CN110923776A - Mixing CO2Conversion to metal carbide coating and O2Molten salt electrochemical process of - Google Patents

Mixing CO2Conversion to metal carbide coating and O2Molten salt electrochemical process of Download PDF

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CN110923776A
CN110923776A CN201911311843.2A CN201911311843A CN110923776A CN 110923776 A CN110923776 A CN 110923776A CN 201911311843 A CN201911311843 A CN 201911311843A CN 110923776 A CN110923776 A CN 110923776A
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metal
carbide coating
electrolysis
metal carbide
molten salt
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肖巍
翁威
曹锦�
肖汉生
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Wuhan University WHU
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/04—Electrolytic coating other than with metals with inorganic materials
    • C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
    • 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

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Abstract

The invention relates to a method for mixing CO2Conversion to metal carbide coating and O2The molten salt electrochemical method of (1), comprising the steps of: using carbonate as electrolyte, high-melting-point metal as cathode and nickel-base metal as inert anode, and adding CO2Continuously introducing into molten electrolyte for electrolysis to obtain metal carbide coating on the surface of the metal cathode and oxygen at the anode. The electrochemical process of the invention is carried out directly with CO2As carbon source, it is directly reacted with metal substrate under electrolysis condition to convert into metal carbide coating and O2On one hand, the method can realize the generation of the metal carbide coating with any shape on the metal surface, the metal carbide coating has high hardness, wear resistance and good hydrogen production performance by catalysis, and in addition, the method can consume CO2And the emission reduction of greenhouse gases is realized.

Description

Mixing CO2Conversion to metal carbide coating and O2Molten salt electrochemical process of
Technical Field
The invention belongs to the technical field of electrochemistry, and particularly relates to a method for preparing CO2Conversion to metal carbide coating and O2The molten salt electrochemical process of (1).
Background
Human industrial process for making CO in atmosphere2The content is continuously increased, and the caused greenhouse effect causes a series of environmental problems of global warming, glacier melting, species accelerated extinction and the like, thereby threatening the sustainable development of human beings.
The carbide has high melting point, strong mechanical property and excellent electrocatalytic activity, so the carbide is widely applied to the fields of wear-resistant devices and electrocatalytic electrodes. Currently, there are two main methods for preparing carbides: one is synthesized by high temperature synthesis of metal and simple carbon in reducing atmosphere or vacuum, such as tungsten powder, molybdenum powder, tantalum powder and graphite powder which are subjected to ball milling are put together in protective atmosphere to synthesize carbide at high temperature in Chinese patent No. CN 201710409843.0. The method has the advantages of high reaction temperature, long reaction time, and difficult collection of generated powder carbide. Another common method is to electrolyze mixed powder of metal oxide and elemental carbon or organic substance in molten salt by an electrochemical method, and to synthesize metal carbide by the carbonization of metal particles generated by the electrolytic reduction of metal oxide and carbon source obtained by the pyrolysis of inorganic carbon or organic substance at high temperature. The product obtained by the method is also powdery carbide, and is not easy to collect efficiently.
In addition, according to the published information at present, the existing technology for preparing carbide by the molten salt electrochemical method uses simple substance carbon or organic carbon source as raw materials, and the emission reduction of greenhouse gases cannot be realized while preparing carbide. In addition, the carbides obtained by the existing method are all powder, and the one-step in-situ generation of a functional metal carbide coating on the surface of a device cannot be realized.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing CO by aiming at the defects in the prior art2Conversion to metal carbide coating and O2The molten salt electrochemical method of (1) can effectively remove CO2The metal carbide coating can enhance the hardness and the wear resistance of the metal device and can be used as a catalyst for the electrolytic catalysis of hydrogen evolution.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
providing a process for the preparation of CO2Conversion to metal carbide coating and O2The molten salt electrochemical method of (1), comprising the steps of: using carbonate as electrolyte, high-melting-point metal as cathode and nickel-base metal as inert anode, and adding CO2Continuously introducing into molten electrolyte for electrolysis to obtain metal carbide coating on the surface of the metal cathode and oxygen at the anode.
According to the scheme, the carbonate is one or more than two of lithium carbonate, sodium carbonate, potassium carbonate, calcium carbonate and magnesium carbonate.
According to the scheme, the high-melting-point metal is one of Fe, Co, Ni, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo and W.
According to the scheme, the nickel-based metal is Ni and Ni11Fe10Cu alloy or NiCr alloy.
According to the above scheme, CO2Continuous introduction of CO into molten electrolyte2The flow rate of (A) is 20 to 100 mL/min.
According to the scheme, the electrolysis temperature is 450-950 ℃, the electrolysis time is 5 min-12 h, the electrolysis mode is one of constant current electrolysis, constant cell voltage electrolysis and pulse electrolysis, wherein the cathode current density of the constant current electrolysis is 0.1-5 Acm-2(ii) a The voltage of constant cell voltage electrolysis is 2.0-3.2V, and the effective value of current density of pulse electrolysis is 0.1-5A cm-2Or the effective voltage value is 2.0-3.2V, the pulse width is 60-5 s, and the pulse interval is 100-5 s.
The invention also provides the material with the metal carbide coating, which is obtained by the method, wherein the thickness of the metal carbide coating is 3-10 mu m.
And the application of the material with the metal carbide coating in the aspects of wear-resistant materials or electrolytic hydrogen evolution.
The invention has the beneficial effects that: 1. the electrochemical process of the invention is carried out directly with CO2As carbon source, it is directly reacted with metal substrate under electrolysis condition to convert into metal carbide coating and O2On the one hand, can realizeFormation of metal carbide coating on the surface of the conformal metal, and consumption of CO2And the emission reduction of greenhouse gases is realized. 2. The hardness of the material with the metal carbide coating layer obtained by the invention is almost 3 times of that of the substrate material, the surface wear resistance is also obviously improved, the material is used on the surfaces of high-revolution running equipment, precision tools, high-precision dies and the like to improve the performance of the material and prolong the service life, in addition, the catalytic hydrogen production performance of the synthesized metal carbide coating layer material is improved in comparison with the substrate material in the hydrogen electrolysis reaction, for example, a molybdenum sheet containing the molybdenum carbide coating layer has a much lower overpotential than a pure molybdenum sheet, namely, the hydrogen production reaction is easier to occur, and the material can be used as a catalyst for hydrogen electrolysis.
Drawings
FIG. 1 is an XRD pattern of an electrolysis product and a starting cathode metal prepared in example 1 of the present invention;
FIG. 2 is an electron micrograph of an electrolytic product prepared in example 1.
FIG. 3 is an XRD pattern of the electrolysis product and the original cathode metal prepared in example 2;
FIG. 4 is an electron micrograph of an electrolytic product prepared in example 2;
fig. 5 is a polarization curve of the electrolysis product prepared in example 1 and the catalytic hydrogen production of the original cathode metal.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings.
Example 1
Mixing CO2Conversion to metal carbide coating and O2The molten salt electrochemical method of (1): placing 250g of lithium carbonate in a high-temperature furnace, heating to 300 ℃, drying for 48h to remove water, heating to 900 ℃ again to melt the molten salt to obtain lithium carbonate molten salt, and introducing CO into the lithium carbonate molten salt at the flow rate of 50mL/min2Using nickel-chromium alloy as anode and molybdenum sheet as cathode, electrolyzing at constant voltage of 3.1V for 2h, taking out cathode after electrolysis, cooling to room temperature, respectively soaking and washing with dilute hydrochloric acid for two to three times, and respectively washing with deionized water and ethanol for three times to remove surfaceAn adherent electrolyte.
6L of carbon dioxide is introduced into the electrolysis process, wherein 30 percent of CO is consumed in the electrolysis process2To yield 1.8L O2。
After XRD analysis, Mo appears on the surface of the metal molybdenum electrode after electrolysis2Diffraction peak of C (see FIG. 1), indicating that Mo is generated2C, analyzing surface Mo by electron microscope2The C plating was about 8 microns thick (see fig. 2). The hardness of the carbide coating is as follows: 3340HV (load 150 g) and a coefficient of friction of 0.25. The hardness of the molybdenum sheet substrate is as follows: 1100HV (load of 150 g), and a coefficient of friction of 0.19.
The molybdenum electrode surface Mo of the metal of the embodiment2C coating electrolysis hydrogen evolution catalysis hydrogen production (electrolyte: 0.5M H)2SO4Using Ag/AgCl electrode as reference electrode, graphite rod as counter electrode, working electrode is molybdenum sheet containing molybdenum carbide coating, scanning speed is 2mV/s), and pure molybdenum sheet is used as working electrode to make comparison, and its polarization curve can be shown at 10mA/cm2The overpotential of the electrode containing the molybdenum carbide coating is 125mV lower than that of a pure molybdenum sheet and is 12mA/cm2The overpotential of the electrode with the molybdenum carbide coating is 110mV lower than that of a pure molybdenum sheet, namely, the electrode is easier to polarize and generate hydrogen evolution reaction (see figure 5).
Example 2
Mixing CO2Conversion to metal carbide coating and O2The molten salt electrochemical method of (1): placing 250g of lithium carbonate in a high-temperature furnace, heating to 300 ℃, drying for 48 hours, then heating to 950 ℃ to melt the molten salt to obtain lithium carbonate molten salt, and introducing CO into the molten salt at the flow rate of 50mL/min2Using metal nickel as anode and tungsten sheet as cathode, pulse electrolyzing for 12h, wherein the effective value of pulse average current density is 5A cm-2And the pulse width is 60ms, the pulse interval is 180ms, after the electrolysis is finished, the cathode is taken out, after the cathode is cooled to room temperature, the cathode is respectively soaked and washed by dilute hydrochloric acid for two to three times, and then deionized water and ethanol are used for washing for three times to remove the electrolyte adhered to the surface, so that the metal tungsten sheet with the tungsten carbide coating on the surface is obtained.
36L of carbon dioxide is introduced into the electrolysis process, wherein 20% of CO is consumed in the electrolysis process2To yield 7.2L O2。
After XRD analysis and electrolysis, a WC diffraction peak appears on the surface of the metal tungsten electrode (see figure 3), which shows that WC is generated, and the thickness of a WC coating on the surface is about 3 microns (see figure 4) through electron microscope analysis. The thickness of the obtained nickel carbide coating is 3 microns, and the hardness of the carbide coating is as follows: 2100HV (load 150 g) and a coefficient of friction of 0.23. The hardness of the tungsten plate substrate is as follows: 700HV (load of 150 g) and a coefficient of friction of 0.15.
Example 3
Mixing CO2Conversion to metal carbide coating and O2The molten salt electrochemical method of (1): mixing lithium carbonate and potassium carbonate (total 250g, mass ratio of 1:1), placing in a high temperature furnace, heating to 300 ℃, drying for 48h, heating to 700 ℃ again to melt the molten salt to obtain mixed molten salt, and introducing CO into the molten salt at a flow rate of 50mL/min2With Ni11Fe10Cu alloy as anode and iron sheet as cathode at 0.1A cm-2Constant current electrolysis for 8h at the current density of (2). And after the electrolysis is finished, taking out the cathode, respectively soaking and washing the cathode for two to three times by using dilute hydrochloric acid after the cathode is cooled to room temperature, then washing the cathode for three times by using deionized water and ethanol, and removing the electrolyte adhered to the surface to obtain the metallic iron sheet with the surface being the iron carbide coating.
24L of carbon dioxide is introduced into the electrolysis process, wherein 25 percent of CO is consumed in the electrolysis process2To yield 6L O2。
The thickness of the iron carbide coating obtained in this example was 4 μm, and the hardness of the carbide coating was: 2340HV (load of 150 g), and the coefficient of friction was 0.24. The hardness of the iron sheet substrate is as follows: 750HV (load of 150 g) and a coefficient of friction of 0.17.
Example 4
Mixing CO2Conversion to metal carbide coating and O2The molten salt electrochemical method of (1): putting lithium carbonate, sodium carbonate and potassium carbonate (the mass ratio is 2: 1:1, and the total is 400g) in a high-temperature furnace with argon protection gas, heating to 300 ℃, drying for 48 hours, heating to 450 ℃ again to melt the molten salt to obtain mixed molten salt, taking a chromium sheet as a cathode, and Ni11Fe10The Cu alloy is used as an anode, and CO is introduced into the molten salt at the flow rate of 50mL/min2Constant cell pressure at 3.2VAnd electrolyzing for 12 hours. And after the electrolysis is finished, taking out the cathode, respectively soaking and washing the cathode for two to three times by using dilute hydrochloric acid after the cathode is cooled to room temperature, and then washing the cathode for three times by using deionized water and ethanol to remove the electrolyte adhered to the surface, thereby obtaining the metal chromium sheet with the chromium carbide coating on the surface.
36L of carbon dioxide is introduced into the electrolysis process, wherein 20% of CO is consumed in the electrolysis process2To yield 7.2L O2。
The thickness of the chromium carbide coating obtained in this example was 5 μm, and the hardness of the carbide coating was: 2850HV (load 150 g) and a coefficient of friction of 0.24. The base hardness of the chromium sheet is as follows: 920HV (load of 150 g) and a coefficient of friction of 0.18.
The above examples are only specific illustrations of the technical solutions of the present invention. The invention relates to a method for mixing CO2Conversion to metal carbide coating and O2The molten salt electrochemical method of (1) is not limited to the experimental scheme and application direction given as examples, but shall be subject to the scope of the claims.

Claims (8)

1. Mixing CO2Conversion to metal carbide coating and O2The molten salt electrochemical method is characterized by comprising the following steps: using carbonate as electrolyte, high-melting-point metal as cathode and nickel-base metal as inert anode, and adding CO2Continuously introducing into molten electrolyte for electrolysis to obtain metal carbide coating on the surface of the metal cathode and oxygen at the anode.
2. The method of claim 1 wherein the CO is2Conversion to metal carbide coating and O2The molten salt electrochemical method of (1), wherein the carbonate is one or more of lithium carbonate, sodium carbonate, potassium carbonate, calcium carbonate and magnesium carbonate.
3. The method of claim 1 wherein the CO is2Conversion to metal carbide coating and O2The molten salt electrochemical method is characterized in that the high-melting-point metal is Fe, Co, Ni, Ti, Zr, Hf, V, Nb, TaCr, Mo, W.
4. The method of claim 1 wherein the CO is2Conversion to metal carbide coating and O2The molten salt electrochemical method is characterized in that the nickel-based metal is Ni and Ni11Fe10Cu alloy or NiCr alloy.
5. The method of claim 1 wherein the CO is2Conversion to metal carbide coating and O2Is characterized by CO2Continuous introduction of CO into molten electrolyte2The flow rate of (A) is 20 to 100 mL/min.
6. The method of claim 1 wherein the CO is2Conversion to metal carbide coating and O2The molten salt electrochemical method is characterized in that the electrolysis temperature is 450-950 ℃, the electrolysis time is 5 min-12 h, the electrolysis mode is one of constant current electrolysis, constant cell voltage electrolysis and pulse electrolysis, wherein the cathode current density of the constant current electrolysis is 0.1-5A cm-2(ii) a The voltage of constant cell voltage electrolysis is 2.0-3.2V, and the effective value of current density of pulse electrolysis is 0.1-5A cm-2Or the effective voltage value is 2.0-3.2V, the pulse width is 60-5 s, and the pulse interval is 100-5 s.
7. A material with a metal carbide coating obtained by the method according to any one of claims 1 to 6, wherein the metal carbide coating has a thickness of 3 to 10 μm.
8. Use of the metal carbide coated material according to claim 7 in wear resistant materials or in electrolytic hydrogen evolution.
CN201911311843.2A 2019-12-18 2019-12-18 Mixing CO2Conversion to metal carbide coating and O2Molten salt electrochemical process of Pending CN110923776A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN112725843A (en) * 2020-12-25 2021-04-30 武汉大学 Molten salt electrochemical preparation method of carbon-coated low-melting-point metal nano material
CN113151851A (en) * 2021-03-31 2021-07-23 清华大学 Carbon dioxide electrolysis device and carbon dioxide electrolysis method
CN113512740A (en) * 2021-06-18 2021-10-19 北京工业大学 Method for preparing WC-Co composite powder by using waste hard alloy
CN113584427A (en) * 2021-07-20 2021-11-02 武汉大学 Carbide coating based on high-melting-point metal and preparation method thereof
CN113718268A (en) * 2021-07-21 2021-11-30 北京工业大学 Method for recycling tungsten waste
CN114875422A (en) * 2022-03-31 2022-08-09 湖北绿钨资源循环有限公司 Method for efficiently and environmentally preparing tungsten carbide powder through molten salt electrolysis

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112725843A (en) * 2020-12-25 2021-04-30 武汉大学 Molten salt electrochemical preparation method of carbon-coated low-melting-point metal nano material
CN112725843B (en) * 2020-12-25 2022-06-03 武汉大学 Molten salt electrochemical preparation method of carbon-coated low-melting-point metal nano material
CN113151851A (en) * 2021-03-31 2021-07-23 清华大学 Carbon dioxide electrolysis device and carbon dioxide electrolysis method
CN113512740A (en) * 2021-06-18 2021-10-19 北京工业大学 Method for preparing WC-Co composite powder by using waste hard alloy
CN113584427A (en) * 2021-07-20 2021-11-02 武汉大学 Carbide coating based on high-melting-point metal and preparation method thereof
CN113718268A (en) * 2021-07-21 2021-11-30 北京工业大学 Method for recycling tungsten waste
CN114875422A (en) * 2022-03-31 2022-08-09 湖北绿钨资源循环有限公司 Method for efficiently and environmentally preparing tungsten carbide powder through molten salt electrolysis
CN114875422B (en) * 2022-03-31 2024-05-31 湖北绿钨资源循环有限公司 Method for efficiently and environmentally preparing tungsten carbide powder by fused salt electrolysis

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