CN110396598A - A kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles - Google Patents

A kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles Download PDF

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Publication number
CN110396598A
CN110396598A CN201910659038.2A CN201910659038A CN110396598A CN 110396598 A CN110396598 A CN 110396598A CN 201910659038 A CN201910659038 A CN 201910659038A CN 110396598 A CN110396598 A CN 110396598A
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lithium
cathode material
manganate cathode
recycles
waste
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卢东亮
齐水冰
蔡东方
李春丽
李可
陈龙
张蕾蕾
江婵
李保庆
王逸飞
陆俞辰
杨帆
罗增勇
毛展冲
毛文涛
黄荣源
陈学威
宋泽洵
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Guangdong Vocational College of Environmental Protection Engineering
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10Obtaining alkali metals
    • C22B26/12Obtaining lithium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/001Dry processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • C22B7/007Wet processes by acid leaching
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/54Reclaiming serviceable parts of waste accumulators
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/84Recycling of batteries or fuel cells

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

Present disclose provides a kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles, steps are as follows: (1) handles lithium manganate anode slice N-Methyl pyrrolidone ultrasonic vibration, precipitating is obtained by filtration;(2) precipitating is calcined, it is cooling, it grinds and is sieved to obtain manganate cathode material for lithium;(3) obtained manganate cathode material for lithium is leached using the mixed solution of sulfuric acid and hydrogen peroxide, leachate is then obtained by filtration;(4) carbon cloth surfaces are activated, the carbon cloth after leachate and activation is then placed in progress incubation water heating reaction in closed container simultaneously;(5) after reaction, carbon cloth is taken out, is washed with deionized, be placed in drying in vacuum oven, obtain the carbon cloth material for having mangaic acid crystalline lithium to surface.The method recycles manganate cathode material for lithium using ultrasonic vibration method, and the recycling of material is carried out using the method for hydro-thermal, and instead of traditional handicraft, reducing environment influences, and reduces recycling energy consumption.

Description

A kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles
Technical field
The disclosure belongs to old and useless battery recovery technology field, and in particular to a kind of waste and old lithium ion battery lithium manganate cathode material The method for expecting to recycle.
Background technique
Ecological Civilization Construction is the theme of current era, and comprehensive utilization of resources is energy-saving and environment-friendly important measures and hand Section.Lithium manganate battery has extensively because of the advantages that its is at low cost, good cycle, high energy density in many fields of production and living Application, and the resource utilization of its old and useless battery to slow down associated materials sustainable growth demand pressure have important reality Meaning.
Recycle waste and old lithium ion battery and eliminate adverse effect, be lithium ion battery sustainable development must be by it Road.Contain a large amount of valuable metal in waste and old lithium ion battery, the recycling of these valuable metals is held to associated materials are slowed down The continuous demand pressure increased has important practical significance.Lithium manganate battery is because its is at low cost, good cycle, energy density are high The advantages that, it is widely used in many fields of production and living, and it is recycled also as research hotspot.Currently, being directed to manganese Sour lithium anode material recycles, and recovery product is usually MnO2、Li2CO3Or manganese alloy, it needs through techniques such as mixed calcinings Manganate cathode material for lithium could be prepared.
Patent CN200910116656.9 discloses one kind and recycles MnO from anode material of wasted lithium manganate battery2Side Method and its application.I.e. in a high pressure reaction kettle, by inorganic Ore Leaching, manganese dioxide salvage material is obtained.Although the patent is returned The MnO of receipts2Good application study is obtained, but acidleach, complex process, equipment investment are carried out using high temperature and pressure in a kettle It is high;And this method does not recycle lithium resource.
Patent CN201010141128.1 discloses a kind of method that valuable metal is recycled from waste lithium manganese oxide battery.I.e. Old and useless battery is crushed, is sieved, Ore Leaching separation and fractional precipitation, finally obtain MnO2And Li2CO3.The patent is although right Manganese and lithium have preferable recycling, but process flow is complicated, and Effect Factors for Sythetic Technology is more, difficulty is big;And the recycling of this method produces Object is difficult to directly apply to lithium ion battery, needs to reprocess to generate manganate cathode material for lithium.
Patent CN201310089509.3 discloses one kind and prepares nickel ion doped by raw material reverse reclamation of waste lithium cell Technique.The method for using electrochemical deposition, the mixed solution of nickel and manganese is placed in electrolytic cell, Ni, Mn oxide is deposited In titanium sheet, Ni, Mn oxide is obtained.Later, nickel ion doped is obtained by the method that lithium source calcining is added.The patent passes through back Receipts provide efficient production lithium ion anode material, but electrodeposition technology is relative complex, and energy consumption is high, difficulty is big, and fail to provide lithium Source effective recycling.
Summary of the invention
Purpose of this disclosure is to provide a kind of methods that waste and old lithium ion battery manganate cathode material for lithium recycles, to reach To low energy consumption, purpose easy to operate.
To achieve the above object, technical solution is as follows:
A kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles, the specific steps of the method are as follows:
(1) lithium manganate anode slice N-Methyl pyrrolidone ultrasonic vibration is handled, precipitating is then obtained by filtration;
(2) precipitating is calcined, is then cooled down, ground and obtain manganate cathode material for lithium after being sieved;
(3) manganate cathode material for lithium obtained after sieving is utilized to the mixed solution leaching of sulfuric acid and hydrogen peroxide, leaching Leachate is obtained by filtration after the completion of out;
(4) carbon cloth surfaces are activated, then by leachate and activation after carbon cloth simultaneously be placed in closed container into The reaction of row incubation water heating;
(5) after reaction, carbon cloth is taken out, is then washed with deionized, be finally placed in drying in vacuum oven, Complete to have to surface the carbon cloth material of mangaic acid crystalline lithium.
The time that ultrasonic vibration is handled in the step (1) is 3-5h.
The temperature calcined in the step (2) is 400-800 DEG C, and the time of calcining is 2-5h;Used in the sieving It is that 200-300 mesh crosses sieve.
The concentration of sulfuric acid is 0.5-2mol/L in the step (3);The mass fraction of preferred hydrogen peroxide is 1-5%;It is excellent The sulfuric acid of choosing and the volume ratio of hydrogen peroxide are (10-15): 1;The solid-to-liquid ratio of the preferred positive electrode and mixed solution is 80- 100g/L。
The temperature leached in the step (3) is 60-90 DEG C, extraction time 4-6h, and the rate of stirring is 80-120r/ min。
The step of carbon cloth surfaces activate in the step (4) are as follows: carbon cloth is used into salt acid soak first, then respectively successively It is cleaned by ultrasonic using acetone, deionized water and dehydrated alcohol, is dried in vacuo later;Then the carbon cloth after drying is placed in dense It flows back in acid solution, uses deionized water and washes of absolute alcohol after reflux again, be finally dried in vacuo again.
The concentration of the hydrochloric acid is 1mol/L, and the time of salt acid soak is 2-3h.
The concentrated acid solution is nitric acid, hydrochloric acid or sulfuric acid, and concentrated acid solution concentration is 10-50mol/L;The preferred reflux Temperature be 30-70 DEG C, return time 1-5h;The preferred vacuum drying temperature is 80-100 DEG C, vacuum drying Time is 1-2h.
The ratio of leachate and carbon cloth additive amount is 10-30mL/cm in the step (4)2;The preferred closed container For water heating kettle;The temperature of the preferred constant temperature is 150-200 DEG C, reaction time 12-18h.
Dry temperature is 60-90 DEG C in the step (5), drying time 12-16h.
The beneficial effect of the disclosure is: providing a kind of side that waste and old lithium ion battery manganate cathode material for lithium recycles Method, the method recycle manganate cathode material for lithium using ultrasonic vibration method, instead of traditional acid leaching process, reduce environment shadow It rings, and recycling energy consumption is reduced, simultaneously instead of traditional high-temperature calcination using the recycling that hydro-thermal method carries out material Material can directly be synthesized on carbon cloth, thus well combine the recycling of material with utilization, it can be effectively to lithium Resource reclaim, and the process flow of the method is easy to operate.
Specific embodiment
Following steps are only to illustrate the technical solution of the disclosure, rather than its limitations;Although referring to These steps The disclosure is described in detail, but those skilled in the art should understand that: it still can be to aforementioned each step Technical solution documented by rapid is modified, or equivalent substitution of some or all of the technical features;And these It modifies or replaces, the range of each step technique scheme of the disclosure that it does not separate the essence of the corresponding technical solution.
Embodiment 1
A kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles, specific steps are as follows:
(1) waste lithium manganese oxide battery remaining capacity is discharged, disassembles battery, take out positive plate, other parts are divided by type Class recycling, positive plate is immersed in N-Methyl pyrrolidone (NMP), using ultrasonic vibration 3h;It is obtained by filtration later with viscous The precipitating of property;
(2) drying will be precipitated, be placed in crucible, 3h is calcined under the conditions of 500 DEG C, natural cooling passes through 200 after grinding Mesh screen is screened, and manganate cathode material for lithium is obtained;
(3) configuration concentration is 0.5mol/L sulfuric acid solution, mass fraction is 1% hydrogen peroxide solution, according to sulfuric acid and dioxygen The volume ratio of water addition is that 10:1 prepares leaching agent, measures 100mL later and is added in flask, then weighs 8g manganese obtained above Sour lithium anode material, which is added in flask, is stirred leaching, and extraction time 4h, extraction temperature is 60 DEG C, stirring rate 80r/ Leachate is obtained by filtration in min after the completion of leaching;
(4) the salt acid soak carbon cloth 2h of 1mol/L is used, it is then clear with acetone, deionized water and dehydrated alcohol ultrasound respectively Wash, be dried in vacuo later, then the carbon cloth after drying is placed in 10mol/L nitric acid, 40 DEG C of reflux 4h, spend later from Sub- water and washes of absolute alcohol, then carry out being dried in vacuo again it is spare, wherein vacuum drying temperature be 80 DEG C, it is vacuum drying Time is 2h;
(5) leachate obtained above is transferred in water heating kettle, the carbon cloth handled well is cut into small pieces and is also placed in hydro-thermal In kettle, then water heating kettle is placed in baking oven, 150 DEG C of reaction 15h of constant temperature, wherein the ratio of leachate and carbon cloth additive amount is 10mL/cm2
(6) after reaction, carbon cloth is taken out, is cleaned 3 times with deionized water, is placed in 60 DEG C of vacuum oven dry 12h may be directly applied to the preparation of lithium ion battery to get the carbon cloth material for having mangaic acid crystalline lithium to surface.
Embodiment 2
A kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles, specific steps are as follows:
(1) waste lithium manganese oxide battery remaining capacity is discharged, disassembles battery, take out positive plate, other parts are divided by type Class recycling, positive plate is immersed in N-Methyl pyrrolidone (NMP), using ultrasonic vibration 5h;It is obtained by filtration later with viscous The precipitating of property;
(2) drying will be precipitated, be placed in crucible, 4h is calcined under the conditions of 500 DEG C, natural cooling passes through 300 after grinding Mesh screen is screened, and manganate cathode material for lithium is obtained;
(3) configuration concentration is 1.5mol/L sulfuric acid solution, mass fraction is 4% hydrogen peroxide solution, according to sulfuric acid and dioxygen The volume ratio of water addition is that 15:1 prepares leaching agent, measures 100mL later and is added in flask, then to weigh 10g obtained above Manganate cathode material for lithium, which is added in flask, is stirred leaching, and extraction time 6h, extraction temperature is 80 DEG C, and stirring rate is Leachate is obtained by filtration in 100r/min after the completion of leaching;
(4) the salt acid soak carbon cloth 3h of 1mol/L is used, it is then clear with acetone, deionized water and dehydrated alcohol ultrasound respectively Wash, be dried in vacuo later, then the carbon cloth after drying is placed in 25mol/L hydrochloric acid, 50 DEG C of reflux 3h, spend later from Sub- water and washes of absolute alcohol, be then dried in vacuo it is spare, wherein vacuum drying temperature be 100 DEG C, the vacuum drying time For 1h;
(5) leachate obtained above is transferred in water heating kettle, the carbon cloth handled well is cut into small pieces and is also placed in hydro-thermal In kettle, then water heating kettle is placed in baking oven, 180 DEG C of reaction 12h of constant temperature, wherein the ratio of leachate and carbon cloth additive amount is 30mL/cm2
(6) after reaction, carbon cloth is taken out, is cleaned 5 times with deionized water, is placed in 80 DEG C of vacuum oven dry 10h may be directly applied to the preparation of lithium ion battery to get the carbon cloth material for having mangaic acid crystalline lithium to surface.

Claims (10)

1. a kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles, which is characterized in that the tool of the method Body step are as follows:
(1) lithium manganate anode slice N-Methyl pyrrolidone ultrasonic vibration is handled, precipitating is then obtained by filtration;
(2) precipitating is calcined, is then cooled down, ground and obtain manganate cathode material for lithium after being sieved;
(3) the mixed solution leaching that the manganate cathode material for lithium obtained after sieving is utilized to sulfuric acid and hydrogen peroxide, has been leached Leachate is obtained by filtration after;
(4) carbon cloth surfaces are activated, the carbon cloth after leachate and activation is placed in closed container simultaneously then and carries out perseverance Warm water thermal response;
(5) after reaction, carbon cloth is taken out, is then washed with deionized, be finally placed in vacuum oven dry, completion Obtain the carbon cloth material for having mangaic acid crystalline lithium to surface.
2. special according to the method that waste and old lithium ion battery manganate cathode material for lithium described in claims 1 recycles Sign is that the time that ultrasonic vibration is handled in the step (1) is 3-5h.
3. special according to the method that waste and old lithium ion battery manganate cathode material for lithium described in claims 1 recycles Sign is that the temperature calcined in the step (2) is 400-800 DEG C, and the time of calcining is 2-5h;It is used in the sieving 200-300 mesh crosses sieve.
4. special according to the method that waste and old lithium ion battery manganate cathode material for lithium described in claims 1 recycles Sign is that the concentration of sulfuric acid is 0.5-2mol/L in the step (3);The mass fraction of preferred hydrogen peroxide is 1-5%;It is preferred that Sulfuric acid and hydrogen peroxide volume ratio be (10-15): 1;The solid-to-liquid ratio of the preferred positive electrode and mixed solution is 80- 100g/L。
5. special according to the method that waste and old lithium ion battery manganate cathode material for lithium described in claims 1 recycles Sign is that the temperature leached in the step (3) is 60-90 DEG C, extraction time 4-6h, and the rate of stirring is 80-120r/ min。
6. special according to the method that waste and old lithium ion battery manganate cathode material for lithium described in claims 1 recycles Sign is, in the step (4) the step of carbon cloth surfaces activation are as follows: carbon cloth is used salt acid soak first, then respectively successively It is cleaned by ultrasonic using acetone, deionized water and dehydrated alcohol, is dried in vacuo later;Then the carbon cloth after drying is placed in dense It flows back in acid solution, uses deionized water and washes of absolute alcohol after reflux again, be finally dried in vacuo again.
7. special according to the method that waste and old lithium ion battery manganate cathode material for lithium described in claims 6 recycles Sign is that the concentration of the hydrochloric acid is 1mol/L, and the time of salt acid soak is 2-3h;Preferably the vacuum drying temperature is 80-100 DEG C, the vacuum drying time is 1-2h.
8. special according to the method that waste and old lithium ion battery manganate cathode material for lithium described in claims 6 recycles Sign is that the concentrated acid solution is nitric acid, hydrochloric acid or sulfuric acid, and concentrated acid solution concentration is 10-50mol/L;The preferred reflux Temperature be 30-70 DEG C, return time 1-5h.
9. special according to the method that waste and old lithium ion battery manganate cathode material for lithium described in claims 1 recycles Sign is that the ratio of leachate and carbon cloth additive amount is 10-30mL/cm in the step (4)2;The preferred closed container For water heating kettle;The temperature of the preferred constant temperature is 150-200 DEG C, reaction time 12-18h.
10. special according to the method that waste and old lithium ion battery manganate cathode material for lithium described in claims 1 recycles Sign is that dry temperature is 60-90 DEG C in the step (5), drying time 12-16h.
CN201910659038.2A 2019-07-22 2019-07-22 A kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles Pending CN110396598A (en)

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CN111593201A (en) * 2020-05-11 2020-08-28 陕西科技大学 Method for short-distance separation of manganese and lithium in waste lithium manganate battery and preparation of functional adsorption material
CN112429799A (en) * 2020-09-25 2021-03-02 先导薄膜材料(广东)有限公司 Method for removing cadmium in wastewater
CN114566730A (en) * 2022-03-05 2022-05-31 贺州学院 Method for preparing positive electrode composite material by using waste lithium manganate battery
CN114583196A (en) * 2022-03-17 2022-06-03 楚能新能源股份有限公司 Method for recycling waste lithium-manganese dioxide battery
CN116199263A (en) * 2021-12-01 2023-06-02 中国科学院福建物质结构研究所 Method for preparing functional adsorption material beta-MnO 2 from waste battery

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CN109449522A (en) * 2018-10-30 2019-03-08 东北师范大学 A kind of metal ion recycling in refuse battery and the method applied to solid lithium battery
CN109659497A (en) * 2019-01-30 2019-04-19 青岛大学 A kind of preparation method of the flexible metatitanic acid lithium electrode based on carbon cloth

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CN109148994A (en) * 2017-06-28 2019-01-04 荆门市格林美新材料有限公司 A kind of recovery method of waste lithium ion cell anode material
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111593201A (en) * 2020-05-11 2020-08-28 陕西科技大学 Method for short-distance separation of manganese and lithium in waste lithium manganate battery and preparation of functional adsorption material
CN112429799A (en) * 2020-09-25 2021-03-02 先导薄膜材料(广东)有限公司 Method for removing cadmium in wastewater
CN116199263A (en) * 2021-12-01 2023-06-02 中国科学院福建物质结构研究所 Method for preparing functional adsorption material beta-MnO 2 from waste battery
CN114566730A (en) * 2022-03-05 2022-05-31 贺州学院 Method for preparing positive electrode composite material by using waste lithium manganate battery
CN114566730B (en) * 2022-03-05 2024-02-06 贺州学院 Method for preparing positive electrode composite material by using waste lithium manganate battery
CN114583196A (en) * 2022-03-17 2022-06-03 楚能新能源股份有限公司 Method for recycling waste lithium-manganese dioxide battery
CN114583196B (en) * 2022-03-17 2023-01-24 楚能新能源股份有限公司 Method for recycling waste lithium-manganese dioxide battery

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Application publication date: 20191101