CN111172562A - Preparation method of fuel aluminum for aluminum-air battery - Google Patents
Preparation method of fuel aluminum for aluminum-air battery Download PDFInfo
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- CN111172562A CN111172562A CN202010064673.9A CN202010064673A CN111172562A CN 111172562 A CN111172562 A CN 111172562A CN 202010064673 A CN202010064673 A CN 202010064673A CN 111172562 A CN111172562 A CN 111172562A
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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
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
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Abstract
The invention belongs to the field of aluminum-air batteries and new energy materials, and particularly relates to a preparation method of fuel aluminum for an aluminum-air battery; the method comprises the following steps: after fuel aluminum (aluminum alloy) is consumed in an aluminum-air battery, Al (OH) containing alloy impurities is generated3After roasting treatment at 500-1200 ℃, aluminum oxide containing alloy oxide is formed; then the aluminum oxide is used as a raw material of the non-carbon anode molten salt aluminum electrolysis process, and the aluminum oxide and alloy oxygen are electrolyzed to directly generate aluminum alloy, namely fuel aluminum; non-carbon anode molten salt aluminum electrolysis process, which adopts ceramic alloy to manufacture non-carbon anode, TiB2-C composite material as cathode; the electrolyte adopts a fluoride salt system, and the electrolysis temperature is 700-950 ℃; non-carbon in electrolytic processThe anode generates oxygen evolution reaction and discharges oxygen; the aluminum and the alloy metal are alloyed when being separated out at the cathode; the method of the invention can lead the production, application and recovery of the fuel aluminum to form a clean and environment-friendly closed cycle, and is safe and environment-friendly.
Description
Technical Field
The invention belongs to the field of aluminum-air batteries and new energy materials, and particularly relates to a preparation method of fuel aluminum for an aluminum-air battery.
Background
The aluminum-air battery is a power generation device which directly converts chemical energy stored in fuel into electric energy, has the advantages of high specific energy, long service life and the like, and is an energy-saving and efficient power generation system. In addition, the aluminum air battery has no pollution emission, and accords with the social idea of cleanness and environmental protection, so the aluminum air battery has very wide application prospect. The aluminum alloy electrode is one of the key components of the aluminum-air battery, and plays a decisive role in the service life of the battery, the electric energy conversion efficiency and the like. The aluminum alloy electrode is made of fuel aluminum through remelting of original aluminum, addition of other metal elements and alloying.
Aluminum has excellent properties such as light weight, good thermal and electrical conductivity, workability, and alloy composition with high strength and corrosion resistance, and is widely used. The aluminum air battery is used for manufacturing automobiles and airplanes, can be light in weight, is more energy-saving and environment-friendly, and is pollution-free when used for aluminum air batteries. However, in the actual industry, the production of primary aluminum requires a significant energy expenditure and is accompanied by a significant amount of greenhouse gas emissions (CO)2、CFx)。
At present, molten salt electrolysis is mainly adopted for producing the raw aluminum, and an industrialized prebaked carbon anode aluminum electrolytic cell is a main device for producing the raw aluminum. Every 1 ton of raw aluminum needs to consume over 13500kWh of alternating current, about 500kg of carbon anode is consumed, and over 1.8 tons of CO are discharged2And CFx. The preparation process of the carbon anode not only discharges CO2And discharging SOx, asphalt smoke, dust, etc., if taking into account CO generated by coal2Greenhouse effect of emissions, and consideration of CFx, is stronger than CO2Ten thousand times, so per 1 ton of raw aluminum produced, equivalent of CO converted2The discharge of (2) is more than 20 tons.
In aluminum air batteries, the aluminum is not generally used as an electrode because an oxide film is easily formed on the surface of the aluminum, so that the electrochemical activity of the aluminum is inhibited, and the potential of the electrode is reduced. In addition, aluminum is subject to hydrogen evolution corrosion in a strongly alkaline electrolyte environment, resulting in a reduction in electrode life and a reduction in current conversion efficiency. It is generally necessary to add other metal elements to improve the defects of the aluminum electrode. From the published documents at present, gallium, indium, magnesium, zinc, lead, bismuth, tin, cadmium, manganese and the like are important additive elements for increasing the activity of the aluminum electrode and inhibiting corrosion; of course, these metal elements are added in very small amounts and need to be alloyed with aluminum before they can function well.
The aluminum alloy is obtained by remelting the original aluminum again, adding the required metal elements, fully mixing, and alloying the added elements with the aluminum by a special process without segregation and burning loss or little burning loss.
Because the current production of the original aluminum increases serious environmental load, the source and the preparation process of the fuel aluminum used by the aluminum alloy electrode are very important, and whether the preparation process of the fuel aluminum is energy-saving and environment-friendly or not can play a decisive role in the actual popularization and application of the aluminum air battery, thereby hindering the popularization and application of the aluminum air battery.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of fuel aluminum capable of meeting the requirements of an aluminum-air battery. After fuel aluminum (aluminum alloy) is consumed in an aluminum-air battery, Al (OH) containing alloy impurities is generated3(ii) a Mixing the Al (OH)3After roasting treatment, forming aluminum oxide containing alloy oxide; the aluminum oxide is used as a raw material of a non-carbon anode molten salt aluminum electrolysis process, and the aluminum oxide and alloy oxygen are directly regenerated into aluminum alloy, namely fuel aluminum through electrolysis.
According to the non-carbon anode molten salt aluminum electrolysis process, oxygen is discharged, and carbon dioxide and isothermal gas are not discharged, so that a clean and environment-friendly closed cycle is formed for production, use and recovery of fuel aluminum.
In order to achieve the above purpose, the invention provides a preparation method of fuel aluminum for an aluminum-air battery, which comprises the following specific steps:
(1) al (OH) containing alloying impurities is generated after fuel aluminum (aluminum alloy) is consumed in an aluminum-air battery3Then, after roasting treatment, aluminum oxide containing alloy oxide is formed;
(2) the electrolytic bath is made of corrosion resistant material, heat insulating material and steel shell; the non-carbon anode of the electrolytic cell is prepared from a ceramic and alloy composite material; the cathode is prepared from a composite material of titanium boride and carbon; the non-carbon anode and the cathode are both connected with the metal guide rod and led out of the electrolytic bath; the molten salt electrolyte in the electrolytic cell is composed of a fluoride salt mixture;
(3) in the electrolysis process, the aluminum oxide containing the alloy oxide obtained in the step (1) is added into a molten salt electrolyte in an electrolytic cell; setting the temperature of molten salt electrolyte and starting the electrolysis process; in the electrolysis process, alumina containing alloy oxide is automatically added by a constant volume blanking device until the concentration of the alumina is 80-95% of the saturated concentration; direct current flows in from the non-carbon anode guide rod and flows out from the cathode guide rod; the alumina and the alloy oxide in the molten salt electrolyte are subjected to decomposition reaction under the action of direct current; oxygen is evolved at the non-carbon anode; aluminum and alloy are separated out and converged at the cathode to form aluminum alloy aluminum liquid; and (3) periodically taking out the aluminum alloy aluminum liquid in the electrolytic cell, and casting the aluminum alloy aluminum liquid into a required shape to obtain the fuel aluminum for the aluminum-air battery.
Preferably, the temperature of the roasting treatment in the step (1) is 500 ℃ to 1200 ℃.
Preferably, in the non-carbon anode of step (2), the ceramic and alloy composite material thereof comprises the components of Ni, Fe and Cu; the ceramic contains NiO (nickel oxide) and NiFe2O4(Nickel ferrite).
Preferably, the fluoride salt mixture in step (2) contains NaF, KF and AlF3、CaF2、MgF2、Na3AlF6、KAlF4Or Al2O3Any 2 or more of them.
Preferably, the non-carbon anode and the cathode in step (2) are arranged in an up-down structure with the non-carbon anode above and the cathode below, or in a vertical structure with the non-carbon anode and the cathode staggered.
Preferably, the molten salt electrolyte temperature in step (3) is 700-950 ℃.
Preferably, when the components of the aluminum alloy aluminum liquid in the electrolytic cell in the step (3) need to be adjusted for certain metal components, the adjustment is realized by adding oxides of corresponding metals into the electrolytic cell; the metal component is one or more of Mg, Zn, Pb, Sn, Ga, In, Bi, Hg, Ca or Sb; the addition amount of the metal oxide is 0.01-10%.
Preferably, when the components of the aluminum alloy aluminum liquid in the electrolytic cell in the step (3) need to be adjusted for certain metal components, the adjustment is realized by adding corresponding metal into the electrolytic cell; the metal is one or more of Mg, Zn, Pb, Sn, Ga, In, Bi, Hg, Ca or Sb; the addition amount of the metal is 0.01-10%.
Preferably, when the components of the aluminum alloy aluminum liquid in the electrolytic cell in the step (3) need to be adjusted for certain metal components, the aluminum alloy aluminum liquid is taken out, and then the adjustment is realized by adding corresponding metal into the aluminum alloy aluminum liquid in the casting process; the metal is one or more of Mg, Zn, Pb, Sn, Ga, In, Bi, Hg, Ca or Sb; the addition amount of the metal is 0.01-10%.
The preparation method of the fuel aluminum for the aluminum-air battery has the following advantages:
(1) the invention combines the carbon-free primary aluminum production process with the fuel aluminum alloying process, the fuel aluminum is prepared in one step, the energy is greatly saved, and O is discharged in the preparation process2And no CO2CFx isothermal chamber gas exhaust.
(2) Miscellaneous Al (OH) produced after use of fuel aluminum in fuel cells3The impure aluminum oxide obtained by drying and roasting treatment can be directly used as a raw material for producing fuel aluminum without impurity removal.
(3) The production, use and recovery of the fuel aluminum form a clean and environment-friendly closed cycle, and the method is safe and environment-friendly and is simple and convenient to operate.
Drawings
FIG. 1 is a schematic view of the structure of an electrolytic cell of example 1; wherein, 1-refractory brick; 2-stainless steel crucible; 3-corundum crucible; 4-electric furnace heating area; 5-temperature control thermocouple; 6-temperature thermocouple; 7-crucible-hearth sealing cover; 8-smoke exhaust pipe; 9-alumina blanking pipe; 10-protective gas (N)2) An inlet; 11-insulating layer of hearth of electric furnace; 12-aluminum water; 13-an electrolyte melt; 14-TiB2-a C composite cathode; 15-a non-carbon anode; 16-electrode guide rod and protective sleeve; 17-an aluminum outlet; 18-protective gas (N)2) An outlet; 19-aluminum outlet plug.
FIG. 2 is a schematic view of the structure of an electrolytic cell of example 2; wherein, 20-refractory brick; 21-stainless steel crucible; 22-TiB2-a composite block of C (cathode); 23-corundum crucibles; 24-electric furnace heating area; 25-temperature control thermocouple; 26-temperature thermocouple; 27-crucible-hearth sealing cover; 28-smoke exhaust pipe; 29-alumina feed pipe; 30-protective gas (N)2) An inlet; 31-insulating layer of electric furnace hearth; 32-aluminum water; 33-an electrolyte melt; 34-a non-carbon anode; 35-electrode guide rod and protective sleeve; 36-an aluminum outlet; 37-cathode guide bar (welded to stainless steel crucible); 38-protective gas (N)2) An outlet; 39-aluminum outlet plug.
Detailed Description
The invention is further described with reference to the following examples, but without limiting its scope.
Example 1:
the structure of the non-carbon anode molten salt aluminum electrolysis cell in the embodiment is shown as a figure (1) in the attached drawings. The electrolytic bath is an external heating type and is composed of an electric heating furnace, a crucible, electrodes, electrolyte and the like. In the figure, 1 is a refractory brick; 2 is a stainless steel crucible; 3 is a corundum crucible; 4 is an electric furnace heating area; 5 is a temperature control thermocouple; 6 is a temperature thermocouple; 7 is a crucible-hearth sealing cover; 8 is a smoke exhaust pipe; 9 is an alumina feeding pipe; 10 is protective gas (N)2) An inlet; 11 is an insulating layer of a hearth of the electric furnace; 12 is molten aluminum; 13 is an electrolyte melt; 14 is TiB2-a C composite cathode; 15 is a non-carbon anode; 16 is an electrode guide rod and a protective sleeve; 17 is an aluminum outlet; 18 is a protective gas (N)2) An outlet; and 19 is an aluminum outlet plug.
Al (OH) containing alloy impurities is generated after fuel aluminum (aluminum alloy) is consumed in an aluminum-air battery3After roasting treatment at 1000 ℃, forming aluminum oxide containing alloy oxide;
the non-carbon anode is made of ceramic alloy, and the ceramic matrix is NiO and NiFe2O4The alloy components are Ni, Fe and Cu; the cathode adopts TiB2-a C composite material; 2 anodes and 1 cathode are adopted, the cathodes and the anodes are in a staggered vertical structure, are all connected with a metal guide rod and are led out of the groove by the guide rod;
the molten salt electrolyte in the electrolytic cell is composed of a fluoride salt mixture; the specific electrolyte adopts KF-NaF-AlF3-Al2O3An electrolyte system, wherein the obtained aluminum oxide containing alloy oxide is added into a molten salt electrolyte to start an electrolysis process; in the electrolysis process, alumina containing alloy oxide is automatically added by a constant-volume blanking device, and the concentration of the alumina is close to 90% of the saturated concentration;
the liquid phase temperature of the molten salt electrolyte is 780 ℃, and the electrolysis temperature is more than 800 ℃; the direct current intensity is 200A; after current is introduced, the non-carbon anode working surface generates oxygen evolution reaction of alumina decomposition; the aluminum and the alloy metal are alloyed when being separated out at the cathode; the obtained alloyed aluminum liquid is gathered at the bottom of the crucible;
and in the operation process, an aluminum discharging spoon is used every 48 hours, aluminum is manually discharged once, and the aluminum is directly cast into a required shape through a die at a high temperature, so that the fuel aluminum for the aluminum-air battery is obtained. An aluminum alloy block with a good shape is selected, an aluminum alloy electrode for a small aluminum-air battery is manufactured through machining, and through testing, the current efficiency of the battery can reach 90.2%.
When the aluminum alloy liquid In the electrolytic bath needs to be adjusted to Al-Zn-Sn-Ga-In alloy, the adjustment is realized by adding oxides of corresponding metals into the electrolytic bath; according to the component analysis of the aluminum liquid, 2 percent of ZnO and 0.15 percent of SnO are added into an aluminum oxide blanking box of an electrolytic cell20.02% of Ga2O3And 0.01% of In2O3。
When the aluminum alloy electrode is consumed in the aluminum-air battery, the recovered battery contains Al (OH)3Filtering, drying and roasting the emulsion to form mixed alumina, and returning the prepared alumina to the electrolytic bath without abnormality in the electrolytic process.
Example 2:
the structure of the non-carbon anode molten salt aluminum electrolysis cell in the embodiment is shown as a figure (2) in the attached drawings. The electrolytic bath is an external heating type and is composed of an electric heating furnace, a crucible, electrodes, electrolyte and the like. Indicated in the drawing, 20 is a refractory brick; 21 is a stainless steel crucible; 22 is TiB2-a composite block of C (cathode); 23 is corundumA crucible; 24 is a heating area of the electric furnace; 25 is a temperature control thermocouple; 26 is a temperature thermocouple; 27 is a crucible-hearth sealing cover; 28 is a smoke exhaust pipe; 29 is an alumina feeding pipe; 30 is protective gas (N)2) An inlet; 31 is an insulating layer of a hearth of the electric furnace; 32 is molten aluminum; 33 is an electrolyte melt; 34 is a non-carbon anode; 35 is an electrode guide rod and a protective sleeve; 36 is an aluminum outlet; 37 is a cathode guide rod (welded with a stainless steel crucible); 38 is a protective gas (N)2) An outlet; and 39 is an aluminum outlet plug.
The non-carbon anode is made of ceramic alloy, and the ceramic matrix is NiO and NiFe2O4The alloy components are Ni, Fe and Cu. The cathode adopts TiB2-a C composite material. The electrode structure is arranged in an upper-lower structure with an anode at the upper part and a cathode at the lower part, and 1 anode and 1 cathode are arranged; the electrolyte adopts NaF-AlF3-Al2O3The electrolyte system has a liquid phase temperature of 850 ℃ and an electrolysis temperature of more than 860 ℃; the DC current intensity is 200A; the alumina adopts Al (OH) generated in an aluminum-air battery3The mixed alumina obtained by roasting at 1000 ℃ is automatically added by a constant-volume blanking device in the electrolytic process; the concentration of alumina is close to 80% of the saturation concentration;
after direct current is introduced, the non-carbon anode working surface generates oxygen evolution reaction of alumina decomposition; the aluminum and the alloy metal are alloyed when being separated out at the cathode; the obtained alloyed aluminum liquid is gathered at the bottom of the crucible. And in the operation process, an aluminum discharging spoon is used every 48 hours, aluminum is manually discharged once, and the aluminum is directly cast into a required shape through a die at a high temperature, so that the fuel aluminum for the aluminum-air battery is obtained. An aluminum block with a good shape is selected, an aluminum alloy electrode for a small aluminum-air battery is manufactured through machining, and through testing, the current efficiency of the battery can reach 91.3%.
When the aluminum alloy composition in the electrolytic bath needs to be adjusted to Al-Bi-Pb-Sb-Ga, the adjustment is realized by adding corresponding metal into the electrolytic bath; according to the component analysis of the aluminum liquid, 1 percent of Bi powder or block, 0.3 percent of Pb powder or block, 0.05 percent of Sb powder or block and 0.01 percent of Ga powder or block are directly added into the aluminum liquid of the electrolytic cell.
When the aluminum alloy electrode is consumed in the aluminum-air batteryThen, Al (OH) is contained in the recovered battery3Filtering, drying and roasting the emulsion to form alumina, and returning the prepared alumina to the electrolytic bath, wherein the electrolysis process is not abnormal.
Description of the drawings: the above embodiments are only used to illustrate the present invention and do not limit the technical solutions described in the present invention; thus, while the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted; as long as the impurity-containing Al (OH) recovered from the aluminum-air battery is used3The method for directly preparing aluminum alloy for aluminum-air battery, namely fuel aluminum by non-carbon anode aluminum electrolysis by using the prepared hybrid aluminum oxide has the advantages that although the specific size, structure, anode composition, electrolyte composition, electrolysis process parameters, current magnitude and the like are changed, the technical scheme and the improvement thereof without departing from the spirit and scope of the invention are all covered in the scope of the claims of the invention.
Claims (9)
1. A preparation method of fuel aluminum for an aluminum-air battery is characterized by comprising the following specific steps:
(1) al (OH) containing alloy impurities is generated after fuel aluminum is consumed in the aluminum-air battery3Then, after roasting treatment, aluminum oxide containing alloy oxide is formed;
(2) the electrolytic bath is made of corrosion resistant material, heat insulating material and steel shell; the non-carbon anode of the electrolytic cell is prepared from a ceramic and alloy composite material; the cathode is prepared from a composite material of titanium boride and carbon; the non-carbon anode and the cathode are both connected with the metal guide rod and led out of the electrolytic bath; the molten salt electrolyte in the electrolytic cell is composed of a fluoride salt mixture;
(3) in the electrolysis process, the aluminum oxide containing the alloy oxide obtained in the step (1) is added into a molten salt electrolyte in an electrolytic cell; setting the temperature of molten salt electrolyte and starting the electrolysis process; in the electrolysis process, alumina containing alloy oxide is automatically added by a constant volume blanking device until the concentration of the alumina is 80-95% of the saturated concentration; direct current flows in from the non-carbon anode guide rod and flows out from the cathode guide rod; the alumina and the alloy oxide in the molten salt electrolyte are subjected to decomposition reaction under the action of direct current; oxygen is evolved at the non-carbon anode; aluminum and alloy are separated out and converged at the cathode to form aluminum alloy aluminum liquid; and (3) periodically taking out the aluminum alloy aluminum liquid in the electrolytic cell, and casting the aluminum alloy aluminum liquid into a required shape to obtain the fuel aluminum for the aluminum-air battery.
2. The method for preparing fuel aluminum for the aluminum-air battery according to claim 1, wherein the temperature of the roasting treatment in the step (1) is 500 ℃ to 1200 ℃.
3. The method for preparing fuel aluminum for an aluminum-air battery according to claim 1, wherein in the step (2), the composition of the alloy in the composite material of the ceramic and the alloy which form the non-carbon anode comprises elements of Ni, Fe and Cu; the ceramic comprises NiO and NiFe2O4。
4. The method for preparing fuel aluminum for an aluminum-air battery according to claim 1, wherein the fluoride salt mixture in the step (2) contains NaF, KF, AlF3, CaF2, MgF2, Na3AlF6, KAlF4 or Al2O3Any 2 or more of them.
5. The method for preparing fuel aluminum for an aluminum-air battery according to claim 1, wherein the non-carbon anode and the cathode are arranged in the step (2) in an up-down structure with the non-carbon anode on top and the cathode on bottom, or in a vertical structure with the non-carbon anode and the cathode staggered.
6. The method for preparing fuel aluminum for the aluminum-air battery according to claim 1, wherein the temperature of the molten salt electrolyte in the step (3) is 700-950 ℃.
7. The method for preparing fuel aluminum for the aluminum-air battery according to claim 1, wherein when the composition of the aluminum alloy aluminum liquid in the electrolytic cell in the step (3) needs to be adjusted for a certain metal composition, the adjustment is realized by adding oxides of the corresponding metals into the electrolytic cell; the metal is one or more of Mg, Zn, Pb, Sn, Ga, In, Bi, Hg, Ca or Sb; the addition amount of the metal oxide is 0.01-10%.
8. The method for preparing fuel aluminum for the aluminum-air battery according to claim 1, wherein when the composition of the aluminum alloy aluminum liquid in the electrolytic cell in the step (3) needs to be adjusted for a certain metal composition, the adjustment is realized by adding a corresponding metal to the electrolytic cell; the metal is one or more of Mg, Zn, Pb, Sn, Ga, In, Bi, Hg, Ca or Sb; the addition amount of the metal is 0.01-10%.
9. The method for preparing fuel aluminum for the aluminum-air battery according to claim 1, wherein when the composition of the aluminum alloy aluminum liquid in the electrolytic cell in the step (3) needs to be adjusted for a certain metal composition, the aluminum alloy aluminum liquid is taken out and then adjusted by adding a corresponding metal to the aluminum alloy aluminum liquid in the casting process; the metal is one or more of Mg, Zn, Pb, Sn, Ga, In, Bi, Hg, Ca or Sb; the addition amount of the metal is 0.01-10%.
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| CN115478303A (en) * | 2021-05-31 | 2022-12-16 | 浙江睿曦绿业新材料科技有限公司 | Oxygen aluminium coproduction does not have carbon and does not have useless electrolysis trough admittedly |
| CN116043276A (en) * | 2023-01-04 | 2023-05-02 | 中铝郑州有色金属研究院有限公司 | A vertical structure inert anode aluminum electrolytic cell |
| CN116426979A (en) * | 2021-12-31 | 2023-07-14 | 浙江睿曦绿业新材料科技有限公司 | Renewable energy consumption device and working method based on carbon-free and solid waste aluminum electrolyzer |
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