WO2022267421A1 - 一种报废正极浆料的处理方法和应用 - Google Patents
一种报废正极浆料的处理方法和应用 Download PDFInfo
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- WO2022267421A1 WO2022267421A1 PCT/CN2021/142947 CN2021142947W WO2022267421A1 WO 2022267421 A1 WO2022267421 A1 WO 2022267421A1 CN 2021142947 W CN2021142947 W CN 2021142947W WO 2022267421 A1 WO2022267421 A1 WO 2022267421A1
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- Prior art keywords
- positive electrode
- slurry
- nmp
- electrode slurry
- phase
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000011267 electrode slurry Substances 0.000 title claims abstract description 39
- 239000002002 slurry Substances 0.000 claims abstract description 34
- 239000007790 solid phase Substances 0.000 claims abstract description 32
- 238000001962 electrophoresis Methods 0.000 claims abstract description 31
- 239000007791 liquid phase Substances 0.000 claims abstract description 28
- 239000007774 positive electrode material Substances 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 150000002739 metals Chemical class 0.000 claims abstract description 11
- 238000011084 recovery Methods 0.000 claims abstract description 11
- 238000005345 coagulation Methods 0.000 claims abstract description 10
- 230000015271 coagulation Effects 0.000 claims abstract description 10
- 239000012074 organic phase Substances 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 24
- 238000001354 calcination Methods 0.000 claims description 17
- 238000003672 processing method Methods 0.000 claims description 13
- 238000004821 distillation Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000000843 powder Substances 0.000 abstract description 7
- 238000003912 environmental pollution Methods 0.000 abstract description 5
- 239000008394 flocculating agent Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000011085 pressure filtration Methods 0.000 abstract 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 56
- 239000000243 solution Substances 0.000 description 20
- 239000008346 aqueous phase Substances 0.000 description 19
- 238000009833 condensation Methods 0.000 description 15
- 230000005494 condensation Effects 0.000 description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 238000002390 rotary evaporation Methods 0.000 description 14
- 239000007787 solid Substances 0.000 description 11
- 239000011230 binding agent Substances 0.000 description 8
- 239000010406 cathode material Substances 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 239000002033 PVDF binder Substances 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 7
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 6
- 239000002910 solid waste Substances 0.000 description 5
- 238000010998 test method Methods 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 239000005416 organic matter Substances 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000011343 solid material Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000006257 cathode slurry Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000005909 Kieselgur Substances 0.000 description 1
- HFCVPDYCRZVZDF-UHFFFAOYSA-N [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O Chemical group [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O HFCVPDYCRZVZDF-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010926 waste battery Substances 0.000 description 1
Classifications
-
- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
-
- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
-
- 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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/02—Obtaining nickel or cobalt by dry processes
- C22B23/021—Obtaining nickel or cobalt by dry processes by reduction in solid state, e.g. by segregation processes
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
-
- 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
-
- 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
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- 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
-
- 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
Definitions
- the invention belongs to the technical field of recycling waste batteries, and in particular relates to a treatment method and application of waste positive electrode slurry.
- Lithium-ion battery positive electrode slurry is composed of positive electrode materials, binders, etc.
- the preparation of positive electrode slurry is an important link in the production of lithium-ion batteries.
- the production process includes mutual mixing, dissolution, and dispersion of liquid and liquid, liquid and positive electrode materials etc.; the quality of slurry dispersion directly affects the quality and performance of lithium-ion batteries.
- the existing publicly reported methods for treating scrap cathode slurry mainly include NMP regeneration and recovery of valuable metals, in which liquid-solid separation is a key step in the recovery process, and currently flocculation-filtration, centrifugal separation, and distillation roasting are mainly used to treat The NMP solution is separated from the cathode material.
- the related art discloses a recycling system for lithium battery positive electrode waste slurry, which adopts a centrifuge for liquid-solid separation, the solid phase is the positive electrode material, and the liquid phase is NMP solution.
- the solid phase is calcined at 300-600°C, followed by crushing and acid leaching to achieve the purpose of recovering valuable metals; the liquid phase adopts a distillation process, and water is removed at 80-100°C to obtain NMP.
- the positive electrode slurry has the characteristics of high viscosity, no coagulation, and fine particles.
- This related technology uses a centrifugal method for solid-liquid separation, which has low separation efficiency and large equipment loss.
- the residual NMP in the solid phase produced is high, and the subsequent calcination process is compact
- the phenomenon is serious and sticky to the wall, which is easy to cause poor material transportation, incomplete removal of organic matter and serious corrosion of roasting equipment, etc., which is not suitable for industrial production; there are many black powder suspensions in the liquid phase, and the black powder in this part of the distillation process will be destroyed. Residues in NMP reduce the recovery rate of valuable metals and seriously affect product quality.
- the present invention aims to solve at least one of the technical problems in the above-mentioned prior art. For this reason, the present invention proposes a treatment method and application of scrapped positive electrode slurry.
- the method uses scrapped positive electrode slurry as a raw material, and uses crushing and sorting, electrophoresis, and gradient roasting processes to recover scrapped positive electrode slurry without introducing flocculants.
- the method has the advantages of completely separating NMP solution from positive electrode powder, high recovery rate of organic matter and valuable metals, and high production efficiency, which not only improves economic benefits, but also reduces environmental pollution.
- the present invention adopts the following technical solutions:
- a processing method for scrap positive electrode slurry comprising the following steps:
- the specific steps of the pretreatment are: separating the scrap positive electrode slurry into bagged materials, and then crushing and sorting the bagged materials to obtain a slurry solution.
- Crushing and sorting the bagged materials is to remove the plastic and massive debris in the bagged materials.
- the material transportation process is very easy to jam; the second is to ensure the uniformity of the solid material, remove the plastic bags and blocky objects in the solid material, and reduce the impact of the debris on the subsequent treatment process of the positive electrode powder ; If there are plastic debris, there will be a phenomenon of melting and shrinkage in the heat treatment step, which will cause the positive electrode powder to be wrapped and affect the recovery rate of the product.
- the direct current used in the electrophoretic coagulation process has a current of 50-70mA and a voltage of 60-65V.
- the current density of the direct current used in the electrophoretic coagulation process is 0.2-0.6 A/m 2 .
- the electrophoresis time is 20-60min.
- a direct current is passed into the slurry solution, and the suspended particles in the slurry solution move directionally under the action of an external direct current electric field, and combine to form large particles to coagulate, and then use a filter press to separate the liquid from the solid to obtain a liquid
- the phase is NMP aqueous solution, and the solid phase is solid material.
- Electrophoretic coagulation is used to settle the positive electrode material in the scrap positive electrode slurry, without using flocculants and reducing the introduction of impurities.
- step (2) it also includes distilling the liquid phase to enrich the organic phase to obtain NMP with a purity greater than 70%.
- the distillation is vacuum rotary distillation or rectification.
- the gauge pressure of the reduced-pressure rotary evaporation is 0.02-0.04 MPa
- the temperature of the reduced-pressure rotary evaporation is 60-80° C.
- the time of the reduced-pressure rotary evaporation is 60-80 minutes.
- the organic phase is enriched to obtain NMP with a purity greater than 99%.
- the rectification conditions are that the pH of the liquid phase is 7.0-10.0, the pressure of the evaporation tank is 7.5-8.0 kPa, and the reflux ratio is 2-2.5.
- the specific process of gradient calcination is to perform three stages of calcination on the solid phase, the temperature of the first stage of calcination is 80-100°C, and the time is 20-60min, and the second stage of calcination is The temperature is 200-250° C. and the time is 30-60 minutes, and the temperature of the third stage of calcination is 350-450° C. and the time is 30-60 minutes to obtain the positive electrode material.
- the second stage of calcination it also includes condensing the gas obtained from calcination to recover NMP.
- the condensation temperature is 25-35°C.
- the temperature of the first stage of calcination is 80-100°C, in order to remove most of the water in the solid phase; the temperature of the second stage of calcination is 200-250°C, in order to remove the residual NMP in the solid phase, and increase the condensation step at the same time.
- NMP is condensed and recovered, and the third-stage calcination temperature is 350-450°C.
- the binder PVDF in the solid phase is removed (the thermal decomposition temperature is 316°C), and finally a positive electrode material without organic components is obtained, which can be used directly. Valuable metals are recovered by leaching.
- the present invention provides the application of the above method in recovering valuable metals.
- the application in recovering valuable metals is to obtain valuable metals through further leaching and aging treatment of positive electrode materials obtained by the above method.
- the invention combines crushing and sorting, electrophoresis, and gradient roasting processes to recycle scrap positive electrode slurry, which has great industrial application prospects.
- the first step is crushing and sorting to remove plastic and massive debris to obtain a slurry solution;
- the second step is to use electrophoresis to coagulate the suspended matter and press filter to obtain a liquid phase and a solid phase;
- the third step is to process the liquid phase Carry out rectification or distillation to obtain NMP organic phase and water phase;
- the fourth step is to use gradient roasting process to remove water and binder, recover NMP, and obtain positive electrode material.
- the method of the present invention uses the scrapped positive electrode slurry as raw material, and uses crushing and sorting, electrophoresis, and gradient roasting processes to recycle the scrapped positive electrode slurry without introducing a flocculant, and has the advantages of completely separating the NMP solution from the positive electrode powder, organic matter and valuable
- the metal recovery rate is as high as 95%, and the production efficiency is high, which not only improves economic benefits, but also reduces environmental pollution.
- the present invention uses electrophoresis to change the non-coagulation characteristics of the positive electrode slurry, thereby separating the liquid phase and the solid phase, and can obtain an NMP organic phase with a purity greater than 99% by rectification, which has high economic value; the final positive electrode produced by gradient roasting
- the material has low organic content and few impurities, which is conducive to subsequent leaching and recovery of valuable metals, and has great industrial application prospects.
- the brs-p-nmp hand-held NMP concentration detector was used to analyze the organic and aqueous phases after rotary evaporation.
- the NMP concentration in the organic phase was 83%; the NMP concentration in the aqueous phase was 6%.
- the NMP concentration recovered by condensation was 87%.
- the solid ignition loss rate of the cathode material in this embodiment is 0.29%.
- the test method of ignition loss rate refers to "Determination of Thermal Ignition Rate of Solid Waste Gravimetric Method” (HJ1024-2019).
- the brs-p-nmp hand-held NMP concentration detector was used to analyze the organic and aqueous phases after rotary evaporation.
- the NMP concentration in the organic phase was 83%; the NMP concentration in the aqueous phase was 6%.
- the NMP concentration recovered by condensation was 87%.
- the solid ignition loss rate of the cathode material in this embodiment is 0.15%.
- the test method of ignition loss rate refers to "Determination of Thermal Ignition Rate of Solid Waste Gravimetric Method” (HJ1024-2019).
- the brs-p-nmp hand-held NMP concentration detector was used to analyze the organic and aqueous phases after rotary evaporation.
- the NMP concentration in the organic phase was 88%; the NMP concentration in the aqueous phase was 13%.
- the concentration of NMP recovered by condensation was 85%.
- the solid ignition loss rate of the cathode material in this embodiment is 0.33%.
- the test method of ignition loss rate refers to "Determination of Thermal Ignition Rate of Solid Waste Gravimetric Method” (HJ1024-2019).
- the brs-p-nmp hand-held NMP concentration detector was used to analyze the organic and aqueous phases after rotary evaporation.
- the NMP concentration in the organic phase was 81%; the NMP concentration in the aqueous phase was 7%.
- the NMP concentration recovered by condensation was 89%.
- the solid ignition loss rate of the cathode material in this embodiment is 0.42%.
- the test method of ignition loss rate refers to "Determination of Thermal Ignition Rate of Solid Waste Gravimetric Method” (HJ1024-2019).
- the brs-p-nmp hand-held NMP concentration detector was used to analyze the organic phase and the aqueous phase after rectification.
- the NMP concentration in the organic phase was 99.5%; the NMP concentration in the aqueous phase was 1.2%.
- the concentration of NMP recovered by condensation was 88%.
- the solid ignition loss rate of the cathode material in this embodiment is 0.33%.
- the test method of ignition loss rate refers to "Determination of Thermal Ignition Rate of Solid Waste Gravimetric Method” (HJ1024-2019).
- the brs-p-nmp hand-held NMP concentration detector was used to analyze the organic and aqueous phases after rotary evaporation.
- the NMP concentration in the organic phase was 85%; the NMP concentration in the aqueous phase was 6%.
- the NMP concentration recovered by condensation was 87%.
- the solid ignition loss rate of the cathode material in this embodiment is 0.36%, and the energy consumption is 0.38 kwh.
- the processing method of the scrap positive electrode slurry of this comparative example comprises the following steps:
- the solid ignition loss rate of this comparative example is 0.36%, the energy consumption is 0.51kwh, and no separate NMP organic phase is produced during the roasting process.
- the present invention combines crushing and sorting, electrophoresis method, and gradient roasting process to recycle the scrapped positive electrode slurry, and the liquid-solid separation is thorough, and the NMP organic phase can be directly obtained.
- the economic value is high, and the output positive electrode
- the organic content of the material is low, the concentration of NMP in the organic phase recovered by condensation or in the organic phase of the rotary distillation/rectification process is greater than 80%, and the ignition loss rate of the positive electrode material is less than 0.5%.
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Abstract
Description
Claims (10)
- 一种报废正极浆料的处理方法,其特征在于,包括以下步骤:(1)将报废正极浆料进行预处理,得到浆料溶液;(2)将所述浆料溶液进行电泳聚沉,压滤,得到液相和固相;(3)对所述固相进行梯度焙烧,得到正极材料。
- 根据权利要求1所述的处理方法,其特征在于,步骤(1)中,所述预处理的具体步骤为:将报废正极浆料分离出袋装物料,再将袋装物料进行破碎分选,得到浆料溶液。
- 根据权利要求1所述的处理方法,其特征在于,步骤(2)中,所述进行电泳聚沉过程中使用的直流电的电流为50-70mA,电压为60-65V。
- 根据权利要求3所述的处理方法,其特征在于,步骤(2)中,所述进行电泳聚沉过程中使用的直流电的电流密度为0.2~0.6A/m 2。
- 根据权利要求1所述的处理方法,其特征在于,步骤(2)中,所述电泳的时间为20-60min。
- 根据权利要求1所述的处理方法,其特征在于,步骤(2)中,还包括对所述液相进行蒸馏,富集有机相,得到纯度大于70%的NMP。
- 根据权利要求6所述的处理方法,其特征在于,所述蒸馏为减压旋蒸或精馏。
- 根据权利要求1所述的处理方法,其特征在于,步骤(3)中,所述梯度焙烧的具体过程为将所述固相进行三段焙烧,第一段焙烧的温度为80~100℃,时间为20-60min,第二段焙烧的温度为200~250℃,时间为30-60min,第三段焙烧的温度为350~450℃,时间为30-60min,得到正极材料。
- 根据权利要求8所述的处理方法,其特征在于,所述第二段焙烧后还包括对焙烧所得的气体进行冷凝,回收NMP。
- 权利要求1-9任一项所述的方法在回收有价金属中应用。
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
MA60459A MA60459A1 (fr) | 2021-06-22 | 2021-12-30 | Procédé de traitement d'une suspension d'électrode positive mise au rebut et application |
ES202390047A ES2959542R1 (es) | 2021-06-22 | 2021-12-30 | Metodo para el tratamiento de lodos de electrodos positivos desechados, y aplicacion |
GB2313095.8A GB2621934A (en) | 2021-06-22 | 2021-12-30 | Method for treating scrapped positive electrode slurry, and application |
HU2200336A HUP2200336A2 (hu) | 2021-06-22 | 2021-12-30 | Hulladék pozitív elektród szuszpenzió kezelési eljárása és alkalmazása |
DE112021005220.9T DE112021005220T5 (de) | 2021-06-22 | 2021-12-30 | Verfahren zur Behandlung von ausgesonderter Positiv-Elektroden-Aufschlämmung und Verwendung |
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GB2621934A (en) | 2024-02-28 |
ES2959542A2 (es) | 2024-02-26 |
US20240039069A1 (en) | 2024-02-01 |
DE112021005220T5 (de) | 2023-08-10 |
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