CN107913721B - Method for preparing defect-rich catalytic material by using magnesiothermic reduction method and catalytic material - Google Patents

Method for preparing defect-rich catalytic material by using magnesiothermic reduction method and catalytic material Download PDF

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CN107913721B
CN107913721B CN201711225700.0A CN201711225700A CN107913721B CN 107913721 B CN107913721 B CN 107913721B CN 201711225700 A CN201711225700 A CN 201711225700A CN 107913721 B CN107913721 B CN 107913721B
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transition metal
rich
catalytic material
defect
metal oxide
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CN107913721A (en
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霍开富
皮超然
高标
张旭明
黄超
付继江
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Wuhan University of Science and Engineering WUSE
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/20—Carbon compounds
    • B01J27/22—Carbides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • 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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention provides a method for preparing a defect-rich catalytic material by a magnesiothermic reduction method, which comprises the following steps: mixing binary transition metal oxide material with NaHCO3Uniformly mixing the magnesium powder with the binary transition metal oxide material, and sealing the mixture in a reaction kettle, wherein the binary transition metal M and N in the binary transition metal oxide material are any two combinations of Mo, V, Mn, W or Nb; and (3) preserving the heat for 1-5 hours at the temperature of 600-900 ℃ in the inert protective atmosphere, and pickling the obtained product to obtain the carbon-coated binary defect-rich carbide catalytic material. The material is rich in defects, can provide a large number of active sites in the electrochemical hydrogen evolution reaction process, and can effectively improve the activity of the catalyst. Meanwhile, the outer surface of the particle is coated with a layer of high-crystallinity carbon, so that the conductivity of the material is improved, the circulating stability of the material is improved, and the dissolution of the material in the catalysis process is inhibited. The method is simple, the obtained product is clear, and the corrosion-resistant effect is achieved, so that a brand new path is provided for improving the activity of the catalyst in the field of electrocatalysis.

Description

Method for preparing defect-rich catalytic material by using magnesiothermic reduction method and catalytic material
Technical Field
The invention relates to the field of material chemistry, in particular to a method for preparing a defect-rich catalytic material by a magnesiothermic reduction method and the catalytic material.
Background
Hydrogen (H)2) Is considered to be a clean energy source that can be used as a substitute for conventional fossil energy sources while having a high calorific value. Realizes effective development of hydrogen energy, thereby successfully realizingThe two key links to replace fossil energy are the production and storage of hydrogen. At present, a plurality of industrial hydrogen production modes are adopted, and hydrogen production by water electrolysis, catalytic steam reforming, hydrogen production by coal gasification, petroleum cracking, catalytic conversion of natural gas and the like are mainly adopted, but the methods all have some defects to be overcome, such as very high energy consumption. Electrolysis of water is one of the simplest and most efficient methods, which has the advantage of high hydrogen purity, but the rate of hydrogen evolution by electrolysis is slow, requiring the use of catalysts to accelerate the kinetics, such as the noble metal platinum (Pt), which is expensive and has limited reserves, eventually limiting its use on a large scale. Therefore, the development of non-noble metal materials as catalysts for electrochemical hydrogen evolution has become a very important issue at present. Transition metal carbides have been extensively studied due to their abundant reserves, low price and excellent catalytic properties. Most catalysts on the market are block materials, and the appearance of the block is lack of effective active sites, so that the catalytic efficiency is low. How to improve the catalytic performance of the material can be started from the following aspects: 1. increasing the specific surface area of the material; 2. the catalyst material is stripped according to layers, so that a rapid ion channel is provided; 3. the conductivity of the material is improved. 4. Too many catalyst boundaries are created, resulting in uneven electron cloud distribution and thus higher activity; the first three methods are to increase the active sites per unit area, and the fourth method can fundamentally change the catalytic effect. Therefore, how to select a proper method to improve the catalytic performance of the material has been a difficulty for those skilled in the art.
Disclosure of Invention
The invention aims to provide a method for preparing a defect-rich catalytic material with ultrahigh catalytic performance by a magnesiothermic reduction method and the prepared catalytic material.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for preparing a defect-rich catalytic material by a magnesiothermic reduction method comprises the following steps:
mixing binary transition metal oxide material with NaHCO3Is even with magnesium powderMixing and sealing in a reaction kettle, wherein binary transition metals M and N in the binary transition metal oxide material are the combination of any two of Mo, V, Mn, W or Nb;
and (3) preserving the heat for 1-5 hours at the temperature of 600-900 ℃ in the inert protective atmosphere, and pickling the obtained product to obtain the carbon-coated binary defect-rich carbide catalytic material.
In the above scheme, the binary transition metal oxide material and NaHCO3The mass ratio of the magnesium powder to the magnesium powder is 1-10:1-10: 1-10.
In the above scheme, the inert protective atmosphere is argon.
In the above embodiment, the particle size of the binary transition metal oxide material powder is in the range of 5 μm to 20 μm.
The catalytic material prepared by the method comprises a carbon net and a plurality of nano particles wrapped in the carbon net, wherein the nano particles are metal M carbide particles and metal N carbide particles which are rich in defect phase and mutually cross-linked in a nano level.
In the above scheme, the size of the inter-crosslinked metal M carbide particles and metal N carbide particles is 20-100 nm.
The reaction principle of the invention is as follows: mg + MNO + NaHCO3＝MgO+MC+NC+CO2(wherein M, N is Mo, V, Mn, W or Nb; MC is a metal carbide of an M element, NC is a metal carbide of an N element, and the molar ratio is not limited to 1: 1). And (3) preserving the heat for 1-5 hours at the temperature of 600-900 ℃ in the protective atmosphere, and pickling to remove magnesium oxide to prepare the nano-scale cross-linked particles with the defect-rich phase. Because the product is obtained by phase separation of the precursor, the obtained two carbides can be simultaneously precipitated but can not be completely separated, so a lattice interface can be formed between the two obtained products, and the interface can provide huge catalytic activity; in the method, carbon dioxide generated by decomposition of sodium bicarbonate is converted into a highly-crystalline carbon network structure with high conductivity through a magnesiothermic reduction reaction, and nanoparticles can be coated on the carbon network. The material is rich in defects, which can provide a large number of active sites in the electrochemical hydrogen evolution reaction processThe catalyst can effectively improve the activity of the catalyst and has excellent performance. The outer surface of the particle is coated with a layer of high-crystallinity carbon, so that the conductivity of the material is improved, the circulating stability of the material is improved, and the dissolution of the material in the catalysis process is inhibited.
The invention has the beneficial effects that:
1. the raw material with micron scale is processed by magnesium thermal reaction, and CO is present2In the case of (b), the pulverization can be efficiently performed and converted into a nano-scale material.
2. The used raw materials are binary components and can be widely obtained in nature, binary transition metal oxide, sodium bicarbonate and magnesium powder are mixed according to a certain proportion and are treated at a certain temperature, so that reduced binary transition metal carbide rich in defects can be obtained, two carbides obtained by phase separation of a precursor can be simultaneously precipitated but cannot be completely separated, a lattice interface can be formed between the two obtained products, the interface can provide huge catalytic activity, the method is easy to operate, and a novel method is provided for preparing a high-performance electrochemical catalyst, and the method is not reported in other documents or patents.
3. In the method, carbon dioxide generated by decomposition of sodium bicarbonate is converted into a highly-crystalline carbon network structure with high conductivity through a magnesiothermic reduction reaction, and simultaneously, a carbonized product corresponding to a metal element can be formed.
4. The method can carry out in-situ phase separation on the binary material, and the obtained product can not be completely separated into individuals which exist in isolation, so that a large number of defects can be obtained at the coherent junction, the improvement of the catalytic performance is facilitated, and the application prospect in the field of electrocatalysis wide.
Drawings
The invention will be further explained with reference to the following figures and examples:
FIG. 1 is an XRD pattern of the product prepared in example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of the product prepared in example 1 of the present invention.
FIG. 3 is a transmission electron micrograph of the product prepared in example 1 of the present invention.
FIG. 4 is a graph showing the electrochemical polarization of the final product prepared in example 1 of the present invention.
FIG. 5 is a comparison of the Tafel slope obtained in example 1 of the present invention.
FIG. 6 is a comparison of the stability of the catalytic performance after recycling of the product prepared in example 1 of the present invention.
FIG. 7 is a Tafel plot of the final product prepared in example 2.
FIG. 8 is a graph showing the electrochemical polarization of the final product prepared in example 2.
FIG. 9 is a Tafel plot of the final product prepared in example 3.
FIG. 10 is a graph showing the electrochemical polarization of the final product prepared in example 3.
FIG. 11 is a Tafel plot of the final product prepared in example 4.
FIG. 12 is a graph showing the electrochemical polarization of the final product prepared in example 4.
FIG. 13 is a graph showing the electrochemical polarization of the final product prepared in example 5.
FIG. 14 is a Tafel plot of the final product prepared in example 5.
FIG. 15 is a graph showing the electrochemical polarization of the final product prepared in example 6.
FIG. 16 is a Tafel plot of the final product prepared in example 6.
FIG. 17 is a schematic diagram of the product obtained by the present invention participating in hydrogen evolution reaction.
Detailed Description
For a more clear understanding of the technical features, objects and effects of the present invention, embodiments of the present invention will now be described in detail with reference to the accompanying drawings.
Example 1
(1) Mixing micron-sized V2MoO8Powder andmagnesium powder and NaHCO3Uniformly mixing the raw materials in a mass ratio of 1:1.5:1.5, and putting the mixture into a sealed reaction kettle;
(2) heating to 800 ℃ under Ar protective atmosphere, and keeping the temperature for 1-2h to obtain Mo2C/V8C7Mixing;
(3) and (3) acid-washing the product obtained in the step (2) to obtain the carbon-coated nano-particles.
The reaction equation of the principle of this reaction is: 2NaHCO3＝Na2CO3+CO2+H2O, decomposition of CO at low temperatures2Then through 2Mg + CO22MgO + C, finally C + V2MoO8---Mo2C+V8C7+CO2And the like.
In this example, V2MoO8The particle size of the powder is 5-20 μm.
The catalytic material comprises a carbon net and a plurality of nano-particles wrapped in the carbon net, wherein the nano-particles are Mo which is rich in defect phase and mutually cross-linked in nano-scale2C particles and V8C7And (3) granules. Crosslinked Mo2C particles and V8C7The size of the particles is 20-100 nm.
The obtained product is subjected to XRD diffraction pattern characterization, and in figure 1, the obtained product is Mo2C/V8C7No other impurity phase except magnesium oxide and sodium carbonate; as can be seen from the scanning electron microscope image in fig. 2, the product prepared in this example has a nano-scale porous structure; as can be seen from the transmission electron microscope image in FIG. 3, the product prepared by the present example is in-situ incomplete phase separation, has abundant defects, and is wrapped by a highly conductive carbon network. FIG. 4 shows the electrocatalytic properties of the reaction products, in comparison with the starting materials and the comparison term Mo2C and V8C7Compared with the catalytic performance, the catalytic performance is greatly improved. FIG. 5 is a Tafel slope diagram, the smaller the Tafel slope value is, the smaller the overpotential required by the reaction is proved to be, i.e. the better the performance is, and the comparison in the diagram shows that the product of the invention is already close to Pt in value and has good electrocatalytic performance. FIG. 6 shows Mo obtained in example 1 of the present invention2C/V8C7AsThe comparison of catalytic performances after 10000 times of catalyst circulation shows that the performance change before and after the circulation is not large, thus showing that the reaction product has good stability and durability.
Example 2
(1) Mixing micron-sized V2MoO8Mixing the powder with magnesium powder and NaHCO3Uniformly mixing the raw materials in a mass ratio of 1:3:10, and putting the mixture into a sealed reaction kettle;
(2) heating to 600 ℃ under Ar protective atmosphere, and keeping the temperature for 1-2h to obtain Mo2C/V8C7Mixing;
(3) and (3) acid-washing the product obtained in the step (2) to obtain the carbon-coated nano-particles.
In this example, V2MoO8The particle size of the powder is 5-20 μm. Crosslinked Mo2C particles and V8C7The size of the particles is 30-100 nm.
FIGS. 7 to 8 are V2MoO8The polarization curve graph and Tafel slope graph obtained by heating to 600 ℃ in Ar can be seen from the curves, and the obtained catalyst material under the condition has excellent performance and can be practically applied.
Example 3
(1) Mixing micron-sized V2MoO8Mixing the powder with magnesium powder and NaHCO3Uniformly mixing the raw materials in a mass ratio of 1:4:2, and putting the mixture into a sealed reaction kettle;
(2) heating to 700 ℃ under Ar protective atmosphere, and keeping the temperature for 1-2h to obtain Mo2C/V8C7Mixing;
(3) and (3) acid-washing the product obtained in the step (2) to obtain the carbon-coated nano-particles.
In this example, V2MoO8The particle size of the powder is 5-20 μm. Crosslinked Mo2C particles and V8C7The size of the particles is 40-60 nm.
FIGS. 9 to 10 are V2MoO8The polarization curve diagram and Tafel slope diagram obtained by heating to 700 ℃ in Ar can be seen from the curves, and the obtained catalyst material under the condition has excellent performance and can be practically applied.
Example 4
(1) Mixing micron-sized V2MoO8Mixing the powder with magnesium powder and NaHCO3Uniformly mixing the raw materials in a mass ratio of 1:1.5:1.5, and putting the mixture into a sealed reaction kettle;
(2) heating to 900 ℃ under Ar protective atmosphere, and keeping the temperature for 1-2h to obtain Mo2C/V8C7Mixing;
(3) and (3) acid-washing the product obtained in the step (2) to obtain the carbon-coated nano-particles.
In this example, V2MoO8The particle size of the powder is 5-20 μm. Crosslinked Mo2C particles and V8C7The size of the particles is 20-100 nm.
FIGS. 11-12 are V2MoO8The polarization curve graph and Tafel slope graph obtained by heating to 900 ℃ in Ar can be seen from the curves, and the obtained catalyst material under the condition has excellent performance and can be practically applied.
Example 5
(1) Mixing micron-sized MnMoO4Mixing the powder with magnesium powder and NaHCO3Uniformly mixing the raw materials in a mass ratio of 1:1.5:1.5, and putting the mixture into a sealed reaction kettle;
(2) heating to 800 ℃ under Ar protective atmosphere, and keeping the temperature for 1-5h to obtain a product;
(3) and (3) acid-washing the product obtained in the step (2) to obtain the carbon-coated nano-particles.
In this example, MnMoO4The particle size of the powder is 5-20 μm. Mn cross-linked with each otherxC particles and MoxThe size of the C particles is 20-100 nm.
FIGS. 13-14 are MnMoO4The polarization curve diagram and Tafel slope diagram obtained by heating to 800 ℃ in Ar can be seen from the curves, and the catalyst material obtained under the condition has excellent performance and can be practically applied, so that the double-element MnMoO4The powder can also obtain two carbonization products without separation, and the carbonization products can be applied to practice.
Example 6
(1) Mixing the micron-sized WMoO4Mixing the powder with magnesium powder and NaHCO3According to the mass ratio1:1:1.5, uniformly mixing and putting into a sealed reaction kettle;
(2) heating to 800 ℃ under Ar protective atmosphere, and keeping the temperature for 1-2h to obtain a product;
(3) and (3) acid-washing the product obtained in the step (2) to obtain the carbon-coated nano-particles.
In this embodiment, WMoO4The particle size of the powder is 5-20 μm. Crosslinked MoxC particles and WXThe size of the C particles is 20-100 nm.
FIGS. 15-16 are WMoO4The polarization curve diagram and Tafel slope diagram obtained by heating to 800 ℃ in Ar can be seen from the curves, and the catalyst material obtained under the condition has excellent performance and can be practically applied, so that the double-element WMoO4The powder can also obtain two carbonization products without separation, and the carbonization products can be applied to practice.
It is understood that the atmosphere of the present invention is not limited to one kind of Ar, and other gases capable of acting as a shielding gas without participating in the reaction may be used, such as helium and nitrogen.
The invention utilizes decomposed CO by a simple magnesiothermic reduction method2To cause the destruction of the micro-materials into nano-catalytic materials. The magnesiothermic reduction method involved therein is reported in the related patent arts, for example, "a method for preparing silicon-carbon composite material by using the magnesiothermic reduction method" (CN106374088A), in which a silica-carbon precursor is mixed with magnesium powder to carry out magnesiothermic reduction, and finally, the silicon-carbon composite material is obtained. For another example, in "a method for preparing porous silicon by magnesiothermic reduction" (CN102259858A), a self-supporting porous silicon material is obtained by treating a mixture of silicon and magnesium oxide, which is formed by using an oxide of silicon as a raw material and by a magnesiothermic reaction. The above 2 patents only reduce the reaction temperature by Mg thermal reduction reaction, and do not relate to the crushing process, and we propose a new way to utilize solid phase reaction and relate to the self-decomposition to produce CO2Thereby generating a crushing effect and realizing a partial phase separation process.
The invention has the innovation point that the main reaction raw material is binary transition metal oxide which can be decomposed with sodium bicarbonate, potassium bicarbonate, calcium carbonate and the like to generate CO2After the raw material and magnesium are mixed, two phases of materials which are not completely separated can be obtained through magnesium thermal reaction, and the boundary effect generated by the two phases generates high activity. Another outstanding advantage of the invention is the CO obtained by decomposition of sodium bicarbonate2After the reaction, the carbon-coated material particles can be reduced as a carbon source to generate high-crystallinity carbon-coated material particles, and excellent conductivity is provided. The method has the advantages that the raw materials are cheap, the binary transition metal oxide, the sodium bicarbonate and the magnesium powder are used as the raw materials, the defect-rich reduction product is obtained through simple magnesium thermal reaction, the production is easy, a new method is provided for preparing the high-quality electrochemical catalyst, and the method can be widely applied to the field of electrocatalysis.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (6)

1. A method for preparing a defect-rich catalytic material by a magnesiothermic reduction method is characterized by comprising the following steps of:
mixing binary transition metal oxide material with NaHCO3Uniformly mixing the double transition metal oxide material with magnesium powder, and sealing the mixture in a reaction kettle, wherein the double transition metal M and N in the double transition metal oxide material are the combination of any two of Mo, V, Mn, W or Nb; and (3) preserving the heat for 1-5 hours at the temperature of 600-900 ℃ in the inert protective atmosphere, and pickling the obtained product to obtain the carbon-coated binary defect-rich carbide catalytic material.
2. The method of claim 1, wherein the binary transition metal oxide material is NaHCO3The mass ratio of the magnesium powder to the magnesium powder is 1-10:1-10: 1-10.
3. The method for preparing a defect-rich catalytic material by a magnesiothermic reduction method according to claim 1, wherein said inert protective atmosphere is argon.
4. The method of claim 1, wherein the binary transition metal oxide material powder has a particle size in the range of 5 μm to 20 μm.
5. The catalytic material prepared by the method of any one of claims 1 to 4, wherein the defect-rich catalytic material comprises a carbon network and a plurality of nanoparticles wrapped in the carbon network, and the nanoparticles are defect-rich phase nanoscale metal M carbide particles and metal N carbide particles which are mutually cross-linked.
6. Catalytic material according to claim 5, characterized in that the size of the inter-crosslinked metal M-carbide particles and metal N-carbide particles is 20-100 nm.
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CN104120457A (en) * 2014-07-10 2014-10-29 上海大学 Preparing method of metal-carbide-containing multi-layer multi-component composite material
CN106374088A (en) * 2016-10-14 2017-02-01 浙江天能能源科技股份有限公司 Method for preparing silicon/carbon composite material with magnesiothermic reduction process

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CN104120457A (en) * 2014-07-10 2014-10-29 上海大学 Preparing method of metal-carbide-containing multi-layer multi-component composite material
CN106374088A (en) * 2016-10-14 2017-02-01 浙江天能能源科技股份有限公司 Method for preparing silicon/carbon composite material with magnesiothermic reduction process

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