GB2621958A - Preparation method for aluminum nitride - Google Patents
Preparation method for aluminum nitride Download PDFInfo
- Publication number
- GB2621958A GB2621958A GB2318477.3A GB202318477A GB2621958A GB 2621958 A GB2621958 A GB 2621958A GB 202318477 A GB202318477 A GB 202318477A GB 2621958 A GB2621958 A GB 2621958A
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- United Kingdom
- Prior art keywords
- reaction
- aluminum nitride
- liquid separation
- solid
- aluminium
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- 239000000843 powder Substances 0.000 claims abstract description 57
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 28
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002699 waste material Substances 0.000 claims abstract description 27
- 239000002244 precipitate Substances 0.000 claims abstract description 25
- 238000000926 separation method Methods 0.000 claims abstract description 24
- 239000007770 graphite material Substances 0.000 claims abstract description 19
- 238000001354 calcination Methods 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 238000007873 sieving Methods 0.000 claims abstract description 17
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 16
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 12
- 239000005751 Copper oxide Substances 0.000 claims abstract description 11
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000007790 solid phase Substances 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 34
- 239000004411 aluminium Substances 0.000 claims description 31
- 229910052782 aluminium Inorganic materials 0.000 claims description 31
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 31
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 29
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 18
- 239000011780 sodium chloride Substances 0.000 claims description 17
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 239000012528 membrane Substances 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 6
- 238000005868 electrolysis reaction Methods 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 15
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 abstract 2
- 229910001388 sodium aluminate Inorganic materials 0.000 abstract 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 27
- 239000010949 copper Substances 0.000 description 26
- 229910052802 copper Inorganic materials 0.000 description 23
- 239000012535 impurity Substances 0.000 description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 10
- 238000002386 leaching Methods 0.000 description 10
- 229910002804 graphite Inorganic materials 0.000 description 9
- 239000010439 graphite Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 5
- 238000003837 high-temperature calcination Methods 0.000 description 5
- -1 Al was 11.34% Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000010008 shearing Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- JRBRVDCKNXZZGH-UHFFFAOYSA-N alumane;copper Chemical compound [AlH3].[Cu] JRBRVDCKNXZZGH-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
- C01B21/0726—Preparation by carboreductive nitridation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
-
- 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
-
- 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
- C22B15/00—Obtaining copper
-
- 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
- C22B15/00—Obtaining copper
- C22B15/0026—Pyrometallurgy
- C22B15/0056—Scrap treating
-
- 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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0073—Leaching or slurrying with acids or salts thereof containing nitrogen
-
- 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
- C22B21/00—Obtaining aluminium
-
- 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
- C22B21/00—Obtaining aluminium
- C22B21/0015—Obtaining aluminium by wet processes
- C22B21/0023—Obtaining aluminium by wet processes from waste materials
-
- 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
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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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- 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
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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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
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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- 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
- C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
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- 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
- C25B15/00—Operating or servicing cells
- C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes
- C25B15/081—Supplying products to non-electrochemical reactors that are combined with the electrochemical cell, e.g. Sabatier reactor
-
- 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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- Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Geochemistry & Mineralogy (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
- Secondary Cells (AREA)
Abstract
The present invention relates to the field of recycling of waste lithium batteries. Disclosed is a preparation method for aluminum nitride. The preparation method comprises the following steps: adding a sodium hydroxide solution to waste positive electrode powder for reaction, and performing solid-liquid separation to obtain a sodium aluminate solution and positive electrode powder; adding acid to the sodium aluminate solution for reaction, performing solid-liquid separation, and extracting a solid phase to obtain an aluminum hydroxide precipitate; performing water washing and sieving on a negative current collector, performing solid-liquid separation, extracting a solid phase, and adding nitric acid for reaction, and performing solid-liquid separation to obtain a graphite material and copper nitrate; mixing the aluminum hydroxide precipitate with the graphite material, granulating the mixture, and then adding copper nitrate for mixing, and performing a calcination reaction to obtain aluminum nitride and copper oxide. According to the present invention, nitrogen does not need to be additionally conveyed in the aluminum nitride synthesis process, and a self-sufficiency state is always kept in the reaction process, so that the reaction is more stable, and the purity of the generated aluminum nitride is high.
Description
-I -
PREPARATION METHOD FOR ALUMINUM NITRIDE TECHNICAL FIELD
The present invention relates to the technical field of recycling waste lithium batteries, and in particular to a method for preparing aluminum nitride.
BACKGROUND
As ecological and environmental protection has been promoted in China, more and more new energy is rising, especially in the lithium battery industry. Lithium batteries are widely used in the field of new energy vehicles, 3C consumer products which refers to an abbreviation of three types of electronic products: computer, communication and consumer electronics, and energy storage batteries, owing to their advantages of high energy density, high operating voltage, long cycle life and large charge-discharge rate. Later, with the use of lithium batteries, a large number of batteries will inevitably be scrapped, which necessitates the treatment on these waste lithium batteries. For the existing dry process of treating the waste lithium batteries, since the recycled battery powder contains a large amount of valuable metals, it costs a lot to remove impurities in later stage, added that the waste residue discarded from the existing process is just accumulated as solid waste, resulting in environmental pollution and waste of resources.
At present, the incineration method and crushing separation method are most commonly used to treat the waste lithium batteries. For the incineration method, it has high energy consumption, long process and low metal recovery, and in particular, the battery powder produced by this method has a high impurity content and a high post-treatment cost. And, due to aluminium in the anode current collector has low melting point, it is easy to melt and infiltrate into the battery powder during heat treatment, resulting in difficulty in separation of valuable metals, which is not conducive to industrial production. For the crushing separation method, it is simple, but it results in a poor production environment, as the dust is dispersed and the equipment is prone to failure, in addition that the product, copper-aluminium mixture, has high content of nickel and cobalt which cannot be easily and effectively recycled and thus is not conducive to production. At present, the process of preparing aluminum nitride mainly involves performing nitridation reaction on ammonia and aluminium directly, and performing pulverization and classification to obtain aluminum nitride powder, or well-mixing aluminium oxide and carbon and performing reduction in an electric furnace at 1700 °C to obtain aluminum nitride. In the process, metallic aluminium needs crushing to micron level, which is very dangerous, and in the reaction process, it may happen that the pipes have not been tightly sealed when being filled with nitrogen gas, resulting in a violent reaction between the internal aluminium powder and air, which is extremely unsafe and unfavorable for process production.
SUMMARY
The present invention is intended to solve at least one of the above-mentioned technical problems existing in the prior art. Therefore, the present invention provides a method for preparing aluminum nitride, which combines physical and chemical methods, satisfies industrial production requirements of environmental friendliness, low energy consumption and high resource recovery, and is safe in process, and produces aluminum nitride with high purity.
In order to achieve the above objective, the present invention uses the following technical solutions.
Provided is a method for preparing aluminum nitride, comprising steps of: (1) adding a sodium hydroxide solution to waste cathode powder to perform reaction, and performing solid-liquid separation to obtain a sodium metaaluminate solution and cathode powder; (2) adding an acid to the sodium metaaluminate solution to perform reaction, and performing solid-liquid separation to obtain an aluminium hydroxide precipitate; (3) washing an anode current collector with water, sieving, and performing solid-liquid separation, adding nitric acid to a resulting solid phase to perform a reaction, and performing solid-liquid separation to obtain a graphite material and copper nitrate; and (4) granulating after mixing the aluminium hydroxide precipitate of step (2) with the graphite material of step (3), then mixing a resulting granule with the copper nitrate of step (3), and performing calcination to obtain aluminum nitride and copper oxide.
Preferably, in the step (I), the waste cathode powder is obtained by disassembling and crushing a waste lithium battery to obtain cathode and anode current collector crushed materials and a separator membrane, carrying out a thermal decomposition on the cathode current collector crushed material, and sieving a resulting reaction product to obtain metal aluminium and the waste cathode powder.
Further preferably, the crushing is shear crushing, and the sieving uses a sieve having 1 cm to 5 cm meshes Further preferably, the thermal decomposition is carried out at a temperature of 400 °C to 600 °C for 0.5 h to 1 h. Further preferably, the sieving uses a sieve having 5 meshes to 20 meshes.
Preferably, in the step (1), the sodium hydroxide solution has a mass concentration of 10 g/L to 30 g/L.
Preferably, in the step (1), a liquid-solid ratio of the sodium hydroxide solution to the waste cathode powder is 1: (1-3) L/8 Preferably, in the step (1), the method further comprises carrying out wet leaching on the cathode powder to recover a valuable metal.
Preferably, in the step (2), the acid is one of hydrochloric acid and nitric acid; when the acid is hydrochloric acid, after performing the solid-liquid separation in the step (2), the aluminium hydroxide precipitate and a sodium chloride solution are obtained Further preferably, the hydrochloric acid has a mass fraction of 20% to 50% Further preferably, the sodium chloride solution is subjected to electrolysis to produce sodium hydroxide, which is returned to the step (1) for use.
More preferably, the electrolysis of the sodium chloride solution is carried out at a voltage of 220 V. Preferably, in the step (3), washing an anode current collector with water is carried out at a liquid-solid ratio of 1: (1-2) L/g, and lasts for 10 min to 30 mm.
Preferably, in the step (3), the sieving uses a sieve having 5 meshes to 10 meshes. Preferably, in the step (3), the nitric acid has a mass fraction of 30% to 50%.
Preferably, in the step (4), a mass ratio of the aluminium hydroxide to the graphite material is (2-3): (1-2).
Preferably, in the step (4), a mass ratio of the copper nitrate to the aluminium hydroxide is (I-3): 1.
Preferably, in the step (4), the resulting granule has a particle diameter of 0.5 mm to 2.0 mm.
Granulation after mixing the aluminium hydroxide with the graphite material are more favorable for the reaction, which is because that if the mixed materials is directly subjected to reaction, the reactants are closely packed, the gas flow capacity is poor, and the contact surface is small, which easily results in incomplete reaction, whereas after granulation, the materials can be rendered with improved bulkiness, larger contact surface, and better gas flow capacity, which facilitates complete reaction.
Preferably, in the step (4), the calcination is carried out in three stages, in which a first stage calcination is carried out at a temperature of 200 °C to 400 °C for 0.5 h to 2 h; a second stage calcination is carried out at a temperature of 1000 °C to 1200 °C for 1 h to 3 h and a third stage calcination is carried out at a temperature of 1400°C to 1600°C for 5 h to 8 It Preferably, in the step (4), the calcination further comprises adding a catalyst for catalysis, wherein the catalyst is a platinum wire The reaction equation in each step of the present invention is shown below: I. Formation of sodium metaaluminate: 2A1+2H20+2NaOH=2NaA102+31-12 t; 2. Formation of aluminium hydroxide with no excess hydrochloric acid: HC1+NaA102+1-120=A1(OH)3 +NaCl; 3 Formation of copper nitrate: H2NO3 (dilute)+Cu=Cu(NO3)2+NO t +H20; 4 Electrolysis of sodium chloride: 2NaC1+2H20=2Na0H+112 '1 +C12 t (electrolysis); Thermal decomposition of copper nitrate: 2Cu(NO3)2=2Cu0+4NO2 '1 +02; 6. Formation of nitrogen: C+02=CO2 (combustion), 2C+02=2C0 (insufficient combustion), C+CO2=2C0 (high temperature), 4C0+2NO2=N2+4CO2 (platinum wire-catalyzed); 7 Formation of alumina: 2A1(OH)3=A1203+3H20 (high temperature); 8 Reduction of copper: CuO+C0=Cu+CO2 (high temperature); and 9. Synthesis of aluminum nitride: A1203+3C+N2=2A1N+3CO. This invention is based on the following processing principle.
The present invention uses a method combining physics and chemistry to treat a waste lithium battery, in which firstly, the waste lithium battery is separated to separately obtain cathode and anode current collectors and a separator membrane which can be sold directly; the cathode and anode current collectors then are separately crushed to obtain cathode and anode current collector crushed materials; and the cathode current collector crushed material is subjected to thermal decomposition and sieving to obtain metal aluminium and waste cathode powder.
Sodium hydroxide is added to waste cathode powder to remove impurities. Sodium hydroxide reacts with aluminium to generate a sodium metaaluminate solution. After solid-liquid separation, a pure cathode powder are separated out. To the filtrate, a small amount of dilute hydrochloric acid is added without excessive amount to perform reaction and to produce an aluminium hydroxide precipitate and a sodium chloride solution. After another solid-liquid separation, the separated aluminium hydroxide is mixed with the graphite material to produce aluminum nitride, and the sodium chloride solution is electrolyzed to produce sodium hydroxide which is recycled, and metallic aluminium which is sold directly. The anode current collector crushed material is washed with water, sieved and press-filtered to obtain metallic copper which is sold directly and graphite powder. To the graphite powder, dilute nitric acid is added to remove impurities and to perform reaction to produce copper nitrate. After solid-liquid separation, the copper nitrate solution and the graphite material are separated out. The graphite material then is mixed with aluminium hydroxide for granulating, and introduced into a tube furnace for high-temperature calcination with copper nitrate to obtain aluminum nitride powder.
Regarding the stage of high-temperature synthesis of aluminum nitride: in a low-temperature stage, copper nitrate is decomposed into copper oxide and nitrogen dioxide, part of the carbon monoxide produced by carbon reacts with nitrogen dioxide to generate nitrogen, and a platinum wire is added as a catalyst in the furnace body; in a medium-temperature stage, aluminium hydroxide is decomposed into alumina powder; and in a high-temperature stage, graphite, alumina and nitrogen are synthesized into aluminum nitride powder, which also reduces the subsequent carbon removal process.
The present invention has the following advantageous effects.
According to the present invention, in the process of synthesizing aluminum nitride, there is no need to additionally supply nitrogen gas, and it is at self-sufficient state during the reaction, thereby making the reaction more stable and producing aluminum nitride with high purity. According to the method of the present invention, the cathode and anode electrodes are treated separately, reducing the difficulty of subsequent impurity removal. For the preparation of aluminium oxide, a chemical dissolution method is used instead of physical crushing, which is also advantageous for removing the impurity from the cathode powder, because on the one hand, an aluminium source is obtained from the cathode powder, and on the other hand, metal aluminium as impurity is removed from the cathode powder, which is advantageous for the subsequent wet leaching of cathode powder, and thus is advantageous for impurity removal. The method of the present invention dose not generate waste residue and wastewater as a whole, and its reaction is relatively stable with simple operation process, and with resources capable of reusing in later production at high recovery rate
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 is a process flow diagram of Example 1 of the present invention
DETAILED DESCRIPTION OF EMBODIMENTS
Hereinafter, the concept of the present invention and the technical effects thereof will be clearly and completely described in conjunction with the examples to fully understand the objectives, features and effects of the present invention. It is obvious that the described examples are only a part of the examples of the present invention, rather than all of them. Based on the examples of the present invention, other examples which can be obtained by those skilled in the art without involving any inventive effort are within the scope of the present invention.
Example 1
In this example, a method for preparing aluminum nitride comprised the following steps.
(1) Single waste lithium batteries were disassembled to obtain separator membranes, cathode current collectors and anode current collectors, separately.
(2) The cathode and anode current collectors were crushed separately for 2 min using a shearing type crusher and a sieve with a mesh diameter of 1 cm to obtain cathode and anode current collector crushed materials.
(3) The cathode current collector crushed material was placed into a muffle furnace for calcining at 450 °C for 1 h. Finally, after sieving with a sieve having 10 meshes, metal aluminium and cathode powder were obtained. In the cathode powder, a measured content of the impurity, Al was 11.34%, and Cu was 0.01%; and in the metal aluminium, Ni was 0.26%, and Co was 0.12%.
(4) 300 g of the cathode powder were added into 300 ml of 15 g/L sodium hydroxide with a liquid-solid ratio being 1: 1, stirred at a speed of 300 r/min for 20 min, and filtered. The filter residue was subjected to wet leaching. To the filtrate, hydrochloric acid having a mass fraction of 50% was added without excessive amount until a precipitate was produced. The addition of hydrochloric acid was stopped once the precipitate started to dissolve. Then, after filtration, an aluminium hydroxide precipitate and a sodium chloride solution were obtained. The sodium chloride solution was electrolyzed to produce sodium hydroxide for use in step (1).
(5) 500 g of the anode current collector crushing material was washed with water for 5 mm under a liquid-solid ratio of 1: 1 at a stirring speed of 200 r/min. After sieving, metallic copper and graphite slurry were obtained. The graphite slurry was press-filtered. In the filter residue, a measured contents of impurity, copper was 9.82% and aluminium was 0.03%. To the residue, 100 ml of nitric acid with a mass fraction of 50% was added, and stirred to perform reaction for 10 min until the impurity copper was completely dissolved. After separation by press-filtration, a solution of copper nitrate and a graphite material were obtained separately. The metallic copper may be sold directly.
(6) The graphite material of step (5) and the aluminium hydroxide precipitate of step (4) were mixed at a mass ratio of 1: 2, and introduced into a pelletizer to make spheres with a size of 1 mm. The copper nitrate solution and aluminium hydroxide with a mass ratio of 2: I, and the spheres, were placed into a tube furnace, together with a small amount of platinum wire inside the furnace, to be subjected to a high-temperature calcination which was designed to have three stages. In the first stage: the temperature was controlled at 200 °C and lasted for 1 h. In the second stage, the temperature was controlled at 1000°C and lasted for 2 h. In the third stage, the temperature was controlled at 1400 °C and lasted for 6 h. Finally, aluminum nitride powder and copper oxide were obtained.
After the above-mentioned steps, the separator membrane, metallic copper, metallic aluminium, cathode powder and aluminum nitride powder were obtained, wherein the separator membrane, metallic copper, metallic aluminium, copper oxide and aluminum nitride may be sold directly, and the cathode powder may be subjected to wet leaching.
Example 2
In this example, a method for preparing aluminum nitride comprised the following steps.
(1) Waste lithium batteries were disassembled to obtain separator membranes, cathode current collectors and anode current collectors, separately.
(2) The cathode and anode current collectors were crushed separately for 2 min using a shearing type crusher and a sieve with a mesh diameter of 1 cm.
(3) The cathode current collector crushed material was placed into a muffle furnace for calcining at 450 °C for 1 h. Finally, after sieving with a sieve having 10 meshes, metal aluminium and cathode powder were obtained. In the cathode powder, a measured content of the impurity, Al was 11.34%, and Cu was 0.01%; and in the metal aluminium, Ni was 0.26%, and Co was 0.12%.
(4) 250 g of the cathode powder were added into 200 ml of 10 g/L sodium hydroxide with a liquid-solid ratio being 1: 1.2, stirred at a speed of 300 r/min for 20 min, and filtered. The filter residue was subjected to wet leaching. To the filtrate, hydrochloric acid having a mass fraction of 40% was added without excessive amount until a precipitate was produced. The addition of hydrochloric acid was stopped once the precipitate started to dissolve. Then, after filtration, an aluminium hydroxide precipitate and a sodium chloride solution were obtained. The sodium chloride solution was electrolyzed to produce sodium hydroxide for use in step (1).
(5) 800 g of the anode current collector crushing material was washed with water for 5 min under al quid-solid ratio of I: 1 at a stirring speed of 200 r/min. After sieving, metallic copper and graphite slurry were obtained. The graphite slurry was press-filtered. In the filter residue, a measured contents of impurity, copper was 9.18% and aluminium was 0.02%. To the residue, 150 ml of nitric acid with a mass fraction of 40% was added, and stirred to perform reaction for 10 min until the impurity copper was completely dissolved. After separation by press-filtration, a solution of copper nitrate and a graphite material were obtained separately. The metallic copper may be sold directly.
(6) The graphite material of step (5) and the aluminium hydroxide precipitate of step (4) were mixed at a mass ratio of 1: 2, and introduced into a pelletizer to make spheres with a size of I mm. The copper nitrate solution and aluminium hydroxide with a mass ratio of 3: I, and the spheres, were placed into a tube furnace, together with a small amount of platinum wire inside the furnace, to be subjected to a high-temperature calcination which was designed to have three stages. In the first stage: the temperature was controlled at 200 °C and lasted for 1 h. In the second stage, the temperature was controlled at 1000 °C and lasted for 2 h. In the third stage, the temperature was controlled at 1400 °C and lasted for 6 h. Finally, aluminum nitride powder and copper oxide were obtained.
After the above-mentioned steps, the separator membrane, metallic copper, metallic aluminium, cathode powder and aluminum nitride powder were obtained, wherein the separator membrane, metallic copper, metallic aluminium, copper oxide and aluminum nitride may be sold directly, and the cathode powder may be subjected to wet leaching.
Example 3
In this example, a method for preparing aluminum nitride comprised the following steps: (1) Waste lithium batteries were disassembled to obtain separator membranes, cathode current collectors and anode current collectors, separately.
(2) The cathode and anode current collectors were crushed separately for 2 min using a shearing type crusher and a sieve with a mesh diameter of 1 cm.
(3) The cathode current collector crushed material was placed into a muffle furnace for calcining at 450 °C for 1 h. finally, after sieving with a sieve having 10 meshes, metal aluminium and cathode powder were obtained. In the cathode powder, a measured content of the impurity, Al was 11.34%, and Cu was 0.01%; and in the metal aluminium, Ni was 0.26%, and Co was 0.12%.
(4) 500 g of the cathode powder were added into 300 ml of 20 g/L sodium hydroxide with a liquid-solid ratio being I: 1.7, stirred at a speed of 300 r/min for 20 min, and filtered. The filter residue was subjected to wet leaching. To the filtrate, hydrochloric acid having a mass fraction of 50% was added without excessive amount until a precipitate was produced. The addition of hydrochloric acid was stopped once the precipitate started to dissolve. Then, after filtration, an aluminium hydroxide precipitate and a sodium chloride solution were obtained. The sodium chloride solution was electrolyzed to produce sodium hydroxide for use in step (1).
(5) 1000 g of the anode current collector crushing material was washed with water for 5 min under a liquid-solid ratio of 1: 1 at a stirring speed of 200 r/min. After sieving, metallic copper and graphite slurry were obtained. The graphite slurry was press-filtered. In the filter residue, a measured contents of impurity, copper was 10.08% and aluminium was 0.04%. To the residue, 200 ml of nitric acid with a mass fraction of 40% was added, and stirred to perform reaction for 10 min until the impurity copper was completely dissolved. After separation by press-filtration, a solution of copper nitrate and a graphite material were obtained separately. The metallic copper may be sold directly.
(6) The graphite material of step (5) and the aluminium hydroxide precipitate of step (4) were mixed at a mass ratio of 1: 1, and introduced into a pelletizer to make spheres with a size of 1 mm. The copper nitrate solution and aluminium hydroxide with a mass ratio of 2: 1, and the spheres, were placed into a tube furnace, together with a small amount of platinum wire inside the furnace, to be subjected to a high-temperature calcination which was designed to have three stages. In the first stage: the temperature was controlled at 200 °C and lasted for 1 h. In the second stage, the temperature was controlled at 1200 °C and lasted for 2 h. In the third stage, the temperature was controlled at 1600 °C and lasted for 6 h. Finally, the resulting product was taken out and decarbonized under air circulation at 500 °C for 1 h, to obtain aluminum nitride powder.
After the above-mentioned steps, the separator membrane, metallic copper, metallic aluminium, cathode powder and aluminum nitride powder were obtained, wherein the separator membrane, metallic copper, metallic aluminium, copper oxide and aluminum nitride may be sold directly, and the cathode powder may be subjected to wet leaching.
Comparative Example 1 In the comparative example, a method for preparing the aluminum nitride powder comprised the following steps: (1) Waste lithium batteries were disassembled to obtain separator membranes, cathode current collectors and anode current collectors, separately.
(2) The cathode and anode current collectors were crushed separately for 2 min using a shearing type crusher and a sieve with a mesh diameter of 1 cm.
(3) The cathode current collector crushed material was placed into a muffle furnace for calcining at 450 °C for 1 h. Finally, after sieving with a sieve having 10 meshes, metal aluminium and cathode powder were obtained. In the cathode powder, a measured content of the impurity, Al was 11.34%, and Cu was 0.01%; and in the metal aluminium, Ni was 0.26%, and Co was 0.12%.
(4) 250 g of the cathode powder were added into 200 ml of 10 g/L sodium hydroxide with a liquid-solid ratio being 1: 1.2, stirred at a speed of 300 r/min for 20 min, and filtered. The filter residue was subjected to wet leaching. To the filtrate, hydrochloric acid having a mass fraction of 40% was added without excessive amount until a precipitate was produced. The addition of hydrochloric acid was stopped once the precipitate started to dissolve. Then, after filtration, an aluminium hydroxide precipitate and a sodium chloride solution were obtained. The sodium chloride solution was electrolyzed to produce sodium hydroxide for in the front end.
(5) 800 g of the anode current collector crushing material was washed with water for 5 mm under a liquid-solid ratio of 1: 1 at a stirring speed of 200 r/min. After sieving, metallic copper and graphite slurry were obtained. The graphite slurry was press-filtered. In the filter residue, a measured contents of impurity, copper was 9.18% and aluminium was 0.02%. To the residue, 100 ml of nitric acid with a mass fraction of 40% was added, and stirred to perform reaction for 10 min until the impurity copper was completely dissolved. After separation by press-filtration, a solution of copper nitrate and a graphite material were obtained separately. The metallic copper may be sold directly.
(6) The graphite material of step (5) and the aluminium hydroxide precipitate of step (4) were mixed at a mass ratio of 1: 2, and introduced into a pelletizer to make spheres with a size of 1 mm.
The spheres were placed into a tube furnace filled with sufficient nitrogen, to be subjected to a high-temperature calcination which was designed to have three stages. In the first stage. the temperature was controlled at 200 °C and lasted for 1 h. In the second stage, the temperature was controlled at 1000 °C and lasted for 2 h. In the third stage, the temperature was controlled at 1400 °C and lasted for a duration of 6 h. Finally, aluminum nitride powder was obtained.
After the above-mentioned steps, the separator membrane, metallic copper, metallic aluminium, cathode powder and aluminum nitride powder were obtained, wherein the separator membrane, metallic copper, metallic aluminium, and aluminum nitride may be sold directly, and the cathode powder may be subjected to wet leaching. But, the copper nitrate requires additional processing treatment.
Element Content Test Results The contents of key elements in the aluminum nitride products prepared in the Examples 1-3 and the Comparative Example 1 of the present invention were measured using ICP (Inductively Coupled Plasma Spectroscopy), and the results were shown in Table 1 below.
Table I Elemental contents in aluminum nitride products prepared in Examples 1-3 and Comparative Example 1 Content Example 1 Example 2 Example 3 Comparative
Element Example 1
AIN 99.2 99.5 98.g 72.5 C 0.02 0,01 0.16 0.01 0 0.12 0.21 0.68 0.45 Cu 0.01 0.02 0.05 0.01 Na 0.13 0.25 0.24 0.44 It can be seen from the data in the table that this process can produce a product with high purity and low impurity content, and has strong feasibility. In the Comparative Example I, the ratio of raw materials was still affected by nitrogen gas; carbon had been completely burnt away in the early stage, resulting in the reaction of nitrogen and alumina in the later stage; the reaction was incomplete, causing high impurity contents, and the remaining copper nitrate in the process required additional processing treatment.
Table 2 Component content of copper oxide Content Example 1 Example 2 Example 3 Comparative
Element Example 1
Cu 96.1 95.8 95.4 35.1 C 0.01 0.01 0.01 15.85 Al 0.05 0,06 0.12 0.01 N 0.25 0.32 0.42 0.01 Na 0.02 0,03 0.12 0.01 It can be seen from Table 2 that heating copper nitrate to obtain copper oxide and then reducing it into metallic copper is highly feasible, and the product has good purity, high sale value and strong recyclability. In the Comparative Example 1, the copper nitrate solution was not treated, thus the substance had high impurity content, and low direct sale value if sold just like that. It needs additional processing, and is toxic and harmful and explosive which is easy to cause a particular hidden danger if not processed in time.
Although the examples of the present invention have been described in detail with reference to the accompanying drawings, the present invention is not limited to the above-described examples, and various changes can be made within the scope of knowledge of a person skilled in the art without departing from the spirit of the present invention. Furthermore, examples of the present invention and features of the examples may be combined with each other without conflict. -1 3-
Claims (10)
- CLAIMSI. A method for preparing aluminum nitride, comprising steps of: (1) adding a sodium hydroxide solution to waste cathode powder to perform reaction, and performing solid-liquid separation to obtain a sodium metaaluminate solution and cathode powder; (2) adding an acid to the sodium metaaluminate solution to perform reaction, and performing solid-liquid separation to obtain an aluminium hydroxide precipitate; (3) washing an anode current collector with water, sieving, and performing solid-liquid separation, adding nitric acid to a resulting solid phase to perform a reaction, and performing solid-liquid separation to obtain a graphite material and copper nitrate; and (4) granulating after mixing the aluminium hydroxide precipitate of step (2) with the graphite material of step (3), then mixing a resulting granule with the copper nitrate of step (3), and performing calcination to obtain aluminum nitride and copper oxide.
- 2. The method according to claim 1, wherein in the step (1), the waste cathode powder is obtained by disassembling and crushing a waste lithium battery to obtain cathode and anode current collector crushed materials and a separator membrane, and carrying out a thermal decomposition on the cathode current collector crushed material, and sieving a resulting reaction product to obtain metal aluminium and the waste cathode powder.
- 3. The method according to claim 2, wherein the thermal decomposition is carried out at a temperature of 400°C to 600 °C for 0.5 h to 1 h.
- 4. The method according to claim 1, wherein in the step (1), a liquid-solid ratio of the sodium hydroxide solution to the waste cathode powder is 1: (1-3) L/g.
- 5. The method according to claim 1, wherein in the step (2), the acid is one of hydrochloric acid and nitric acid; and when the acid is hydrochloric acid, after performing the solid-liquid separation in the step (2), the aluminium hydroxide precipitate and a sodium chloride solution are obtained.
- 6. The method according to claim 5, wherein the sodium chloride solution is subjected to electrolysis to produce sodium hydroxide, which is returned to the step (1) for use.
- 7. The method according to claim 1, wherein in the step (3), the nitric acid has a mass fraction of 30% to 50%.
- 8. The method according to claim 1, wherein in the step (4), a mass ratio of the copper nitrate to the aluminium hydroxide is (1-3): 1
- 9. The method according to claim 1, wherein in the step (4), the calcination is carried out in three stages, in which a first stage calcination is carried out at a temperature of 200 °C to 400 °C for 0.5 h to 2 h; a second stage calcination is carried out at a temperature of 1000 °C to 1200 °C for 1 h to 3 11; and a third stage calcination is carried out at a temperature of 1400 °C to 1600 °C for 5 h to 8 h.
- 10. The method according to claim 1, wherein in the step (4), the calcination further comprises adding a catalyst for catalysis, which is a platinum wire.
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