CN112458323B - Method for preparing nickel-based alloy by recycling waste nickel-hydrogen battery - Google Patents
Method for preparing nickel-based alloy by recycling waste nickel-hydrogen battery Download PDFInfo
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- CN112458323B CN112458323B CN202011163026.XA CN202011163026A CN112458323B CN 112458323 B CN112458323 B CN 112458323B CN 202011163026 A CN202011163026 A CN 202011163026A CN 112458323 B CN112458323 B CN 112458323B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/02—Obtaining nickel or cobalt by dry processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention provides a method for preparing nickel-based alloy by recycling waste nickel-hydrogen batteries, which comprises the following steps of (a) crushing and separating the waste nickel-hydrogen batteries to obtain nickel-rich particles; (b) adding the nickel-rich particles and the separating agent into a high-temperature resistant container, stirring and preserving heat after the nickel-rich particles and the separating agent are completely melted; (c) adjusting the temperature of a high-temperature resistant container to 1430-1480 ℃, adding a certain amount of slag removing agent into a molten product in the high-temperature resistant container, stirring and preserving heat, and finally casting the molten liquid after scum removal to form a nickel ingot; (d) detecting the metal components of the nickel ingot, supplementing corresponding metals into the nickel ingot according to the requirements of the metal components of the nickel-based alloy, adding the nickel ingot and the supplemented corresponding metals into a vacuum smelting furnace filled with inert gas, stirring and preserving heat after the nickel ingot and the supplemented corresponding metals are completely melted, then adding a certain amount of reducing agent to prepare nickel liquid, and casting the nickel liquid to form the nickel-based alloy. The invention has simple and novel process, high product purity and less pollution.
Description
Technical Field
The invention relates to a method for preparing a nickel-based alloy by recycling waste nickel-hydrogen batteries.
Background
Environmental pollution and petroleum energy crisis problems jointly promote the development of energy-saving and new energy automobiles. With the rapid development of domestic electric vehicles, the usage amount of power batteries is gradually increased. However, power batteries have a certain service life, and need to be replaced after a period of use to generate more waste batteries, and the waste nickel-hydrogen batteries contain metal nickel, cobalt, manganese, iron, rare earth and the like, and these elements, if not treated, will have a great threat to the natural environment and human health, and will generate great resource waste. After the traditional waste nickel-metal hydride battery is pretreated, active substance powder, a diaphragm and the like can be sorted out, and the active substance powder is subjected to wet treatment.
Disclosure of Invention
The invention aims to provide a method for preparing a nickel-based alloy by recycling waste nickel-hydrogen batteries, which has the advantages of simple and novel process, high product purity and less pollution.
The invention is realized by the following scheme:
a method for preparing a nickel-based alloy by recycling waste nickel-metal hydride batteries comprises the following steps:
(a) crushing the waste nickel-metal hydride battery, separating active substance powder, a diaphragm and mixed particles containing plastic iron and nickel, and putting the mixed particles containing plastic iron and nickel into a magnetic separation device to separate plastic particles, iron-rich particles and nickel-rich particles; the nickel-rich particles generally contain nickel and a small amount of diaphragm, cobalt, iron, manganese, rare earth metals and oxides thereof; during specific production, plastic particles are partially selected from the upper part of the magnetic separation device, nickel-rich particles are partially selected from the middle part of the magnetic separation device, and iron materials are selected from the lower part of the magnetic separation device by adjusting basic parameters such as magnetic strength of the magnetic separation device;
(b) adding the nickel-rich particles separated in the step (a) and a separating agent into a high-temperature resistant container, heating the high-temperature resistant container to 1500-1580 ℃, stirring and preserving heat for 20-30 min after the nickel-rich particles and the separating agent are completely melted, and removing surface scum in the stirring process, wherein most of the oxides of metals such as diaphragms, active substance powder, plastics, nickel, iron, cobalt, manganese, rare earth and the like in the nickel-rich particles are removed as scum;
(c) adjusting the temperature of a high-temperature resistant container to 1430-1480 ℃, adding a certain amount of slag removing agent into a molten product in the high-temperature resistant container, stirring and preserving heat for 10-15 min, removing surface scum in the stirring process, and finally casting the molten liquid after scum removal to form a nickel ingot; in the step, a small amount of rare earth metal left in the nickel-rich particles forms scum to be separated from the melt, and simultaneously, a small amount of nickel-cobalt-manganese oxide left in the nickel-rich particles is reduced, so that high-purity melt containing a small amount of cobalt and manganese is obtained;
(d) detecting the metal components of the nickel ingot obtained in the step (c), supplementing corresponding metals into the nickel ingot according to the requirements of the metal components of the nickel-based alloy, adding the nickel ingot and the supplemented corresponding metals into a vacuum smelting furnace filled with inert gas, heating the vacuum smelting furnace to 1650-1750 ℃, stirring and preserving heat for 5-10 min after the nickel ingot and the supplemented corresponding metals are completely melted, then adding a certain amount of reducing agent into the molten product in the vacuum smelting furnace under the condition that the temperature of the vacuum smelting furnace is not changed, stirring and removing surface scum, namely surface trace oxygen to prepare nickel liquid, standing for 15-25 min, and casting the nickel liquid to form the nickel-based alloy. The inert gas is generally argon or helium, and argon is often used in view of cost.
Further, in the step (b), the addition amount of the separating agent is 6-15% of the mass of the nickel-rich particles.
Further, in the step (b), the separating agent is a mixture of sodium chloride particles, sodium hexafluoroaluminate particles and aluminum fluoride particles, and the mass ratio of the sodium chloride particles to the sodium hexafluoroaluminate particles to the aluminum fluoride particles is 64-76: 14-20: 6 to 20.
Further, in the step (c), the slag removing agent is one of trees, heavy oil, light diesel oil and natural gas, the pressure of the natural gas is 0.2Mpa, and the adding amount of the slag removing agent is 3-8% of the mass of the melting product in the high-temperature resistant container.
Further, in the step (d), the reducing agent is one or two of carbon and silicon, and the adding amount of the reducing agent is 0.01-0.1% of the mass of the melting product in the vacuum melting furnace. When the reducing agent is a mixture of carbon and silicon, the mass ratio of carbon to silicon can be adjusted as necessary.
The method for preparing the nickel-based alloy by recycling the waste nickel-hydrogen batteries has the advantages of simple and novel process, high production efficiency, high purity of recycled alloy products which can reach more than 99 percent, low energy consumption, high safety and little pollution, and is suitable for large-scale treatment of nickel materials recycled from the waste nickel-hydrogen batteries.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the description of the examples.
Example 1
A method for preparing a nickel-based alloy by recycling waste nickel-metal hydride batteries comprises the following steps:
(a) crushing the waste nickel-metal hydride battery, separating active substance powder, a diaphragm and mixed particles containing plastic iron and nickel, and putting the mixed particles containing plastic iron and nickel into a magnetic separation device to separate plastic particles, iron-rich particles and nickel-rich particles; the nickel-rich particles generally contain nickel and a small amount of diaphragm, cobalt, iron, manganese, rare earth metals and oxides thereof; during specific production, plastic particles are partially selected from the upper part of the magnetic separation device, nickel-rich particles are partially selected from the middle part of the magnetic separation device, and iron materials are selected from the lower part of the magnetic separation device by adjusting basic parameters such as magnetic strength of the magnetic separation device;
(b) adding the nickel-rich particles separated in the step (a) and a separating agent into a high-temperature resistant container, wherein the adding amount of the separating agent is 10% of the mass of the nickel-rich particles, the separating agent is a mixture of sodium chloride particles, sodium hexafluoroaluminate particles and aluminum fluoride particles, and the mass ratio of the sodium chloride particles to the sodium hexafluoroaluminate particles to the aluminum fluoride particles is 68: 18: 14, heating the high-temperature resistant container to 1530 ℃, stirring and preserving heat for 20min after the nickel-rich particles and the separating agent are completely melted, and removing surface scum in the stirring process, wherein most of diaphragms, active substance powder, plastics, oxides of metals such as nickel, cobalt, manganese, rare earth and the like in the nickel-rich particles are removed as scum;
(c) firstly, adjusting the temperature of a high-temperature resistant container to 1460 ℃, then adding heavy oil with the mass of 5% of that of a molten product in the high-temperature resistant container into the molten product in the high-temperature resistant container, then stirring and preserving heat for 10min, removing surface scum in the stirring process, and finally casting the molten liquid with scum removed to form a nickel ingot; in the step, a small amount of rare earth metal left in the nickel-rich particles forms scum to be separated from the melt, and simultaneously, a small amount of nickel-cobalt-manganese oxide left in the nickel-rich particles is reduced, so that high-purity melt containing a small amount of cobalt and manganese is obtained;
(d) detecting the metal components of the nickel ingot obtained in the step (c), supplementing corresponding metals into the nickel ingot according to the requirements of the metal components of the nickel-based alloy, adding the nickel ingot and the supplemented corresponding metals into a vacuum smelting furnace filled with argon, heating the vacuum smelting furnace to 1750 ℃, stirring and preserving heat for 8min after the nickel ingot and the supplemented corresponding metals are completely melted, then adding carbon with the mass of 0.05% of the melting product in the vacuum smelting furnace into the melting product in the vacuum smelting furnace under the condition that the temperature of the vacuum smelting furnace is not changed, stirring and removing surface scum, namely trace oxygen on the surface to prepare nickel liquid, and casting the nickel liquid into the nickel-based alloy after standing for 15 min.
The nickel-based alloy prepared in the steps is subjected to metal component detection, the detection results are shown in table 1, and the data in table 1 meet the requirements of the metal components of the nickel-based alloy.
TABLE 1 detection data of various metal components of nickel-base alloy
Example 2
The steps of the method for preparing the nickel-based alloy by recycling the waste nickel-metal hydride batteries are basically the same as the steps of the method for preparing the nickel-based alloy by recycling the waste nickel-metal hydride batteries in the embodiment 1, and the difference is that:
1. in the step (b), the addition amount of the separating agent is 15% of the mass of the nickel-rich particles, and the mass ratio of the sodium chloride particles to the sodium hexafluoroaluminate particles to the aluminum fluoride particles in the separating agent is 70: 20: 10, heating the high-temperature resistant container to 1580 ℃, stirring and keeping the temperature for 25min after the nickel-rich particles and the separating agent are completely melted;
2. in the step (c), the temperature of the high-temperature resistant container is adjusted to 1480 ℃, the heat preservation time of adding the deslagging agent is 12min, the deslagging agent is natural gas, the pressure of the natural gas is 0.2Mpa, and the adding amount of the deslagging agent is 8 percent of the mass of the melting product in the high-temperature resistant container;
3. in the step (d), the vacuum smelting furnace is heated to 1700 ℃, after the nickel ingot and the supplemented corresponding metal are completely melted, the nickel ingot is stirred and the temperature is kept for 5min, the surface scum is removed, and then the nickel ingot and the supplemented corresponding metal are kept still for 20min, wherein the reducing agent is silicon, and the adding amount of the reducing agent is 0.1 percent of the mass of the melting product in the vacuum smelting furnace.
The nickel-based alloy prepared in the above steps is subjected to metal component detection, the detection results are shown in table 2, and the data in table 2 all meet the requirements of the metal components of the nickel-based alloy.
TABLE 2 detection data of various metal components of nickel-base alloy
Example 3
The steps of the method for preparing the nickel-based alloy by recycling the waste nickel-metal hydride batteries are basically the same as the steps of the method for preparing the nickel-based alloy by recycling the waste nickel-metal hydride batteries in the embodiment 1, and the difference is that:
1. in the step (b), the addition amount of the separating agent is 6% of the mass of the nickel-rich particles, and the mass ratio of the sodium chloride particles to the sodium hexafluoroaluminate particles to the aluminum fluoride particles in the separating agent is 75: 16: 9, heating the high-temperature resistant container to 1500 ℃, stirring and preserving heat for 30min after the nickel-rich particles and the separating agent are completely melted;
2. in the step (c), the temperature of the high-temperature resistant container is adjusted to 1430 ℃, the heat preservation time of adding the slag removing agent is 15min, the slag removing agent is light diesel oil, and the adding amount of the slag removing agent is 3 percent of the mass of the melting product in the high-temperature resistant container;
3. in the step (d), the vacuum smelting furnace is heated to 1650 ℃, the nickel ingot and the supplemented corresponding metal are stirred and insulated for 10min after being completely melted, the surface scum is removed and then the mixture is kept stand for 25min, and the adding amount of the reducing agent is 0.02 percent of the mass of the melting product in the vacuum smelting furnace.
The nickel-based alloy prepared in the above steps is subjected to metal component detection, the detection results are shown in table 3, and the data in table 3 all meet the requirements of the metal components of the nickel-based alloy.
TABLE 3 detection data of various metal components of nickel-base alloy
Claims (6)
1. A method for preparing nickel-based alloy by recycling waste nickel-hydrogen batteries is characterized by comprising the following steps: the method comprises the following steps:
(a) crushing the waste nickel-metal hydride battery, separating active substance powder, a diaphragm and mixed particles containing plastic iron and nickel, and putting the mixed particles containing plastic iron and nickel into a magnetic separation device to separate plastic particles, iron-rich particles and nickel-rich particles;
(b) adding the nickel-rich particles separated in the step (a) and a separating agent into a high-temperature resistant container, heating the high-temperature resistant container to 1500-1580 ℃, stirring and keeping the temperature for 20-30 min after the nickel-rich particles and the separating agent are completely melted, and removing the surface scum in the stirring process; the separating agent is a mixture of sodium chloride particles, sodium hexafluoroaluminate particles and aluminum fluoride particles;
(c) adjusting the temperature of a high-temperature resistant container to 1430-1480 ℃, adding a certain amount of slag removing agent into a molten product in the high-temperature resistant container, stirring and preserving heat for 10-15 min, removing surface scum in the stirring process, and finally casting the molten liquid after scum removal to form a nickel ingot;
(d) detecting the metal components of the nickel ingot obtained in the step (c), supplementing corresponding metals into the nickel ingot according to the requirements of the metal components of the nickel-based alloy, adding the nickel ingot and the supplemented corresponding metals into a vacuum smelting furnace filled with inert gas, heating the vacuum smelting furnace to 1650-1750 ℃, stirring and preserving heat for 5-10 min after the nickel ingot and the supplemented corresponding metals are completely melted, then adding a certain amount of reducing agent into the molten product in the vacuum smelting furnace under the condition that the temperature of the vacuum smelting furnace is not changed, stirring and removing surface scum to prepare nickel liquid, standing for 15-25 min, and casting the nickel liquid to form the nickel-based alloy.
2. The method for preparing the nickel-based alloy by recycling the waste nickel-hydrogen battery as claimed in claim 1, wherein the method comprises the following steps: in the step (b), the addition amount of the separating agent is 6-15% of the mass of the nickel-rich particles.
3. The method for preparing the nickel-based alloy by recycling the waste nickel-hydrogen battery as claimed in claim 2, wherein the method comprises the following steps: in the step (b), the mass ratio of the sodium chloride particles to the sodium hexafluoroaluminate particles to the aluminum fluoride particles is 64-76: 14-20: 6 to 20.
4. The method for preparing the nickel-based alloy by recycling the waste nickel-metal hydride batteries as claimed in any one of claims 1 to 3, wherein the method comprises the following steps: in the step (c), the slag removing agent is one of trees, heavy oil, light diesel oil and natural gas, the pressure of the natural gas is 0.2Mpa, and the adding amount of the slag removing agent is 3-8% of the mass of the melting product in the high-temperature resistant container.
5. The method for preparing the nickel-based alloy by recycling the waste nickel-metal hydride batteries as claimed in any one of claims 1 to 3, wherein the method comprises the following steps: in the step (d), the reducing agent is one or two of carbon and silicon, and the addition amount of the reducing agent is 0.01-0.1% of the mass of the melting product in the vacuum melting furnace.
6. The method for preparing the nickel-based alloy by recycling the waste nickel-hydrogen battery as claimed in claim 4, wherein the method comprises the following steps: in the step (d), the reducing agent is one or two of carbon and silicon, and the addition amount of the reducing agent is 0.01-0.1% of the mass of the melting product in the vacuum melting furnace.
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