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WO2025154800A1 - Procédé de production de liquide concentré en lithium - Google Patents

Procédé de production de liquide concentré en lithium

Info

Publication number
WO2025154800A1
WO2025154800A1 PCT/JP2025/001366 JP2025001366W WO2025154800A1 WO 2025154800 A1 WO2025154800 A1 WO 2025154800A1 JP 2025001366 W JP2025001366 W JP 2025001366W WO 2025154800 A1 WO2025154800 A1 WO 2025154800A1
Authority
WO
WIPO (PCT)
Prior art keywords
lithium
carbonate
calcium
liquid
carbonation reaction
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.)
Pending
Application number
PCT/JP2025/001366
Other languages
English (en)
Japanese (ja)
Inventor
那奈子 今崎
浩志 林
亮介 佐藤
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.)
Mitsubishi Materials Corp
Original Assignee
Mitsubishi Materials 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 Mitsubishi Materials Corp filed Critical Mitsubishi Materials Corp
Priority to JP2025567386A priority Critical patent/JPWO2025154800A1/ja
Publication of WO2025154800A1 publication Critical patent/WO2025154800A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/08—Carbonates; Bicarbonates
    • 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
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • lithium has been recovered and reused from lithium-containing materials such as crushed lithium-ion batteries.
  • a method for recovering lithium from a lithium-containing material as disclosed in, for example, Patent Documents 1 and 2, there is known a method in which lithium ion battery waste is roasted to obtain battery dregs, which are then immersed in an acidic solution to leach lithium into the acidic solution, and lithium is recovered from the obtained lithium leachate.
  • the lithium leachate from which lithium has been leached also contains metals other than lithium, such as cobalt and aluminum.
  • metals other than lithium such as cobalt and aluminum.
  • the metals other than lithium are mainly precipitated, and solid-liquid separation is then performed to separate the lithium-containing liquid from the other substances.
  • Carbonic acid is then added to the lithium-containing liquid to recover the lithium as lithium carbonate.
  • Patent Document 1 proposes a technical method for concentrating lithium in a lithium-containing solution using a nanofiltration (NF) membrane or a reverse osmosis (RO) membrane.
  • Patent Document 2 proposes a method for concentrating lithium in a lithium-containing solution using an electrodialysis device having an ion exchange membrane.
  • Patent Document 2 it is not easy to reduce the calcium content to 10 mg/L or less without precipitating lithium, and it is difficult to sufficiently suppress the decrease in the permeation flow rate through the membrane due to calcium precipitation.
  • carbonate ions remain in the lithium-containing liquid, carbon dioxide gas may be generated in the permeable membrane module, decreasing the permeation flow rate of the membrane.
  • calcium carbonate when the lithium-containing liquid is concentrated, calcium carbonate may be precipitated, decreasing the permeation flow rate of the membrane.
  • the method for producing a lithium concentrated liquid according to aspect 1 of the present invention is characterized by comprising a carbonation reaction step of adding a soluble carbonate compound to a lithium-containing liquid in which calcium ions coexist to produce calcium carbonate, a solid-liquid separation step of separating the calcium carbonate produced in the carbonation reaction step from the lithium-containing liquid, a decarbonation step of adding an inorganic acid to the lithium-containing liquid separated in the solid-liquid separation step to remove the dissolved carbonate compound from the lithium-containing liquid as carbon dioxide gas, and a membrane separation step of obtaining a lithium concentrated liquid in which the lithium ions in the lithium-containing liquid are concentrated using a reverse osmosis membrane after the decarbonation step.
  • the method for producing a lithium concentrated liquid according to aspect 1 of the present invention includes a decarbonation process prior to the membrane separation process, in which an inorganic acid is added to the lithium-containing liquid separated in the solid-liquid separation process to remove dissolved carbonate compounds from the lithium-containing liquid as carbon dioxide gas.
  • This sufficiently reduces the amount of carbonate compounds contained in the lithium-containing liquid supplied to the membrane separation process, inhibits the generation of carbon dioxide gas in the permeable membrane module, and inhibits the precipitation of calcium carbonate even when the lithium-containing liquid is concentrated.
  • This ensures a sufficient permeation flow rate through the reverse osmosis membrane in the membrane separation process, making it possible to efficiently and stably concentrate the lithium ions contained in the lithium-containing liquid.
  • the calcium concentration supplied to the carbonation reaction step is 10 mg/L or more, it is possible to obtain the effect of removing calcium by the carbonation reaction step and the solid-liquid separation step, and by sufficiently reducing the amount of carbonate compounds by the decarbonation step, it is possible to reliably suppress the precipitation of calcium carbonate when the lithium-containing solution is concentrated.
  • the method for producing a lithium concentrate according to the third aspect of the present invention is characterized in that, in the method for producing a lithium concentrate according to the first or second aspect, the pH in the carbonation reaction step is 8.0 or more and 12.0 or less. According to the method for producing a lithium concentrated solution of aspect 3 of the present invention, the pH in the carbonation reaction step is set to 8.0 or more and 12.0 or less, so that the production of calcium carbonate can be promoted and the amount of calcium in the lithium-containing solution can be efficiently reduced.
  • the method for producing a lithium concentrated solution according to a seventh aspect of the present invention is characterized in that, in the method for producing a lithium concentrated solution according to any one of the first to sixth aspects, sulfuric acid, hydrochloric acid, nitric acid, or a mixed solution thereof is used as the inorganic acid used in the decarbonation step.
  • sulfuric acid, hydrochloric acid, nitric acid, or a mixed solution of two or more selected from these is used as the inorganic acid used in the decarbonation step, so that carbonate compounds can be efficiently removed as carbon dioxide gas in the decarbonation step.
  • FIG. 1 is a flow diagram showing a method for recovering lithium using a method for producing a lithium concentrated solution according to one embodiment of the present invention.
  • FIG. 2 is a flow diagram showing an impurity removing step in FIG. 1 .
  • FIG. 2 is a flow diagram showing a method for producing a lithium-concentrated solution according to one embodiment of the present invention, which is applied as the lithium-containing solution concentrating step in FIG. 1.
  • FIG. 2 is a flow diagram showing a lithium carbonate production process in FIG.
  • the method for producing a lithium concentrate according to the present embodiment is applied to a process for recovering lithium from lithium-containing materials such as crushed waste lithium-ion batteries.
  • a lithium recovery method to which the method for producing a lithium concentrated solution according to the present embodiment is applied will be described with reference to FIG.
  • the lithium recovery method includes a leaching process S01, an impurity removal process S02, a lithium-containing liquid concentration process S03, a lithium carbonate production process S04, and a lithium carbonate purification process S05.
  • the impurity removal step S02 includes a first calcium compound addition step S21, a first solid-liquid separation step S22, a second calcium compound addition step S23, and a second solid-liquid separation step S24, as shown in FIG.
  • the first calcium compound is added to the lithium leachate to generate metal hydroxide and calcium fluoride. These metal hydroxide and calcium fluoride are precipitated in the liquid as solid phases.
  • the first calcium compound is added, for example, while stirring the lithium leachate.
  • the first calcium compound is not particularly limited as long as it is basic, and solid calcium compounds such as calcium carbonate, calcium hydroxide, calcium oxide, or mixtures thereof can be used.
  • the pH of the lithium leachate when producing metal hydroxide and calcium fluoride is adjusted to be 8.0 or more and 12.0 or less.
  • the metal hydroxide and calcium fluoride produced in the first calcium compound addition step S21 are removed from the lithium leachate.
  • an appropriate solid-liquid separation method such as gravity settling separation, centrifugal separation, or cloth filtration using a filter press or the like can be selected and used.
  • the precipitated calcium carbonate can be flocculated into larger flocs so that they do not remain in the supernatant liquid, and solid-liquid separation can be performed more reliably even when solid-liquid separation is performed by a gravity settling separation method such as a thickener.
  • the concentration of aluminum sulfate in the lithium-containing liquid is preferably 0 mg/L or more and 110 mg/L or less, more preferably 27 mg/L or more and 83 mg/L or less. If the concentration of aluminum sulfate is less than 27 mg/L, aggregation is not performed sufficiently, which is not preferable.
  • the concentration of aluminum sulfate is more than 110 mg/L, the volume of solids including calcium carbonate that precipitates becomes large, which is not preferable because the settling equipment must be large in order to perform solid-liquid separation sufficiently by the gravity settling separation method.
  • polymer flocculants include Diaflock AP825 manufactured by MT Aqua Polymer Co., Ltd. and Diaflock NP500 manufactured by MT Aqua Polymer Co., Ltd.
  • the concentration of the polymer flocculant in the lithium-containing liquid is preferably 1 to 10 ppm. For example, 2 mL of a 0.05% AP825 solution is added per 1 L of lithium-containing liquid. Also, 1 mL of a 0.1% NP500 solution is added per 1 L of lithium-containing liquid.
  • the lithium concentration in the lithium-containing liquid to be treated is 1 g/L or more and 15 g/L or less, and the calcium concentration is 10 mg/L or more and 100 mg/L or less.
  • the lithium concentration in the lithium-containing liquid to be treated is more preferably 1 g/L or more, and even more preferably 5 g/L or more.
  • the lithium concentration in the lithium-containing liquid to be treated is more preferably 15 g/L or less, and even more preferably 13 g/L or less.
  • the calcium concentration in the lithium-containing liquid to be treated is more preferably 10 mg/L or more, and even more preferably 20 mg/L or more.
  • the calcium concentration in the lithium-containing liquid to be treated is preferably 100 mg/L or less, and even more preferably 50 mg/L or less.
  • an inorganic acid is added to the lithium-containing liquid separated in the solid-liquid separation step S32, and the dissolved carbonate compounds are removed from the lithium-containing liquid as carbon dioxide gas.
  • the inorganic acid to be added may be, for example, sulfuric acid, nitric acid, hydrochloric acid, or a mixed acid of two or more selected from these.
  • the pH of the lithium-containing liquid in the decarbonation step S33 is more preferably 3.0 or more, and even more preferably 6.0 or more.
  • the pH of the lithium-containing liquid in the decarbonation step S33 is more preferably 7.0 or less, and even more preferably 6.5 or less.
  • the membrane separation step S34 after the decarbonation step S33, lithium ions in the lithium-containing liquid are concentrated using a reverse osmosis membrane.
  • a reverse osmosis membrane for example, a reverse osmosis membrane having a hollow fiber type, a spiral type, a tubular type, or the like structure made of a material such as cellulose acetate can be used.
  • the lithium concentration is preferably 18 g/L or more.
  • the upper limit of the lithium concentration in the lithium concentrated solution is preferably 35 g/L or less in consideration of the solubility of lithium sulfate.
  • the lithium carbonate production process S04 includes a first carbonation reaction process S41, a first solid-liquid separation process S42, a second carbonation reaction process S43, and a second solid-liquid separation process S44, as shown in Fig. 4.
  • a first soluble carbonate compound (first water-soluble carbonate compound) is added to a lithium concentrate in which lithium ions and calcium ions coexist, and the lithium concentrate is heated to generate calcium carbonate.
  • the lithium concentrate may be heated after the addition of the first soluble carbonate compound, or the first soluble carbonate compound may be added while heating the lithium concentrate.
  • the first soluble carbonate compound for example, sodium carbonate or sodium bicarbonate can be used in the form of a solution or powder. It is also possible to solubilize the first soluble carbonate compound by blowing in carbon dioxide gas, thereby allowing it to react with the dissolved calcium.
  • the amount of substance (number of moles) of the first soluble carbonate compound to be added and the amount of substance (number of moles) of calcium in the lithium concentrated solution are in the range of 1.0 or more and 10.0 or less in terms of stoichiometric ratio (CO 3 2 ⁇ /Ca 2+ ) (molar ratio).
  • stoichiometric ratio (CO 3 2 ⁇ /Ca 2+ ) is 1.0 or more, calcium ions can be sufficiently precipitated as calcium carbonate, whereas when the stoichiometric ratio (CO 3 2 ⁇ /Ca 2+ ) is 10.0 or less, precipitation of lithium as lithium carbonate can be suppressed.
  • the stoichiometric ratio (CO 3 2 ⁇ /Ca 2+ ) in the first carbonation reaction step S41 is more preferably 2.0 or more, and even more preferably 3.0 or more.
  • the stoichiometric ratio (CO 3 2 ⁇ /Ca 2+ ) in the first carbonation reaction step S41 is more preferably 7.0 or less, and even more preferably 5.0 or less.
  • the heating temperature in the first carbonation reaction step S41 is preferably within the range of 40°C or higher and 95°C or lower. By setting the heating temperature in the first carbonation reaction step S41 to 40° C. or higher, it is possible to promote the production of calcium carbonate. On the other hand, by setting the heating temperature in the first carbonation reaction step S41 to 95° C. or lower, an increase in pressure in the reaction tank is suppressed, and it is possible to stably carry out the first carbonation reaction step S41.
  • the heating temperature in the first carbonation reaction step S41 is more preferably 60° C. or higher, and further preferably 90° C. or higher.
  • the amount of the second soluble carbonate compound added so that the ratio (CO 3 2 ⁇ /2Li + ) of the amount (molar number) of carbonate ions (CO 3 2 ⁇ ) in the second soluble carbonate compound to twice the amount (molar number) of lithium ions contained in the lithium concentrate is 1.0 to 5.0. This makes it possible to reduce the amounts of Ca and Al contained in the produced lithium carbonate.
  • the lithium concentrated liquid may be heated after the addition of the second soluble carbonate compound, or the second soluble carbonate compound may be added while heating the lithium concentrated liquid.
  • the second soluble carbonate compound it is preferable to add the second soluble carbonate compound at 15 to 25°C (room temperature) and then heat the lithium concentrated liquid, as described below.
  • the heating temperature in the second carbonation reaction step S43 is preferably within the range of 80°C or higher and 95°C or lower. By setting the heating temperature in the second carbonation reaction step S43 to 80° C. or higher, it is possible to promote the production of lithium carbonate. On the other hand, by setting the heating temperature in the second carbonation reaction step S43 to 95° C.
  • the heating temperature in the second carbonation reaction step S43 is more preferably 85°C or higher, and even more preferably 90°C or higher.
  • the lower the temperature of the lithium concentrate when sodium carbonate is added the slower the crystal growth of the lithium carbonate produced, and the less the amount of impurities contained therein.
  • the temperature of the lithium concentrate is preferably 1 mass % or less.
  • the lithium carbonate production step S04 it is preferable to return the carbonate compound containing calcium carbonate recovered in the first solid-liquid separation step S42 to the first carbonation reaction step S41.
  • the production of calcium carbonate can be promoted by using the returned calcium carbonate as seed crystals.
  • the lithium carbonate produced together with the calcium carbonate can be returned to the first carbonation reaction step S41, which makes it possible to improve the recovery efficiency of lithium.
  • the lithium carbonate produced in the second carbonation reaction step S43 is separated from the mother liquor.
  • an existing solid-liquid separation method such as a gravity settling separation method, a centrifugal separation method, or a filter cloth filtration method such as a filter press can be appropriately selected and used.
  • lithium carbonate is produced. Note that this lithium carbonate may contain calcium at a concentration of 400 ppm by mass or more.
  • the lithium carbonate purification step S05 includes a slurrying step S51, a bicarbonation step S52, a first solid-liquid separation step S53, a purified lithium carbonate crystallization step S54, a second solid-liquid separation step S55, and a mother liquor returning step S56.
  • the pH in the decarbonation process S33 is set to 3.0 or higher and 7.0 or lower, damage to the reverse osmosis membrane in the membrane separation process S34 can be suppressed and the generation of carbon dioxide gas can be further promoted.
  • the production of calcium carbonate in the carbonation reaction process S31 can be promoted and calcium can be efficiently removed.
  • the solid matter was filtered using a membrane filter having a pore size of 0.45 ⁇ m.
  • the calcium concentration in the lithium-containing liquid after filtration is shown in Table 1.
  • sulfuric acid was added to adjust the pH of the lithium-containing liquid to a value shown in Table 1.
  • Comparative Examples 1 and 3 sulfuric acid was not added, and the pH of the lithium-containing liquid was not adjusted.
  • the lithium-containing liquid was passed through a reverse osmosis membrane module (HOLLOSEP® BC membrane, manufactured by Toyobo MC Co., Ltd.) to obtain a lithium-concentrated liquid.
  • HOLLOSEP® BC membrane manufactured by Toyobo MC Co., Ltd.
  • the permeation flow rate in the membrane separation step and the lithium concentration of the resulting lithium concentrated solution were evaluated.
  • the evaluation results are shown in Table 1.
  • the lithium concentration and calcium concentration were measured by ICP emission spectroscopy (iCAP7600Duo, manufactured by Thermo Fisher Scientific).
  • the permeation flow rate was calculated from the amount of the lithium concentrated solution that passed through the reverse osmosis membrane module at a certain time.
  • Comparative Example 1 the carbonation reaction process was not carried out, and no pH adjustment was carried out by adding sulfuric acid. As a result, the calcium concentration in the lithium-containing liquid was high, the pH was high, and the permeation flow rate in the membrane separation process was slow. In addition, the lithium concentration in the obtained lithium concentrated liquid was low, and lithium could not be concentrated efficiently.
  • the method for producing lithium concentrate of this embodiment is suitable for use in the process of recovering lithium from lithium-containing materials such as crushed lithium-ion batteries.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Metallurgy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
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  • Electrochemistry (AREA)
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  • Nanotechnology (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

Ce procédé de production de liquide concentré en lithium (S03) est caractérisé en ce qu'il comprend : une étape de réaction de carbonatation (S31) dans laquelle un composé d'acide carbonique soluble est ajouté à un liquide contenant du lithium contenant des ions calcium coexistant dans celui-ci pour produire du carbonate de calcium ; une étape de séparation solide-liquide (S32) dans laquelle le carbonate de calcium produit dans l'étape de réaction de carbonatation (S31) et le liquide contenant du lithium sont séparés ; une étape de décarbonatation (S33) dans laquelle un acide inorganique est ajouté au liquide contenant du lithium séparé dans l'étape de séparation solide-liquide (S32) et le composé d'acide carbonique dissous est éliminé du liquide contenant du lithium en tant que dioxyde de carbone gazeux ; et une étape de séparation par membrane (S34) dans laquelle, après l'étape de décarbonatation (S33), une membrane d'osmose inverse est utilisée pour obtenir un liquide concentré de lithium dans lequel des ions lithium dans le liquide contenant du lithium sont concentrés.
PCT/JP2025/001366 2024-01-19 2025-01-17 Procédé de production de liquide concentré en lithium Pending WO2025154800A1 (fr)

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JP2024-006790 2024-01-19
JP2024006790 2024-01-19
JP2024006659 2024-01-19
JP2024006655 2024-01-19
JP2024-006655 2024-01-19
JP2024-006659 2024-01-19

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PCT/JP2025/001366 Pending WO2025154800A1 (fr) 2024-01-19 2025-01-17 Procédé de production de liquide concentré en lithium
PCT/JP2025/001347 Pending WO2025154798A1 (fr) 2024-01-19 2025-01-17 Procédé de production de carbonate de lithium

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JP2020132952A (ja) * 2019-02-20 2020-08-31 株式会社ササクラ リチウム回収方法
CN111235591A (zh) * 2020-03-04 2020-06-05 杭州科锐环境能源技术有限公司 一种由锂辉石硫酸浸出液制备单水氢氧化锂的方法
JP2022164547A (ja) * 2021-04-15 2022-10-27 Ｄｏｗａエコシステム株式会社 リチウムイオン二次電池からのリチウムの回収方法
JP2023106309A (ja) * 2022-01-20 2023-08-01 Ｄｏｗａエコシステム株式会社 有価物の回収方法

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