WO2014066776A1 - Processus de récupération d'alliage ab5 à partir d'accumulateurs nickel/hydrure métallique usagés et/ou de leurs cellules - Google Patents

Processus de récupération d'alliage ab5 à partir d'accumulateurs nickel/hydrure métallique usagés et/ou de leurs cellules Download PDF

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Publication number
WO2014066776A1
WO2014066776A1 PCT/US2013/066835 US2013066835W WO2014066776A1 WO 2014066776 A1 WO2014066776 A1 WO 2014066776A1 US 2013066835 W US2013066835 W US 2013066835W WO 2014066776 A1 WO2014066776 A1 WO 2014066776A1
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Prior art keywords
nickel hydroxide
intermetallic alloy
nickel
slurry
solids
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PCT/US2013/066835
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English (en)
Inventor
W. Novis Smith
Scott Swoffer
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Retriev Technologies Incorporated
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Priority claimed from US13/661,922 external-priority patent/US8696788B1/en
Application filed by Retriev Technologies Incorporated filed Critical Retriev Technologies Incorporated
Publication of WO2014066776A1 publication Critical patent/WO2014066776A1/fr

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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
    • H01M6/00—Primary cells; Manufacture thereof
    • H01M6/52—Reclaiming serviceable parts of waste cells or batteries, e.g. recycling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
    • B09B3/80—Destroying solid waste or transforming solid waste into something useful or harmless involving an extraction step
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/24—Electrodes for alkaline accumulators
    • H01M4/32—Nickel oxide or hydroxide electrodes
    • 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 the recovery of AB 5 alloy from spent nickel/metal hydride (NIMH) storage batteries and/or the electrode cells. More particularly, there is provided a process for the selective recovery of AB 5 alloy from NIMH storage batteries without thermal melting or dissolving the AB 5 alloy into solution.
  • NIMH nickel/metal hydride
  • the rare earth materials are found in NIMH batteries in the unique hydrogen absorbing AB 5 metal alloy anode (about 32% are earth metals, primarily lanthanum in amounts of 18-25%) powder which is the key anode material found in most NIMH batteries.
  • AB 5 alloys combine a hydride forming metal A, usually a rare earth metal (La, Ce, Nd, Pr, Y or their mixture known as misch metal), with a non-hydride forming element, nickel.
  • the AB 5 can be doped with other metals, such as Co, Sn or Al, to improve materials stability or to adjust equilibrium hydrogen pressure and temperature required for its charging discharging with hydrogen.There is a significant amount of energy and loss of material in separating then converting a rare-earth ore to the purified rare earth compound mix (18-25% lanthanum).
  • the correct rare earth oxide mix is converted to the highly reactive rare earth metal mixture (misch metal) under vacuum and very high temperatures (>1400°C) under vacuum.
  • This misch metal then must be mixed with the correct amount of nickel metal and re-melted in a vacuum induction furnace and then cooled rapidly and then ground to a -325 mesh powder under inert atmosphere due to its reactivity.
  • the very hard alloy is difficult to grind. This is a very energy intensive and costly process.
  • the invention is more preferably used in a cell containing a negative electrode having hydrogen storage alloy materials of the so-called AB 5 -type, a common example of which is described in the basic formula and M s Ni 5 (Al x Mn 4 Co 3 ) x wherein M s represents a lanthanum-rich misch metal (REM), which includes various rare earth metals and wherein 2.5 ⁇ r ⁇ 5.0, 0 ⁇ s ⁇ 2.5, 0 ⁇ t ⁇ 0.5, and 0 ⁇ u ⁇ 0.5.
  • Hydrogen absorbing alloys of this class i.e., AB5 are disclosed, for instance, in U.S. Patent Nos. 4,216,274 (Bruning et al) and 4,375,257 (Bruning, et al).
  • the typical AB 5 -type materials as currently envisioned and similarly TiNi 2 and typically have the basic atomic structure Ni-Ti-V-Cr-Zr-X-Y wherein X and Y can be other elements of various selection.
  • the invention is more preferably used in a cell containing a negative electrode having hydrogen storage intermetallic alloy materials of the so-called AB 5 -type, a common example of which is described in the basic formula MmNi r Co s Mn t Al u , wherein Mm represents a lanthanum-rich misch metal, which includes various rare earth metals, and wherein 2.5 ⁇ r ⁇ 5.0, 0 ⁇ s ⁇ 2.5, 0 ⁇ t ⁇ 0.5, and 0 ⁇ u ⁇ 0.5 and M s NiAl x Mn 4 Co 3 .
  • Negative electrode alloys used in NiMH batteries typically comprise La Pr and Nd as rare earth elements and Zn, Mg and Ni. Cobalt, manganese and aluminum are common additives.
  • the components of a NIMH battery include nickel metal grid, Ni(OH) 2 , nickel coated iron, potassium hydroxide electrolyte, and most importantly a nickel metal alloy powder of up to 25-30%) by weight.
  • This alloy powder has been developed to absorb considerable hydrogen and is the source of the descriptor "nickel metal hydride" battery. Under charging conditions, this nickel alloy absorbs significant amounts of hydrogen as the metal hydride is formed electrochemically. Under battery discharge conditions this absorbed hydrogen reacts electrochemically back to hydroxide and water providing the electrical current of the battery.
  • AB 5 The currently most well known nickel alloy used is termed AB 5 which is an alloy consisting of one part misch metal (mostly lanthanum or REM) to five parts nickel on a mole basis— theoretically 32.1% (REM) on a weight basis. Therefore, the naturally occurring rare earth oxide mixture is used to form the misch metal which avoids the expense of separating the rare earth oxides into the individual elements before reducing them to the mixed metal and not to the pure metal such as pure lanthanum metal. This metal mixture which is used is called misch metal. Therefore the AB 5 alloy is an alloy of a mixture of lanthanum group metals and nickel with some cobalt and other metals added in small amounts for optimized hydrogen formation and storage. This AB 5 component is the most expensive raw material cost for this type of battery.
  • misch metal mostly lanthanum or REM
  • a process for the recovery of AB 5 intermetallic alloy from spent nickel metal hydride batteries and/or cells comprises the steps of:
  • step B) screening the product of step A) to separate the metal particles from the slurry which is formed;
  • step C) treating the slurry from step B) with a non-oxidizing non-halogenated acid to
  • step D) recovering the AB 5 intermetallic alloy solids from the product of step C) by allowing the AB5 intermetallic alloy solids to settle while decanting off a suspension comprised of undissolved nickel hydroxide and dissolved nickel hydroxide (binder may also be present in the suspension).
  • Another embodiment of the invention provides a process for the recovery of AB 5 intermetallic alloy from spent nickel metal hydride batteries and/or cells which comprises the steps of:
  • step B) screening the product of step A) to separately recover the metal particles and the slurry formed
  • step D) recovering the AB 5 intermetallic alloy solids from the product of step C) by
  • step F) recovering dissolved nickel hydroxide from the filtrate obtained in step E) by precipitation with base.
  • Yet another embodiment of the present invention provides a process comprising the steps of: (a) wet crushing nickel metal hydride batteries and/or cells, (b) screening the product of step (a) to recover the coarser metal particles from the resultant slurry of fine particles, (c) selectively partially dissolving Ni(OH) 2 present in the slurry at a pH of about 2- 5 without dissolving the AB 5 intermetallic alloy and lanthanum; (d) agitating the resultant slurry to suspend and decant the undissolved nickel hydroxide slurry in the form of a suspension while not disturbing the settled heavier AB 5 ; (e) resuspending the heavier AB 5 in water and filtering this suspension and washing the solids; (f) drying the solids under an inert atmosphere and recovering the AB 5 containing the lanthanum; (g) filtering the decanted suspension of step (d) to recover the undissolved nickel hydroxide; and then (h) adding a base such as sodium hydroxide to the filtrate from step
  • the Ni(OH) 2 is selectively partially dissolved by a non-oxidizing non-halogenated acid.
  • the acid treatment conditions are selected such that only about 20% to about 60% or about 25% to about 50% of the nickel hydroxide is actually dissolved (i.e., converted to a water-soluble species), with the rest of the nickel hydroxide remaining undissolved in fine particulate form.
  • the invention thus provides ways to purify a mixture containing hydrogen storage intermetallic AB 5 which is obtained from the electrodes of spent nickel metal hydride batteries and/or the crushed batteries.
  • the invention further provides ways to obtain AB 5 containing the lanthanum from electrodes of spent nickel metal hydride batteries.
  • a method for the purification and isolation of hydrogen storage intermetallic alloy AB 5 and any lanthanum present from material obtained from spent nickel metal hydride batteries and cells which comprises the steps of:
  • step B) screening the product of step A) to separately recover the metal particles and the slurry formed;
  • step C) selectively partially dissolving the nickel hydroxide in the slurry of step C) with a non-oxidizing non-halogenated acid without dissolving said AB 5 intermetallic alloy solids and any lanthanum present;
  • step F recovering the dissolved nickel hydroxide (which is typically in the form of a soluble acid salt such as nickel acetate) from the filtrate obtained in step E) by precipitation with base.
  • nickel hydroxide which is typically in the form of a soluble acid salt such as nickel acetate
  • step D) the AB 5 intermetallic alloy solids, by virtue of their higher density, settle out of the aqueous mixture obtained as a result of step C) more rapidly than the remaining undissolved particles of nickel hydroxide, which tend to remain in suspension longer.
  • the decanted suspension (supernatant) also contains dissolved nickel hydroxide.
  • the process is carried out under an inert atmosphere.
  • the non-oxidizing non-halogenated acid is preferably selected from the group consisting of acetic acid, glycolic acid, formic acid, sulfuric acid and combinations thereof.
  • step B) The product of step B) can be screened through a 25 mesh screen and then through a - 200 mesh screen.
  • step C) is carried out at a pH of 2-4. .
  • the present process may involve the crushing of steel cased battery or cells in a water mist, preferably in a hammer mill and under an inert atmosphere.
  • the wet heavy separator mat which entangles much of the coarse grid collector metal on the top of a shaker table (+1/4") is screened off. This may be sold for its coarse nickel metal content. It can also be pyrolyzed to remove the organic separator yielding all of the contained nickel metal powder and pieces free of organic material, also suitable for sale.
  • the rest of the water slurry after removing the +1/4" material may be further screened to -200 mesh to yield a slurry containing 85% of the starting electrode material including the AB 5 anode metal powder material and the nickel hydroxide cathode material with some binder.
  • This -200 mesh slurry may be neutralized to pH 5 with a non-oxidizing acid such as acetic acid.
  • the acid e.g., commercial grade acetic acid
  • the acid is preferably added to the aqueous slurry under an inert atmosphere in an estimated 50-95% of the theoretical amount needed to dissolve the calculated molar mount of nickel hydroxide present (in the case of acetic acid, for example, two moles of acetic acid per mole of nickel hydroxide).
  • This addition may be at room temperature with high shear stirring and cooling may be maintained at about 18-25°C for four hours.
  • the slurry is allowed to settle briefly to just allow the dense AB 5 to settle.
  • the suspension (supernatant) containing the undissolved nickel hydroxide and dissolved nickel acetate or other acid salt (with some cobalt acetate) both from the cathode may be decanted off and filtered.
  • the nickel hydroxide cake is recovered and dried, and the dissolved nickel is recovered from the filtrate solution by adding a base such as an alkali hydroxide (e.g., 50% sodium hydroxide) to a pH of 10-1 1, for example, and filtering the precipitated nickel hydroxide off and drying.
  • a base such as an alkali hydroxide (e.g., 50% sodium hydroxide)
  • the acetic acid may be recovered from this filtrate for recycling back to the process by distilling off the water and then acidifying this filtrate with sulfuric acid (e.g., to pH 3.5) and distilling off the formed acetic acid.
  • the wash decantation of the AB 5 metal powder may need to be carried out several times to purge the residual binder from the AB 5 powder. (This can also be accomplished in a continuous controlled cyclic wash with filtration of the circulating system).
  • the cleaned AB 5 may be filtered and recovered under inert atmosphere. It may be dried under vacuum with heating (e.g., at 100°C), cooled and screened (e.g., through -325 mesh).
  • the assay of the AB 5 thus obtained typically is 18-25% La and an oxygen content of ⁇ 1.0 to 2%.
  • the other rare earths including the cerium and neodymium typically add up to about 6% with a few percent cobalt and aluminum.
  • the nickel metal is the balance to typically about 65%. The overall recovery is about 60-80% of the contained AB 5 metal in the electrode mix.
  • the initial slurry after screening the metal particles may be treated with a magnet to remove any small casing particles.
  • This selective dissolution/purification procedure will work on any mixture of the nickel metal hydride and the Ni(OH) 2 cathode material. It can be applied to those mixtures recovered from the processing and recycling of NIMH batteries. It can also be applied to electrode powders recovered from nickel/hydrogen batteries.
  • Ten Prius battery cells (1510 g) were stripped of their bus bars and plastic covers (1 155 g after) and were run through a hammer mill with an internal water spray and under nitrogen. The resulting slurry was directed onto a shaker table with 1 ⁇ 4" slots and the slurry passed through a 25 mesh screen (72 g +25 mesh -1/4") and then through a -200 mesh screen (61 g +200 mesh/-25 mesh). The damp mat cake on the shaker table contained coarse metal pieces and weighed 262 g dry. (Pyrolysis of this mat cake at 280°C under inert atmosphere gave 220 g of nickel metal powder and pieces for recovery.) The -200 mesh slurry was filtered to reduce the water content and dried under vacuum.
  • This mixed electrode cake consisting of AB 5 metal powder and nickel hydroxide cathode material weighed 564 g dry. (All steps were processed under nitrogen when possible.) The dry cake contained 12% lanthanum, which serves as a marker for the purity of the AB 5 which contains about 18-25%) lanthanum. This cake was about 48% AB 5 at this point of recovery.
  • This electrode mix was processed by the addition of slightly less than stoichiometric amounts (0.5 to 0.9) of 70% glycolic acid (in mole ratios of two glycolic acid molecules for each nickel hydroxide molecule present). The analysis of the lanthanum level was indicative of the purity along with the oxygen level.
  • a slurry of 80 g of the electrode mix (12% La) prepared in accordance with Example 1 in 200 ml of water was prepared with high speed mixing under nitrogen. (Calculated to contain 41.6 g nickel hydroxide-0.45 moles). The slurry was adjusted to pH 5 with sulfuric acid and then 78 g (70%) glycolic acid (85% of theory) was slowly added with only slight warm up. The stirring was maintained for four hours and then the slurry was allowed to settle only enough to allow the dense AB 5 to settle but to keep the fine brown gelatinous binder particles suspended. The total solution and binder were decanted off. This was repeated three times. The AB 5 was isolated by filtration and drying under vacuum and finally screening through -325 mesh. A magnet was used to remove any nickel metal fines which may still be present. The La content was 25% with 0.89% oxygen and the yield was 26 g, which was 68% based on the calculated amount in the cake.
  • a slurry of 80 g of the electrode mix (12% La) prepared in accordance with Example 1 in 200 ml of water was prepared with high speed mixing under nitrogen. (Calculated to contain 41.6 g nickel hydroxide-0.45 moles). The slurry was adjusted to pH 5 with sulfuric acid and then 54 g acetic acid (90% of theory) was slowly added with only slight warm up. The stirring was maintained four hours and then the slurry was allowed to settle only enough to allow the dense AB 5 to settle but keeping the fine brown undissolved nickel hydroxide particles suspended. The total solution and binder were decanted off. This was repeated three times. The AB 5 was isolated by filtration and drying under vacuum and finally screening through -325 mesh. A magnet was used to remove any nickel metal fines which may still be present. The La content was 25% with 0.99% oxygen and the yield was 29 g, which was 76% based on the calculated amount in the cake.

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  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
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Abstract

L'invention concerne un processus de récupération d'alliage AB5 à partir d'accumulateurs de stockage nickel/hydrure usagés et/ou de leurs cellules sans fusion thermique ou dissolution de l'alliage AB5. Le processus comprend une étape de dissolution partielle du Ni(OH)2 et de séparation de l'alliage AB5 contenant toujours du métal lanthane.
PCT/US2013/066835 2012-10-26 2013-10-25 Processus de récupération d'alliage ab5 à partir d'accumulateurs nickel/hydrure métallique usagés et/ou de leurs cellules WO2014066776A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US13/661,922 US8696788B1 (en) 2010-08-23 2012-10-26 Process for the Recovery of AB5 Alloy from Used Nickel/Metal Hydride Batteries
US13/661,922 2012-10-26

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WO2014066776A1 true WO2014066776A1 (fr) 2014-05-01

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019108120A1 (fr) * 2017-11-28 2019-06-06 Nilar International Ab Broyage de matériau d'électrode négative récupéré
CN112699618A (zh) * 2020-12-18 2021-04-23 赣江新区澳博颗粒科技研究院有限公司 一种离子型稀土矿原地浸矿过程数值模拟方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5478664A (en) * 1993-04-05 1995-12-26 Santoku Metal Industry Co., Ltd. Method of recovering reusable metals from nickel-hydrogen rechargeable battery
US5980841A (en) * 1996-02-13 1999-11-09 Santoku Metal Industry Co., Ltd. Method for recovering reusable elements from rare earth-nickel alloy
US20020124691A1 (en) * 1998-10-27 2002-09-12 Mitsui Mining & Smelting Co., Ltd. Process and system for recovering valent metals from refuse secondary batteries
US8246717B1 (en) * 2010-08-23 2012-08-21 Toxco, Inc. Process for the recovery of metals from used nickel/metal hydride batteries
US8252085B1 (en) * 2010-08-23 2012-08-28 Toxco, Inc. Process for the recovery of metals from used nickel/metal hydride batteries

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5478664A (en) * 1993-04-05 1995-12-26 Santoku Metal Industry Co., Ltd. Method of recovering reusable metals from nickel-hydrogen rechargeable battery
US5980841A (en) * 1996-02-13 1999-11-09 Santoku Metal Industry Co., Ltd. Method for recovering reusable elements from rare earth-nickel alloy
US20020124691A1 (en) * 1998-10-27 2002-09-12 Mitsui Mining & Smelting Co., Ltd. Process and system for recovering valent metals from refuse secondary batteries
US8246717B1 (en) * 2010-08-23 2012-08-21 Toxco, Inc. Process for the recovery of metals from used nickel/metal hydride batteries
US8252085B1 (en) * 2010-08-23 2012-08-28 Toxco, Inc. Process for the recovery of metals from used nickel/metal hydride batteries

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019108120A1 (fr) * 2017-11-28 2019-06-06 Nilar International Ab Broyage de matériau d'électrode négative récupéré
CN112699618A (zh) * 2020-12-18 2021-04-23 赣江新区澳博颗粒科技研究院有限公司 一种离子型稀土矿原地浸矿过程数值模拟方法
CN112699618B (zh) * 2020-12-18 2023-01-17 赣江新区澳博颗粒科技研究院有限公司 一种离子型稀土矿原地浸矿过程数值模拟方法

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