CN113832473B - Molten salt electrochemical method for co-producing metal/carbon composite material and hydrogen - Google Patents
Molten salt electrochemical method for co-producing metal/carbon composite material and hydrogen Download PDFInfo
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- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/04—Electrolytic production, recovery or refining of metals by electrolysis of melts of magnesium
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- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
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- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
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- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/34—Electrolytic production, recovery or refining of metals by electrolysis of melts of metals not provided for in groups C25C3/02 - C25C3/32
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- C—CHEMISTRY; METALLURGY
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- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/36—Alloys obtained by cathodic reduction of all their ions
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- 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 relates to a molten salt electrochemical method for co-producing metal/carbon composite material and hydrogen. In the chloride molten salt electrolyte containing oxygen ions, low-melting-point metal is used as a cathode, methane is introduced to the surface of an anode, direct current is conducted between the anode and the cathode, the anode potential is controlled between partial oxidation hydrogen evolution potential of the methane and oxidation oxygen evolution potential of the oxygen ions during electrolysis, methane oxidation reaction is carried out on the anode to generate hydrogen, and carbon in the methane is combined with liquid metal at the cathode to generate a metal/carbon composite material. The method has simple steps, can take the greenhouse gas methane as a hydrogen source and a carbon source at the same time, obtains high-purity hydrogen at the anode, and simultaneously fixes carbon atoms of the methane at a low-melting-point metal cathode in a solid form to obtain a metal/carbon composite material, thereby realizing effective separation of hydrogen and carbon as products. Realizes the conversion of methane into hydrogen and high added value carbon, and the added value utilization of low-melting point metal.
Description
Technical Field
The invention belongs to the field of material metallurgy and also belongs to the field of energy efficient conversion, and particularly relates to a molten salt electrochemical method for co-producing a metal/carbon composite material and hydrogen.
Background
The rapid development of economy is accompanied by an increasing consumption of fossil energy, thereby causing various energy crisis and environmental pollution. Therefore, research on green energy and energy storage technology is widely focused.
In the aspect of energy storage, the carbon nanomaterial is applied to the field of electrochemical energy storage due to stable chemical properties, various morphology structures and good electric conduction performance. However, the conventional carbon material anode has a low theoretical capacity. The carbon material and the metal are compounded, so that the obtained metal/carbon material has higher theoretical capacity on one hand, and on the other hand, the problems of agglomeration, volume expansion and the like of the metal with high energy density can be effectively prevented, and the energy storage performance of the metal/carbon material is effectively improved.
In the aspect of green energy, the hydrogen energy has the advantages of high heat value, convenient storage, easy regeneration, zero pollution and the like, so that the demand of the hydrogen energy in the industrial field is increased year by year. Methane reforming is an important mode for hydrogen production at present, but how to safely and efficiently separate hydrogen from other byproducts in the hydrogen production process is always a difficult problem to be solved. In addition, the large amount of carbon deposited as a solid by-product is extremely liable to cause catalyst deactivation during the catalytic reaction, incomplete reaction and CO 2 Emission and the like, and the difficult reuse of carbon products and the like are also a waste of resources.
In view of the materials disclosed at present, the existing methane hydrogen production process faces the great challenges of high purification of hydrogen and improvement of the added value of carbon products, and the reaction temperature of the existing methane hydrogen production process is high and difficult to control.
Disclosure of Invention
The invention aims to provide a molten salt electrochemical method capable of co-producing a metal/carbon composite material and hydrogen, wherein methane is used as a hydrogen source and a carbon source at the same time, the methane is anodized into hydrogen, and carbon is fixed on a low-melting-point metal electrode to obtain the metal/carbon composite material.
In order to achieve the above purpose, the invention adopts the following technical scheme:
in the fused salt electrochemical method for co-producing metal/carbon composite material and hydrogen gas, in the chloride fused salt electrolyte containing oxygen ion, low-melting point metal is used as cathode, methane is fed into the surface of anode, and between anode and cathode a direct current is fed, and during electrolysis the anode potential is controlled between partial oxidation hydrogen-evolution potential of methane and oxygen ion oxidation oxygen-evolution potential so as to make anode produce methane oxidation reaction to produce hydrogen gas, at the same time the carbon in methane is combined with low-melting point metal at cathode, and the cathode product is collected, washed and dried so as to obtain the metal/carbon composite material.
Preferably, the molten salt electrolyte comprises a chloride molten salt and an additional oxide.
Preferably, the chloride molten salt is optionally selected from LiCl, naCl, KCl, caCl 2 Or MgCl 2 One or more of the following; the additional oxide is selected from Li 2 O，Na 2 O，K 2 O，CaO，CO 2 One or more of the following.
Preferably, the low melting point metal is in a liquid state during electrolysis.
Preferably, the low-melting-point metal is selected from one of Zn, sn, ga, al, mg, bi, pb and Cu, or an alloy consisting of any two or more of Zn, sn, ga, al, mg, bi, pb and Cu.
Preferably, the anode is made of Au, ag, pt, ni, cu and RuO 2 Any one of NiFe alloy, niFeCu alloy, ni-YSZ, co-YSZ, cu-GDC, ru-GDC, LSM.
Preferably, during electrolysis, the current or potential is controlled such that the anode potential is between the methane partial oxidation hydrogen evolution potential and the oxygen ion oxidation oxygen evolution potential, i.e. the anode potential is more positive than the methane partial oxidation hydrogen evolution potential and more negative than the oxygen ion oxidation oxygen evolution potential. Further, the anode potential is between 0.4 and 1.4V vs. Ag/AgCl.
Preferably, the electrolysis time is 15 min-24 h.
Preferably, the electrolysis temperature is between 400 and 850 ℃.
Preferably, the methane is a mixture of methane and inert gas, wherein the volume fraction of methane is 0.001% -99.99%. Further preferably, the inert gas component is nitrogen, argon or helium.
In the electrolytic process, methane is electrooxidized to H at the anode 2 And CO production 3 2－ CO produced 3 2－ The metal oxide and carbon are obtained by chemical reaction with a liquid metal cathode, the metal oxide is reduced into metal by electrochemical reaction of the cathode, and meanwhile, CO 3 2－ Reduced to carbon on the liquid metal electrode. The process can effectively separate hydrogen and carbon products in space to obtain high-purity hydrogen, and carbon and cathode liquid metal are combined and converted into a metal/carbon composite material, so that the composite material has good conductivity, can be widely applied to the fields of electrocatalysis, batteries, capacitors and the like, improves the added value of solid carbon, realizes the value-added and utilization of low-melting-point metal, and simultaneously realizes the effective conversion of methane.
The method has simple steps and mild reaction conditions, and can effectively control the formation of the carbon-coated metal structure of the cathode product and the content of metal and carbon in the product by controlling the reaction time, the temperature and the electrolytic potential. Particularly, methane is used as a hydrogen source and a carbon source at the same time, the methane is anodized into hydrogen, and carbon is fixed on a low-melting-point metal electrode to obtain a metal/carbon composite material, so that high-purity hydrogen can be obtained, and the added value of the carbon material and the added value utilization of the low-melting-point metal are improved.
Drawings
FIG. 1 XRD pattern of the electrolytic product of example 1;
FIG. 2 is an electron micrograph of a metal Zn/carbon composite material obtained by electrolysis in example 1;
FIG. 3 example 1 potentiostatic electrolysis corresponds to the variation of the product concentration of the anode gas;
FIG. 4 XRD pattern of the electrolytic product of example 2;
FIG. 5 an electron micrograph of the metal/carbon composite obtained by electrolysis in example 2;
FIG. 6 is an electron micrograph of a carbon material obtained by cathodic electrolysis of a refractory metal of comparative example 1.
Detailed Description
For a better understanding of the present invention, the following examples are further illustrative of the present invention, but the contents of the present invention are not limited to the following examples only.
The invention will be further illustrated with reference to specific examples, but the scope of the invention is not limited thereto. Insubstantial modifications and variations in the form and content of the invention as per the principles of the invention are within the scope of the invention as per the claims of this patent.
Example 1:
by CaCl 2 500g of molten salt (molar ratio: 52:48) was used as an electrolyte, 20g of CaO was added thereto, and the mixture was poured into a crucible after uniform mixing. Heating to 250 ℃ at 5 ℃/min, and preserving heat for 24 hours to completely volatilize water in the molten salt. Then heating to 850 ℃ at 5 ℃/min, introducing argon as a protective atmosphere, preserving heat for 3 hours, and cooling and maintaining the temperature at 700 ℃. The metal Au sheet is used as an anode, 3vol% methane is introduced to the surface of the metal Au sheet, liquid Zn is used as a cathode, 0.8V vs. Ag/AgCl is used for electrolysis for 5 hours, meanwhile, the online gas chromatograph is used for monitoring that hydrogen is synchronously separated out from the anode region (see figure 3), and other gases except methane and argon are not monitored, namely methane is cracked into hydrogen at the anode. After the electrolysis is finished, the liquid Zn electrode is taken out, and is respectively washed by deionized water and absolute ethyl alcohol for three times, so that a metal Zn/carbon composite material (shown in the attached drawings 1 and 2) is obtained, namely, carbon in methane and a liquid zinc cathode are composited and converted into a Zn/carbon composite material.
Example 2:
by CaCl 2 500g of molten salt of NaCl (molar ratio 52:48) is used as electrolyte, and the mixture is poured into a crucible after being uniformly mixed. Heating to 300 ℃ at 5 ℃/min, and preserving heat for 24 hours to completely volatilize water in the molten salt. Then the temperature is raised to 850 ℃ at 5 ℃/min, argon is simultaneously introduced as a protective atmosphere, the temperature is kept for 3 hours, and then the temperature is reduced to 850 ℃ and kept at 850 ℃. CO is processed by 2 Introducing into molten salt medium at a speed of 100mL/min as an additional oxide, introducing 10vol% methane into the surface of a metal Ru-GDC sheet serving as an anode, using liquid SnBi alloy as a cathode, electrolyzing for 1h at a potential of 1.2V vs. Ag/AgCl, synchronously monitoring the anode region by using online gas chromatography to synchronously separate out hydrogen, and removing methane and CO 2 No other gases were detected. After the electrolysis is finished, taking out the liquid SnBi alloy electrode was washed three times with deionized water and absolute ethanol, respectively, to obtain metal SnBi/carbon composite material (see FIG. 4 and FIG. 5).
Comparative example 1:
introducing 10vol% methane on the surface of metal Ru-GDC sheet, using high melting point metal Mo as cathode, electrolyzing for 1 hr with potential of 1.2V vs. Ag/AgCl, synchronously monitoring the anode region by online gas chromatography to synchronously separate out hydrogen, removing methane and CO 2 No other gases were detected. After the electrolysis is finished, the solid Mo electrode is taken out, and is respectively washed three times by deionized water and absolute ethyl alcohol to obtain the carbon material (see figure 6).
Example 3
500g of LiCl and NaCl (molar ratio 1:1) are used as electrolyte, and 20g of Na is added 2 And O, pouring the mixture into a crucible after uniformly mixing. Heating to 300 ℃ at 5 ℃/min, and preserving heat for 24 hours to completely volatilize water in the molten salt. Then the temperature is raised to 850 ℃ at 5 ℃/min, argon is simultaneously introduced as a protective atmosphere, the temperature is kept for 3 hours, and then the temperature is reduced to 650 ℃ and kept at 650 ℃. Taking a metal Cu net as an anode, introducing methane on the surface of the metal Cu net, taking liquid Ga as a cathode, and taking the liquid Ga as a cathode at a concentration of 40mA/cm 2 The anode potential was monitored to be 0.81vs. Ag/AgCl during electrolysis for 12 h. Simultaneously, the online gas chromatography is used for monitoring that the anode synchronously separates out hydrogen, and other gases except methane are not monitored. And after the electrolysis is finished, taking out the liquid Ga electrode, respectively cleaning the liquid Ga electrode with deionized water and absolute ethyl alcohol for three times, and analyzing the product by XRD to obtain the metal Ga/carbon composite material.
Example 4:
with KCl and NaCl (mass ratio of 48:52) 500g molten salt as electrolyte, 10g Na is added 2 And O, pouring the mixture into a crucible after uniformly mixing. Heating to 250 ℃ at 5 ℃/min, and preserving heat for 24 hours to completely volatilize water in the molten salt. Then heating to 700 ℃ at 5 ℃/min, introducing argon as a protective atmosphere, preserving heat for 3 hours, and cooling and maintaining the temperature at 600 ℃. Taking a metal Ni-YSZ sheet as an anode, introducing 50vol% methane on the surface of the metal Ni-YSZ sheet, taking liquid Al as a cathode, and taking the concentration of 5mA/cm 2 The anode potential during electrolysis was monitored to be 0.43V vs. Ag/AgCl for 9 h. At the same time use on-line gas chromatographyThe anode was tested for simultaneous evolution of hydrogen and no other gases other than methane were monitored. And after the electrolysis is finished, taking out the liquid Al electrode, respectively cleaning the liquid Al electrode with deionized water and absolute ethyl alcohol for three times, and analyzing the product by XRD to obtain the metal Al/carbon composite material.
Example 5:
500g of molten salt is taken as electrolyte, liCl and KCl (molar ratio is 1:1), and 10g of Li is added 2 And pouring the mixture into a crucible after uniformly mixing the O. Heating to 300 ℃ at 5 ℃/min, and preserving heat for 24 hours to completely volatilize water in the molten salt. Then heating to 400 ℃ at 5 ℃/min, simultaneously introducing argon as a protective atmosphere, preserving heat for 3 hours, and then keeping the temperature at 550 ℃. Taking metal foam Au as an anode, introducing methane on the surface of the metal foam Au, taking liquid Mg as a cathode, and taking the average current density as 80mA/cm 2 The on-off ratio is 100s: the electrolysis was carried out for 3h with a pulsed current of 20s, and the anode potential was monitored to be 1.31V vs. Ag/AgCl during the electrolysis. Simultaneously, the online gas chromatography is used for monitoring that the anode synchronously separates out hydrogen, and other gases except methane are not monitored. And after the electrolysis is finished, taking out the liquid Mg electrode, respectively cleaning the liquid Mg electrode with deionized water and absolute ethyl alcohol for three times, and analyzing the product by XRD to obtain the metal Mg/carbon composite material.
Example 6:
500g of molten salt was used as an electrolyte at LiCl, KCl, naCl (molar ratio 1:1:1). Heating to 300 ℃ at 5 ℃/min, and preserving heat for 24 hours to completely volatilize water in the molten salt. Then heating to 400 ℃ at 5 ℃/min, introducing argon as a protective atmosphere, preserving heat for 3 hours, and then keeping at 400 ℃. CO is processed by 2 Introducing the metal NiFeCu alloy sheet as anode into molten salt medium at a speed of 100mL/min as an added oxide, introducing methane on the surface of the metal NiFeCu alloy sheet, using liquid Pb as cathode, electrolyzing for 3h at a potential of 1.4V vs. Ag/AgCl, simultaneously monitoring the synchronous separation of hydrogen from the anode by using online gas chromatography, removing methane and CO 2 No other gases were detected. And after the electrolysis is finished, taking out the liquid Pb electrode, respectively cleaning the liquid Pb electrode with deionized water and absolute ethyl alcohol for three times, and analyzing the product by XRD to obtain the metal Pb/carbon composite material.
While the invention has been described with respect to the preferred embodiments, it will be understood that the invention is not limited thereto, but is capable of modification and variation without departing from the spirit of the invention, as will be apparent to those skilled in the art.
Claims (7)
1. A molten salt electrochemical method for co-producing metal/carbon composite material and hydrogen is characterized in that in a chloride molten salt electrolyte containing oxygen ions, low-melting-point metal is used as a cathode, methane is introduced to the surface of an anode, direct current is introduced between the anode and the cathode, and the anode potential is controlled between partial oxidation hydrogen evolution potential of the methane and oxygen ion oxidation oxygen evolution potential during electrolysis, so that methane oxidation reaction is carried out on the anode to generate hydrogen, and meanwhile, carbon in the methane is combined with the low-melting-point metal at the cathode to generate the metal/carbon composite material;
the molten salt electrolyte comprises chloride molten salt and externally added oxide;
the low-melting-point metal is in a liquid state in the electrolysis process;
in the electrolytic process, the anode potential is between 0.4 and 1.4V vs. Ag/AgCl.
2. The molten salt electrochemical method for co-producing metal/carbon composite and hydrogen of claim 1, wherein said chloride molten salt is optionally selected from LiCl, naCl, KCl, caCl 2 Or MgCl 2 One or more of the following; the oxygen ions are derived from Li 2 O，Na 2 O，K 2 O，CaO，CO 2 One or more of the following.
3. The molten salt electrochemical method for co-producing metal/carbon composite material and hydrogen according to claim 1, wherein the low melting point metal is any one selected from Zn, sn, ga, al, mg, bi, pb, cu, or an alloy consisting of any two or more of Zn, sn, ga, al, mg, bi, pb, cu.
4. A molten salt electrochemical method of co-producing metal/carbon composite and hydrogen according to claim 1, whichIs characterized in that the anode adopts Au, ag, pt, ni, cu and RuO as materials 2 Any one of NiFe alloy, niFeCu alloy, ni-YSZ, co-YSZ, cu-GDC, ru-GDC, LSM.
5. The molten salt electrochemical method for co-producing metal/carbon composite material and hydrogen according to claim 1, wherein the electrolysis time is 15min to 24h.
6. The molten salt electrochemical method for co-producing metal/carbon composite and hydrogen of claim 1 wherein the electrolysis temperature is between 400 and 450 ℃.
7. The molten salt electrochemical method for co-producing metal/carbon composite material and hydrogen according to claim 1, wherein the methane is a mixture of methane and inert gas, and the volume fraction of methane is 0.001% -99.99%.
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| GB1215002A (en) * | 1967-02-02 | 1970-12-09 | Courtaulds Ltd | Coating carbon with metal |
| CN110257848A (en) * | 2019-06-10 | 2019-09-20 | 武汉大学 | Middle low-temperature oxidation methane is the melten salt electriochemistry method of hydrogen and carbon monoxide |
| CN110359068A (en) * | 2019-08-07 | 2019-10-22 | 武汉大学 | A method of carbon nanotube metal material for coating is prepared based on melten salt electriochemistry method |
| 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 |
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| GB1215002A (en) * | 1967-02-02 | 1970-12-09 | Courtaulds Ltd | Coating carbon with metal |
| CN110257848A (en) * | 2019-06-10 | 2019-09-20 | 武汉大学 | Middle low-temperature oxidation methane is the melten salt electriochemistry method of hydrogen and carbon monoxide |
| CN110359068A (en) * | 2019-08-07 | 2019-10-22 | 武汉大学 | A method of carbon nanotube metal material for coating is prepared based on melten salt electriochemistry method |
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