the pH value of the electrolyte is 10-14.
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