CN114959254A - Method for separating and recovering cobalt and lithium in lithium cobaltate - Google Patents
Method for separating and recovering cobalt and lithium in lithium cobaltate Download PDFInfo
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- CN114959254A CN114959254A CN202210454898.4A CN202210454898A CN114959254A CN 114959254 A CN114959254 A CN 114959254A CN 202210454898 A CN202210454898 A CN 202210454898A CN 114959254 A CN114959254 A CN 114959254A
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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
- C22B1/08—Chloridising roasting
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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
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching 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
- 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
- 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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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
- C25C1/10—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of chromium or manganese
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention relates to a method for separating and recovering cobalt and lithium in lithium cobaltate. The invention provides a simple, efficient and clean method for separating and recovering cobalt and lithium from lithium cobaltate, and can solve the problems of complicated steps, low recovery rate and large pollution in the recovery process in the existing technology for recovering lithium cobaltate. The technical scheme of the invention mainly comprises the following steps: 1) converting lithium cobaltate into halide and dissolving the halide into a solution; 2) evaporating the solution to dryness to obtain a solid, dissolving, centrifuging for many times, and taking supernatant; 3) repeating the step 2) for 3-5 times to obtain a clear and transparent solution; 4) separating out cobalt ions in the solution; 5) and separating out lithium ions in the residual solution.
Description
Technical Field
The invention belongs to the technical field of metal cobalt and lithium recovery, and particularly relates to a method for separating and recovering cobalt and lithium in lithium cobaltate.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The problems of resource shortage and environmental pollution become the most serious problems in all countries in the world, and how to effectively solve the problems of resources and environment has important significance to the whole personal society. Lithium ion batteries are widely used in portable electronic products, electric vehicles, and various fields thereof due to their high energy density and long cycle life. In recent years, the capacity of lithium ion batteries has increased rapidly to meet market demand, and it is estimated that by 2020, china will consume 250 billion lithium ion batteries. At such a huge consumption, the recycling work of the lithium ion battery is not negligible because the life of the lithium ion battery is generally only several years.
As is known, lithium cobaltate is the first commercial positive electrode material of lithium ion batteries, and has a leading role in the fields of computers, communications, and the like, so the problem of recycling lithium cobaltate has been studied. Currently, thermochemical and wet chemical processes are common methods for recovering lithium cobaltate. The advantages of wet chemistry are mild conditions and high recovery, but its important step is acid leaching (typically H) 2 SO 4 、HNO 3 ) A large amount of toxic by-products, such as SO, is inevitably produced X 、NO X And the like. While the thermochemical process, although less contaminated, consumes a significant amount of energyThe heat energy and the recovery rate are not satisfactory.
In summary, the existing technologies for recovering lithium cobaltate have the problem of high pollution, and cannot combine reduction of environmental pollution with improvement of recovery rate, so it is important to propose a new scheme for recovering lithium cobaltate.
Disclosure of Invention
Based on the above technical background, the present invention aims to provide a simple and efficient way for recovering lithium cobaltate, which is more environmentally friendly. Meanwhile, the recovery method provided by the invention does not adopt acidolysis, and belongs to a clean recovery mode.
The invention firstly provides a method for separating and recovering cobalt and lithium in lithium cobaltate, which is characterized by comprising the following steps: mixing lithium cobaltate (LiCoO) 2 ) Reacting with chloride to obtain lithium chloride (LiCl) and cobalt chloride (CoCl) 2 ) And then the lithium chloride and the solution of the cobalt chloride are processed for separation to obtain the simple metal substances of the cobalt and the lithium, cobalt compounds or lithium compounds.
The recovery method mainly comprises two steps of preparation and separation of chloride, wherein lithium cobaltate and the chloride can be calcined through a tubular furnace, and the separation of the cobalt compound and the lithium compound in the solution of lithium chloride and cobalt chloride can be further separated through chemical reagent sedimentation or electrochemical precipitation. The recovery process has simple steps and low cost, and can be used for industrially recovering a large amount of lithium cobaltate.
In addition, the recovery method provided by the invention does not generate common toxic byproducts such as SOx, NOx and the like in the recovery process, and the recovery process is cleaner and more environment-friendly.
Finally, the recovery method provided by the invention can obtain different products according to different recovery modes of cobalt compounds and lithium compounds, wherein the different products comprise compounds containing the metal ions in the form of simple metal substances of cobalt and lithium. The skilled person can select the manner of separation and recovery according to the use requirements of the recycled material. The recovery rate of the metal cobalt and lithium in the lithium cobaltate is high, the recovery rate of the cobalt can reach 70-99 percent, and the recovery rate of the lithium can reach 50-99 percent.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an", and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As described in the background art, it is important to provide a simple, efficient and clean method for recovering lithium cobaltate material, and in order to solve the above technical problems, the present invention provides a method for separating and recovering cobalt and lithium in lithium cobaltate.
In a first aspect of the present invention, there is provided a method for separating and recovering cobalt and lithium from lithium cobaltate, the method comprising: mixing lithium cobaltate (LiCoO) 2 ) Reacting with chloride to obtain lithium chloride (LiCl) and cobalt chloride (CoCl) 2 ) And then the lithium chloride and the solution of the cobalt chloride are processed for separation to obtain the simple metal substances of the cobalt and the lithium, cobalt compounds or lithium compounds.
Preferably, one example of the chloride is CCl 4 Said LiCoO 2 And CCl 4 Calcining to obtain lithium chloride and cobalt chloride, wherein the reaction steps are as follows: subjecting LiCoO to condensation 2 Placed in a tube furnace, the CCl 4 And blowing inert gas into the tubular furnace for calcination, and dissolving the calcined product in water to obtain a solution of lithium chloride and cobalt chloride.
Further, the CCl 4 The reagent is maintained at a temperature of 1-50 deg.C before being blown into the tube furnace at a blowing rate of 10-300 sccm.
Further, the inert gas is one or more of helium, neon, argon, krypton, xenon and radon. In a specific example, the inert gas is argon.
Furthermore, the calcining temperature of the tubular furnace is 500-1000 ℃, and the calcining time is 1-50 hours. In a further embodiment, the calcination temperature of the tube furnace is 550 to 800 ℃, and the temperature rise rate of the tube furnace calcination is 2 to 20 ℃/min.
Further, the calcined product is dissolved in water and centrifuged to obtain a supernatant part of the solution, the supernatant part is evaporated to dryness to obtain lithium chloride and cobalt chloride solids, and the evaporated lithium chloride and cobalt chloride solids are dissolved in water or ethanol again to repeat the steps until clear and transparent lithium chloride and cobalt chloride solutions are obtained.
Further, the centrifugation speed is 5000-.
After the solution of lithium chloride and cobalt chloride is obtained according to the method, the solution can be converted into other components with different solubilities for separation, or metal ions in the mixed solution of lithium chloride and cobalt chloride can be separated out in an electrochemical mode.
In one embodiment, lithium hydroxide (LiOH) is added to the mixed solution of lithium chloride and cobalt chloride, the cobalt chloride is separated by converting it to a cobalt hydroxide precipitate, and the separated solution is evaporated to dryness to obtain a mixed powder of lithium chloride and lithium hydroxide.
In another embodiment, the solution of lithium chloride and cobalt chloride is used as a reaction solution for an electrochemical reaction, and metallic cobalt is obtained at a working electrode by electrolysis while the working electrode is held in the reaction solution having a pH of 1 to 6; and after the electrolytic reaction is finished, evaporating the residual solution to dryness to obtain lithium chloride solid powder.
In the above embodiment, the reference electrode of the electrochemical reaction is a saturated calomel electrode, the voltage is 0 to-10 v, the current is 0.0001 to 0.1A, and the time is 10 to 80 hours.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1
A simple, efficient and clean method for separating and recovering cobalt and lithium from lithium cobaltate comprises the following steps:
first, lithium cobaltate is converted into a halide, and it is dissolved into a solution. 0.4078g of LiCoO were weighed out 2 In an alumina crucible, put into a tube furnace, and blown with argon into CCl at 30 ℃ in the tube furnace 4 Reagent, the bubbling rate was 50 sccm. The tube furnace was raised to 750 ℃ at a rate of 10 ℃ per minute and was allowed to cool naturally after 20 hours of holding at this condition. After cooling, the tube wall and the crucible are cleaned by deionized water, and the product is completely transferred to the aqueous solution.
Secondly, the solution is evaporated to dryness to obtain a solid, and then the solid is dissolved, and after multiple times of centrifugal cleaning, a supernatant is taken. Repeating for 3-5 times to obtain clear and transparent solution. And (3) preserving the heat of the suspension obtained after cleaning at 130 ℃ for 18 hours, evaporating the suspension to dryness to obtain a solid, and dissolving the solid, wherein the purpose is to concentrate the solution to facilitate subsequent treatment. Centrifuging the concentrated solution at 13000 rpm for 3 minutes, repeating the centrifuging for three times, and concentrating the supernatant to 100ml as a chloride solution of cobalt ions and lithium ions.
And thirdly, separating out the cobalt ions in the solution. 0.7533g of LiOH was added to the volume-fixed solution, and the reaction was stirred for 3 hours, whereby a large amount of precipitate was formed. Centrifuging for three times at 13000 r/min for 3 min to obtain Co (OH) 2 The solid was washed with deionized water and dried under vacuum at 60 deg.C for 24 hours, and finally weighed to obtain 0.3616g of Co (OH) 2 The recovery rate of cobalt ions was calculated to be 97.3%.
Finally, the lithium ions in the remaining solution are separated. Evaporating the supernatant obtained after centrifugation to dryness to obtain a solid, washing and evaporating to dryness for multiple times, wherein the evaporation temperature is 130 ℃ each time, and the time is 24 hours. A mixed powder of LiCl and LiOH was obtained, and the recovery rate of lithium ions was calculated to be 72.4%.
Example 2
A simple, efficient and clean method for separating and recovering cobalt and lithium from lithium cobaltate comprises the following steps:
firstly, the methodLithium cobaltate is converted to a halide and dissolved as a solution. 0.4580g of LiCoO were weighed out 2 In an alumina crucible, put into a tube furnace, and blown with argon into CCl at 10 ℃ in the tube furnace 4 Reagent, the bubbling rate was 120 sccm. The tube furnace was raised to 700 ℃ at a rate of 10 ℃ per minute and was allowed to cool naturally after being held for 25 hours under these conditions. After cooling, the tube wall and the crucible are cleaned by deionized water, and the product is completely transferred to the aqueous solution.
Secondly, the solution is evaporated to dryness to obtain a solid, and then the solid is dissolved, and after multiple times of centrifugal cleaning, a supernatant is taken. Repeating for 3-5 times to obtain clear and transparent solution. And (3) preserving the heat of the suspension obtained after cleaning at 130 ℃ for 18 hours, evaporating the suspension to dryness to obtain a solid, and dissolving the solid, wherein the purpose is to concentrate the solution to facilitate subsequent treatment. Centrifuging the concentrated solution at 13000 rpm for 3 minutes, repeating the centrifuging for three times, and concentrating the supernatant to 100ml as a chloride solution of cobalt ions and lithium ions.
And thirdly, separating out the cobalt ions in the solution. The solution after constant volume is put into a reactor, a saturated calomel electrode is used as a reference electrode, the voltage is set to be-1.2 v, the current is set to be 0.01A, a KOH solution is used as a counter electrode, the concentration is 1mol/L, and the pH value of a working electrode needs to be kept at 2, so that hydrochloric acid needs to be continuously added to the end of the working electrode in the reaction. 0.2291g of metallic cobalt were obtained at the working electrode after 30 hours of electrolysis, and the recovery of cobalt ions was calculated to be 83.0%.
Finally, the lithium ions in the remaining solution are separated. And (3) evaporating the residual electrolyte to obtain a solid, washing and evaporating to dryness for multiple times, wherein the evaporation temperature is 130 ℃ each time, and the time is 24 hours. A white powder of LiCl was obtained, and the recovery rate of lithium ions was 77.4% by calculation.
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 separating and recovering cobalt and lithium in lithium cobaltate, which is characterized in that: reacting lithium cobaltate with chloride to obtain lithium chloride and cobalt chloride, and then processing the solution of lithium chloride and cobalt chloride to separate to obtain simple metal substances, cobalt compounds or lithium compounds of cobalt and lithium.
2. The method for separating and recovering cobalt and lithium contained in lithium cobaltate according to claim 1, wherein the chloride is CCl 4 Said LiCoO 2 And CCl 4 Calcining to obtain lithium chloride and cobalt chloride, wherein the reaction steps are as follows: subjecting LiCoO to condensation 2 Placing in a tube furnace, the CCl 4 And blowing inert gas into the tubular furnace for calcination, and dissolving the calcined product in water to obtain a solution of lithium chloride and cobalt chloride.
3. The method for separating and recovering cobalt and lithium from lithium cobaltate according to claim 2, wherein CCl is a gas phase separation catalyst 4 The temperature should be maintained at 1-50 ℃ before blowing into the tube furnace, with a blowing rate of 10-300 sccm.
4. The method for separating and recovering cobalt and lithium from lithium cobaltate according to claim 2, wherein the calcination temperature of the tube furnace is 500 ℃ to 1000 ℃ and the calcination time is 1 to 50 hours.
5. The method for separating and recovering cobalt and lithium from lithium cobaltate according to claim 4, wherein the calcining temperature of the tube furnace is 550 to 800 ℃, and the heating rate of the calcining in the tube furnace is 2 to 20 ℃/min.
6. The method for separating and recovering cobalt and lithium in lithium cobaltate according to claim 2, wherein the calcined product is dissolved in water and centrifuged to obtain a supernatant part of the solution, the supernatant part is evaporated to dryness to obtain solid lithium chloride and cobalt chloride, and the evaporated solid lithium chloride and cobalt chloride are dissolved in water or ethanol again to repeat the steps until clear and transparent lithium chloride and cobalt chloride solutions are obtained.
7. The method for separating and recovering cobalt and lithium in lithium cobaltate as claimed in claim 6, wherein the centrifugation speed is 5000-15000 rpm, and the centrifugation time is 1-20 minutes.
8. The method for separating and recovering cobalt and lithium from lithium cobaltate according to claim 2, wherein lithium hydroxide is added to the solution of lithium chloride and cobalt chloride to convert the cobalt chloride into a cobalt hydroxide precipitate for separation, and the separated solution is evaporated to dryness to obtain a mixed powder of lithium chloride and lithium hydroxide.
9. The method for separating and recovering cobalt and lithium from lithium cobaltate according to claim 2, wherein the solution of lithium chloride and cobalt chloride is used as a reaction solution for an electrochemical reaction, and a working electrode is maintained in the reaction solution at a pH of 1 to 6, and metallic cobalt is obtained at the working electrode by electrolysis; and after the electrolytic reaction is finished, evaporating the residual solution to dryness to obtain lithium chloride solid powder.
10. The method for separating and recovering cobalt and lithium in lithium cobaltate according to claim 9, wherein the reference electrode of the electrochemical reaction is a saturated calomel electrode, the voltage is 0 to-10 v, the current is 0.0001 to 0.1A, and the time is 10 to 80 hours.
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