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WO1999033137A1 - Systemes de fixation integres - Google Patents

Systemes de fixation integres Download PDF

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Publication number
WO1999033137A1
WO1999033137A1 PCT/CA1998/001156 CA9801156W WO9933137A1 WO 1999033137 A1 WO1999033137 A1 WO 1999033137A1 CA 9801156 W CA9801156 W CA 9801156W WO 9933137 A1 WO9933137 A1 WO 9933137A1
Authority
WO
WIPO (PCT)
Prior art keywords
fixation
soluble metal
soluble
fixation reagent
reagents
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/CA1998/001156
Other languages
English (en)
Inventor
William C. Webster
Noel Evan Spindler
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.)
Solucorp Industries Ltd USA
Original Assignee
Solucorp Industries Ltd USA
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
Priority claimed from CA002225367A external-priority patent/CA2225367A1/fr
Application filed by Solucorp Industries Ltd USA filed Critical Solucorp Industries Ltd USA
Priority to AU16569/99A priority Critical patent/AU1656999A/en
Priority to PCT/CA1999/000383 priority patent/WO1999056867A2/fr
Priority to CA2372985A priority patent/CA2372985C/fr
Priority to EP99918998A priority patent/EP1062035A1/fr
Priority to EP20030078630 priority patent/EP1435674A1/fr
Priority to AU36954/99A priority patent/AU3695499A/en
Priority to US09/646,544 priority patent/US6838504B1/en
Publication of WO1999033137A1 publication Critical patent/WO1999033137A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
    • 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
    • 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
    • C22B17/00—Obtaining cadmium
    • 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
    • C22B43/00—Obtaining mercury
    • 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
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J61/00—Gas-discharge or vapour-discharge lamps
    • H01J61/02—Details
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J61/00—Gas-discharge or vapour-discharge lamps
    • H01J61/70—Lamps with low-pressure unconstricted discharge having a cold pressure < 400 Torr
    • H01J61/72—Lamps with low-pressure unconstricted discharge having a cold pressure < 400 Torr having a main light-emitting filling of easily vaporisable metal vapour, e.g. mercury
    • 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
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2203/00—Aspects of processes for making harmful chemical substances harmless, or less harmful, by effecting chemical change in the substances
    • A62D2203/10—Apparatus specially adapted for treating harmful chemical agents; Details thereof
    • 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
    • H01M10/06—Lead-acid accumulators
    • 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
    • H01M10/24—Alkaline accumulators
    • H01M10/30—Nickel accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2200/00—Safety devices for primary or secondary batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2200/00—Safety devices for primary or secondary batteries
    • H01M2200/10—Temperature sensitive devices
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling
    • 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 is m the field of apparatuses and methods for controlling release of solubilized metal wastes, particularly those metals which are the subject of environmental regulations.
  • the containers of the present invention provide capsules or absorbent mats which are adapted to release compositions that are capable of reacting with solubilized metals to produce insoluble metal compounds.
  • Ni-Cd batteries Cadmium, nickel
  • Zinc-carbon batteries Mercury, zinc
  • Silver oxide batteries Cadmium, silver, zinc
  • Lead-acid batteries have often been segregated from other waste for disposal. Facilities have been established to crush the batteries and reclaim the elemental lead. However, such batteries may leak during storage prior to disposal. Also, lead-acid batteries contain sulfuric acid, which is capable of dissolving the lead. As a result of these problems, it is common for the recycling sites to have contaminated soil and ground water, resulting in the need for expensive environmental remediation at such sites.
  • SLI Starting-lighting-ignition
  • BCI Battery Council International
  • Secondary lead Recycling lead from spent SLI batteries, referred to as secondary lead, is a major source of the annual production of lead. Currently, about 68% of the yearly U.S. consumption of lead is from secondary sources, the majority of which (about 90%) is from recycled SLI batteries. In 1997, in the U.S., 30 plants were actively engaged in the production of secondary lead.
  • lead-acid batteries When improperly disposed of, lead-acid batteries can corrode and release soluble lead and lead contaminated sulfuric acid into the environment, which in turn can pollute lakes, rivers, streams, ground water and eventually drinking water. In the event that lead-acid batteries are incinerated, lead will be released into the air and/or remain in the ash; in either case, a potentially dangerous environmental condition exists.
  • Ni-Cd batteries Rechargeable nickel-cadmium (Ni-Cd) batteries are ubiquitous in modern society as power sources for a wide variety of articles such as cellular and cordless phones, camcorders, CD players, laptop computers and cordless power tools.
  • the number of Ni-Cd batteries produced each year may be m the hundreds of millions in the U.S. alone.
  • Ni-Cd batteries When initially introduced, Ni-Cd batteries were typically and inadvertently disposed of in MSW. However, in 1996, m the U.S. a Federal law, The Mercury Containing and Rechargeable Battery Act (Public Law 104-142) was enacted to facilitate the efficient recycling of rechargeable Ni-Cd batteries, as well as to restrict the manufacture and use of certain mercury-containing batteries. Title I of that Act establishes uniform national labeling requirements for Ni-Cd batteries, small sealed lead-acid batteries, and certain other regulated batteries. Each battery or battery pack must bear a recycling symbol and recycling phrase appropriate to its electrical chemistries. Recovery of the metals in Ni-Cd batteries is currently conducted at only one facility m the United States.
  • thermometer contains 0.5g to 3 g, thermostats 3 g, mercury switches 3.5 g, and fluorescent lights 10 mg to 40 mg .
  • MSW soluble-metal-contaming devices
  • EPA has developed the Synthetic Precipitation Leaching Procedure (SPLP, described in EPA SW-846 Method 1312, incorporated herein by reference) which utilizes synthetic rainwater rather than the stronger extraction fluids wnich are used m the TCLP.
  • SPLP Synthetic Precipitation Leaching Procedure
  • Table 2 summarizes the existing TCLP limits and the proposed UTS limits for solubilized metals in soils and other non-waste waters. Such limits are set out merely as examples and may change from time to time and may differ from one jurisdiction to another .
  • radioactive metals including radioactive cobalt, uranium, plutonium, americium, thorium, cesium and strontium.
  • the invention provides an apparatus comprising a barrier separating a soluble metal from a fixation reagent.
  • the soluble metal and fixation reagent may be housed in the apparatus, le . tney are together retame ⁇ as parts of the apparatus.
  • the barrier is rupturable to expose the soluble metal to the fixation reagent.
  • a reaction may occur, under appropriate conditions, between the soluble metal and the fixation reagent to form a fixed metal compound that is less soluble than the soluble metal.
  • the fixed metal compound may be a substantially insoluble metal compound.
  • the barrier of the invention may form part of a fixation reagent container, housing the fixation reagent in or around the apparatus.
  • a fixation reagent container may comprise a fibrous mat impregnated with the fixation reagent.
  • the fibrous mat may in turn De coated with a rupturable polymer.
  • the fixation reagent container may comprise a rupturable capsule.
  • the fixation reagent container may comprise a gasket positioned to seal the apparatus against leakage of the soluble metal.
  • the barrier in the apparatus may form part of a soluble metal container, housing the soluble metal in the apparatus.
  • housing or “housed” is not to be understood as limiting the relevant structures to enclosures that completely encase a material. Rather, a housing denotes a physical connection that brings parts together as, for example, parts of the apparatus of the invention are housed in the apparatus in the sense that they are kept together as parts of the apparatus. Accordingly, soluble metals or fixation reagents may be housed in various embodiments of the invention by their incorporation into a single apparatus, and the apparatus need not encase or surround these parts of the apparatus .
  • the soluble metal may be selected from the group consisting of the following elements and compounds thereof: lead, nickel, cadmium, mercury, zinc, silver, vanadium, arsenic, beryllium, selenium, antimony, barium, chromium, thallium, cobalt, uranium, plutonium, thorium, strontium, cesium and americium.
  • the soluble metal is selected from the group consisting of the following elements and their compounds: lead, cadmium, and mercury.
  • the fixation reagent may be selected from the group consisting of sulfides, phosphates, hydroxides, silicates and carbonates. In one embodiment, the fixation reagent is selected from the group consisting of sulfides and phosphates. Where the fixation reagent is a sulfide, the fixed metal compound may be a substantially insoluble sulfide of the soluble metal. Where the fixation reagent is a phosphate, the fixed metal compound may be a substantially insoluble phosphate of the soluble metal.
  • the apparatus housing the fixation reagents and the soluble metal may be a battery, and the battery may have an electrode that comprises the soluble metal.
  • the battery may be a lead-acid battery wherein the soluble metal comprises lead.
  • the lead-acid battery may have an external casing, and a portion of the casing may house the fixation reagent.
  • the battery may be a nickel-cadmium battery wherein the soluble metal comprises cadmium or nickel, and a portion of the casing of the nickel- cadmium battery may house the fixation reagent.
  • One aspect of the invention provides a method of stabilizing a soluble metal comprising the steps of:
  • the present invention involves the utilization of integrated fixation systems in the manufacture of apparatuses, including devices, instruments, or appliances which contain metals in a form which can leach into the environment.
  • integrated waste treatment systems are provided in which various apparatuses are adapted to ameliorate leaching of soluble metals into the environment.
  • lead-acid batteries which contain soluble lead
  • Ni- Cd batteries which contain soluble cadmium and nickel
  • fixation systems and compositions of the present invention include sulfide and phosphate fixation systems which react with the solubilized metals to produce relatively insoluble metal sulfides and phosphates.
  • Other fixation systems may be used, either alone or in combination, including, among others, pH control, oxidizers, reducers, cementitious systems, and sorbents.
  • the quantity of the reactive composition provided in the apparatus is measured to achieve a generally stoichiometric reaction with the solubilized metal component of the apparatus, without providing an excess of reagent.
  • a container for fixation reagents may be provided, as a part of an integrated fixation system, to prevent release into the environment of soluble metals from various apparatuses.
  • fixation reagent containers of the present invention are adapted to provide a mechanism whereby soluble metals may be reacted with fixation reagents while the metals are still contained within the apparatus or in the vicinity thereof.
  • the fixation reagents may react with the solubilized metals to form insoluble metal compounds when the reagents are either released from the container or the reagents are accessed by the solubilized metals while the reagents are within the fixation reagent container.
  • Apparatuses of the invention may include, among other things, various types of batteries, mercury switches, ballast from fluorescent lights, electronic circuit boards, solar panels or cells and the like.
  • the reagent containers of the invention may include, among other things, capsules, impregnated mats and the like.
  • Reagents of the invention may include, among other things, sulfides, phosphates, buffers and the like in either liquid, slurry or solid form.
  • the reagent container may be integrated into the apparatus, such that reagents are generally released or made accessible when the useful life of the apparatus has been completed, either during storage prior to disposal of the apparatus or on disposal of the apparatus.
  • Figure 1 is a schematic side elevational, cross-sectional view of a lead-acid battery comprising six compartments, each with various adaptations for housing fixation reagents and soluble metals.
  • FIG. 2 is an isometric view of a nickel-cadmium (Ni-Cd) battery comprising a polyethylene insulator/fixation reagent container .
  • the present invention involves the utilization of integrated soluble metal fixation systems in the manufacture of various apparatuses, including devices, instruments, or appliances, which contain soluble metals in a form which can leach into the environment.
  • soluble metal fixation systems for example, lead-acid batteries, which contain soluble lead, and Ni-Cd batteries, which contain soluble cadmium and nickel, may be modified in accordance with the invention to ameliorate leaching of solubilized lead, cadmium, and nickel from such devices when they are damaged or discarded.
  • fixation reagents and compositions of the present invention include sulfide and phosphate fixation reagents which react with soluble metals to produce relatively insoluble metal sulfides and phosphates.
  • Other fixation systems may be used, either alone or in combination, including, among others, pH control, oxidizers, reducers, cementitious systems, and sorbents .
  • the quantity of fixation reagents provided in the container is measured to optimize the reaction between the fixation reagents and the soluble metal component (s) of the apparatus.
  • the optimum fixation reagent combination can be used in the correct dosage, avoiding concerns with either over dosing or under dosing of the fixation reagents.
  • Under dosing fixation reagents may fail to adequately control leaching of soluble metals because of incomplete fixation, resulting in environmental releases of solubilized metals. Over dosing of fixation reagents, beyond the cost disadvantage, may also create problems with particular fixation reagents.
  • overdosing of sulfide fixation reagents could result in reactive sulfides being released into the environment, or the release of toxic hydrogen sulfi ⁇ e (H 2 S) gas produced from the reactive sulfide fixation reagents.
  • H 2 S toxic hydrogen sulfi ⁇ e
  • the application of fixation reagents to soluble metal contaminants before they are released from an apparatus in effect reduces the volume of waste to be treated and facilitates more efficient reaction of the fixation reagents with the soluble metals .
  • apparatus has its ordinary meaning, encompassing in various embodiments of the invention any device, instrument, appliance or other thing that contains soluble metals in a form that can leach into the environment during storage, use, or disposal of the apparatuses.
  • apparatuses include, but are not limited to, lead-acid automotive batteries, nickel-cadmium rechargeable batteries, mercury batteries, mercury switches, ballasts from fluorescent light fixtures, electronic circuit boards, solar panels/cells and the like, such as are listed in Table 1.
  • soluble metals are metals, or metal compounds or complexes, that are capable of becoming solubilized, i.e. entrained in a solvent, and hence capable of leaching into the environment.
  • Solubilized metals are generally ionic, or in an equilibrium state with an ionic form, and may be complexe ⁇ with other compounds.
  • Soluble metals may be soluble in aqueous or non- aqueous media, and may become solubilized directly by a solvent or with the assistance of other factors such as heat, light or microbiological action. Metals may be present in an apparatus in a soluble form, or may become soluble during use, storage, or disposal of an apparatus.
  • the term 'soluble metal' specifically includes those metals which are the subject of regulations promulgated from time-to-time by the U.S. EPA relating to the disposal of the metal or the concentration level of the metal in the environment (or the subject of similar environmental regulations in other jurisdictions).
  • fixation is the chemical reaction of a fixation reagent with a soluble metal to form a fixed metal compound that is less soluble than the soluble metal.
  • the fixation reaction produces an insoluble metal compound that is substantially insoluble in aqueous media.
  • the fixation reaction provides fixed metal compounds that are soluble at rates which make the solubilized metal available in the environment at concentrations below limits which are acceptable in accordance with prevailing environmental regulations, such as regulations promulgated from time-to-time by the U.S. EPA or similar agencies in other jurisdictions.
  • a "barrier” may be any means for physically separating soluble metals and fixation reagents, such as polymeric, metallic or vitreous members and equivalents thereof. Such barriers may be ruptured physically or chemically so that they break down to expose fixation reagents to soluble metals. In some embodiments, barriers may be adapted to rupture when an apparatus is crushed. Alternatively, an actuator may be provided on an apparatus for rupturing a barrier in the apparatus automatically or manually. Alternatively, the barrier may be rupturable by degradation over time, for example biodegradable barriers may be provided that are susceptible to decay after an article is disposed of.
  • a "fixation reagent container” may be any receptacle or means for retaining fixation reagents apart from the soluble metals with which they would otherwise react.
  • a "soluble metal container” may be any receptacle or means for retaining soluble metals apart from the fixation reagents with which they would otherwise react.
  • containers may include capsules and equivalent structures that enclose fixation reagents or soluble metals.
  • containers may include impregnated materials such as mats that may be impregnated or coated with fixation reagents or soluble metals, and equivalents thereof. In some embodiments, mats may be enclosed in capsules.
  • More than one container may be used in a particular apparatus.
  • capsules and mats may both be integrated into the construction of an apparatus.
  • Capsules may be rupturable by being breakable, degradable or dissolvable, or any other means of rupture, to facilitate release of fixation reagents or soluble metals at an appropriate time.
  • mats may be integrated into the construction of an apparatus in a manner that facilitates the occurrence of a fixation reaction between a fixation reagent and a soluble metal when a soluble metal is released from an apparatus in the vicinity of the mat.
  • fixation reagents may be used in particular embodiments of the present invention.
  • the specific reagents to be used in any given application may be selected by those skilled in the art of the invention depending upon the requirements of that application.
  • Different fixation reagents may be considered suitable from a technical point of view, and the factors that will determine which reagent is selected will include the solubility of fixed metal compounds that are formed by the reaction between the fixation reagent and the soluble metal, the stability of the fixation reagent over time under the relevant conditions in the apparatus, and other technical attributes affecting the suitability of the reagent for the specific application as understood by those skilled in the art, as well as the practical considerations of the availability of the reagent and cost.
  • Fixation systems that use relatively high dosages of reagents may not be suitable for certain applications, as higher dosages result in the use of more space in the apparatus .
  • fixation systems that may be used in accordance with various aspects of the present invention are described below. The following discussion is not intended to limit the type of fixation system or systems that may be utilized by the invention. In accordance with the present invention, those skilled in the art can evaluate alternative fixation systems and select a suitable fixation system for each application of the invention.
  • fixation reagents and systems that may be useful in various embodiments of the present invention are disclosed in: "Chemical fixation and solidification of hazardous wastes" J. R. Conner, Van Nostrand Remhold (1990); U.S. Patent No. 5,202,033 (Stanforth et al); U.S. Patent No. 5,527,982 (Pal et al); U.S. Patent No.
  • the reagents are selected on the basis of their ability to ameliorate the leaching of soluble metals from a specific type of apparatus by reacting with the soluble metal in the apparatus to form an fixed metal compound that is less soluble than the soluble metal compound.
  • the suitability of a fixation system may be routinely assayed using established protocols such as the U.S. EPA's TCLP or SPLP.
  • the control of pH may be used in accordance with the present invention to fix soluble metals.
  • Precipitation of solubilized metals as hydroxides may be accomplished by the use of calcium compounds such as quicklime (CaO) , hydrated lime (Ca(OH) 2 ) or carbonate (CaC0 3 ) ; magnesium compounds such as oxide (MgO) or hydroxide (Mg(OH) 2 ); or sodium compounds such as sodium hydroxide (NaOH) or sodium carbonate (Na 2 C0 3 ) .
  • CaO quicklime
  • Ca(OH) 2 hydrated lime
  • CaC0 3 carbonate
  • magnesium compounds such as oxide (MgO) or hydroxide (Mg(OH) 2 )
  • sodium compounds such as sodium hydroxide (NaOH) or sodium carbonate (Na 2 C0 3 ) .
  • metal hydroxides are amphoteric; that is, they are resolubilized at both high and low pHs .
  • hydroxide fixation reagents may be contraindicated where the soluble metal forms amphoteric hydroxides.
  • Dosage rates which are established based on passing the aggressive, low pH extraction fluid of the TCLP may result in failures when the less aggressive extraction fluid of the SPLP is applied. Accordingly, pH control may not be the best fixation method in certain circumstances. In some situations, it may be desirable to combine pH control with other fixation systems in order to obtain the most favourable results.
  • a neutralization reaction involving the fixation reagents in the case of acidic waste streams, may be extremely exothermic. This may present operational problems. The use of quicklime raises this concern, in that an exothermic slaking reaction contributes additional heat. Also, the use of a carbonate may release C0 2 , which could limit its acceptability in confined spaces (such as some of the battery applications noted below).
  • the base is a carbonate, such as calcium carbonate
  • the reaction of the base with an acidic solution of soluble metal may cause effervescence. An appropriate amount of such effervescence may facilitate the fixation reaction by improving the mixing of the fixation reagent with the soluble metal.
  • An alternative fixation process involves cementitious systems. Portland cement, high alumina cement, and other cements may be used as fixation reagents. Soluble silicates may be used in combination with Portland cement. The soluble metals present n the waste may be reacted to some extent to form insoluble silicates, or in the case of high alumina cement, aluminates. Such fixation reactions may produce a low porosity, hardened fixed metal product with high tortuosity, which in turn encapsulates the metals (whether reacted or not) .
  • Alkaline pHs are typical in the cementitious treated waste, as may be measured in the final extraction pH in the TCLP test, often in the optimal range for limiting solubility of the soluble metals.
  • the treated materials may pass the TCLP, due partially to the alkalinity of the treated waste, they may nevertheless fail the SPLP or leach high concentrations of amphoteric metals in the high pH condition which is associated with more normal disposal conditions.
  • Fairly high dosage rates of fixation reagents may be required, in the 10% to 25% range in some embodiments, by wet weight of waste.
  • byproducts from such processes as cement or lime production, coal combustion and the like may be utilized as a replacement or partial replacement for cement in fixation processes of the invention that are similar in nature to cement fixation systems.
  • Such byproducts include, among others, cement kiln dust, lime kiln dust, various types of coal fly ashes, and silica fume.
  • Byproducts may be combined with Portland cement in some applications. Generally, the usefulness and limitations of these systems are similar to the Portland cement systems, but higher dosages of the byproducts may be required.
  • Oxidation or reduction reactions may play a part in fixation systems of the invention.
  • Certain metals have solubility and toxicity concerns related to the valance state of the metal.
  • Cr +fc compounds are generally highly soluble and very toxic, whereas CO compounds generally are not.
  • As +3 compounds are generally more toxic, and may be more soluble depending on the fixation system used, than As +5 compounds. Therefore it is important to consider the possible need or utility of an oxidation or reduction treatment step as a part of the fixation regimen of the invention.
  • Common oxidizers that may be used in accordance with this aspect of the invention include permanganate, hypochlorite, peroxide and chemical equivalents thereof.
  • Common reducers include ferrous sulfate, sodium sulfites, various sulfides and equivalents thereof (aspects of which are discussed below in Example 3) .
  • pH adjustments may be used to enhance the oxidation or reduction step of a fixation system.
  • fixation systems which incorporate appropriate oxidation or reduction reactions.
  • sulfide reagents can be used for reduction and precipitation of hexavalent chromium.
  • Sulfide precipitation systems may be used in accordance with the present invention. Both soluble and relatively insoluble sulfide reagents may be used, at very low dosage rates in some embodiments, to react with metallic compounds in waste and precipitate the metals as sulfides. Most metal sulfides have extremely low solubilities over a wider range of pH than the corresponding oxides or hydroxides and they may therefore be more effective than cement-based systems in preventing solubilized metal releases into the environment. However, in some embodiments, there may be concerns that sulfide treatment may release HS, a toxic gas, during treatment. Also, fixed metal sulfides may resolubilize under oxidizing conditions.
  • an absorbent mat may be provided comprising a hydrophilic fibrous material having incorporated therein as a fixation reagent a reactive metal sulfide, the reactive metal sulfide being capable of reacting with a soluble metal to form a fixed metal compound that is less soluble than the soluble metal.
  • the mat may comprise a cellulosic material having zinc sulfide incorporated therein, such as is disclosed in U.S. Patent No. 4,280,925 issued to Kiefer 28 July 1981, which is incorporated herein by reference.
  • Phosphate precipitation systems may also be used in accordance with the present invention to fix soluble metals as phosphates.
  • Soluble and relatively insoluble phosphate reagents may be used.
  • orthophosphates may be preferred.
  • these systems may advantageously be used in an alkaline environment, often with the addition of an alkaline additive, and may, for example, be effective in reducing the leaching of solubilized lead, zinc, cadmium, and copper from wastes.
  • relatively low dosage rates may be required, in some embodiments in the range of 5% to 10% phosphate by weight of soluble metal waste, in combination with 5% to 10% alkaline reagent by weight of waste. Resolubilization of metal phosphates in acid conditions may be a concern, and some metal phosphates may also resolubilize at high pHs .
  • a combination of sulfide and phosphate precipitation may be used as another aspect of the present invention.
  • Combinations of sulfide and phosphate reagents may be effective for reducing the leaching of soluble metals over a wide range of pH conditions.
  • the addition of the phosphates may prevent oxidation of the fixed metal sulfide compounds, providing long term stability for the fixed metal sulfide reaction products.
  • Such sulfide and phosphate fixation reagents are, for example, the subject of copending, commonly owned U.S.
  • Patent Applications 08/823,627 and 08/705,794, incorporated herein by reference (and may be available under the trade name Molecular Bonding SystemTM (MBSTM) from Solucorp Industries of West Nyack, New York) .
  • MBSTM Molecular Bonding SystemTM
  • Very low dosage rates of phosphate and sulfide may be required, in the range of 2% to 6% total dry reagent weight as a percentage of the total soluble metal waste wet weight, in some embodiments.
  • sorbents may also be used as fixation reagents in the present invention. Such sorbents may be used in combination with other fixation reagents, to capture and fix soluble metals. In some embodiments, this approach involves the sorption of soluble metal compounds into the interior or onto the surface of the absorbing or adsorbing material. Fixation reagents may subsequently be added to the sorbed metals.
  • Materials that may be used as sorbents include activated carbon; metal oxides; synthetic materials such as activated alumina, organic polymers, zeolites and equivalents thereof; natural materials such as clays
  • diatomaceous earth with or without modification
  • peat moss peat moss
  • vermiculite vermiculite
  • natural zeolites and equivalents thereof.
  • the fixation reagents may be novel or selected from reagents known in the art, such as those discussed above, and equivalents thereof, so that the fixation reaction will occur within the specific apparatus, or in the vicinity of that apparatus, resulting in the amelioration of migration of solubilized metals from the apparatus into the environment.
  • the system that is selected for each application will preferably provide an appropriate type and quantity of reagents to effectively prevent release of soluble metals from the apparatus of the invention.
  • lead-acid battery generally refers to a secondary storage battery in which the electrodes comprise lead, and the electrolyte comprises diluted sulfuric acid.
  • a major use of lead- acid batteries is in vehicle starting applications. Most vehicles use a 12-volt battery with a capacity in the range of 40-60 Ah.
  • a typical battery weighs about 14.5 Kg or 32 lb, and has a sufficient high-rate capacity to deliver the 450-650A necessary to start an automobile engine. Approximately 60% of the battery's weight is lead or lead components.
  • a lead-acid battery is typically comprised of multiple cells, typically six cells in an automotive battery, with each individual cell containing lead plates and sulfuric acid.
  • Soluble lead waste may be released from a lead-acid battery as a result of breakage, spillage or leakage from the battery.
  • Such lead waste may be produced within the battery via a sulfation process in which lead sulfate is produced on the positive and/or negative plates of a lead-acid battery during discharge as the result of a chemical reaction between sulfuric acid and lead dioxide of the positive electrode, or between sulfuric acid and the metallic lead of the negative electrode.
  • a mat may be added to the outer casing of a lead-acid battery.
  • the mat may be made of absorbent material (such as hard cardboard, ceramic, natural or synthetic fabric, diatomaceous earth, vermiculite or equivalents thereof) selected so that it can absorb and retain fixation chemicals within its matrix.
  • fixation reagents for example, Molecular Bonding SystemTM (MBSTM) reagents
  • the mat may be placed inside the battery casing during its construction, in a manner that provides a guard against release of liquids from the bottom and sides of the battery in the event that the battery casing is cracked.
  • the mat may also be coated with a polymeric or alternative coating that is rupturable to expose the mat to the soluble metal.
  • casing mat 10 may be housed between inner battery casing 12 and outer battery casing 14.
  • Fixation reagents impregnating casing mat 10 may react with soluble metals that are released if cracks form in inner battery casing 12. Such cracks may for example occur during the removal, transport, handling or storage of a lead-acid battery.
  • Inner battery casing 12 thereby constitutes a rupturable barrier between the fixation reagents and the soluble metal housed in the battery.
  • Capsules 16 of fixation reagents may be used, as shown in the embodiment of Figure 1, either alone or in combination with casing mat 10. Capsules 16 containing fixation reagents may be housed in each cell 8 of lead-acid battery 6.
  • the barrier formed by the outer surface of capsule 16 may be adapted to maintain the integrity of the capsule during normal use of the battery, but to rupture and allow release of fixation reagents preferably after the useful life of the battery is complete.
  • Breakable capsule materials such as glass, plastic and equivalent materials may be used to facilitate the release of fixation reagents by breaking the capsule. Alternatively, other materials, such as polymers and gels, may be used that dissolve over time to release reagents.
  • release of the fixation reagents from capsules 16 may be activated manually or automatically in response to the lapse of time or a change in the condition of the battery, such as a pH change.
  • Capsules may be used to release fixation reagents that work to fix soluble metals and optionally to neutralize sulfuric acid or absorb free liquids in the battery.
  • capsule 16 comprising a neutralizing fixation reagent such as sodium hydroxide, calcium hydroxide or other neutralizing reagent may be positioned on wall 20 of each battery cell 8.
  • a neutralizing fixation reagent such as sodium hydroxide, calcium hydroxide or other neutralizing reagent
  • Capsule 16 be manually broken with plunger 18, preferably at the end of the useful life of the battery.
  • capsule 16 may be automatically ruptured by an actuated plunger (not shown) .
  • Plunger 18 may be actuated, for example, in response to a pH change in the battery which is monitored by a sensor (not shown) that triggers a plunger actuator (not shown) .
  • Capsules 16 may have an outer coating of glass, plastic or other equivalent breakable material that forms a breakable capsule.
  • Plunger 18 may slidmgly extend through a seal (not shown) in the top of the battery casings 12, 14.
  • a venting mechanism (not shown) may be included in casings 12, 14 to allow for the release of pressure that may build up within cells 8 when neutralizing fixation reagents are released from capsule 16 (such pressure build up may be due to the heat from an exothermic neutralization reaction) .
  • Capsule 16 may contain a sufficient amount of a neutralizing fixation reagent to bring the sulfuric acid solution in each cell 8 to a pH level between about 4 and about 9, and preferably near neutral. In a typical embodiment of a standard automobile battery where there are six cells, six capsules may be utilized.
  • the amount of neutralization reagent that is used in each cell 8 may be predetermined based on the size of the battery cells 8 and the strength of the sulfuric acid in the battery 6. In one embodiment of a typical 12-volt automotive battery, approximately V OZ. of sodium hydroxide, or an equivalent base, may be required in each cell 8. When capsule 16 is ruptured in the presence of a sulfuric acid solution, an exothermic reaction may occur while the solution is neutralized.
  • Cell mat 4 comprising fixation reagents may be provided along the bottom of each cell 8 (with or without alternative casing mat 10) .
  • Cell mat 4 may have a heat labile coating, so that an exothermic reaction caused by the release of neutralizing fixation reagents from capsule 16 will melt the coating of cell mat 4.
  • the heat labile coating of cell mat 4 constitutes a rupturable barrier between fixation reagents and a soluble metal.
  • such a coating may be polymeric, such as a heat sensitive or pH sensitive plastic coating.
  • polycarbonate plastics may be used as coatings in formulations that are acid resistant but have weak resistance at alkaline pHs .
  • capsule 16 may be dissolvable, adapted to automatically release neutralizing fixation reagents at some point in time, preferably near the end of the life of the battery.
  • an additional plunger may be provided for rupturing cell mat 4, or a single plunger may serve to rupture both capsule 16 and cell mat 4, the plunger being adapted to break capsule 16 first and then, with further actuation, to break open cell mat 4.
  • fixation reagents such as calcium sulfide, triple superphosphate, calcium carbonate and calcium hydroxide, in dry form, may be encapsulated in a breakable glass or polymeric material in a cell of the battery without a plunger.
  • the fixation reagents may remain in the capsule, in their solid form, until such time as the battery casing is crushed.
  • the casing and the container are ruptured and the soluble metal and the fixation reagents may react to form insoluble lead compounds, thereby immobilizing soluble lead ions present in the spent sulfuric acid, and also having the potential in some embodiments to form a reaction layer of lead sulfide on the surface of the remaining metallic lead of the battery electrode, to help prevent further solubilization of the lead.
  • An absorbent material may be included in alternative embodiments of capsules that may be adapted for neutralization of battery acid.
  • the absorbent may be vermiculite, diatomaceous earth, and equivalents thereof which would absorb the liquid in the battery.
  • Such absorbents may be used in combination with fixation reagents, including neutralizing fixation reagents.
  • capsule (s) containing fixation reagents may be positioned at or near the bottom of a cell(s) where they may be ruptured, preferably at the end of the useful life of the battery.
  • the capsules may contain a sufficient amount of fixation reagent to react with lead sulfate that has accumulated in the bottom of the battery during the battery's life.
  • the release of the fixation reagents may be triggered by the heat released from a neutralization reaction or a change in pH associated with a neutralization reaction triggered by the rupture of capsules as described above.
  • Capsules, mats or equivalent alternative containerization means for retaining fixation reagents known to those in the art may be utilized in various embodiments of the invention.
  • a capsule may be positioned on the bottom of each cell; the capsule including a highly absorbent material, a neutralizing fixation reagent, and additional metal stabilizing fixation reagent (s), such that the battery acid may be absorbed and neutralized and the soluble metals fixed when the capsule is ruptured.
  • the integrated fixation system of the invention offers dual protection against hazardous lead-acid contamination.
  • One mode of protection being a casing mat (as previously described) , which protects against the premature and accidental release of contamination through breakage of the casing of the lead-acid battery.
  • the other mode of protection being capsules or mats that are rupturable at an appropriate time to provide internal protection (preferably after the useful life of the battery) against spillage during handling, storage, recycling or illegal dumping.
  • Various embodiments may comprise multiple mats and capsules which will neutralize the battery's sulfuric acid solution and stabilize soluble metals. Absorbents may also be included in various embodiments of such mats and capsules to ameliorate fluid leakage.
  • Ni-Cd rechargeable battery generally refers to a secondary storage battery in which the positive electrode comprises primarily nickel hydroxide, in some embodiments as a coating over a sintered nickel substrate, and the negative electrode comprises cadmium, also over a sintered nickel substrate in some embodiments.
  • the electrolyte in a typical embodiment, is an alkaline compound such as potassium hydroxide or other hydroxide.
  • the electrolyte may be absorbed within a non-woven nylon or polypropylene fabric which serves as a separator between the electrodes. In a typical embodiment, no free electrolyte is present in the dry cell configuration.
  • a "jelly-roll" construction is typical in cylindrical cell embodiments, in which the positive electrode, separator and negative electrode are rolled up together and placed in a nickel- plated cylinder.
  • the cover which acts as the positive terminal is typically connected to the nickel-plated case, which acts as the negative terminal, with the incorporation of an insulating seal.
  • Figure 2 shows an embodiment of a cylindrical rechargeable Ni-Cd battery that incorporates these features.
  • Ni-Cd battery leakage may contain cadmium and nickel.
  • the leakage may also be alkaline. When batteries are left in equipment, the leaks can damage or ruin the equipment. Improper disposal of Ni-Cd batteries can result in leaching of cadmium and nickel from the metallic components of the battery into the environment.
  • a seal or insulating member of a Ni-Cd battery may be supplemented by the addition of a fixation reagent container.
  • the container may take the form of an O-ring, which is inserted between a seal member and the battery casing.
  • the O-ring may be made of an absorbent material that can absorb and retain fixation chemicals within its matrix.
  • the O-ring may be made of absorbent fiber which has been pretreated with sulfide or phosphate or combinations thereof with or without a base, as described in Example 3 herein.
  • a mat may be provided as an alternative or in addition to an O-ring.
  • Such a mat may be made of an absorbent material which has been impregnated with fixation reagents and coated to prevent premature release, or of a sandwich-type material, with the fixation ingredients in the middle of the sandwich. It would be positioned as a liner on the inside of the cylinder.
  • a rupturable barrier such as a polymeric or vitreous material, which material may be nonconductive.
  • the O-ring or mat may be coated with a thin plastic sheet, such as polyethylene.
  • a Ni-Cd AA battery may contain approximately 13 to 22% cadmium, 20 to 32% nickel, and 4% hydroxide.
  • An AA Ni- Cd battery may weigh about 26 grams. Accordingly, in such an example, approximately 5 grams of cadmium and 7 grams of nickel would be present. In order for this amount of cadmium and nickel to be fixed, about gram of fixation reagents may be provided in o-ring and/or mat containers.
  • fixation reagents may be suitable for use in a variety of containers in various Ni-Cd batteries.
  • the fixation reagents of the present invention may be a combination of a sulfide and phosphate, and optionally a base (sometimes referred to herein as the "MBSTM" reagents).
  • MBSTM a base
  • the present invention provides a process for treating soluble metals comprising:
  • a sulfide selected from the group consisting of calcium sulfide, calcium polysulfide, sodium sulfide, sodium hydrosulfide and iron sulfide,
  • an inorganic phosphate and (iii) a base, preferably including calcium hydroxide.
  • a base preferably including calcium hydroxide.
  • calcium sulfide is a preferred component of the fixation reagents.
  • Water may be provided in the apparatus, for example in the composition in the capsule.
  • the amount of water may be selected to adjust consistency of the fixation reagents at the time of reaction with the soluble metal so as to assist mass transfer.
  • the sulfide, phosphate or other reactive component of the fixation reagents may be provided in an amount optimized for approximately stoichiometric reaction with the soluble metal in the waste.
  • the sulfide may be used in an amount that is approximately the stoichiometic equivalent of the soluble metal in the apparatus.
  • the phosphate may be used in an amount that is approximately the stoichiometic equivalent of the soluble metal in the apparatus.
  • the sulfide and phosphate together may be used in an amount that is approximately the stoichiometic equivalent of the soluble metal in the apparatus.
  • the phosphate in the capsule composition may precipitate ferric iron that is present in the waste, so that the redox potential of the waste environment is rendered insufficient to oxidize the fixed sulfide metal compound.
  • orthophosphates are preferred phosphates in the fixation reagents.
  • preferred phosphates are calcium phosphate, phosphorus anhydride (P 2 0 5 ) , and triple super phosphate, alone or in combination.
  • a base may be provided as a component of the fixation reagents.
  • an amount of base is provided which is calculated to act rapidly to bring the initial pH of the soluble metal-containing mixture in the apparatus to above 8.0 when the barrier separating the fixation reagent and soluble metal is ruptured.
  • the base may comprise calcium carbonate or calcium hydroxide or both.
  • the base is preferably of small particle size.
  • the base component may be used in an amount sufficient to provide 2 or more times the amount of neutralization capability as there is acid generation potential in the sulfide used as a fixation reagent.
  • the amount of base may be adapted to suppress the generation of hydrogen sulfide gas from a sulfide fixation reagent.

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  • Processing Of Solid Wastes (AREA)

Abstract

L'invention concerne des barrières pouvant se rompre, placées entre des métaux solubles et des réactifs de fixation, constituant une partie de systèmes de fixation intégrés dans des appareils logeant des métaux solubles, pour réduire la libération dans l'environnement de métaux solubilisés. Les réactifs de fixation peuvent être contenus dans un contenant dont la surface comporte une barrière pouvant se rompre. Lorsque la barrière qui les sépare est rompue, les réactifs de fixation réagissent avec les métaux solubles pour former des composés métalliques moins solubles. Cela peut se produire lorsque les réactifs sont libérés d'un contenant ou mis en contact avec une autre substance quand ils se trouvent dans le contenant. Des appareils selon l'invention peuvent être différents types de piles, de commutateurs au mercure, de ballasts provenant de lampes fluorescentes, de plaquettes de circuits électroniques, de panneaux solaires usagés et analogues. Les contenants pour réactifs de fixation selon l'invention peuvent être des capsules, des mats imprégnés et analogues. Lesdits réactifs peuvent être des ciments, des sulfures, des phosphates, des tampons, des absorbants et analogues, se présentant sous la forme d'un liquide, d'une pâte ou d'un solide. Selon un aspect de la présente invention, le contenant est intégré lors de la production d'un appareil commercial, de sorte que les réactifs sont libérés ou mis en contact avec une substance lorsque la vie utile de l'appareil est terminée, soit pendant le stockage avant la mise au rebut de l'appareil, soit lors de la mise au rebut de l'appareil.
PCT/CA1998/001156 1997-12-19 1998-12-21 Systemes de fixation integres Ceased WO1999033137A1 (fr)

Priority Applications (7)

Application Number Priority Date Filing Date Title
AU16569/99A AU1656999A (en) 1997-12-19 1998-12-21 Integrated fixation systems
PCT/CA1999/000383 WO1999056867A2 (fr) 1998-05-06 1999-05-06 Systemes de fixation integres
CA2372985A CA2372985C (fr) 1998-05-06 1999-05-06 Systemes de fixation integres
EP99918998A EP1062035A1 (fr) 1998-05-06 1999-05-06 Systemes de fixation integres
EP20030078630 EP1435674A1 (fr) 1998-05-06 1999-05-06 Systèmes de fixation integrés
AU36954/99A AU3695499A (en) 1998-05-06 1999-05-06 Integrated fixation systems
US09/646,544 US6838504B1 (en) 1998-05-06 1999-05-06 Integrated fixation systems

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
CA2,225,367 1997-12-19
CA002225367A CA2225367A1 (fr) 1997-12-19 1997-12-19 Appareil de conteneurisation de metaux
US7277198A 1998-05-06 1998-05-06
US09/072,771 1998-05-06

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Cited By (3)

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EP1719563A1 (fr) * 2005-05-06 2006-11-08 AGILENT TECHNOLOGIES, INC. (A Delaware Corporation) Appareil contenant une matière toxique et méthode pour réduire la toxicité de la matière dans l'appareil
WO2023070546A1 (fr) * 2021-10-29 2023-05-04 宁德时代新能源科技股份有限公司 Dispositif à libération lente pour batterie, et batterie secondaire le comprenant
US12347894B2 (en) 2021-08-26 2025-07-01 Contemporary Amperex Technology (Hong Kong) Limited Tank, battery cell, battery, and electrical device

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EP1719563A1 (fr) * 2005-05-06 2006-11-08 AGILENT TECHNOLOGIES, INC. (A Delaware Corporation) Appareil contenant une matière toxique et méthode pour réduire la toxicité de la matière dans l'appareil
US12347894B2 (en) 2021-08-26 2025-07-01 Contemporary Amperex Technology (Hong Kong) Limited Tank, battery cell, battery, and electrical device
WO2023070546A1 (fr) * 2021-10-29 2023-05-04 宁德时代新能源科技股份有限公司 Dispositif à libération lente pour batterie, et batterie secondaire le comprenant

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