CN111468285A - Method for recovering nickel, cobalt and manganese from waste ternary lithium ion battery - Google Patents
Method for recovering nickel, cobalt and manganese from waste ternary lithium ion battery Download PDFInfo
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- CN111468285A CN111468285A CN202010301416.2A CN202010301416A CN111468285A CN 111468285 A CN111468285 A CN 111468285A CN 202010301416 A CN202010301416 A CN 202010301416A CN 111468285 A CN111468285 A CN 111468285A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B9/00—General arrangement of separating plant, e.g. flow sheets
- B03B9/06—General arrangement of separating plant, e.g. flow sheets specially adapted for refuse
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/005—Pretreatment specially adapted for magnetic separation
- B03C1/015—Pretreatment specially adapted for magnetic separation by chemical treatment imparting magnetic properties to the material to be separated, e.g. roasting, reduction, oxidation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
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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
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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
- C22B47/00—Obtaining manganese
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B9/00—General arrangement of separating plant, e.g. flow sheets
- B03B9/06—General arrangement of separating plant, e.g. flow sheets specially adapted for refuse
- B03B2009/066—General arrangement of separating plant, e.g. flow sheets specially adapted for refuse the refuse being batteries
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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
- Y02W30/52—Mechanical processing of waste for the recovery of materials, e.g. crushing, shredding, separation or disassembly
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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
Abstract
The invention provides a method for recovering nickel, cobalt and manganese from waste ternary lithium ion batteries. The method comprises the following steps: s1, disassembling and crushing the waste ternary lithium ion battery to obtain a crushed material; s2, carrying out low-temperature pyrolysis on the crushed material at the temperature of 600-650 ℃ in a protective atmosphere to obtain a pyrolysis material; s3, cleaning and grading the pyrolysis material to obtain coarse-fraction particles, medium-fine-fraction particles and fine-fraction particles, wherein the particle size of the coarse-fraction particles is larger than that of the medium-fine-fraction particles, and the particle size of the medium-fine-fraction particles is larger than that of the fine-fraction particles; and S4, respectively carrying out magnetic separation on the coarse-fraction particles, the medium-fine-fraction particles and the fine-fraction particles to obtain the nickel-cobalt-manganese product. The method adopts the processes of disassembly and crushing, low-temperature pyrolysis, cleaning and grading, and magnetic separation recovery to recover nickel, cobalt and manganese in the waste ternary lithium ion battery, and effectively solves the problems of complex process flow and high recovery cost when the nickel, cobalt and manganese are recovered from the waste ternary lithium ion battery.
Description
Technical Field
The invention relates to the technical field of waste ternary lithium ion battery resource recovery, in particular to a method for recovering nickel, cobalt and manganese from waste ternary lithium ion batteries.
Background
At present, the recovery process of the waste ternary lithium ion battery is roughly pretreatment of discharging, dismantling, crushing, sorting and the like, then plastic, an iron shell and an electrode material after dismantling are separated, and then the electrode material is extracted after alkali leaching, acid leaching and impurity removal; or directly incinerating the disassembled fragments at high temperature to recover metals and further recovering the incineration residues by adopting a wet method. According to the principle of the process, the method can be divided into two categories of physical recovery and chemical recovery, and the main processes are pyrometallurgical method and hydrometallurgical method.
The high-temperature metallurgical process is relatively simple, the high-temperature metallurgical process is suitable for large-scale treatment of various waste lithium batteries, the battery material can provide a large amount of energy consumption required by incineration, the residual volume can be reduced to the maximum extent, but atmospheric pollution is easily caused by combustion of other components in battery electrolytes and electrodes, and the pressure for treating incineration tail gas is large. The hydrometallurgical process mainly comprises the steps of directly dissolving and leaching nickel, cobalt and manganese in the anode material, and then respectively recovering metal ions in a solution obtained after dissolving and leaching, wherein the leaching process generally comprises the following steps: alkaline leaching, acid leaching and bioleaching. In order to improve the extraction efficiency of metals, the process requires that the waste lithium batteries are finely classified according to different chemical compositions of the batteries before crushing so as to be matched with a leachate chemical system. In addition, there are also combined pyrogenic-wet processes, such as the Val' Eas process of dimirore, belgium, for recovering cobalt from spent batteries.
However, the recovery of nickel, cobalt and manganese by using a pyrometallurgical process requires a higher temperature, which increases the recovery cost, and the composition of the waste ternary lithium ion battery is complex, so that the obtained nickel, cobalt and manganese alloy contains more other metals, the content of slag metal is higher, the investment is high, and the operation cost is high. The wet process directly treats the crushed materials, and can obtain high-grade nickel, cobalt and manganese, but has long process flow and complex separation and purification process flow. In a word, the two methods have the defects of complex process flow and higher recovery cost.
Disclosure of Invention
The invention mainly aims to provide a method for recovering nickel, cobalt and manganese from waste ternary lithium ion batteries, and aims to solve the problems of complex process flow and high recovery cost in the prior art when the nickel, cobalt and manganese are recovered from the waste ternary lithium ion batteries.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for recovering nickel, cobalt and manganese from a waste ternary lithium ion battery, comprising the steps of: s1, disassembling and crushing the waste ternary lithium ion battery to obtain a crushed material; s2, carrying out low-temperature pyrolysis on the crushed material under the conditions of protective atmosphere and temperature of 600-650 ℃ to obtain a pyrolysis material; s3, cleaning and grading the pyrolysis material to obtain coarse-fraction particles, medium-fine-fraction particles and fine-fraction particles, wherein the particle size of the coarse-fraction particles is larger than that of the medium-fine-fraction particles, and the particle size of the medium-fine-fraction particles is larger than that of the fine-fraction particles; and S4, respectively carrying out magnetic separation on the coarse-fraction particles, the medium-fine-fraction particles and the fine-fraction particles to obtain the nickel-cobalt-manganese product.
Further, in the step S2, the temperature of the low-temperature pyrolysis is 610-640 ℃.
Further, in the step S2, the time of low-temperature pyrolysis is 0.5-6 h.
Further, in the step S1, in the process of disassembling and crushing the waste ternary lithium ion battery, the crushed particle size is below 50mm, so as to obtain a crushed material.
Further, in step S3, the particle size of the coarse fraction particles is not less than 2mm, preferably 2-5 mm, the particle size of the fine fraction particles is not more than 0.45mm, preferably 0.10-0.45 mm, and the particle size of the medium and fine fraction particles is between the particle sizes of the coarse fraction particles and the fine fraction particles.
Further, step S4 includes: carrying out two-stage magnetic separation on the coarse fraction particles in sequence to obtain a first product; carrying out first-stage magnetic separation on the medium and fine particle-grade particles to obtain a second product; carrying out first-stage magnetic separation on the fine-fraction particles to obtain a third product; the first product, the second product and the third product jointly form a nickel-cobalt-manganese product.
Further, in the step of sequentially carrying out two-stage magnetic separation on the coarse fraction particles, the magnetic field intensity of the first-stage magnetic separation is 200-280 kA/m, and the magnetic field intensity of the second-stage magnetic separation is 40-80 kA/m; in the step of carrying out first-stage magnetic separation on the medium and fine particle-grade particles, the magnetic field intensity is 200-280 kA/m; in the step of carrying out first-stage magnetic separation on the fine-fraction particles, the magnetic field intensity is 200-280 kA/m.
Further, the protective atmosphere is nitrogen, argon, or carbon dioxide.
Further, before the step of disassembling and crushing the waste ternary lithium ion battery, step S1 further includes a step of discharging the waste ternary lithium ion battery.
Further, in step S3, the pyrolysis material is cleaned and classified by using a wet type vibration screen.
The method for recovering nickel, cobalt and manganese from waste ternary lithium ion batteries provided by the invention comprises the process steps of dismantling and crushing, low-temperature roasting, cleaning and grading, and magnetic separation and recovery. The disassembled and crushed battery is roasted at low temperature under the protective atmosphere, so that organic matters including a plastic shell of the battery and polyvinylidene fluoride (PVDF) and the like covering the positive electrode of the battery can be separated from materials. Particularly, through the low-temperature roasting process, nickel, cobalt and manganese in the waste ternary lithium ion battery are converted from non-magnetism to magnetism, so that the nickel, cobalt and manganese can be recovered through magnetic separation. Because the size of the particle fraction is uneven after the waste ternary lithium ion battery is disassembled and crushed and a plurality of negative electrode materials are attached, partial black powder can be generated after the organic matter is cracked in the roasting process, in order to improve the separation efficiency of nickel, cobalt and manganese in the next stage, the invention firstly cleans and grades the pyrolysis material, and then respectively performs magnetic separation on the graded product, thereby obtaining the nickel, cobalt and manganese product.
The method adopts the process steps of disassembly and crushing, low-temperature pyrolysis, cleaning and grading, and magnetic separation recovery to recover the nickel, cobalt and manganese in the waste ternary lithium ion battery, has short treatment process, low energy consumption and low cost, and can form high-efficiency enrichment of the nickel, cobalt and manganese. In a word, the method provided by the invention effectively solves the problems of complex process flow and high recovery cost when the nickel, cobalt and manganese are recovered from the waste ternary lithium ion battery in the prior art.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
Fig. 1 shows a flow chart of a method for recovering nickel, cobalt and manganese from a waste ternary lithium ion battery according to an embodiment of the invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
As described in the background art, the problems of complex process flow and high recovery cost exist when recovering nickel, cobalt and manganese from the waste ternary lithium ion battery in the prior art.
In order to solve the above problems, the present invention provides a method for recovering nickel, cobalt and manganese from a waste ternary lithium ion battery, as shown in fig. 1, the method comprises the following steps: s1, disassembling and crushing the waste ternary lithium ion battery to obtain a crushed material; s2, carrying out low-temperature pyrolysis on the crushed material under the conditions of protective atmosphere and temperature of 600-650 ℃ to obtain a pyrolysis material; s3, cleaning and grading the pyrolysis material to obtain coarse-fraction particles, medium-fine-fraction particles and fine-fraction particles, wherein the particle size of the coarse-fraction particles is larger than that of the medium-fine-fraction particles, and the particle size of the medium-fine-fraction particles is larger than that of the fine-fraction particles; and S4, respectively carrying out magnetic separation on the coarse-fraction particles, the medium-fine-fraction particles and the fine-fraction particles to obtain the nickel-cobalt-manganese product.
The method for recovering nickel, cobalt and manganese from waste ternary lithium ion batteries comprises the process steps of dismantling and crushing, low-temperature pyrolysis, cleaning and grading, and magnetic separation and recovery. The disassembled and crushed battery is roasted at low temperature under the protective atmosphere, so that organic matters including a plastic shell of the battery and polyvinylidene fluoride (PVDF) and the like covering the positive electrode of the battery can be separated from materials. The low-temperature pyrolysis mainly cracks organic matters on the battery to form carbon, the positive electrode material nickel cobalt manganese becomes magnetic in the process, the black powder refers to the original negative electrode material graphite of the battery and the carbon generated in the low-temperature pyrolysis process, and the material composition after the low-temperature pyrolysis is as follows: nickel cobalt manganese, copper sheets, aluminum sheets, iron sheets, black powder (graphite and carbon). Because the grain size of graphite and black powder is very small (generally, the grain size is fine powder less than 0.074mm), and the grain size of copper sheets, aluminum sheets, iron sheets and part of the positive electrode material (nickel, cobalt and manganese) is larger (greater than 0.074mm), the black powder and most of nickel, cobalt and manganese can be separated by cleaning and grading. Particularly, through the low-temperature roasting process, nickel, cobalt and manganese in the waste ternary lithium ion battery are converted from non-magnetism to magnetism, so that the nickel, cobalt and manganese can be separated from other copper sheets, aluminum sheets and black powder through magnetic separation. Because the size of the particle fraction is uneven after the waste ternary lithium ion battery is disassembled and crushed and a plurality of negative electrode materials are attached, partial black powder can be generated after the organic matter is cracked in the roasting process, in order to improve the separation efficiency of nickel, cobalt and manganese in the next stage, the invention firstly cleans and grades the pyrolysis material, and then respectively performs magnetic separation on the graded product, thereby obtaining the nickel, cobalt and manganese product.
The method adopts the process steps of disassembly and crushing, low-temperature roasting, cleaning and grading, and magnetic separation recovery to recover the nickel, cobalt and manganese in the waste ternary lithium ion battery, has short treatment process, low energy consumption and low cost, and can form high-efficiency enrichment of the nickel, cobalt and manganese. In a word, the method provided by the invention effectively solves the problems of complex process flow and high recovery cost when the nickel, cobalt and manganese are recovered from the waste ternary lithium ion battery in the prior art.
In order to pyrolyze the organic components more sufficiently and convert the nickel, cobalt and manganese in the battery from non-magnetic to magnetic more sufficiently, in a preferred embodiment, the temperature of the low-temperature pyrolysis in step S2 is 610-640 ℃. More preferably, in the step S2, the time for low-temperature pyrolysis is 0.5-6 h.
In a preferred embodiment, in the step S1, during the process of disassembling and crushing the waste ternary lithium ion battery, the crushed particle size is below 50mm, so as to obtain a crushed material. The battery is crushed to the particle size range, on one hand, the battery is favorable for more sufficient reaction in the low-temperature pyrolysis process, on the other hand, the effect of subsequent cleaning and grading can be improved, the magnetic separation effect is further improved, and the nickel, cobalt and manganese are more effectively enriched.
In a preferred embodiment, in step S3, the particle size of the coarse fraction is greater than or equal to 2mm, preferably 2-5 mm, the particle size of the fine fraction is less than or equal to 0.45mm, preferably 0.10-0.45 mm, and the particle size of the medium-fine fraction is between the particle sizes of the coarse fraction and the fine fraction. The size of each grade of particles is controlled within the range, so that the targeted treatment of the subsequent magnetic separation process is facilitated, and the treatment efficiency and the nickel-cobalt-manganese enrichment effect are further facilitated to be improved.
As described above, since the nickel-cobalt-manganese is converted into the magnetic substance during the low-temperature roasting process, the magnetic separation process can separate and enrich the magnetic substance, and in order to further improve the separation effect of the nickel-cobalt-manganese, in a preferred embodiment, the step S4 includes: carrying out two-stage magnetic separation on the coarse fraction particles in sequence to obtain a first product; carrying out first-stage magnetic separation on the medium and fine particle-grade particles to obtain a second product; carrying out first-stage magnetic separation on the fine-fraction particles to obtain a third product; the first product, the second product and the third product jointly form a nickel-cobalt-manganese product. More preferably, in the step of sequentially carrying out two-stage magnetic separation on the coarse fraction particles, the magnetic field intensity of the first-stage magnetic separation is 200-280 kA/m, and the magnetic field intensity of the second-stage magnetic separation is 40-80 kA/m; in the step of carrying out first-stage magnetic separation on the medium and fine particle-grade particles, the magnetic field intensity is 200-280 kA/m; in the step of carrying out first-stage magnetic separation on the fine-fraction particles, the magnetic field intensity is 200-280 kA/m. The coarse fraction adopts a two-stage magnetic separation process, the first stage magnetic separation obtains coarse concentrate under the high magnetic field intensity, and the coarse concentrate of the first stage magnetic separation is subjected to two-stage magnetic separation under the low magnetic field intensity to further remove impurities. And the magnetic separation magnetic field intensity of each grade is controlled in the range, so that the separation and enrichment effects of nickel, cobalt and manganese are further improved. The first product, the second product and the third product can be used as nickel-cobalt-manganese products respectively, and of course, the nickel-cobalt-manganese obtained by three size fraction magnetic separation can be combined into one product.
In the practical operation process, the magnetic separation equipment of coarse fraction is preferably dry or wet magnetic roller and magnetic pulley, the medium-fine fraction and fine-fraction classification products are preferably wet magnetic roller, and the magnetic medium can be electrically excited or permanent magnet.
In a preferred embodiment, the protective atmosphere is nitrogen, argon, or carbon dioxide.
In a preferred embodiment, step S1 further includes a step of discharging the waste ternary lithium ion battery before the step of disassembling and crushing the waste ternary lithium ion battery. When the ternary lithium ion battery is scrapped, the residual electric quantity has explosion danger in the storage and crushing processes, the explosion danger can be reduced by utilizing the discharging step, and the problems of fire and the like easily caused by the residual electric quantity in the crushing process are avoided being disassembled.
In a preferred embodiment, in step S3, the pyrolysis material is washed and classified using a wet vibrating screen.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
The method is characterized in that a square waste ternary lithium ion battery in a certain factory in Jiangsu is discharged, crushed to be below 30mm and roasted for 2 hours at the temperature of 620 ℃ in a protective atmosphere of nitrogen. Cleaning the pyrolysis material, classifying the pyrolysis material into three size fractions of 3mm, 0.45-3 mm and 0.45mm, carrying out first-stage magnetic separation on a product with the size fraction of 3.0mm under the magnetic field strength of 240kA/m, and carrying out second-stage magnetic separation on concentrate subjected to the first-stage magnetic separation under the magnetic field strength of 40kA/m to remove impurity iron. The iron content in the square battery is not high, after two-stage magnetic separation is carried out on the grain size of 3mm, the iron grade of the magnetic separation concentrate is 38.32%, and the grades of nickel, cobalt and manganese in the magnetic separation tailings are 32.71%, 14.83% and 14.45% respectively. Under the condition that the magnetic field intensity is 240kA/m, the medium-fine fraction and the fine fraction are respectively subjected to first-stage magnetic separation, and after the obtained nickel-cobalt-manganese intermediate products are combined, the grades of nickel, cobalt and manganese are respectively 36.90%, 16.21% and 16.57%. After all nickel-cobalt-manganese products obtained by magnetic separation are combined, the grades of nickel, cobalt and manganese are respectively 36.10%, 15.74% and 15.81%, and the recovery rates are respectively 94.98%, 94.37% and 91.27%.
Example 2
The method is characterized in that a square waste ternary lithium ion battery in a certain factory in Jiangsu is discharged, crushed to be less than 30mm and roasted for 1.5 hours at 640 ℃ in a protective atmosphere of nitrogen. Cleaning the pyrolysis material, classifying the pyrolysis material into three size fractions of 3mm, 0.45-3 mm and 0.45mm, carrying out first-stage magnetic separation on a product with the size fraction of 3.0mm under the magnetic field strength of 240kA/m, and carrying out second-stage magnetic separation on concentrate subjected to the first-stage magnetic separation under the magnetic field strength of 40kA/m to remove impurity iron. The square battery has low iron content, and after two-stage magnetic separation is carried out on the grain size of 3mm, the iron grade of the magnetic separation concentrate is 37.68%, and the grades of nickel, cobalt and manganese in the magnetic separation tail tailings are 31.98%, 15.11% and 14.05%. Under the condition that the magnetic field intensity is 240kA/m, the grading products of medium and fine fractions are respectively subjected to first-stage magnetic separation, and after the obtained nickel-cobalt-manganese intermediate products are combined, the grades of nickel, cobalt and manganese are respectively 36.24%, 16.81% and 16.12%. After all the nickel, cobalt and manganese products obtained by magnetic separation are combined, the grades of nickel, cobalt and manganese are respectively 35.98%, 15.37% and 15.09%, and the recovery rates are respectively 95.86%, 95.79% and 92.76%.
Example 3
The method is characterized in that a square waste ternary lithium ion battery in a certain factory in Jiangsu is discharged, crushed to be less than 30mm and roasted for 3 hours at the temperature of 610 ℃ in a protective atmosphere of nitrogen. Cleaning the pyrolysis material, classifying the pyrolysis material into three size fractions of 3mm, 0.45-3 mm and 0.45mm, carrying out first-stage magnetic separation on a product with the size fraction of 3.0mm under the magnetic field strength of 240kA/m, and carrying out second-stage magnetic separation on concentrate subjected to the first-stage magnetic separation under the magnetic field strength of 40kA/m to remove impurity iron. The square battery has low iron content, and after two-stage magnetic separation is carried out on the grain size of 3mm, the iron grade of the magnetic separation concentrate is 37.98%, and the grades of nickel, cobalt and manganese in the magnetic separation tail tailings are 33.87%, 14.76% and 14.59%. Under the condition that the magnetic field intensity is 240kA/m, the medium-fine fraction and the fine fraction are respectively subjected to first-stage magnetic separation, and after the obtained nickel-cobalt-manganese intermediate products are combined, the grades of nickel, cobalt and manganese are respectively 36.93%, 16.89% and 16.45%. After all the nickel, cobalt and manganese products obtained by magnetic separation are combined, the grades of nickel, cobalt and manganese are respectively 36.11%, 15.74% and 15.42%, and the recovery rates are respectively 93.26%, 94.13% and 90.89%.
Example 4
The method is characterized in that a square waste ternary lithium ion battery in a certain factory in Jiangsu is discharged, crushed to be less than 30mm and roasted for 2 hours at the temperature of 600 ℃ in a protective atmosphere of nitrogen. Cleaning the pyrolysis material, classifying the pyrolysis material into three size fractions of 3mm, 0.45-3 mm and 0.45mm, carrying out first-stage magnetic separation on a product with the size fraction of 3.0mm under the magnetic field strength of 240kA/m, and carrying out second-stage magnetic separation on concentrate subjected to the first-stage magnetic separation under the magnetic field strength of 40kA/m to remove impurity iron. The square battery has low iron content, and after two-stage magnetic separation is carried out on the grain size of 3mm, the iron grade of the magnetic separation concentrate is 34.21%, and the grades of nickel, cobalt and manganese in the magnetic separation tail tailings are 31.24%, 13.58% and 12.98%. Under the condition that the magnetic field intensity is 240kA/m, the medium-fine fraction and the fine fraction are respectively subjected to first-stage magnetic separation, and after the obtained nickel-cobalt-manganese intermediate products are combined, the grades of nickel, cobalt and manganese are respectively 35.26%, 15.49% and 15.13%. After all the nickel, cobalt and manganese products obtained by magnetic separation are combined, the grades of nickel, cobalt and manganese are 34.89%, 14.75% and 14.26% respectively, and the recovery rates are 91.26%, 90.76% and 90.36% respectively.
Example 5
The method is characterized in that a square waste ternary lithium ion battery in a certain factory in Jiangsu is discharged, crushed to be less than 30mm and roasted for 1.5 hours at the temperature of 650 ℃ in a protective atmosphere of nitrogen. Cleaning the pyrolysis material, classifying the pyrolysis material into three size fractions of 3mm, 0.45-3 mm and 0.45mm, carrying out first-stage magnetic separation on a product with the size fraction of 3.0mm under the magnetic field strength of 240kA/m, and carrying out second-stage magnetic separation on concentrate subjected to the first-stage magnetic separation under the magnetic field strength of 40kA/m to remove impurity iron. The square battery has low iron content, and after two-stage magnetic separation is carried out on the grain size of 3mm, the iron grade of the magnetic separation concentrate is 31.69%, and the nickel, cobalt and manganese grades in the magnetic separation tail tailings are 26.89%, 13.45% and 13.62%. Under the condition that the magnetic field intensity is 240kA/m, the grading products of medium and fine fractions are respectively subjected to first-stage magnetic separation, and after the obtained nickel-cobalt-manganese intermediate products are combined, the grades of nickel, cobalt and manganese are respectively 30.16%, 13.29% and 13.11%. After all the nickel, cobalt and manganese products obtained by magnetic separation are combined, the grades of nickel, cobalt and manganese are respectively 29.22%, 13.02% and 12.93%, and the recovery rates are respectively 90.26%, 88.26% and 87.46%.
Example 6
The method is characterized in that a square waste ternary lithium ion battery in a certain factory in Jiangsu is broken to be less than 10mm after being discharged, and is roasted for 2 hours at the temperature of 620 ℃ in a protective atmosphere of nitrogen. Cleaning the pyrolysis material, classifying the cleaned pyrolysis material into three size fractions of 2mm, 0.30-2 mm and 0.30mm, carrying out first-stage magnetic separation on the product of the size fraction of 2mm under the magnetic field strength of 240kA/m, and carrying out second-stage magnetic separation on the concentrate subjected to the first-stage magnetic separation under the magnetic field strength of 40kA/m to remove impurity iron. The square battery has low iron content, and after two-stage magnetic separation is carried out on the 2mm grain size fraction, the iron grade of the magnetic separation concentrate is 35.48%, and the grades of nickel, cobalt and manganese in the magnetic separation tail tailings are 30.45%, 13.56% and 13.28%. Under the condition that the magnetic field intensity is 240kA/m, the grading products of medium and fine fractions are respectively subjected to first-stage magnetic separation, and after the obtained nickel-cobalt-manganese intermediate products are combined, the grades of nickel, cobalt and manganese are respectively 33.59%, 14.24% and 14.38%. After all the nickel, cobalt and manganese products obtained by magnetic separation are combined, the grades of nickel, cobalt and manganese are respectively 32.89%, 13.68% and 13.91%, and the recovery rates are respectively 94.47%, 94.02% and 90.89%.
Example 7
The method is characterized in that a square waste ternary lithium ion battery in a certain factory in Jiangsu is broken to be less than 50mm after being discharged, and is roasted for 2 hours at the temperature of 620 ℃ in a protective atmosphere of nitrogen. Cleaning the pyrolysis material, classifying the cleaned pyrolysis material into three size fractions of 5mm, 0.45-5 mm and 0.45mm, carrying out first-stage magnetic separation on a product of the size fraction of 5mm under the magnetic field strength of 240kA/m, and carrying out second-stage magnetic separation on concentrate subjected to the first-stage magnetic separation under the magnetic field strength of 40kA/m to remove impurity iron. The iron content in the square battery is not high, after two-stage magnetic separation is carried out on the grain size of more than 5mm, the iron grade of the magnetic separation concentrate is 37.53%, and the grades of nickel, cobalt and manganese in the magnetic separation tail tailings are 30.28%, 13.26% and 12.94%. Under the condition that the magnetic field intensity is 240kA/m, the medium-fine fraction and the fine fraction are respectively subjected to first-stage magnetic separation, and after the obtained nickel-cobalt-manganese intermediate products are combined, the grades of nickel, cobalt and manganese are respectively 32.49%, 13.84% and 13.26%. After all the nickel, cobalt and manganese products obtained by magnetic separation are combined, the grades of nickel, cobalt and manganese are 31.49%, 13.70% and 13.11% respectively, and the recovery rates are 93.56%, 93.47% and 92.01% respectively.
Example 8
The method is characterized in that a square waste ternary lithium ion battery in a certain factory in Jiangsu is discharged, crushed to be below 30mm and roasted for 2 hours at the temperature of 620 ℃ in a protective atmosphere of nitrogen. Cleaning the pyrolysis material, classifying into three size fractions of 3mm, 0.45-3 mm and 0.45mm, carrying out first-stage magnetic separation on a product of the size fraction of 3mm under the magnetic field intensity of 280kA/m, and carrying out second-stage magnetic separation on concentrate subjected to the first-stage magnetic separation under the magnetic field intensity of 80kA/m to remove impurity iron. The square battery has low iron content, and after two-stage magnetic separation is carried out on the grain size of 3mm, the iron grade of the magnetic separation concentrate is 29.56%, and the nickel, cobalt and manganese grades in the magnetic separation tail tailings are 29.42%, 12.14% and 12.62%. Under the condition that the magnetic field intensity is 280kA/m, the medium-fine fraction and the fine fraction are respectively subjected to first-stage magnetic separation, and after the obtained nickel-cobalt-manganese intermediate products are combined, the grades of nickel, cobalt and manganese are respectively 31.13%, 13.29% and 12.99%. After all the nickel, cobalt and manganese products obtained by magnetic separation are combined, the grades of nickel, cobalt and manganese are respectively 30.89%, 12.83% and 12.80%, and the recovery rates are respectively 94.20%, 94.34% and 92.87%.
Example 9
The method is characterized in that a square waste ternary lithium ion battery in a certain factory in Jiangsu is discharged, crushed to be below 30mm and roasted for 2 hours at the temperature of 620 ℃ in a protective atmosphere of nitrogen. Cleaning the pyrolysis material, classifying the cleaned pyrolysis material into three size fractions of 3mm, 0.45-3 mm and 0.45mm, carrying out first-stage magnetic separation on a product with the size fraction of 3mm under the magnetic field strength of 200kA/m, and carrying out second-stage magnetic separation on concentrate subjected to the first-stage magnetic separation under the magnetic field strength of 40kA/m to remove impurity iron. The square battery has low iron content, and after two-stage magnetic separation is carried out on the grain size of 3mm, the iron grade of the magnetic separation concentrate is 38.83 percent, and the nickel, cobalt and manganese grades in the magnetic separation tail tailings are 32.92 percent, 14.93 percent and 14.86 percent. Under the condition that the magnetic field intensity is 200kA/m, the grading products of the medium-fine fraction and the fine fraction are respectively subjected to first-stage magnetic separation, and after the obtained nickel-cobalt-manganese intermediate products are combined, the grades of nickel, cobalt and manganese are respectively 37.02%, 16.46% and 16.83%. After all the nickel, cobalt and manganese products obtained by magnetic separation are combined, the grades of nickel, cobalt and manganese are 36.40%, 15.86% and 15.99% respectively, and the recovery rates are 93.26%, 92.71% and 90.76% respectively.
Example 10
The method is characterized in that a square waste ternary lithium ion battery in a certain factory in Jiangsu is discharged, crushed to be below 30mm and roasted for 2 hours at the temperature of 620 ℃ in a protective atmosphere of nitrogen. Cleaning the pyrolysis material, classifying the pyrolysis material into three size fractions of 3mm, 0.45-3 mm and 0.45mm, carrying out first-stage magnetic separation on a product with the size fraction of 3mm under the magnetic field intensity of 180kA/m, and carrying out second-stage magnetic separation on concentrate obtained by the first-stage magnetic separation under the magnetic field intensity of 80kA/m to remove impurity iron. The square battery has low iron content, and after two-stage magnetic separation is carried out on the grain size of 3mm, the iron grade of the magnetic separation concentrate is 39.12 percent, and the nickel, cobalt and manganese grades in the magnetic separation tail tailings are 30.49 percent, 12.89 percent and 12.23 percent. Under the condition that the magnetic field intensity is 90kA/m, the medium-fine fraction and the fine fraction are respectively subjected to first-stage magnetic separation, and after the obtained nickel-cobalt-manganese intermediate products are combined, the grades of nickel, cobalt and manganese are respectively 32.16%, 13.27% and 12.37%. After all the nickel, cobalt and manganese products obtained by magnetic separation are combined, the grades of nickel, cobalt and manganese are respectively 31.79%, 13.11% and 12.30%, and the recovery rates are respectively 90.26%, 89.77% and 90.06%.
Example 11
The cylindrical ternary lithium ion battery in a factory in Hubei province is crushed to be less than 50mm after being discharged, and is roasted for 1.5h at the temperature of 620 ℃ in a protective atmosphere. And cleaning the pyrolysis material, and grading into three size fractions of >5mm, 0.15-5 mm and <0.15 mm. And (3) carrying out primary magnetic separation on the product with the size fraction of more than 5mm under the magnetic field strength of 200kA/m, and carrying out fine separation on the concentrate subjected to the primary magnetic separation under the magnetic field strength of 50kA/m to remove impurities, wherein the iron grade in the impurities is 35.89%, and the iron recovery rate is 93.78%. The fraction of 0.15 mm-5 mm size fraction is obtained by magnetic separation under the condition that the magnetic field intensity is 220kA/m, and the grades of the nickel-cobalt-manganese product obtained by the magnetic separation at one stage are respectively as follows: 26.30%, 14.15% and 15.88%, and the recovery rates are respectively as follows: 5.26%, 3.64% and 5.98%. Under the condition that the magnetic field intensity of the product with the size fraction of less than 0.15mm is 220kA/m, the grade of the obtained nickel-cobalt-manganese product is 31.86 percent, 14.95 percent and 16.73 percent respectively, and the recovery rate is 89.60 percent, 92.67 percent and 88.48 percent respectively. The grades of nickel, cobalt and manganese obtained by magnetic separation are respectively 30.85%, 14.57% and 16.81%, and the recovery rates are respectively 95.86%, 97.44% and 95.68%.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for recovering nickel, cobalt and manganese from waste ternary lithium ion batteries is characterized by comprising the following steps:
S1, disassembling and crushing the waste ternary lithium ion battery to obtain a crushed material;
S2, carrying out low-temperature pyrolysis on the crushed material under the conditions of protective atmosphere and temperature of 600-650 ℃ to obtain a pyrolysis material;
S3, cleaning and grading the pyrolysis material to obtain coarse-fraction particles, medium-fine-fraction particles and fine-fraction particles, wherein the particle size of the coarse-fraction particles is larger than that of the medium-fine-fraction particles, and the particle size of the medium-fine-fraction particles is larger than that of the fine-fraction particles;
And S4, respectively carrying out magnetic separation on the coarse fraction particles, the medium and fine fraction particles and the fine fraction particles to obtain a nickel-cobalt-manganese product.
2. The method according to claim 1, wherein in the step S2, the temperature of the low-temperature pyrolysis is 610-640 ℃.
3. The method according to claim 2, wherein in the step S2, the time for the low-temperature pyrolysis is 0.5-6 h.
4. The method according to claim 1, wherein in the step S1, the crushed material is obtained by crushing the waste ternary lithium ion battery to a particle size of 50mm or less in the process of disassembling and crushing the waste ternary lithium ion battery.
5. The method according to claim 4, wherein in step S3, the coarse fraction particles have a particle size of 2mm or more, preferably 2-5 mm, the fine fraction particles have a particle size of 0.45mm or less, preferably 0.10-0.45 mm, and the medium fine fraction particles have a particle size between the particle sizes of the coarse fraction particles and the fine fraction particles.
6. The method according to any one of claims 1 to 5, wherein the step S4 includes:
Sequentially carrying out two-stage magnetic separation on the coarse fraction particles to obtain a first product;
Carrying out first-stage magnetic separation on the medium and fine fraction particles to obtain a second product;
Carrying out first-stage magnetic separation on the fine-fraction particles to obtain a third product;
The first product, the second product and the third product jointly form the nickel-cobalt-manganese product.
7. The method of claim 6,
In the step of sequentially carrying out two-stage magnetic separation on the coarse fraction particles, the magnetic field intensity of the first-stage magnetic separation is 200-280 kA/m, and the magnetic field intensity of the second-stage magnetic separation is 40-80 kA/m;
In the step of carrying out first-stage magnetic separation on the medium and fine fraction particles, the magnetic field intensity is 200-280 kA/m;
And in the step of carrying out first-stage magnetic separation on the fine-fraction particles, the magnetic field intensity is 200-280 kA/m.
8. The method according to any one of claims 1 to 5, characterized in that the protective atmosphere is nitrogen, argon, or carbon dioxide.
9. The method according to any one of claims 1 to 5, wherein the step S1 further comprises a step of discharging the waste ternary lithium ion battery before the step of dismantling and crushing the waste ternary lithium ion battery.
10. The method as claimed in any one of claims 1 to 5, wherein in the step S3, the pyrolysis material is washed and classified by using a wet vibrating screen.
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