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WO2018028167A1 - Procédé de récupération de pièce d'électrode négative pour batterie au lithium-ion - Google Patents

Procédé de récupération de pièce d'électrode négative pour batterie au lithium-ion Download PDF

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Publication number
WO2018028167A1
WO2018028167A1 PCT/CN2017/074130 CN2017074130W WO2018028167A1 WO 2018028167 A1 WO2018028167 A1 WO 2018028167A1 CN 2017074130 W CN2017074130 W CN 2017074130W WO 2018028167 A1 WO2018028167 A1 WO 2018028167A1
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WO
WIPO (PCT)
Prior art keywords
lithium
negative electrode
metal
battery
electrode sheet
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2017/074130
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English (en)
Chinese (zh)
Inventor
曹乃珍
徐川
陈欣
高洁
钟兆资
李仕红
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tianqi Lithium Corp
Original Assignee
Tianqi Lithium Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tianqi Lithium Corp filed Critical Tianqi Lithium Corp
Publication of WO2018028167A1 publication Critical patent/WO2018028167A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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

Definitions

  • the invention relates to a method for recovering a negative electrode sheet of a metal lithium battery, and belongs to the technical field of batteries.
  • the composition of the lithium metal negative electrode sheet that a small amount of copper and a battery separator (generally PP or PE film) are mainly contained in the metal lithium or lithium alloy. If you can remove the copper and separator, you can regain high-purity, expensive battery-grade lithium metal or lithium alloy.
  • a battery separator generally PP or PE film
  • the first type is the recovery of metallic lithium for metallic lithium (such as lithium oxide, lithium nitride, etc.) having a surface which does not require a product, for example, metal lithium having a desired surface on the surface as mentioned in ZL201110296543.9
  • metallic lithium for metallic lithium (such as lithium oxide, lithium nitride, etc.) having a surface which does not require a product, for example, metal lithium having a desired surface on the surface as mentioned in ZL201110296543.9
  • the reaction with nitrogen forms lithium nitride and then reacts with carbon dioxide to form lithium carbonate, and then the formed lithium carbonate is reacted with hydrochloric acid to form lithium chloride, and the metal lithium is melted and electrolytically recovered.
  • This method is mainly for the recovery of surface products, and other large amounts of lithium metal are not recovered.
  • the process route is complicated, and the energy consumption, labor, and equipment cost are relatively high, which is equivalent to the whole process of re-preparing metal lithium, and the degree of application is low.
  • the second method is mainly for recovering metallic lithium from a waste lithium ion secondary battery, for example, as mentioned in ZL201010199758.4, all the reversible lithium ions on the negative electrode sheets of the used battery are transferred to the positive electrode, and formed on the positive electrode sheet.
  • a lithium salt a lithium salt
  • the battery after the discharge treatment is mechanically disassembled and the positive electrode sheet is completely taken out and dried
  • the lithium metal or lithium-clad material is used as a negative electrode sheet to match each positive electrode treated by the previous step.
  • the positive and negative sheet groups are respectively connected to the positive and negative bus bars of the DC power source, and subjected to externalization treatment to reversible lithium ions from the positive electrode sheets.
  • the invention mainly adopts the method of extracting lithium from the positive and negative electrodes respectively after pretreatment, but the method of subsequently extracting lithium is not described, and the key to extracting metallic lithium is the processing method on the pole piece.
  • the lithium extraction efficiency of the method is low, generally only reaches 70% to 90%, and the requirements for equipment, environment, operation and the like are high, and the recovery cost is also high.
  • the technical problem to be solved by the present invention is to provide a method for recovering a negative electrode sheet of a metal lithium battery, which extracts metal lithium or a lithium alloy from a negative electrode sheet of a metal lithium battery.
  • the method for recovering the negative electrode sheet of the metal lithium battery of the invention comprises the following steps:
  • the metal lithium battery negative electrode sheet is immersed in white oil
  • heating heating the white oil immersed in the negative electrode sheet of the metal lithium battery to 180-220 ° C, and stirring;
  • step b Insulation filtration: the white oil heated in step b is subjected to heat preservation filtration, and the filtrate is taken;
  • Degreasing Vacuum degreasing the solid metal lithium or lithium alloy to obtain a metallic lithium liquid or a lithium alloy liquid;
  • the soaking time is not less than 1 hour, preferably 1 hour.
  • the stirring rate is 100 to 150 rpm; the stirring time is 15 to 30 minutes.
  • the filter is subjected to thermal insulation filtration, and the filter has an accuracy of 15 to 30 ⁇ m, preferably a filter precision of 15 ⁇ m.
  • step d filtration is performed using a filter having an accuracy of 5 to 10 ⁇ m.
  • the vacuum deoiling temperature in the e step is 240 to 260 ° C
  • the degree of vacuum is 0.8 to 1.2 Pa, preferably the vacuum deoiling temperature is 250 ° C, and the degree of vacuum is 1 Pa.
  • the source of the negative electrode sheet of the metal lithium battery is a negative electrode sheet of a metal lithium battery negative electrode scrap, scrap or a metal lithium battery.
  • the metal lithium battery is a metal lithium primary battery, a metal lithium secondary battery, a lithium alloy primary battery, or a lithium alloy secondary battery.
  • the recycled material for the method of the present invention is the recovery of lithium metal or lithium alloy on the negative electrode sheet of the metal lithium battery, and the recovery process is to use white oil to purify and remove impurities, and recover high-purity metal lithium. Or lithium alloy, no need to re-electrolytic refining, the process is simple, low energy consumption, low comprehensive cost, easy to implement.
  • the recovered product has high purity and is easy to be added to the industrial process control.
  • the main reaction medium used is white oil. Recycle after treatment to reduce costs.
  • the method for recovering the negative electrode sheet of the metal lithium battery of the invention comprises the following steps:
  • the metal lithium battery negative electrode sheet is immersed in white oil
  • heating heating the white oil immersed in the negative electrode sheet of the metal lithium battery to 180-220 ° C, and stirring;
  • step b Insulation filtration: the white oil heated in step b is subjected to heat preservation filtration, and the filtrate is taken;
  • Degreasing Vacuum degreasing the solid metal lithium or lithium alloy to obtain a metallic lithium liquid or a lithium alloy liquid;
  • the white oil of the present invention is an industrial grade white oil obtained by petroleum refining, and the main component is a mixture of saturated cycloalkane and paraffin.
  • step a a certain amount of white oil is added to fully soak the negative electrode sheet of the metal lithium battery, and the separator attachment is gradually dissolved after contact with the white oil in the soaking process, and finally completely dissolved in the white oil.
  • the amount of white oil added is preferably a immersion metal lithium battery negative electrode sheet, and the immersion time is not less than 1 hour, preferably 1 hour.
  • step b as the temperature increases, the lithium metal or lithium alloy on the negative electrode sheet melts in the white oil, and the internal embedded impurities are released by stirring, wherein the stirring rate is 100 to 150 rpm, and the stirring reaction time is 15 to 30 minutes.
  • the reaction material is subjected to thermal filtration using a filter of a certain precision; copper and nitride and other deposits are deposited in the filter residue by filtration, and the filter has an accuracy of 15 to 30 ⁇ m.
  • step d the filtrate is cooled and filtered again to obtain a solid metal lithium or lithium alloy; the liquid metal lithium or lithium alloy is solidified in white oil and solidified, and the filtrate is white oil.
  • the filter accuracy is preferably 5 to 10 ⁇ m.
  • the vacuum degreasing temperature in the e step is 240 to 260 ° C, and the degree of vacuum is 0.8 to 1.2 Pa.
  • the vacuum deoiling temperature of the e step is 250 ° C and the degree of vacuum is 1 Pa.
  • the e step may be performed by placing lithium metal in a vacuum de-oiling tank to control the deoiling temperature at 250 ° C, and removing the volatile oil stain under the condition of a vacuum of 1 Pa.
  • the metal lithium liquid or the lithium alloy liquid obtained by de-oiling the e step is again filtered in a glove box under an argon atmosphere, and the filtrate is poured and cooled to obtain a battery-grade metal lithium ingot or a lithium alloy ingot.
  • the filter accuracy is preferably 5 to 10 ⁇ m.
  • Filtration of the f step of the invention is carried out under an inert atmosphere.
  • lithium nitride and lithium oxide are prevented from being formed, and on the other hand, lithium nitride, lithium oxide or the like contained in the raw material can be further removed by filtration.
  • the inert atmosphere is argon.
  • the invention mainly utilizes the scrap material of the negative electrode sheet of the metal lithium battery, the scrap or the negative electrode sheet disassembled by the metal lithium battery, and extracts the lithium metal or lithium alloy with higher purity.
  • the metal lithium battery is a metal lithium primary battery, a metal lithium secondary battery, a lithium alloy primary battery, or a lithium alloy secondary battery.
  • the metal lithium primary battery or the metal lithium secondary battery can be recovered by the method of the invention to obtain battery-grade metallic lithium
  • the lithium alloy primary battery or the lithium alloy secondary battery can be recovered by the method of the invention to obtain a relatively pure lithium alloy.
  • a lithium battery in which lithium metal or a lithium alloy is used as a negative electrode can be recovered without simply peeling off metallic lithium or a lithium alloy.
  • On the negative electrode sheet of the metal lithium battery there may be a deposit of the battery separator, a deposit of copper, and a surface deposit formed by the reaction of the metal lithium and the electrolytic solution.
  • the white oil is used for purification and impurity removal of the reaction medium, and the copper, the separator and other deposits therein can be removed to obtain a metal lithium or a lithium alloy with higher purity.
  • the lithium metal is recovered by the following method:
  • the reactor is heated so that the temperature of the white oil reaches 200 ° C and is fully stirred, and the stirring rate is 110 r / min; as the temperature increases, the metallic lithium on the pole piece melts in the white oil and is released by stirring.
  • reaction material is incubated with a 15 ⁇ m precision filter; the copper and nitride and other deposits are deposited in the filter residue by filtering;
  • the obtained metallic lithium is vacuum-depleted, and the metallic lithium is placed in a vacuum de-oiling tank to control the deoiling temperature to be 250 ° C, and the vacuum degree is 1 Pa to remove volatile oil, thereby obtaining a metallic lithium liquid.
  • the metal lithium liquid is again filtered in a glove box under an argon atmosphere, and the filtrate is poured and cooled to obtain a battery grade metal lithium ingot.
  • the filter has an accuracy of 5 to 10 ⁇ m.
  • the lithium metal is recovered by the following method:
  • the 100 g of the negative electrode sheet of the metal lithium secondary battery is placed in the reactor, and 100 ml of white oil is added to fully soak for 60 min. During the process, the separator deposit is gradually dissolved after contact with the white oil, and finally completely dissolved in the white oil;
  • the reactor is heated so that the temperature of the white oil reaches 180 ° C and is fully stirred, and the stirring rate is 100 r / min; as the temperature increases, the metallic lithium on the pole piece melts in the white oil and is released by stirring.
  • reaction material is incubated with a 15 ⁇ m precision filter; the copper and nitride and other deposits are deposited in the filter residue by filtering;
  • the obtained metallic lithium is vacuum-depleted, and the metallic lithium is placed in a vacuum de-oiling tank to control the deoiling temperature to be 240 ° C, and the vacuum degree is 0.8 Pa to remove the volatile oil stain to obtain a metallic lithium liquid.
  • the metal lithium liquid is again filtered in a glove box under an argon atmosphere, and the filtrate is poured and cooled to obtain a battery grade metal lithium ingot.
  • the filter has an accuracy of 5 to 10 ⁇ m.
  • the lithium metal is recovered by the following method:
  • the reactor is heated so that the temperature of the white oil reaches 180 ° C and is fully stirred, the stirring rate is 150 r / min; as the temperature increases, the metallic lithium on the pole piece melts in the white oil and is released by stirring. Internally embedded impurities;
  • reaction material is incubated with 30 ⁇ m precision filter; the copper and nitride and other deposits are deposited in the filter residue by filtering;
  • the obtained metallic lithium is vacuum-depleted, and the metallic lithium is placed in a vacuum de-oiling tank to control the deoiling temperature to be 240 ° C, and the vacuum degree is 0.8 Pa to remove the volatile oil stain to obtain a metallic lithium liquid.
  • the metal lithium liquid is again filtered in a glove box under an argon atmosphere, and the filtrate is poured and cooled to obtain a battery grade metal lithium ingot.
  • the filter has an accuracy of 5 to 10 ⁇ m.
  • the battery grade metallic lithium according to the present invention has the composition shown in Table 1.
  • the lithium alloy is recovered by the following method:
  • the lithium alloy primary battery negative electrode scrap 100g is placed in the reactor, and 800ml white oil is added and fully immersed for 60min. During the process, the separator attachment is gradually dissolved after contact with the white oil, and finally completely dissolved in the white oil;
  • the reactor is heated so that the temperature of the white oil reaches 180 ° C and is fully stirred, the stirring rate is 150 r / min; as the temperature increases, the lithium alloy on the pole piece melts in the white oil and is released by stirring.
  • reaction material is incubated with 30 ⁇ m precision filter; the copper and nitride and other deposits are deposited in the filter residue by filtering;
  • the filtrate is cooled and filtered again to obtain a solid lithium alloy; the liquid lithium alloy is cooled and solidified in white oil, and the filtrate is white oil;
  • the obtained lithium alloy is vacuum degreased, and the lithium alloy is placed in a vacuum degreaser to control the deoiling temperature to be 240 ° C, and the vacuum degree is 0.8 Pa to remove the volatile oil stain to obtain a lithium alloy liquid.
  • the metal lithium alloy liquid is again filtered in a glove box under an argon atmosphere, and the filtrate is poured and cooled to obtain a battery grade metal lithium ingot.
  • the filter has an accuracy of 5 to 10 ⁇ m.
  • the composition of the battery grade lithium alloy is shown in Table 2.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Secondary Cells (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

La présente invention concerne un procédé de récupération pour une pièce d'électrode négative d'une batterie au lithium-métal, concernant le domaine technique des batteries. Le problème technique résolu par la présente invention est de fournir un procédé de récupération pour une pièce d'électrode négative d'une batterie au lithium-métal, de manière à extraire du métal lithium ou un alliage de lithium de la pièce d'électrode négative de la batterie au lithium-métal. Le procédé comprend les étapes suivantes : a. immersion des matières résiduelles de la pièce d'électrode négative de la batterie au lithium-métal dans de l'huile blanche; b. chauffer l'huile blanche dans laquelle la pièce d'électrode négative de la batterie au lithium-métal est immergée à une température de 180 à 220 °C et agiter l'huile blanche; c. maintenir la température et le filtrage pour obtenir un filtrat; d. refroidir le filtrat et filtrer pour obtenir un métal semi-conducteur de lithium ou un alliage de lithium; e. effectuer un dégraissage sous vide sur le métal semi-conducteur de lithium ou l'alliage de lithium pour obtenir un liquide de métal de lithium ou un liquide d'alliage de lithium; et f. filtrer et verser: filtrer le liquide de métal de lithium ou le liquide d'alliage de lithium dans une atmosphère inerte, puis verser le filtrat obtenu après filtration pour former un lingot de métal de lithium de qualité de batterie ou un lingot d'alliage de lithium. Par rapport à l'état de la technique, le produit récupéré par le procédé de la présente invention a une pureté élevée; le procédé de récupération ne nécessite pas de raffinage par une deuxième électrolyse; et l'invention est simple à mettre en œuvre et présente une faible consommation d'énergie et un coût global et est facile à mettre en œuvre.
PCT/CN2017/074130 2016-08-11 2017-02-20 Procédé de récupération de pièce d'électrode négative pour batterie au lithium-ion Ceased WO2018028167A1 (fr)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
FR3095076A1 (fr) * 2019-04-15 2020-10-16 Blue Solutions Procédé d’extraction de lithium d’une batterie électrique comprenant du lithium métallique solide.

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CN106159367B (zh) * 2016-08-11 2018-08-03 天齐锂业股份有限公司 金属锂电池负极片的回收方法
CN108879013B (zh) * 2018-07-18 2019-11-01 大同新成新材料股份有限公司 一种锂电池负极片二次加工装置及其加工方法
CN109244499B (zh) * 2018-09-29 2020-08-18 杨倩 一种锂电池负极片二次回收加工用除油浇注一体化设备
CN109355506B (zh) * 2018-10-22 2023-05-05 天齐锂业（江苏）有限公司 一种金属锂废渣的无害化处理方法及系统
CN109371240B (zh) * 2018-10-23 2024-04-30 天齐锂业（江苏）有限公司 一种金属锂渣回收处理设备及方法
CN109852802B (zh) * 2019-01-10 2020-12-11 东南大学 一种锂金属电池负极回收再利用的方法
CN113839114A (zh) * 2020-06-24 2021-12-24 天津中能锂业有限公司 金属锂负极回收
CN112920494A (zh) * 2021-02-05 2021-06-08 保定风帆美新蓄电池隔板制造有限公司 一种用铅酸蓄电池pe隔板废料制备再生物的方法
FR3161803A1 (fr) * 2024-04-24 2025-10-31 Blue Solutions Dispositif de support de cellule électrochimique à recycler

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CN106159367B (zh) 2018-08-03

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