CN111139367A - Method for deeply removing fluorine from LiCl solution recovered from waste battery - Google Patents
Method for deeply removing fluorine from LiCl solution recovered from waste battery Download PDFInfo
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- CN111139367A CN111139367A CN201911399832.4A CN201911399832A CN111139367A CN 111139367 A CN111139367 A CN 111139367A CN 201911399832 A CN201911399832 A CN 201911399832A CN 111139367 A CN111139367 A CN 111139367A
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- fluorine
- licl solution
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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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
- 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
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
-
- 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 discloses a method for deeply removing fluorine from a LiCl solution recovered from a waste battery, which takes the LiCl solution as a raw material to prepare battery-grade lithium carbonate and comprises the following steps: A. preparing raw materials; B. activating a fluorine removal agent; C. adjusting the pH value of the system; removing fluorine from the LiCl solution; E. and (4) regenerating the fluorine removal agent. According to the invention, a small amount of fluorine removal agent is added into the LiCl solution to remove fluorine deeply, and then the LiCl solution is regenerated and recycled. The method has good fluorine removal effect, is simple and rapid, and the fluorine removal agent can be recycled through multiple regeneration, thereby greatly reducing the production cost; meanwhile, the method has the advantages of short process flow, high fluorine removal efficiency, simplicity in operation, environmental friendliness and the like, and can realize large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of battery recovery, in particular to a method for deeply removing fluorine in LiCl solution recovered from waste batteries.
Background
Lithium is the lightest and most active metal element in the nature, lithium and compounds thereof are widely applied to the fields of ceramics, glass, medicines, aluminum products, synthetic rubber, plastics, lithium batteries, refrigerants, military industry, high technology and the like in the life and production of human beings, and lithium has the reputation of 'energy metal promoting the progress of human beings'.
Therefore, the recovery and reuse of lithium resources are also an important issue. The recovery of various waste batteries in the lithium resource recovery is important. At present, domestic waste batteries are mainly refined by a wet method, and in the process, due to the existence of electrolyte in the waste batteries and the limitation of a process flow, fluorine ions are inevitably enriched in the process of preparing lithium salt compounds, so that the serious problems of standard exceeding of fluorine content, environmental pollution and the like are caused.
At present, the mature defluorination method comprises a coagulating sedimentation method, an adsorption method, an ion exchange method and the like. In the methods, the key point is to find a fluorine removal agent with large fluorine removal amount, high speed, high efficiency and low cost. Wherein the calcium salt is widely used defluorinating agent and is used to generate insoluble CaF2The fluorine is removed by precipitation, but only the coarse fluorine removal can be realized in LiCl solution, and the fluorine cannot be removedThe purpose of deep fluorine removal is achieved; among them, CN110205502A discloses a method for removing fluorine by adding aluminum sulfate salt into neutral leachate of lepidolite ore, but the method has large investment, high fluorine removal cost, difficult filter pressing and unfavorable production.
Disclosure of Invention
The invention provides a method for deeply removing fluorine from a LiCl solution recovered from a waste battery in order to overcome the defects in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for deeply removing fluorine from a LiCl solution recovered from a waste battery comprises the following steps:
A. preparing raw materials: taking a certain amount of LiCl solution prepared by recovering waste batteries, and calculating the addition of a fluorine removal agent according to the fluorine content in the LiCl solution according to different addition times;
B. activation of a fluorine removal agent: adding the fluorine removing agent into inorganic acid according to a certain solid-liquid ratio, mixing and stirring to prepare activated fluorine removing agent slurry;
C. adjusting the pH of the system: adding the defluorinating agent slurry into a LiCl solution, and then adding acid or alkali to adjust the pH value to 5-7;
D. and (3) removing fluorine from LiCl solution: mixing and stirring for 0.5-1.5 h, and performing filter pressing to obtain LiCl purified liquid and fluorine-containing slag;
E. and (3) regenerating a fluorine removal agent: and D, adding a sodium hydroxide solution into the fluorine-containing slag obtained in the step D according to a certain solid-to-liquid ratio, reacting for 1.0-2.0 h at the temperature of 85-95 ℃, and after the reaction is completed, carrying out filter pressing, washing and drying to obtain the regenerated fluorine removal agent.
Preferably, the defluorinating agent is a composite material made of alumina, porous carbon and a small amount of rare earth elements.
Preferably, the addition amount of the fluorine removal agent in the step A is 10-40 times of the fluorine content in the LiCl solution.
Preferably, the inorganic acid in the step B is one or a combination of more than one of hydrochloric acid, sulfuric acid and nitric acid, and the solid-liquid ratio is 1: 2-5.
Preferably, the acid in step C is one or more of hydrochloric acid, sulfuric acid and nitric acid, and the base is one or more of sodium hydroxide, ammonia water and sodium carbonate.
Preferably, the concentration of the sodium hydroxide solution in the step E is 30-50 g/L, and the solid-to-liquid ratio of the fluorine-containing slag to the sodium hydroxide solution is 1: 3-6.
The design key point of the invention is that the impressing device adopts a magnetic flux winding framework which is electrified instantly to generate a magnetic field, under the action of the magnetic field, the front iron core is attracted to be quickly close to the magnetic flux winding framework, a driving ejector block on the iron core is rushed to a driven ejector block, a center deviation interval for accelerating the iron core is arranged between the driving ejector block and the driven ejector block, when the instant initial speed reaches a certain value, the driving ejector block can instantly eject a carving plate mounting seat, so that a carving plate on the carving plate mounting seat can be instantly impressed, the upper surface of the carving plate is better matched with the surface of a rod body of an aluminum rod, and the upper surface of the carving plate is designed to have a certain slight radian when the carving plate is designed, so that label codes on the carving plate can be conveniently impressed on the copper rod.
In addition, the processing operation of the copper bar feeding device is automatically controlled by a PLC electrical system, the upper hopper opening of the copper bar feeding hopper can be connected with a discharging and feeding machine, so that the copper bar feeding device can be directly butted with a copper bar production line, the discharging and feeding machine is used for neatly and transversely placing copper bars into the copper bar feeding hopper, and the hopper openings (openings) below the copper bar feeding hopper directly enable the copper bars to slide out, so that the copper bars are fed one by one.
Compared with the prior art, the method takes LiCl solution recovered from waste batteries as a raw material, and achieves the purpose of deep fluorine removal by adding the fluorine removal agent, thereby solving the problems of corrosion of fluorine ions to equipment and overproof fluorine content in lithium carbonate products. And the defluorinating agent can be regenerated by the sodium hydroxide solution, the process is simple, and the production cost is low.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
As shown in fig. 1, the method for deeply removing fluorine from the recovered LiCl solution of waste batteries according to the present invention is operated according to the process flow of fig. 1.
Example 1:
A. preparing raw materials: the LiCl solution obtained in 10L waste battery recovery is measured to have the fluorine ion content of 98ppm, and the mass of the required defluorinating agent is 19.6g calculated according to 20 times of the F content in the LiCl solution.
B. Activation of a fluorine removal agent: 78.4ml of hydrochloric acid solution of 2mol/L is added into the defluorinating agent according to the solid-to-liquid ratio of 1:4, and the mixture is uniformly mixed and stirred to prepare defluorinating agent slurry.
C. Adjusting the pH of the system: adding the defluorinating agent slurry into LiCl solution, and adding dilute hydrochloric acid to adjust the pH value of the system to 5.
D. And (3) removing fluorine from LiCl solution: mixing and stirring for 1h, and performing suction filtration to obtain fluorine-containing slag and a defluorinated LiCl solution, wherein the content of fluorine ions is measured to be 3.5 ppm.
E. And (3) regenerating a fluorine removal agent: mixing fluorine-containing slag according to the proportion of 1:4, adding 35g/L of sodium hydroxide solution into the solution at the solid-to-liquid ratio, heating to 90 ℃, reacting for 1h, then carrying out suction filtration, washing with deionized water, and drying in an oven to obtain the regenerated defluorinating agent.
F. And (3) regenerating a fluorine removal agent to remove fluorine: the procedure of example 1 was repeated to carry out secondary defluorination of the regenerated defluorinating agent, and the content of fluorine ions in the defluorination solution was found to be 4.2 ppm.
Example 2:
A. preparing raw materials: the LiCl solution obtained in 10L of waste battery recovery is taken, the content of fluorine ions is measured to be 67ppm, and the mass of the required defluorinating agent is 10g calculated according to 15 times of the F content in the LiCl solution.
B. Activation of a fluorine removal agent: 40ml of 2mol/L hydrochloric acid solution is added into the defluorinating agent according to the solid-to-liquid ratio of 1:4, and the defluorinating agent slurry is prepared by uniformly mixing and stirring.
C. Adjusting the pH of the system: adding the defluorinating agent slurry into LiCl solution, and adding sodium carbonate to adjust the pH value of the system to 5.
D. And (3) removing fluorine from LiCl solution: mixing and stirring for 1h, and performing suction filtration to obtain fluorine-containing slag and a defluorinated LiCl solution, wherein the content of fluorine ions is measured to be 3.8 ppm.
E. And (3) regenerating a fluorine removal agent: adding 40g/L sodium hydroxide solution into fluorine-containing slag according to the solid-to-liquid ratio of 1:4, heating to 90 ℃, reacting for 1h, then carrying out suction filtration, washing with deionized water, and drying in an oven to obtain the regenerated defluorinating agent.
F. And (3) regenerating a fluorine removal agent to remove fluorine: the procedure of example 2 was repeated to carry out secondary defluorination of the regenerated defluorinating agent, and the content of fluoride ions in the defluorination solution was measured to be 4.3 ppm.
Example 3:
A. preparing raw materials: the LiCl solution obtained in the recovery of 5L of waste batteries is measured to have the fluorine ion content of 84ppm, and the mass of the required defluorinating agent is 6.3g calculated according to 15 times of the F content in the LiCl solution.
B. Activation of a fluorine removal agent: 78.4ml of hydrochloric acid solution of 2mol/L is added into the defluorinating agent according to the solid-to-liquid ratio of 1: 5, and the mixture is mixed and stirred evenly to prepare defluorinating agent slurry.
C. Adjusting the pH of the system: adding the defluorinating agent slurry into LiCl solution, and adding dilute hydrochloric acid to adjust the pH value of the system to 5.
D. And (3) removing fluorine from LiCl solution: mixing and stirring for 1h, performing suction filtration to obtain fluorine-containing slag and a defluorinated LiCl solution, and measuring the fluorine ion content of the solution to be 2.1 ppm.
E. And (3) regenerating a fluorine removal agent: adding 45g/L sodium hydroxide solution into fluorine-containing slag according to the solid-to-liquid ratio of 1:4, heating to 90 ℃, reacting for 1h, then carrying out suction filtration, washing with deionized water, and drying in an oven to obtain the regenerated defluorinating agent.
F. And (3) regenerating a fluorine removal agent to remove fluorine: the procedure of example 3 was repeated to carry out secondary defluorination of the regenerated defluorinating agent, and the content of fluoride ions in the defluorinating liquid was found to be 3.2 ppm.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the patent and protection scope of the present invention should be subject to the appended claims.
Claims (6)
1. A method for deeply removing fluorine from LiCl solution recovered from waste batteries is characterized by comprising the following steps:
A. preparing raw materials: taking a certain amount of LiCl solution prepared by recovering waste batteries, and calculating the addition of a fluorine removal agent according to the fluorine content in the LiCl solution according to different addition times;
B. activation of a fluorine removal agent: adding the fluorine removing agent into inorganic acid according to a certain solid-liquid ratio, mixing and stirring to prepare activated fluorine removing agent slurry;
C. adjusting the pH of the system: adding the defluorinating agent slurry into a LiCl solution, and then adding acid or alkali to adjust the pH value to 5-7;
D. and (3) removing fluorine from LiCl solution: mixing and stirring for 0.5-1.5 h, and performing filter pressing to obtain LiCl purified liquid and fluorine-containing slag;
E. and (3) regenerating a fluorine removal agent: and D, adding a sodium hydroxide solution into the fluorine-containing slag obtained in the step D according to a certain solid-to-liquid ratio, reacting for 1.0-2.0 h at the temperature of 85-95 ℃, and after the reaction is completed, carrying out filter pressing, washing and drying to obtain the regenerated fluorine removal agent.
2. The method for deeply removing fluorine from LiCl solution recovered from waste batteries according to claim 1, characterized in that: the defluorinating agent is a composite material prepared from alumina, porous carbon and a small amount of rare earth elements.
3. The method for deeply removing fluorine from LiCl solution recovered from waste batteries according to claim 1, characterized in that: and the addition amount of the fluorine removal agent in the step A is 10-40 times of the fluorine content in the LiCl solution.
4. The method for deeply removing fluorine from LiCl solution recovered from waste batteries according to claim 1, characterized in that: the inorganic acid in the step B is one or a composition of more than one of hydrochloric acid, sulfuric acid and nitric acid, and the solid-liquid ratio is 1: 2-5.
5. The method for deeply removing fluorine from LiCl solution recovered from waste batteries according to claim 1, characterized in that: and C, acid in the step C is one or more of hydrochloric acid, sulfuric acid and nitric acid, and alkali is one or more of sodium hydroxide, ammonia water and sodium carbonate.
6. The method for deeply removing fluorine from LiCl solution recovered from waste batteries according to claim 1, characterized in that: and E, the concentration of the sodium hydroxide solution in the step E is 30-50 g/L, and the solid-to-liquid ratio of the fluorine-containing slag to the sodium hydroxide solution is 1: 3-6.
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Cited By (7)
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CN112142081A (en) * | 2020-09-28 | 2020-12-29 | 江西永兴特钢新能源科技有限公司 | Method for preparing battery-grade lithium carbonate by using lepidolite |
CN112267023A (en) * | 2020-09-25 | 2021-01-26 | 衢州华友钴新材料有限公司 | Two-stage defluorination method for fluorine-containing material |
CN112853120A (en) * | 2020-12-31 | 2021-05-28 | 衢州华友资源再生科技有限公司 | LiHCO recovered and leached from waste lithium battery3Method for deeply removing fluorine from solution |
CN113897490A (en) * | 2021-12-13 | 2022-01-07 | 矿冶科技集团有限公司 | Defluorination method and application of lithium ion battery anode material leaching solution |
WO2023050805A1 (en) * | 2021-09-30 | 2023-04-06 | 广东邦普循环科技有限公司 | Method for removing fluorine in waste lithium batteries |
WO2023050804A1 (en) * | 2021-09-28 | 2023-04-06 | 广东邦普循环科技有限公司 | Method for efficiently removing fluorine from spent lithium battery |
WO2023071353A1 (en) * | 2021-10-26 | 2023-05-04 | 广东邦普循环科技有限公司 | Method for removing fluorine in positive electrode leachate of lithium batteries |
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Cited By (10)
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CN112267023A (en) * | 2020-09-25 | 2021-01-26 | 衢州华友钴新材料有限公司 | Two-stage defluorination method for fluorine-containing material |
CN112267023B (en) * | 2020-09-25 | 2022-07-08 | 衢州华友钴新材料有限公司 | Two-stage defluorination method for fluorine-containing material |
CN112142081A (en) * | 2020-09-28 | 2020-12-29 | 江西永兴特钢新能源科技有限公司 | Method for preparing battery-grade lithium carbonate by using lepidolite |
CN112853120A (en) * | 2020-12-31 | 2021-05-28 | 衢州华友资源再生科技有限公司 | LiHCO recovered and leached from waste lithium battery3Method for deeply removing fluorine from solution |
CN112853120B (en) * | 2020-12-31 | 2023-05-09 | 衢州华友资源再生科技有限公司 | LiHCO is leached in old and useless lithium cell recovery 3 Solution deep defluorination method |
WO2023050804A1 (en) * | 2021-09-28 | 2023-04-06 | 广东邦普循环科技有限公司 | Method for efficiently removing fluorine from spent lithium battery |
WO2023050805A1 (en) * | 2021-09-30 | 2023-04-06 | 广东邦普循环科技有限公司 | Method for removing fluorine in waste lithium batteries |
WO2023071353A1 (en) * | 2021-10-26 | 2023-05-04 | 广东邦普循环科技有限公司 | Method for removing fluorine in positive electrode leachate of lithium batteries |
GB2623240A (en) * | 2021-10-26 | 2024-04-10 | Guangdong Brunp Recycling Technology Co Ltd | Method for removing fluorine in positive electrode leachate of lithium batteries |
CN113897490A (en) * | 2021-12-13 | 2022-01-07 | 矿冶科技集团有限公司 | Defluorination method and application of lithium ion battery anode material leaching solution |
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