CN108155434B - Method for recovering lithium from waste electrolyte of lithium ion battery - Google Patents

Method for recovering lithium from waste electrolyte of lithium ion battery Download PDF

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CN108155434B
CN108155434B CN201711423808.0A CN201711423808A CN108155434B CN 108155434 B CN108155434 B CN 108155434B CN 201711423808 A CN201711423808 A CN 201711423808A CN 108155434 B CN108155434 B CN 108155434B
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lithium
chloride
reaction
solution
ion battery
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CN108155434A (en
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陈亚
曹利涛
关杰豪
甘辉
陈白珍
石西昌
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Central South University
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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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/84—Recycling of batteries or fuel cells

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  • Manufacturing & Machinery (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Secondary Cells (AREA)

Abstract

The invention relates to a method for recovering lithium from waste electrolyte of a lithium ion battery, belonging to the technical field of resource recycling. The invention aims to provide a method for recovering lithium from waste electrolyte of a lithium ion battery, which is characterized in that the waste electrolyte is mixed with halide solution containing large cation radiusReaction, PF in electrolyte6 ‑And (3) integrally separating, and carrying out deep purification and lithium precipitation treatment on the lithium-containing solution obtained after separation to obtain lithium carbonate, thereby achieving the purpose of cleanly and efficiently utilizing the waste electrolyte of the lithium ion battery.

Description

Method for recovering lithium from waste electrolyte of lithium ion battery
Technical Field
The invention relates to a method for recovering lithium from waste electrolyte of a lithium ion battery; belongs to the technical field of resource recycling.
Technical Field
The lithium ion battery has the advantages of high specific energy, long cycle life, no memory effect and the like, so that the lithium ion battery is widely applied to the mobile electronic communication market and becomes one of the preferred power batteries of the pure electric vehicle at present. With the rapid development of the lithium ion battery industry, the demand for relevant battery materials continues to increase. In the preparation of electrode materials for lithium ion batteries, either early LiCoO2Is also LiMn developed gradually in the later period2O4、LiFePO4Or ternary materials and the like, without exception, high-purity lithium salt is required to be used as a raw material, and lithium carbonate or lithium hydroxide is mainly used. Because of the influence of reaction activity and the like, lithium phosphate is rarely directly used for producing the lithium ion battery anode material. In addition, high-purity lithium salt is also needed as a raw material when preparing lithium ion battery electrolyte, lithium metatitanate and other cathode materials.
In order to meet the demand of the vigorous development of the lithium ion battery industry, a great deal of research work is carried out at home and abroad around the technology of extracting lithium carbonate or lithium hydroxide from spodumene, lepidolite and salt lake brine, and industrial production is carried out. Meanwhile, in order to realize efficient recycling of limited resources, attention is paid to technical researches on valuable metal recovery from waste lithium ion batteries at home and abroad at present, but a great deal of research and production technical work mainly focuses on recovering metals such as Co, Ni and the like in electrode materials, technical researches on efficient lithium recovery are rarely reported, and especially, researches on lithium recovery from waste electrolyte are rarely carried out. When the electrode material is recovered, the waste electrolyte and the pole piece cleaning water are mainly mixed, a large amount of waste electrolyte enters the cleaning water to be hydrolyzed, lithium in the waste electrolyte is converted into lithium fluoride and lithium phosphate, and a large amount of hydrogen fluoride gas is released at the same time. On one hand, the problem that the hydrogen fluoride gas pollutes the environment and harms the health of field workers is caused, and on the other hand, the obtained lithium salt can be used for synthesizing the lithium ion battery material again only after being subjected to complex subsequent conversion. Therefore, there is a need to develop a technology for efficiently and cleanly recovering lithium from the electrolyte of the waste lithium ion battery.
Disclosure of Invention
The invention aims to provide a method for recovering lithium from waste electrolyte of a lithium ion battery, which is characterized in that the waste electrolyte is mixed with chloride solution containing large cation radius for reaction, so that cations with large ionic radius are mixed with PF6 -The ions are converted into sparingly soluble or poorly soluble salts by reaction, thereby reacting the lithium ions with PF6 -And (3) separating ions, and performing deep purification and lithium precipitation treatment on the lithium-containing solution obtained after separation to obtain lithium carbonate, so as to achieve the purpose of cleanly and efficiently utilizing the waste lithium ion battery electrolyte.
The invention relates to a method for recovering lithium from waste electrolyte of a lithium ion battery, which comprises the following steps:
step one
Preparing a chloride aqueous solution containing large cation radius, slowly adding waste electrolyte into the chloride aqueous solution to perform stirring reaction, filtering after the reaction is completed, and standing the filtrate to obtain a lithium-containing solution; the radius of the large cation is more than or equal to 0.133 nm;
step two
Adding soluble alkali into the lithium-containing solution, stirring for reaction, and filtering after the reaction is completed to obtain a purified solution;
step three
And adding soluble carbonate into the purified solution, heating for reaction, immediately filtering after the reaction is completed, and washing and drying a filter cake to obtain the lithium carbonate.
The invention relates to a method for recovering lithium from waste electrolyte of a lithium ion battery, in the step one, the chloride with large cation radius comprises at least one of potassium chloride, ammonium chloride, rubidium chloride, cesium chloride, tetraethylammonium chloride, tetrapropylammonium chloride, tetrabutylammonium chloride, nickel hexammine dichloride, potassium bromide, ammonium bromide, rubidium bromide, cesium bromide, tetraethylammonium bromide, tetrapropylammonium bromide, tetrabutylammonium bromide and nickel hexammine dibromide, and in order to facilitate operation and recovery treatment of mother liquor after lithium precipitation, at least one of the chlorides is preferably selected; more preferably at least one of potassium chloride, ammonium chloride, tetraethylammonium chloride, tetrabutylammonium chloride and nickel hexammine dichloride. In order to improve the recovery rate of lithium and the purity of products; preferably, the chloride with large cation radius consists of potassium chloride and tetraethylammonium chloride. As a further preferred scheme, the chloride with large cation radius consists of potassium chloride and tetraethylammonium chloride according to the molar ratio of 1: 2-5. Still more preferably 1: 3-5. By adopting the scheme, unexpected effects are obtained on the yield of lithium.
In order to improve the recovery rate of lithium and the purity of products; preferably, the chloride with large cation radius consists of potassium chloride and nickel hexammine dichloride. As a further preferred scheme, the chloride with large cation radius consists of potassium chloride and nickel hexammine dichloride according to the molar ratio of 1: 2-5. Still more preferably 1: 3-4. By adopting the scheme, unexpected effects are obtained on the yield of lithium.
In order to improve the recovery rate of lithium and the purity of products; preferably, the chloride with large cation radius consists of potassium chloride and tetrabutylammonium chloride. As a further preferable scheme, the chloride with large cation radius consists of potassium chloride and tetrabutylammonium chloride according to the molar ratio of 1: 1.5-5. Still more preferably 1: 1.5-3. By adopting the scheme, unexpected effects are obtained on the yield of lithium.
The invention relates to a method for recovering lithium from waste electrolyte of a lithium ion battery, wherein the concentration of chloride with large ionic radius in the step I is 0.5-2 mol/L.
The invention relates to a method for recovering lithium from waste electrolyte of a lithium ion battery, which comprises the following steps that in the first step, the reaction temperature is 20-60 ℃, the reaction time is 30-180 minutes, preferably 20-30 ℃, and the reaction time is 90-180 minutes.
The invention relates to a method for recovering lithium from waste electrolyte of a lithium ion battery, wherein in the second step, soluble alkali is at least one of sodium hydroxide, ammonia water and potassium hydroxide, and potassium hydroxide is preferred.
The invention relates to a method for recovering lithium from waste electrolyte of a lithium ion battery, which comprises the step two of adding soluble alkali, adjusting the pH value of the solution to 10-13, preferably 12-13, and reacting. Preferably, the pH value of the system is controlled to be 10-13 in the reaction process.
The invention relates to a method for recovering lithium from waste electrolyte of a lithium ion battery, wherein in the second step, the reaction temperature is 25-60 ℃, and the reaction time is 30-60 minutes. Preferably, the reaction temperature in the second step is 40-60 ℃ and the reaction time is 30-60 minutes.
The invention relates to a method for recovering lithium from waste electrolyte of a lithium ion battery, wherein in the third step, soluble carbonate is at least one of potassium carbonate, ammonium carbonate or sodium carbonate.
The method for recovering lithium from the waste electrolyte of the lithium ion battery comprises the third step of heating and reacting at the temperature of 60-90 ℃ for 30-120 minutes, preferably at the temperature of 70-90 ℃, for 60-90 minutes
Principles and advantages
The invention mixes and reacts the waste electrolyte of the lithium ion battery with a chloride solution containing large cation radius, on one hand, halogen anions in the solution prevent PF in the electrolyte6 -Ion hydrolysis to make it stable in aqueous solution and promote cation with large ionic radius and PF6 -Ion reaction to produce slightly soluble or insoluble salt, and using original PF as phosphorus and fluorine element in the solution6 -The form is recovered integrally, thereby lithium ions are mixed with PF6 -Ion separation, namely deeply purifying the lithium-containing solution obtained after separation and depositing lithium to obtain lithium carbonate, thereby achieving the aim of cleanly and efficiently utilizing the electricity of the waste lithium ion batteryThe purpose of the liquid is to decompose the liquid.
Compared with the prior art, the technical thought and the technical principle of the invention have obvious characteristics and technical advantages, which are specifically shown in the following steps:
(1) the invention provides a method for preparing a halogen salt with a large cation radius and LiPF in electrolyte6Reaction, stabilization of PF by halogen ions6 -To prevent hydrolysis thereof by cations having a large ionic radius with PF6 -The ion reaction generates slightly soluble or insoluble salt, thereby avoiding generating toxic gases such as HF and the like to harm the environment and the health of workers;
(2) removal of PF from spent lithium ion battery electrolytes by the process of the present invention6 -The obtained lithium halide solution can be used for preparing lithium carbonate after deep purification, a large amount of lithium phosphate or lithium fluoride which is difficult to treat is not generated in the recovery process, and the recovery process flow is short;
(3) the method of the invention can recover lithium from the waste electrolyte of the lithium ion battery without the procedures of roasting or burning and the like, and has simple equipment requirement and low energy consumption.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
The waste electrolyte of the lithium ion battery comprises waste electrolyte generated in the recovery process of the waste lithium ion battery, waste electrolyte generated in processes such as liquid injection and the like in the production process of the lithium ion battery or unqualified electrolyte generated in the production process of the lithium ion battery.
Unless otherwise specified, each of the reagents used in the present invention is a commercially available product or a product obtainable by a known method.
The specific embodiment of the invention is as follows:
example one
The preparation contains 0.1mol/L KCl and 0.4mol/L C8H20And adding 310 ml of ClN mixed solution into 150 ml of waste lithium ion electrolyte at room temperature while stirring, and continuing to stir for reaction for 180 minutes after the addition is finished. After the stirring reaction is finished, the precipitate and the lithium-containing solution are separated by filtration. Adding KOH into the separated lithium-containing solution to adjust the pH value to 13, heating and reacting for 60 minutes at 60 ℃, and filtering after the solution is cooled to obtain purified solution. Heating the purified solution to 90 ℃, adding 30mL of 300g/L sodium carbonate solution while stirring, continuing to react for 120 minutes after the addition is finished, immediately filtering after the reaction is finished, washing the obtained lithium carbonate with hot water, drying at 100 ℃ for 12 hours, and weighing and calculating to obtain the lithium recovery rate of 82.1%. The purity of the lithium carbonate obtained was 98.8%.
Example two
The operation process is the same as that of the first example, except that KCl and NH are prepared4205 ml of mixed solution with Cl concentration of 1mol/L, adding 150 ml of waste lithium ion electrolyte at 60 ℃ while stirring, and continuing to stir for reaction for 60 minutes after the addition is finished. After the stirring reaction is finished, the precipitate and the lithium-containing solution are separated by filtration. Adding KOH into the separated lithium-containing solution to adjust the pH value to 10, heating the solution at 40 ℃ for reaction for 30 minutes, and filtering the solution after the solution is cooled to obtain purified solution. Heating the purified solution to 70 ℃, adding 30mL of 300g/L sodium carbonate solution while stirring, continuing to react for 30 minutes after the addition is finished, immediately filtering after the reaction is finished, washing the obtained lithium carbonate with hot water, drying at 100 ℃ for 12 hours, and weighing and calculating to obtain the lithium recovery rate of 74.4%. The purity of the lithium carbonate obtained was 98.6%.
EXAMPLE III
The operation process is the same as that of example one, except that 0.5mol/L KCl and 0.5mol/L Ni (NH) are prepared3)6Cl2155 ml of the mixed solution is added with 150 ml of the lithium ion waste electrolyte under stirring at the temperature of 30 ℃, and the stirring reaction is continued for 90 minutes after the addition is finished. After the stirring reaction is finished, the precipitate and the lithium-containing solution are separated by filtration. Adding KOH into the separated lithium-containing solution to adjust the pH value to 12, heating and reacting for 60 minutes at 60 ℃, and filtering after the solution is cooled to obtain the purified solution. Heating the purified solution to 90 ℃, adding 30mL of 300g/L sodium carbonate solution while stirring, and continuing to add after the addition is finishedThe reaction was carried out for 60 minutes, immediately after completion of the reaction, filtration was carried out, and the obtained lithium carbonate was washed with hot water and then dried at 100 ℃ for 12 hours, and the recovery rate of lithium was weighed and calculated to be 85.2%. The purity of the lithium carbonate obtained was 98.1%.
Example four
The procedure is as in example one except that the formulation contains 0.2mol/L KCl and 0.4mol/L C16H36260 ml of mixed solution of ClN, adding 150 ml of waste lithium ion electrolyte at 30 ℃ while stirring, and continuing to stir for reaction for 120 minutes after the addition is finished. After the stirring reaction is finished, the precipitate and the lithium-containing solution are separated by filtration. Adding KOH into the separated lithium-containing solution to adjust the pH value to 12, heating and reacting for 40 minutes at 60 ℃, and filtering after the solution is cooled to obtain purified solution. Heating the purified solution to 90 ℃, adding 30mL of 300g/L sodium carbonate solution while stirring, continuing to react for 90 minutes after the addition is finished, immediately filtering after the reaction is finished, washing the obtained lithium carbonate with hot water, drying at 100 ℃ for 12 hours, and weighing and calculating to obtain the lithium recovery rate of 86.7%. The purity of the lithium carbonate obtained was 98.4%.
EXAMPLE five
The operation process is the same as that of example one, except that the preparation solution contains 0.5mol/L NH4Cl and 0.1mol/L C12H28300 ml of ClN mixed solution is added with 150 ml of waste lithium ion electrolyte under stirring at 60 ℃, and stirring reaction is continued for 120 minutes after the addition is finished. After the stirring reaction is finished, the precipitate and the lithium-containing solution are separated by filtration. Adding KOH into the separated lithium-containing solution to adjust the pH value to 11, heating and reacting for 40 minutes at 60 ℃, and filtering after the solution is cooled to obtain the purified solution. Heating the purified solution to 90 ℃, adding 30mL of 300g/L sodium carbonate solution while stirring, continuing to react for 90 minutes after the addition is finished, immediately filtering after the reaction is finished, washing the obtained lithium carbonate with hot water, drying at 100 ℃ for 12 hours, and weighing and calculating the recovery rate of lithium to be 76.8%. The purity of the lithium carbonate obtained was 98.4%.
EXAMPLE six
The operation process is the same as the first embodiment, only 300 ml of 0.5mol/L KCl solution is prepared, 150 ml of the waste lithium ion electrolyte is added at 60 ℃ while stirring, and the stirring reaction is continued for 120 minutes after the addition is finished. After the stirring reaction is finished, the precipitate and the lithium-containing solution are separated by filtration. Adding KOH into the separated lithium-containing solution to adjust the pH value to 11, heating and reacting for 40 minutes at 60 ℃, and filtering after the solution is cooled to obtain the purified solution. Heating the purified solution to 90 ℃, adding 30mL of 300g/L sodium carbonate solution while stirring, continuing to react for 90 minutes after the addition is finished, immediately filtering after the reaction is finished, washing the obtained lithium carbonate with hot water, drying at 100 ℃ for 12 hours, and weighing and calculating the recovery rate of lithium to be 69.8%. The purity of the lithium carbonate obtained was 98.6%.
Comparative example 1
The operation process is the same as the first embodiment, only 300 ml of NaCl solution containing 0.5mol/L is prepared, 150 ml of lithium ion waste electrolyte is added under stirring at 60 ℃, and stirring reaction is continued for 180 minutes after the addition is finished. After the stirring reaction is finished, the precipitate and the lithium-containing solution are separated by filtration. Adding NaOH into the separated lithium-containing solution to adjust the pH value to 13, heating and reacting at 60 ℃ for 40 minutes, and filtering after the solution is cooled to obtain purified solution. Heating the purified solution to 90 ℃, adding 30mL of 300g/L sodium carbonate solution while stirring, continuing to react for 90 minutes after the addition is finished, immediately filtering after the reaction is finished, washing the obtained lithium carbonate with hot water, drying at 100 ℃ for 12 hours, and weighing and calculating the recovery rate of the lithium to be 37.8%. The purity of the lithium carbonate obtained was 97.4%.

Claims (9)

1. A method for recovering lithium from waste electrolyte of a lithium ion battery is characterized by comprising the following steps:
step one
Preparing a chloride aqueous solution containing large cation radius, slowly adding waste electrolyte into the chloride aqueous solution to carry out stirring reaction, and filtering after the reaction is completed to obtain a lithium-containing solution; the radius of the large cation is more than or equal to 0.133 nm;
step two
Adding soluble alkali into the lithium-containing solution, stirring for reaction, and filtering after the reaction is completed to obtain a purified solution; in the second step, the soluble alkali is at least one of sodium hydroxide, ammonia water and potassium hydroxide;
step three
And adding soluble carbonate into the purified solution, heating for reaction, immediately filtering after the reaction is completed, and washing and drying a filter cake to obtain the lithium carbonate.
2. The method of claim 1, wherein the method comprises the steps of: in the step one, the chloride with large cation radius comprises at least one of potassium chloride, ammonium chloride, rubidium chloride, cesium chloride, tetraethylammonium chloride, tetrapropylammonium chloride, tetrabutylammonium chloride and nickel hexammoniadichloride.
3. The method of claim 2, wherein the lithium is recovered from the spent electrolyte of the lithium ion battery by: the chloride with large cation radius is at least one selected from potassium chloride, ammonium chloride, tetraethylammonium chloride, tetrabutylammonium chloride and nickel hexammine dichloride.
4. The method of claim 1, wherein the method comprises the steps of: in the chloride aqueous solution containing large cation radius in the step one, the concentration of the chloride containing large cation radius is 0.5-2 mol/L.
5. The method of claim 1, wherein the method comprises the steps of: in the first step, the reaction temperature is 20-60 ℃, and the reaction time is 30-180 minutes; and filtering after the reaction is completed to obtain the lithium-containing solution.
6. The method of claim 1, wherein the method comprises the steps of: and adding soluble alkali in the second step, adjusting the pH value of the solution to 10-13, and reacting.
7. The method of claim 1, wherein the method comprises the steps of: in the second step, the reaction temperature is 25-60 ℃, and the reaction time is 30-60 minutes.
8. The method of claim 1, wherein the method comprises the steps of: in the third step, the soluble carbonate is at least one of potassium carbonate, ammonium carbonate or sodium carbonate.
9. The method of claim 1, wherein the method comprises the steps of: the heating reaction temperature in the third step is 60-90 ℃, and the reaction time is 30-120 minutes.
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CN109119713B (en) * 2018-08-24 2020-07-31 广西师范大学 Method for recovering positive active material in lithium ion battery
CN109193062B (en) * 2018-10-29 2021-04-02 山西根复科技有限公司 Waste battery electrolyte recycling method
CN109585963B (en) * 2018-11-30 2021-12-21 先进储能材料国家工程研究中心有限责任公司 Method for recycling and treating waste lithium ion battery electrolyte
CN110034351A (en) * 2019-04-29 2019-07-19 浙江华友钴业股份有限公司 A kind of innoxious minimizing technology of used Li ion cell electrolyte
CN112259819B (en) * 2020-10-20 2022-02-25 清华大学深圳国际研究生院 Disassembling and recycling method of lithium ion battery
CN114759286A (en) * 2022-05-30 2022-07-15 清华大学深圳国际研究生院 Method for recovering waste electrolyte of lithium ion battery
CN115259184B (en) * 2022-09-29 2022-12-16 广州天赐高新材料股份有限公司 Method for recovering high-purity hexafluorophosphate and lithium carbonate from waste lithium ion battery electrolyte

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CN102751549B (en) * 2012-07-04 2014-12-24 中国科学院过程工程研究所 Full-component resource reclamation method for waste positive electrode materials of lithium ion batteries
CN103114211B (en) * 2013-02-19 2014-06-11 宁波莲华环保科技股份有限公司 Method for extracting lithium from primary lithium extraction solution of lithium ore
CN106745099A (en) * 2016-12-05 2017-05-31 天津二八科技股份有限公司 A kind of method that utilization lithium phosphate prepares lithium carbonate

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