CN113638004B - Preparation method and application of bimetallic catalyst - Google Patents
Preparation method and application of bimetallic catalyst Download PDFInfo
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- CN113638004B CN113638004B CN202110908388.5A CN202110908388A CN113638004B CN 113638004 B CN113638004 B CN 113638004B CN 202110908388 A CN202110908388 A CN 202110908388A CN 113638004 B CN113638004 B CN 113638004B
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- 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
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- 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
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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
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- 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
Abstract
The invention belongs to the technical field of electrochemical catalytic synthesis of ammonia, and particularly relates to a preparation method and application of a bimetallic catalyst, which comprises the following steps: adopting an electrochemical double-electrode system, taking a carbon rod as a cathode, taking metallic iron as an anode, taking a cobalt nitrate solution as an electrolyte, and carrying out electrochemical stripping to obtain nanoscale iron; after the electrode positions are exchanged, carbon stripping is carried out; after the double-electrode stripping is finished, coprecipitation is carried out, centrifugal separation is carried out, and the bimetallic catalyst is obtained after drying. The nanometer bimetal electrode is used for electrochemically catalyzing and synthesizing ammonia in a water system to obtain higher ammonia yield and Faraday efficiency, and the ammonia yield can reach 591.43mg h ‑ 1 m ‑2 The Faraday efficiency can reach 33.36%.
Description
Technical Field
The disclosure belongs to the technical field of electrochemical catalytic synthesis of ammonia, and particularly relates to a preparation method and application of a bimetallic catalyst.
Background
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Ammonia is an important chemical product, which is a raw material of products such as nitrogen fertilizer, fiber, explosive and the like, and is a non-carbon hydrogen storage medium, a refrigerant fluid and a clean combustion fuel. Currently, the industry is primarily using the Haber-Bosch process, which has a centuries history. The Haber-Bosch process is generally a catalytic synthesis from fossil fuels (coal, petroleum, natural gas, etc.) powered and hydrogen sources using iron-based catalysts at high temperatures (400 ℃ C. -500 ℃ C.) and high pressures (200-. More than 90% of the world's ammonia is reported to be produced industrially by the Haber-Bosch process, which consumes about 3% -5% of the world's natural gas production annually, accounting for about 1% -2% of the world's energy supply; at the same time, about 400Mt of CO is released during the production of ammonia 2 Accounting for 1.5% of all greenhouse gas emissions. With the increasing global population, the increasing exhaustion of fossil fuels and the increasing awareness of environmental safety, an alternative and sustainable method is being developed, and a new green process capable of synthesizing ammonia under mild conditions by using renewable resources rather than fossil fuels is being developed.
One of the current research hotspots is the electrochemical catalytic reduction of nitrogen to synthesize ammonia (NRR), and the electrochemical catalytic synthesis of NH 3 It was reported since 1985. Compared with other nitrogen activation processes, the electrochemical transmission electron has obvious advantages, thermodynamic limitation can be broken through, high-temperature and high-pressure reaction can be realized at normal temperature and normal pressure, the power source can be non-fossil energy such as wind power, water power, solar energy, nuclear energy and the like, the power cost is low, and the method is easy to promote to industrialization. The nitrogen or air is used as a nitrogen source, and the water is used as a proton source, so that the problems of fossil energy consumption and carbon emission in the H-B process are solved. However, the inventors have found that NH is synthesized electrochemically 3 In the process, the preparation of the electrode is complex due to the catalytic effect of the catalystThe poor results in poor performance of electrodes for electrochemical ammonia synthesis, low ammonia yield and faraday efficiency, not to mention the prospects of industrialization. Therefore, how to prepare a catalyst for synthesizing ammonia with better performance and prepare an electrode with better performance by a simple and quick method is very important.
Disclosure of Invention
In order to overcome the problems and limitations of the electrode preparation process in the existing electrochemical ammonia synthesis technology, a preparation method and application of a bimetallic catalyst are provided, wherein a carrier is used for loading a nano bimetallic catalyst, and the prepared electrode is adopted to carry out the technical scheme of electrochemical ammonia synthesis at normal temperature and normal pressure.
Specifically, the technical scheme of the present disclosure is as follows:
in a first aspect of the present disclosure, a method of preparing a bimetallic catalyst comprises: adopting an electrochemical double-electrode system, taking a carbon rod as a cathode, taking metallic iron as an anode, taking a cobalt nitrate solution as an electrolyte, and carrying out electrochemical stripping to obtain nanoscale iron; after the electrode positions are interchanged, carbon stripping is carried out; after the double-electrode stripping is finished, coprecipitation is carried out, centrifugal separation is carried out, and the bimetallic catalyst is obtained after drying.
In a second aspect of the present disclosure, a bimetallic catalyst is obtained by the above-described preparation method.
In a third aspect of the disclosure, a bimetallic catalyst electrode for ammonia electrochemical synthesis is prepared by mixing the bimetallic catalyst and a binder.
In the fourth aspect of the present disclosure, the electrochemical synthesis of ammonia is performed by using the bimetallic catalyst electrode as a working electrode, a Pt electrode as a counter electrode, a calomel electrode as a reference electrode, a potassium phosphate solution as an electrolyte solution, and a constant voltage method.
One or more technical schemes in the disclosure have the following beneficial effects:
(1) the electrode material is prepared by adopting an electrode stripping method, the method is a convenient and efficient method, the prepared material is a nano-scale bimetallic system, can be well enriched on a carrier, has good dispersibility, and can be conveniently prepared into a working electrode by adding a binder into the obtained sample powder and pressing the sample powder into a tablet.
(2) The provided nanometer bimetal electrode is used for synthesizing ammonia by electrochemical catalysis of a water system, and higher ammonia yield and Faraday efficiency can be obtained, wherein the ammonia yield can reach 591.43mg h -1 m -2 The Faraday efficiency can reach 33.36%.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure, illustrate embodiments of the disclosure and together with the description serve to explain the disclosure and are not to be construed as limiting the disclosure.
FIG. 1: x-ray diffraction pattern for the catalyst of example 1;
FIG. 2: an X-ray photoelectron spectrum for the catalyst of example 1;
FIG. 3: scanning electron microscope SEM images of the catalyst of example 1;
FIG. 4 is a schematic view of: is a low power transmission electron microscope TEM image of the catalyst charge of example 1.
Detailed Description
The disclosure is further illustrated with reference to specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present disclosure. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out according to conventional conditions or according to conditions recommended by the manufacturers.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The reagents or starting materials used in the present invention can be purchased from conventional sources, and unless otherwise specified, the reagents or starting materials used in the present invention can be used in a conventional manner in the art or in accordance with the product specifications. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are exemplary only.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present disclosure. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise, and it should also be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the features, steps, operations and/or combinations thereof.
At present, the existing catalyst for electrochemically synthesizing ammonia has poor catalytic effect, and the preparation method of the electrode for preparing the electrochemically synthesized ammonia is complex, so that the performance of the synthesized ammonia is poor, the ammonia yield and the Faraday efficiency are low, and the industrial application is difficult to realize.
In one embodiment of the present disclosure, a method of preparing a bimetallic catalyst comprises: adopting an electrochemical double-electrode system, taking a carbon rod as a cathode, taking metallic iron as an anode, taking a cobalt nitrate solution as an electrolyte, and carrying out electrochemical stripping to obtain nanoscale iron; after the electrode positions are exchanged, carbon stripping is carried out; after the double-electrode stripping is finished, coprecipitation is carried out, centrifugal separation is carried out, and the bimetallic catalyst is obtained after drying.
In the preparation method, an alkaline solution is added to ensure that cobalt and iron are coprecipitated under the participation of stripping carbon to obtain a mixture. Compared with the existing preparation method of other catalysts, the method adopts an electrochemical stripping method, can conveniently prepare the nano-grade dispersed bimetallic catalyst, can improve the uniform dispersion and controllable preparation of the catalyst, and has better catalytic effect on improving the synthesis of ammonia.
Among them, carbon is required to be involved in the co-precipitation of cobalt and iron in order to obtain a uniform dispersion effect. The nano-scale particles are easy to agglomerate, and carbon participates in coprecipitation, so that the agglomeration phenomenon can be effectively inhibited, and the prepared iron-cobalt nano-particles are uniformly dispersed.
Wherein, the preparation of the cobalt nitrate solution comprises the following steps: weighing Co (NO) of different quality 3 ) 2 ·6H 2 Adding deionized water into the O solid, stirring until the O solid is dissolved, then fixing the volume, and respectively preparing 0.5-5M Co (NO) 3 ) 2 And (5) preparing an aqueous solution for later use. Preferably, of cobalt nitrate solutionThe concentration was 2.0M. In this step, Co (NO) 3 ) 2 ·6H 2 The O solid is readily soluble in water and deionized water is used to avoid the effect of other ions in the water on the reaction.
Adopting a constant voltage method, setting the voltage to be 1-5.0V, and carrying out electrochemical stripping. Uniform nano-iron can be obtained within the voltage range, agglomeration can be caused by overhigh voltage, and the stripping effect is poor due to overlow voltage.
The time of electrochemical stripping is 2-5.0 h; alternatively, the electrochemical peeling is performed at normal temperature and pressure. The optimal time for electrochemical stripping is 3.0h, and at this time, the nano iron is uniform and does not agglomerate.
The centrifugal separation rotating speed is 4000-10000 rpm; the temperature of vacuum drying is 50-120 ℃, and the vacuum degree is 10-60 mmHg. In the vacuum drying process, it is necessary to control the temperature, and too high temperature easily causes oxidation or cracking of the material.
In one embodiment of the present disclosure, a bimetallic catalyst is obtained by the above-described preparation method.
In one embodiment of the disclosure, a bimetallic catalyst electrode for ammonia electrochemical synthesis is prepared by mixing the bimetallic catalyst with a binder. Adding binder, pressing into tablet, trimming into square electrode slice, and clamping on electrode clamp with good conductivity to obtain working electrode. The preparation method is very simple and efficient, and is favorable for exerting the catalytic performance of the catalyst.
The binder is selected from sodium carboxymethylcellulose (CMC), polyvinylidene fluoride (PVDF), styrene butadiene rubber or polytetrafluoroethylene; preferably, polyvinylidene fluoride (PVDF).
In one embodiment of the present disclosure, a method for electrochemically synthesizing ammonia is provided, in which a bimetallic catalyst electrode for electrochemically synthesizing ammonia is used as a working electrode, a Pt electrode is used as a counter electrode, a calomel electrode is used as a reference electrode, a potassium phosphate solution is used as an electrolyte solution, and the ammonia is electrochemically synthesized by catalysis in a constant voltage method.
The voltage of the constant voltage method is-1.0-2.0V; or, the concentration of potassium phosphate solution is 0.1-2.0M, preferably 1.0M, under the synthesis conditions, ammonia yield and faraday efficiency can be improved.
In order to make the technical solutions of the present disclosure more clearly understood by those skilled in the art, the technical solutions of the present disclosure will be described in detail below with reference to specific embodiments.
Example 1
Cobalt nitrate hexahydrate (Co (NO) was weighed 3 ) 2 ·6H 2 O)29.103g, adding a small amount of deionized water, stirring, dissolving, and transferring to a 200ml volumetric flask for later use. The carbon rod is respectively put in ethanol and deionized water for ultrasonic treatment for 30min, and is taken out and then is polished by fine sand paper, so that the surface is rough, and the stripping is facilitated.
Adopting a double-electrode system, taking a metal iron electrode as a counter electrode, taking a carbon rod electrode as a working electrode, and taking 0.5M Co (NO) 3 ) 2 Putting 120ml of the solution into a 150ml conventional electrolytic cell to be used as an electrolyte solution, and carrying out electrochemical stripping in a Princeton electrochemical workstation by adopting a constant voltage method, wherein the voltage is set to be 5V, the time per point is 0.05s, and the duration is 7200 s; the electrochemical treatment was carried out under the same conditions using a carbon rod electrode as a counter electrode and metallic iron as a working electrode.
After the electrode stripping step is finished, adding an alkaline solution to ensure that the cobalt solution and the iron are coprecipitated under the participation of stripping carbon, carrying out centrifugal separation on the obtained mixture at the rotating speed of 4000rpm, putting the separated precipitate into a vacuum drying oven, and carrying out vacuum drying at the vacuum degree of 40mmHg and the temperature of 60 ℃ for 4 hours. And adding a polytetrafluoroethylene electrode binder into the obtained sample powder for bonding, and finally tabletting and shaping by a tabletting machine. And trimming and polishing the obtained electrode slice into a square with the side length of 1cm, and taking the electrode slice as an electrochemical synthesis ammonia electrode slice.
The prepared bimetallic electrode is used as a working electrode, the Pt electrode is used as a counter electrode, the calomel electrode is used as a reference electrode, a potassium phosphate solution with the concentration of 1.0M is used as an electrolyte solution, and an electrochemical catalytic synthesis ammonia performance experiment is carried out by using an electrochemical workstation constant voltage method and the voltage of 1.0V. The ammonia content of the system is detected by indophenol blue spectrophotometry, and the result shows that the ammonia yield of the electro-catalysis synthesis ammonia is 303.6mg h -1 m -2 The Faraday efficiency reaches 20.4%.
Example 2
Cobalt nitrate hexahydrate (Co (NO) was weighed 3 ) 2 ·6H 2 O)58.206g, adding a small amount of deionized water, stirring, dissolving, and transferring to a 200ml volumetric flask for later use. The carbon rod is respectively put in ethanol and deionized water for ultrasonic treatment for 30min, and is taken out and then is polished by fine sand paper, so that the surface is rough, and the stripping is facilitated.
Adopting a double-electrode system, taking a metal iron electrode as a counter electrode, taking a carbon rod electrode as a working electrode, and taking 1.0M of Co (NO) 3 ) 2 Putting 120ml of the solution into a 150ml conventional electrolytic cell to be used as an electrolyte solution, and carrying out electrochemical stripping in a Princeton electrochemical workstation by adopting a constant voltage method, wherein the voltage is set to be 10V, the time per point is 0.05s, and the duration is 7200 s; the electrochemical treatment was carried out under the same conditions using a carbon rod electrode as the counter electrode and metallic iron as the working electrode.
After the electrode stripping is finished, adding an alkaline solution to ensure that the cobalt solution and the iron are coprecipitated under the action of stripping carbon, carrying out centrifugal separation on the obtained mixture at the rotating speed of 4000rpm, putting the separated precipitate into a vacuum drying oven, and carrying out vacuum drying at the vacuum degree of 40mmHg for 4 hours at the temperature of 60 ℃. And adding the obtained sample powder into a styrene butadiene rubber electrode binder for bonding, and finally tabletting and shaping by a tabletting machine. And trimming and polishing the obtained electrode slice into a square with the side length of 1cm, and taking the electrode slice as an electrochemical synthesis ammonia electrode slice.
The prepared bimetallic electrode is used as a working electrode, the Pt electrode is used as a counter electrode, the calomel electrode is used as a reference electrode, 2.0M potassium phosphate solution is used as electrolyte solution, and an electrochemical catalytic synthesis ammonia performance experiment is carried out by using an electrochemical workstation constant voltage method with the voltage of 2.0V. The ammonia content of the system is detected by indophenol blue spectrophotometry, and the result shows that the ammonia yield of the electro-catalysis synthesis ammonia is 286.6mg h -1 m -2 The Faraday efficiency reaches 18.6%.
Example 3
Cobalt nitrate hexahydrate (Co (NO) was weighed 3 ) 2 ·6H 2 O)116.412g，Adding a small amount of deionized water, stirring, dissolving, and transferring to a 200ml volumetric flask for later use. The carbon rod is respectively put in ethanol and deionized water for ultrasonic treatment for 30min, and is taken out and then is polished by fine sand paper, so that the surface is rough, and the stripping is facilitated.
Adopting a double-electrode system, taking a metal iron electrode as a counter electrode, taking a carbon rod electrode as a working electrode, and taking 2.0M Co (NO) 3 ) 2 Putting 120ml of the solution into a 150ml conventional electrolytic cell to serve as an electrolyte solution, and performing electrochemical stripping in a Princeton electrochemical workstation by adopting a constant voltage method, wherein the voltage is set to be 5V, the time at each point is 0.05s, and the duration is 18000 s; the electrochemical treatment was carried out under the same conditions using a carbon rod electrode as a counter electrode and metallic iron as a working electrode.
After the electrode stripping is finished, adding an alkaline solution to ensure that the cobalt solution and the iron are coprecipitated under the action of stripping carbon, carrying out centrifugal separation on the obtained mixture at the rotating speed of 4000rpm, putting the separated precipitate into a vacuum drying oven, and carrying out vacuum drying at the vacuum degree of 40mmHg for 4 hours at the temperature of 60 ℃. And adding the obtained sample powder into a sodium carboxymethylcellulose electrode binder for bonding, and finally tabletting and shaping by a tabletting machine. And trimming and polishing the obtained electrode slice into a square with the side length of 1cm, and taking the electrode slice as an electrochemical synthesis ammonia electrode slice.
The prepared bimetallic electrode is used as a working electrode, the Pt electrode is used as a counter electrode, the calomel electrode is used as a reference electrode, a potassium phosphate solution with the concentration of 1.0M is used as an electrolyte solution, and an electrochemical catalytic synthesis ammonia performance experiment is carried out by using an electrochemical workstation constant voltage method and the voltage of-0.5V. And detecting the ammonia content of the system by indophenol blue spectrophotometry. The results showed that the yield of ammonia in the electrocatalytic synthesis of ammonia was 591.43mg h -1 m -2 The Faraday efficiency reaches 33.36 percent.
Example 4
Cobalt nitrate hexahydrate (Co (NO) was weighed 3 ) 2 ·6H 2 O)291.03g, adding a small amount of deionized water, stirring, dissolving, and transferring to a 200ml volumetric flask for later use. The carbon rod is respectively placed in ethanol and deionized water for ultrasonic treatment for 30min, and is taken out and then is polished by fine abrasive paper, so that the surface is rough, and stripping is facilitated.
Adopting a double-electrode system, taking a metal iron electrode as a counter electrode, taking a carbon rod electrode as a working electrode, and taking 5.0M Co (NO) 3 ) 2 Putting 120ml of the solution into a 150ml conventional electrolytic cell to serve as an electrolyte solution, and performing electrochemical stripping in a Princeton electrochemical workstation by adopting a constant voltage method, wherein the voltage is set to be 10V, the time at each point is 0.05s, and the duration is 18000 s; the electrochemical treatment was carried out under the same conditions using a carbon rod electrode as a counter electrode and metallic iron as a working electrode.
After the electrode stripping is finished, adding an alkaline solution to ensure that the cobalt solution and the iron are coprecipitated under the action of stripping carbon, carrying out centrifugal separation on the obtained mixture at the rotating speed of 6000rpm, putting the separated precipitate into a vacuum drying oven, and carrying out vacuum drying at the vacuum degree of 50mmHg for 4 hours at the temperature of 80 ℃. And adding polyvinylidene fluoride (PVDF) electrode binder into the obtained sample powder for bonding, and finally tabletting and shaping by a tabletting machine. And trimming and polishing the obtained electrode plate into a square with the side length of 1cm to be used as an electrode plate for electrochemical synthesis of ammonia.
The prepared bimetallic electrode is used as a working electrode, the Pt electrode is used as a counter electrode, the calomel electrode is used as a reference electrode, a potassium phosphate solution with the concentration of 0.1M is used as an electrolyte solution, and an electrochemical catalytic synthesis ammonia performance experiment is carried out by using an electrochemical workstation constant voltage method and the voltage of-1.0V. The ammonia content of the system is detected by indophenol blue spectrophotometry, and the result shows that the ammonia yield of the electro-catalysis synthesis ammonia is 412.8mg h -1 m -2 The Faraday efficiency reaches 23.7%.
Comparative example 1:
compared with example 1, the differences are: taking a metal iron electrode as a counter electrode and a carbon rod electrode as a working electrode, and directly adding an alkaline solution for coprecipitation without exchanging the positions of the electrodes after electrochemical stripping. The catalyst is prepared into an electrode plate and then used for electrochemically synthesizing ammonia, and the specific steps are the same as those in example 1. The ammonia content of the system is detected by indophenol blue spectrophotometry, and the result shows that the ammonia yield of the electro-catalysis synthesis ammonia is only 101.6mg h -1 m -2 The faradaic efficiency is only 6.80%.
It can be seen that carbon is required to participate in the co-precipitation of cobalt and iron. Carbon participates in coprecipitation, so that agglomeration can be effectively inhibited, the prepared iron-cobalt nanoparticles are uniformly dispersed, and the ammonia yield and the Faraday efficiency are obviously improved.
Comparative example 2:
compared with example 1, the difference is that: cobalt nitrate was replaced with nickel nitrate. The catalyst is used for electrochemically synthesizing ammonia after being prepared into an electrode plate, and the specific steps are the same as those in example 1. The ammonia content of the system is detected by indophenol blue spectrophotometry, and the result shows that the ammonia yield of the electro-catalysis synthesis ammonia is only 86.8mg h -1 m -2 The faraday efficiency is only 5.81%.
Therefore, the iron-cobalt bimetallic catalyst prepared by the method has a synergistic effect, and the cobalt metal is replaced by the nickel metal, so that the catalytic effect is weakened, and the synergistic effect is avoided.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described above, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing a bimetallic catalyst, which is characterized by comprising the following steps: adopting an electrochemical double-electrode system, taking a carbon rod as a cathode, taking metallic iron as an anode, taking a cobalt nitrate solution as an electrolyte, and carrying out electrochemical stripping to obtain nanoscale iron; after the electrode positions are exchanged, carbon stripping is carried out; after the double-electrode stripping is finished, carrying out coprecipitation, centrifugal separation and drying to obtain a bimetallic catalyst;
adopting a constant voltage method, setting the voltage to be 1-5V, and carrying out electrochemical stripping;
the time of the electrochemical stripping is 2-5 h; electrochemical stripping is carried out at normal temperature and normal pressure;
the concentration of the cobalt nitrate solution is 0.5-5M.
2. The process for preparing a bimetallic catalyst as in claim 1, wherein said cobalt nitrate solution has a concentration of 2.0M.
3. The method for preparing a bimetallic catalyst as in claim 1, wherein the centrifugal separation rotation speed is 4000 to 10000 rpm; the temperature of vacuum drying is 50-120 ℃, and the vacuum degree is 10-60 mmHg.
4. A bimetallic catalyst, characterized by being obtained by the process of any one of claims 1 to 3.
5. A bimetallic catalyst electrode for the electrochemical synthesis of ammonia, characterized in that the electrode is prepared by mixing the bimetallic catalyst of claim 4 with a binder.
6. The bimetallic catalyst electrode of claim 5, wherein the binder is sodium carboxymethylcellulose (CMC), polyvinylidene fluoride (PVDF), styrene butadiene rubber or polytetrafluoroethylene.
7. The bimetallic catalyst electrode of claim 6, wherein the binder is polyvinylidene fluoride (PVDF).
8. A method for electrochemically synthesizing ammonia, characterized in that the electrochemical synthesis ammonia of claim 5 or 6 is carried out by taking a bimetallic catalyst electrode as a working electrode, a Pt electrode as a counter electrode, a calomel electrode as a reference electrode, a potassium phosphate solution as an electrolyte solution and a constant voltage method.
9. The method for the electrochemical synthesis of ammonia as claimed in claim 8, wherein the constant voltage method has a voltage of-1.0-2.0V and the concentration of potassium phosphate solution is 0.1-2.0M.
10. The process for the electrochemical synthesis of ammonia according to claim 9, wherein the concentration of potassium phosphate solution is 1.0M.
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| CN111719165A (en) * | 2020-06-24 | 2020-09-29 | 江南大学 | Method for preparing Bi nanosheet by electrochemical stripping method |
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