WO2015046218A1 - Procédé de traitement d'un électrolyte liquide contenant du fluor - Google Patents

Procédé de traitement d'un électrolyte liquide contenant du fluor Download PDF

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Publication number
WO2015046218A1
WO2015046218A1 PCT/JP2014/075227 JP2014075227W WO2015046218A1 WO 2015046218 A1 WO2015046218 A1 WO 2015046218A1 JP 2014075227 W JP2014075227 W JP 2014075227W WO 2015046218 A1 WO2015046218 A1 WO 2015046218A1
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Prior art keywords
fluorine
vaporization
vaporized gas
containing electrolyte
waste battery
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PCT/JP2014/075227
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English (en)
Japanese (ja)
Inventor
林　浩志
浩一郎 平田
英範 鶴巻
龍太郎 藤澤
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三菱マテリアル株式会社
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Publication of WO2015046218A1 publication Critical patent/WO2015046218A1/fr

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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
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566—Liquid materials
    • 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
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0025—Organic electrolyte
    • H01M2300/0028—Organic electrolyte characterised by the solvent
    • H01M2300/0034—Fluorinated solvents
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • 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 present invention relates to a safe processing method for a fluorine-containing electrolytic solution used in a lithium ion battery or the like.
  • This application claims priority on September 30, 2013 based on Japanese Patent Application No. 2013-204126 for which it applied to Japan, and uses the content here.
  • Electrolytic solutions used in lithium ion batteries and the like contain fluorine compounds (LiPF 6 , LiBF 4, etc.) that serve as electrolytes and volatile organic solvents, which are mainly carbonates. It is a flammable substance. Moreover, when LiPF 6 reacts with water, it hydrolyzes to generate toxic hydrogen fluoride. For this reason, a safe processing method is required.
  • fluorine compounds LiPF 6 , LiBF 4, etc.
  • the following treatment methods are known as a treatment method for a lithium ion battery and its electrolytic solution.
  • Patent Document 1 Processing method to separate (Patent Document 1), (B) Battered used lithium battery, crushing the baked product and separating it into a magnetic material and a non-magnetic material, with a large amount of useful metals such as aluminum and copper Treatment method (Patent Document 2), (C) a lithium battery is opened with ultra-high pressure water, and an electrolytic solution is recovered using an organic solvent (Patent Document 3), (D) used battery is crushed Then, after washing with water, the positive electrode is peeled off to recover Al, Cu, Ni and Co, and Li is extracted from the remaining liquid by solvent extraction (Patent Document 4), (E) used batteries are crushed , washed with water to elute the LiPF 6, cobalt oxide lithium is peeled off cathode While recovering, the washing solution after the addition of hot acid decomposes LiPF 6 phosphate and fluorine, this was added slaked lime, processing method of recovering a mixture of fluoride Ca and phosphate Ca (JP 5).
  • Patent Document 2
  • the said processing method (A) requires a freezing equipment in order to disassemble and crush a lithium battery under freezing, it is difficult to implement.
  • a fluorine is processed as a combustion gas in the roasting process of a lithium battery, a highly pure fluorine component cannot be collect
  • recovered electrolyte solution becomes a problem.
  • the electrolyte solution contains a flammable organic solvent, and the fluorine compound in the electrolyte solution reacts with water to generate toxic hydrogen fluoride, so that safe treatment is required.
  • cleaning containing an organic solvent becomes a problem.
  • the present invention solves the above-mentioned problems in conventional processing methods, and an object thereof is to provide a method for safely processing an electrolytic solution containing a volatile fluorine compound (LiPF 6 or the like) and an organic solvent. .
  • the present invention is a method for treating a fluorine-containing electrolytic solution having the following constitution.
  • First vaporization in which water is added to a fluorine-containing electrolyte solution, the fluorine-containing electrolyte solution is heated to vaporize a volatile component contained in the fluorine-containing electrolyte solution, and a vaporized gas from which the volatile component is vaporized is recovered.
  • heating gas is fed while heating the residual liquid of the first vaporization step to vaporize volatile components contained in the residual liquid and recover the vaporized gas from which the volatile components have vaporized A second vaporization step, and the fluorine contained in the vaporized gas or a vaporized gas condensate obtained by condensing the vaporized gas is reacted with calcium and fixed as calcium fluoride, and further the organic solvent contained in the vaporized gas A method for treating a fluorine-containing electrolyte for recovering components.
  • fluorine-containing electrolyte is an electrolyte in a waste battery, an electrolyte in a state where the waste battery is cut or crushed, an electrolyte before use, or an electrolyte extracted from the waste battery
  • the fluorine-containing electrolytic solution is an electrolytic solution in a waste battery, and after the alkali is injected into the waste battery or the waste battery is immersed in the alkaline solution, the waste battery is heated and the first battery is heated.
  • the fluorine-containing electrolytic solution is an electrolytic solution in a waste battery, and after cutting or crushing the waste battery and adding a powdered alkali or an alkaline solution, the waste battery is heated to perform the first vaporization step.
  • a second vaporization step of feeding a heated gas is performed after the first vaporization step performed by adding moisture to the fluorine-containing electrolyte.
  • This two-stage vaporization treatment can increase the fluorine recovery rate. Specifically, in the normal first vaporization step, the fluorine recovery rate is around 70%, but the fluorine recovery rate can be increased to about 75% to 85% by the two-stage vaporization treatment.
  • fluorine can be recovered from the vaporized gas as calcium fluoride having high purity.
  • calcium fluoride having a purity of 80% or more can be obtained.
  • This calcium fluoride can be reused as a raw material for producing hydrofluoric acid or as a raw material for cement.
  • the recovered organic solvent component can be used as a fuel or an alternative fuel. Since the organic solvent component recovered by the treatment method of the present invention is separated from fluorine, no harmful substances such as hydrogen fluoride are generated when used as a fuel and can be used safely.
  • the electrolytic solution is vaporized and taken out, so that the battery can be treated safely without being frozen or burned at a high temperature.
  • Electrolytic solutions used in lithium ion batteries and the like contain an electrolyte fluorine compound and an organic solvent.
  • the fluorine compound is mainly lithium hexafluorophosphate (LiPF 6 )
  • the organic solvent is dimethyl carbonate (DMC), ethyl methyl carbonate (EMC), diethyl carbonate (DEC), propylene carbonate (PC), ethylene carbonate (EC).
  • DMC, EMC and DEC are flammable substances.
  • the treatment method of the present embodiment is such a fluorine-containing electrolyte solution, which is an electrolyte solution in a waste battery, an electrolyte solution obtained by cutting or crushing a waste battery, an electrolyte solution before use, or a waste battery.
  • This is a method for treating the electrolyte extracted from the liquid.
  • step S1 After adding water to the fluorine-containing electrolyte, a vaporization process is performed to heat the fluorine-containing electrolyte and vaporize volatile components contained in the electrolyte.
  • water may be either liquid or gas (water vapor). It is preferable to perform vaporization treatment by adding water of 1 to 30% by mass of the electrolytic solution amount to the electrolytic solution and heating the electrolytic solution until the electrolytic solution temperature becomes 130 ° C. or higher.
  • DMC, EMC, and DEC are vaporized by heating so that the temperature of the electrolytic solution is 130 ° C. or higher.
  • the boiling point of EC is 244 ° C., when EC is vaporized, it is preferable to heat it to about 250 ° C. In addition, it is preferable that heating temperature is 280 degrees C or less.
  • the first vaporization process is completed when the electrolyte temperature has passed 130 ° C or has passed 250 ° C.
  • Gas that vaporizes volatile components (vaporized gas) is guided to the recovery process (steps S3 and S4), and the fluorine contained in the vaporized gas or the vaporized gas condensate condensed with vaporized gas is reacted with calcium and fixed as calcium fluoride. (Step S3). Further, the organic solvent component contained in the vaporized gas is recovered (step S4).
  • a vaporized residual liquid (hereinafter referred to as “residual liquid in the first vaporization step”) that is a fluorine-containing electrolyte solution that has undergone the first vaporization step after the first vaporization step (step S1).
  • a heating gas is sent in while heating, and a vaporization process is performed to further vaporize the volatile components of the residual liquid.
  • the heating gas water vapor of about 80 ° C. to about 110 ° C., vapor of an organic solvent, or heated air is used.
  • DMC or EMC vapor can be used as the vapor of the organic solvent.
  • the heated gas is preferably sent while bubbling into the residual liquid in the first vaporization step.
  • the amount of the heated gas may be 50 to 500% by mass of the residual liquid in the first vaporization step. Preferably, it is 100 to 300% by mass.
  • the vaporized gas obtained by the second vaporization step (the gas from which the volatile components have been vaporized) is guided to the recovery step (steps S3 and S4) in the same manner as the first vaporization step.
  • the heating in the second vaporization step may be performed at the same heating temperature as in the first vaporization step. Since the second vaporization step is performed after the first vaporization step, the first and second vaporization steps can be performed by providing a two-stage vaporization facility. Alternatively, the second vaporization step can be performed after the first vaporization step using one vaporization facility.
  • the vaporization of fluorine contained in the residual liquid in the first vaporization process is promoted by feeding a heated gas such as water vapor, organic solvent vapor, or heated air into the residual liquid in the first vaporization process.
  • the vaporization treatment may be repeated until the fluorine concentration in the vaporized gas is 1000 mg / L or less. Alternatively, the vaporization treatment may be continued until the fluorine concentration in the vaporized gas becomes 1000 mg / L or less.
  • Such a second vaporization step can increase the amount of fluorine recovered.
  • About 70% of the fluorine contained in the electrolytic solution is recovered by the first vaporization step, about 5 to 15% is further recovered by the second vaporization step, and finally about 75 to 85% of fluorine is recovered. be able to.
  • the used waste battery is heated after being discharged, and the volatile components contained in the electrolyte solution are first and second vaporization steps. Vaporize by.
  • a safety valve is provided in a battery to lower an excessive internal pressure, the safety valve is opened to connect a pipe, and the waste battery is heated to vaporize volatile components contained in the electrolyte.
  • the cut or crushed waste battery is in a state where the electrolyte inside the battery is exposed to the outside together with the electrode material, so that the electrolyte can be processed. Cutting or crushing the waste battery may be performed in an inert gas atmosphere so that the electrolyte does not ignite.
  • the internal temperature becomes high, so that volatile components are easily vaporized.
  • the atmospheric pressure conversion temperature becomes 170 ° C. to 251 ° C.
  • the pressure may be reduced to 1 kPa to 0.1 kPa and heated to 80 ° C. to 120 ° C.
  • the volatile component may be vaporized by heating the container as it is.
  • the waste battery which passed through the 1st and 2nd vaporization process is cut
  • the crushed material obtained as a result is separated and recycled according to the raw material.
  • the first and second vaporization steps may be performed on the cut or crushed waste battery, and the obtained crushed material may be separated and recycled.
  • the vaporized gas obtained in the first vaporization step and the vaporized gas obtained in the second vaporization step may be combined and guided to the recovery step, and the vaporized gas obtained in the first vaporization step and the second vaporization step may be processed.
  • the vaporized gas obtained in step 1 may be separately led to the recovery step.
  • the fluorine and the organic solvent contained in the vaporized gas can be recovered, for example, by any of the following steps (A) to (C).
  • B) A calcium compound is added to the vaporized gas condensate to precipitate calcium fluoride for solid-liquid separation, and then the organic solvent component is recovered from the separated liquid.
  • C) The vaporized gas is passed through the calcium packed bed to generate calcium fluoride, and the organic solvent component is recovered from the condensate obtained by condensing the gas that has passed through the packed bed.
  • the vaporized gas is introduced into a water-cooled trap, and the organic solvent and hydrogen fluoride in the vaporized gas are condensed and collected. These are separated into two layers, an aqueous phase and an organic phase.
  • the aqueous phase contains a fluorine component in the vaporized gas and is generally acidic with a pH of 2 or less.
  • a calcium compound (calcium carbonate, slaked lime, quicklime, etc.) is added to the aqueous phase (fluorine-containing water) to neutralize it, and the fluorine and calcium in the liquid are reacted to precipitate calcium fluoride.
  • the calcium fluoride is recovered by solid-liquid separation.
  • the fluorine concentration was analyzed by the fluoride ion electrode method. Specifically, 5 ml of an ionic strength adjusting agent (TISAB (A total ionic strength adjustment buffer) manufactured by Kanto Chemical Co., Inc.) was added to 100 mL of the measurement target solution, and the fluorine concentration was measured at a liquid temperature of 20 ° C. A fluoride ion electrode 6561-10C manufactured by Horiba was used as the fluoride ion electrode.
  • TISAB Total ionic strength adjustment buffer
  • a fluoride ion electrode 6561-10C manufactured by Horiba was used as the fluoride ion electrode.
  • Example 1 A two-stage vaporization process was performed on the lithium ion waste battery. After discharging the lithium ion waste battery (containing 100 mL of electrolyte), remove the safety valve of the lithium battery, connect the conduit to the safety valve, and add additives (water, water vapor, organic solvent vapor, heated air) through the conduit. It was introduced inside the battery. Further, the vaporized gas was led to the outside through the pipe line. As the first vaporization step, 20 g of water was added to the waste battery and heated to 120 ° C. under a reduced pressure of 20 kPa to perform vaporization treatment for 2 hours.
  • additives water, water vapor, organic solvent vapor, heated air
  • Table 2 shows the fluorine concentration of the recovered liquid according to the number of treatments in the second vaporization step of Example 1.
  • the collected liquid was sampled in 5 portions every 10 minutes from the start of the treatment. Since the fluorine concentration in the fifth sampling solution was below 1000 ppm, the second vaporization step was completed.
  • Example 2 A two-stage vaporization treatment was performed on a commercially available electrolytic solution (100 mL, 120.1 g in weight).
  • As the first vaporization step 20.0 g of water was added to the electrolytic solution, heated to 120 ° C. under a reduced pressure of 20 kPa, and vaporized for 2 hours. 70.1% of fluorine was recovered from the liquid (recovered liquid) condensed by cooling the vaporized gas to 2 ° C.
  • the residual liquid in the first vaporization step was 41.2 g, and the fluorine concentration was 82000 ppm.
  • As the second vaporization step heating was performed at 120 ° C. while continuously feeding EMC vapor to the residual liquid in the first vaporization step.
  • the fluorine concentration of the cooling liquid was 950 ppm
  • the second vaporization step was completed. 10.7% of the electrolyte was recovered from the recovered liquid in the second vaporization step.
  • the residual liquid in the second vaporization step was 35.9 g, and the fluorine concentration was 49000 ppm.
  • the total fluorine recovery rate was 80.8%. This two-step process reduced the residual liquid weight by 5.3 g.
  • Table 3 the charge amount in the first vaporization step is the amount of the electrolytic solution
  • the charge amount in the second vaporization step is the weight of the residual liquid in the first vaporization step.
  • the fluorine recovery rate is a ratio with respect to the amount of fluorine in the electrolytic solution.
  • Example 3 A two-stage vaporization treatment was performed on a commercially available electrolytic solution (100 mL, 120.6 g in weight). In the second vaporization step, the same treatment as in Example 2 was performed except that dimethyl carbonate (DMC) vapor was fed into the residual liquid in the first vaporization step. The first vaporization step recovered 69.8% of the fluorine, and the second vaporization step recovered 10.2% of the fluorine (total recovery rate of 80%). The fluorine concentration of the recovered liquid at the end of the second vaporization step was 720 ppm. This two-stage process reduced the residual liquid weight by 5.3 g. The results are shown in Table 4.
  • DMC dimethyl carbonate
  • the amount charged in the first vaporization step is the amount of the electrolytic solution
  • the amount charged in the second vaporization step is the weight of the residual liquid in the first vaporization step.
  • the fluorine recovery rate is a ratio with respect to the amount of fluorine in the electrolytic solution.
  • Example 4 A two-stage vaporization treatment was performed on a commercially available electrolytic solution (100 mL, weight of 120.4 g). In the 2nd vaporization process, it processed like Example 2 except sending water vapor
  • the amount charged in the first vaporization step is the amount of the electrolytic solution
  • the amount charged in the second vaporization step is the weight of the residual liquid in the first vaporization step.
  • the fluorine recovery rate is a ratio with respect to the amount of fluorine in the electrolytic solution.
  • Example 5 A two-stage vaporization treatment was performed on a commercially available electrolytic solution (100 mL, weight of 120.4 g). In the 2nd vaporization process, it processed like Example 2 except sending heated air (80 degreeC) into the residual liquid of a 1st vaporization process. In the first vaporization step, 70.5% of the fluorine was recovered, and in the second vaporization step, 4.5% of the fluorine was recovered (total recovery rate of 75%). This two-step process reduced the residual liquid weight by 4.6 g. The results are shown in Table 6. In Table 6, the amount charged in the first vaporization step is the amount of the electrolytic solution, and the amount charged in the second vaporization step is the weight of the residual liquid in the first vaporization step. The fluorine recovery rate is a ratio with respect to the amount of fluorine in the electrolytic solution.
  • an electrolyte containing a fluorine compound and an organic solvent can be safely treated.
  • the lithium battery containing a fluorine-containing electrolyte solution can be processed safely.

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Abstract

La présente invention concerne un procédé de traitement d'un électrolyte liquide contenant du fluor, faisant appel aux étapes suivantes : une première étape de vaporisation durant laquelle de l'eau est ajoutée à un électrolyte liquide contenant du fluor, ledit électrolyte liquide contenant du fluor est ensuite chauffé de façon à y vaporiser un constituant volatile, et un gaz résultant de la vaporisation dudit constituant volatile est récupéré ; et une seconde étape de vaporisation durant laquelle, après la première étape de vaporisation, tandis qu'un résidu liquide de la première étape de vaporisation est en cours de chauffe, un gaz chauffé lui est appliqué, vaporisant ainsi un constituant volatile dans le résidu liquide, et un gaz résultant de la vaporisation dudit constituant volatile est récupéré. Le fluor qui se trouve soit dans les gaz mentionnés précédemment soit dans un condensat desdits gaz réagit avec du calcium et est ainsi fixé sous la forme de fluorure de calcium, et un composé à base de solvant organique se trouvant dans lesdits gaz est également récupéré.
PCT/JP2014/075227 2013-09-30 2014-09-24 Procédé de traitement d'un électrolyte liquide contenant du fluor WO2015046218A1 (fr)

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Cited By (1)

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US20210143489A1 (en) * 2019-11-12 2021-05-13 Hulico LLC Battery deactivation

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JP6562212B2 (ja) * 2015-12-19 2019-08-21 三菱マテリアル株式会社 リチウムイオン電池の熱分解処理方法および処理装置

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JP2005026089A (ja) * 2003-07-02 2005-01-27 Toyota Motor Corp リチウム電池、その製造方法ならびに処理方法
JP2012186150A (ja) * 2011-02-15 2012-09-27 Sumitomo Chemical Co Ltd 電池廃材からの活物質の回収方法
JP2012204000A (ja) * 2011-03-23 2012-10-22 Toyota Motor Corp 電池パックのリサイクル方法及び処理装置

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JP2000030741A (ja) * 1998-07-09 2000-01-28 Morita Kagaku Kogyo Kk 六フッ化リン酸リチウムを含有する有機電解液の処理方 法
JP2005026089A (ja) * 2003-07-02 2005-01-27 Toyota Motor Corp リチウム電池、その製造方法ならびに処理方法
JP2012186150A (ja) * 2011-02-15 2012-09-27 Sumitomo Chemical Co Ltd 電池廃材からの活物質の回収方法
JP2012204000A (ja) * 2011-03-23 2012-10-22 Toyota Motor Corp 電池パックのリサイクル方法及び処理装置

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Publication number Priority date Publication date Assignee Title
US20210143489A1 (en) * 2019-11-12 2021-05-13 Hulico LLC Battery deactivation
US12021202B2 (en) * 2019-11-12 2024-06-25 Hulico LLC Battery deactivation

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