WO2021070230A1 - Plaque d'électrode positive, batterie de stockage au plomb et procédé de fabrication associé - Google Patents

Plaque d'électrode positive, batterie de stockage au plomb et procédé de fabrication associé Download PDF

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Publication number
WO2021070230A1
WO2021070230A1 PCT/JP2019/039529 JP2019039529W WO2021070230A1 WO 2021070230 A1 WO2021070230 A1 WO 2021070230A1 JP 2019039529 W JP2019039529 W JP 2019039529W WO 2021070230 A1 WO2021070230 A1 WO 2021070230A1
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WO
WIPO (PCT)
Prior art keywords
positive electrode
active material
electrode plate
fiber
electrode active
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Application number
PCT/JP2019/039529
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English (en)
Japanese (ja)
Inventor
祐一 利光
隆之 木村
素子 原田
Original Assignee
昭和電工マテリアルズ株式会社
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.)
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Application filed by 昭和電工マテリアルズ株式会社 filed Critical 昭和電工マテリアルズ株式会社
Priority to JP2021550961A priority Critical patent/JP7223870B2/ja
Priority to PCT/JP2019/039529 priority patent/WO2021070230A1/fr
Publication of WO2021070230A1 publication Critical patent/WO2021070230A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • H01M4/14—Electrodes for lead-acid accumulators
    • H01M4/16—Processes of manufacture
    • H01M4/20—Processes of manufacture of pasted 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

Definitions

  • the present invention relates to a positive electrode plate, a lead storage battery, and a method for manufacturing them.
  • Lead-acid batteries are widely used for industrial purposes, for example, as a battery for automobiles, a backup power source, and a main power source for electric vehicles.
  • the positive electrode in a lead storage battery is required to improve the utilization rate of the positive electrode active material held in the current collector.
  • a positive electrode having an excellent utilization rate of the positive electrode active material is used, for example, the amount of the positive electrode active material used to obtain a predetermined discharge capacity can be reduced, and as a result, the weight of the lead storage battery can be reduced.
  • Patent Document 1 in order to increase the utilization rate of the positive electrode active material, basic lead sulfate and graphite are added to the positive electrode active material, and phosphoric acid is 1% by mass or less in the electrolytic solution.
  • the contained lead-acid battery is disclosed.
  • an object of the present invention is to provide a positive electrode plate for a lead storage battery having an excellent utilization rate of a positive electrode active material, and a lead storage battery provided with the positive electrode plate.
  • One aspect of the present invention includes a positive electrode current collector and a positive electrode active material held by the positive electrode current collector, and the positive electrode active material shrinks irregularly and is represented by the following formula (1).
  • a positive electrode plate for a lead storage battery containing fibers having a ratio of 45% or more hereinafter, also referred to as “shrinkage fibers”).
  • Shrinkage rate (%) (yx) / yx100 ... (1) (In the formula, x represents the shortest distance from one end to the other end of the fiber, and y represents the length along the longitudinal direction of the fiber.)
  • Another aspect of the present invention includes a step of holding the positive electrode active material in the positive electrode current collector, and the positive electrode active material shrinks irregularly, and the shrinkage rate represented by the above formula (1) is 45%.
  • This is a method for manufacturing a positive electrode plate for a lead storage battery, which contains the above fibers.
  • the shrinkage rate may be 80% or less, and the fibers may contain polymer fibers.
  • Another aspect of the present invention is a lead-acid battery provided with the above-mentioned positive electrode plate.
  • Another aspect of the present invention is a lead-acid battery manufacturing method including a step of manufacturing a positive electrode plate by the above-mentioned manufacturing method and a step of assembling a lead-acid battery including the positive electrode plate.
  • a positive electrode plate for a lead storage battery having an excellent utilization rate of a positive electrode active material, and a lead storage battery provided with the positive electrode plate.
  • FIG. 1 It is a perspective view which shows the overall structure and the internal structure of the lead storage battery which concerns on one Embodiment. It is a perspective view which shows the electrode group of the lead storage battery shown in FIG. It is a schematic diagram which shows one Embodiment of a shrink fiber.
  • FIG. 1 is a perspective view showing the overall configuration and internal structure of the lead storage battery according to the embodiment.
  • the lead-acid battery 1 includes an electric tank 2 having an open upper surface and a lid 3 that closes the opening of the electric tank 2.
  • the battery case 2 and the lid 3 are made of polypropylene, for example.
  • the lid 3 is provided with a negative electrode terminal 4, a positive electrode terminal 5, and a liquid port plug 6 for closing the liquid injection port provided in the lid 3.
  • FIG. 2 is a perspective view showing the electrode group 7.
  • the electrode group 7 includes a negative electrode plate 9, a positive electrode plate 10, and a separator 11 arranged between the negative electrode plate 9 and the positive electrode plate 10.
  • the negative electrode plate 9 includes a negative electrode current collector (negative electrode lattice body) 12 and a negative electrode active material 13 held by the negative electrode current collector 12.
  • the positive electrode plate 10 includes a positive electrode current collector (positive electrode lattice body) 14 and a positive electrode active material 15 held by the positive electrode current collector 14.
  • negative electrode active material negative electrode active material
  • positive electrode plate after chemical conversion from which the positive electrode current collector is removed is referred to as "positive electrode active material”.
  • positive electrode active material the positive electrode plate after chemical conversion from which the positive electrode current collector is removed
  • the electrode group 7 has a structure in which a plurality of negative electrode plates 9 and positive electrode plates 10 are alternately laminated in a direction substantially parallel to the opening surface of the battery case 2 via a separator 11. That is, the negative electrode plate 9 and the positive electrode plate 10 are arranged so that their main surfaces extend in the direction perpendicular to the opening surface of the battery case 2.
  • the ears 12a of each of the negative electrode current collectors 12 in the plurality of negative electrode plates 9 are collectively welded by the negative electrode side strap 16.
  • the ears 14a of each of the positive electrode current collectors 14 of the plurality of positive electrode plates 10 are collectively welded by the positive electrode side strap 17.
  • the negative electrode side strap 16 and the positive electrode side strap 17 are connected to the negative electrode terminal 4 and the positive electrode terminal 5 via the negative electrode column 8 and the positive electrode column, respectively.
  • the separator 11 is formed in a bag shape, for example, and houses the negative electrode plate 9.
  • the separator 11 is made of, for example, polyethylene (PE), polypropylene (PP), or the like.
  • the separator 11 may have inorganic particles such as SiO 2 and Al 2 O 3 adhered to a woven fabric, a non-woven fabric, a porous film, or the like formed of these materials.
  • the negative electrode current collector 12 and the positive electrode current collector 14 are each made of a lead alloy.
  • the lead alloy may be an alloy containing tin, calcium, antimony, selenium, silver, bismuth and the like in addition to lead. Specifically, for example, an alloy containing lead, tin and calcium (Pb-Sn). -Ca-based alloy) may be used.
  • the negative electrode active material 13 contains at least Pb as a Pb component, and further contains a Pb component other than Pb (for example, PbSO 4) and an additive, if necessary.
  • the negative electrode active material 13 preferably contains porous spongy lead.
  • the content of the Pb component may be 90% by mass or more or 95% by mass or more, and may be 99% by mass or less or 98% by mass or less, based on the total mass of the negative electrode active material.
  • the total mass of the negative electrode active material is, for example, the mass of the negative electrode measured after the negative electrode (negative electrode current collector and negative electrode active material) is taken out from the lead storage battery, washed with water, and the negative electrode is sufficiently dried, and the negative electrode current collection. It can be calculated from the difference from the mass of the body. Drying is carried out, for example, at 50 ° C. for 24 hours.
  • additives include resins having a sulfo group and / or a sulfonic acid base, barium sulfate, carbon materials (excluding carbon fibers) and fibers (acrylic fibers, polyethylene fibers, polypropylene fibers, polyethylene terephthalate fibers, carbon fibers, etc.). Can be mentioned.
  • Resins having a sulfo group and / or a sulfonic acid base include lignin sulfonic acid, lignin sulfonate, and a condensate of phenols, aminoaryl sulfonic acid, and formaldehyde (for example, bisphenol, aminobenzene sulfonic acid, and formaldehyde). It may be at least one selected from the group consisting of condensates).
  • the carbon material include carbon black and graphite. Examples of carbon black include furnace black, channel black, acetylene black, thermal black and Ketjen black.
  • the positive electrode active material 15 contains PbO 2 which is a Pb component and shrink fibers.
  • the positive electrode active material 15 may further contain a Pb component (for example, PbSO 4 ) other than PbO 2 and an additive, if necessary.
  • the positive electrode active material 15 preferably contains ⁇ -PbO 2 as a Pb component.
  • the positive electrode active material 15 may further contain ⁇ -PbO 2 as a Pb component. That is, the positive electrode active material 15 may contain only ⁇ -PbO 2 as a Pb component in one embodiment, and contains ⁇ -PbO 2 and ⁇ -PbO 2 as Pb components in another embodiment. Good.
  • the content of the Pb component is preferably 90% by mass or more, more preferably 95% by mass or more, based on the total mass of the positive electrode active material, from the viewpoint of further improving the low temperature and high rate discharge performance and the cycle performance.
  • the content of the Pb component is preferably 99.9% by mass or less, more preferably 98% by mass or less, based on the total mass of the positive electrode active material, from the viewpoint of reducing the production cost and weight.
  • the total mass of the positive electrode active material is, for example, the mass of the positive electrode measured after taking out the positive electrode (positive electrode current collector and positive electrode active material) from the lead storage battery, washing the positive electrode with water, and sufficiently drying the positive electrode, and the positive electrode current collection. It can be calculated from the difference from the mass of the body. Drying is carried out, for example, at 50 ° C. for 24 hours.
  • FIG. 3 is a schematic diagram showing an embodiment of shrink fibers.
  • the shrink fiber 18 is irregularly shrunk.
  • the shrinking fibers 18 are different from the fibers that are regularly shrinking (for example, coiled (spiral) fibers).
  • the shape (shrinking method) of the shrinking fiber 18 is arbitrary as long as it satisfies the shrinkage rate described later.
  • the shrink fiber has a shrinkage rate of 45% or more.
  • the shrinkage ratio is expressed by the following formula (1).
  • Shrinkage rate (%) (yx) / yx100 ...
  • x represents the shortest distance from one end 18a of the shrinking fiber 18 to the other end 18b (the distance of a straight line connecting one end 18a and the other end 18b of the shrinking fiber 18).
  • y represents the length of the shrink fiber 18 along the longitudinal direction (the length of the shrink fiber 18 itself).
  • x and y can be calculated from the SEM image of the shrink fiber 18. For example, y can be calculated as the sum of the lengths of the plurality of straight lines by dividing the longitudinal direction of the shrinking fiber 18 and approximating it to a plurality of straight lines (for example, 10 straight lines).
  • the shrinkage rate of the shrink fiber 18 may be 50% or more, 55% or more, 60% or more, 65% or more, or 70% or more, and 80% or less, 75% or less, 70% or less, or 65% or less. It may be.
  • the shrinkage ratio of the shrinkage fiber 18 can be adjusted, for example, by applying a predetermined stress in the longitudinal direction of the fiber for a certain period of time. The greater the stress applied and the longer the stress is applied, the greater the shrinkage rate tends to be.
  • the shrinkage fiber 18 may contain, for example, a polymer fiber, a carbon fiber, or the like.
  • the polymer fiber include polyolefin fiber (fiber containing polyethylene, polypropylene, etc.), polyester fiber (fiber containing polyethylene terephthalate, etc.), and acrylic fiber (fiber containing polyacrylate, polymethacrylate, etc.).
  • the shrinkage fiber 18 preferably contains a polymer fiber, more preferably an acrylic fiber, from the viewpoint of obtaining excellent charge / discharge performance (charge acceptance performance, low temperature high rate discharge performance, etc.).
  • the content of the shrinkage fiber 18 is preferably 0.5% by mass or more, more preferably 1% by mass or more, still more preferably 1% by mass or more, based on the total mass of the positive electrode active material, from the viewpoint of further improving the utilization rate of the positive electrode active material. Is 2% by mass or more.
  • the content of the shrinkage fiber 18 is preferably 30% by mass or less, more preferably 20% by mass or less, still more preferably 10% by mass, based on the total mass of the positive electrode active material from the viewpoint of reducing the electrical resistance of the positive electrode plate. It is as follows.
  • Examples of the additive include carbon materials (excluding shrink fibers (carbon fibers)).
  • Examples of the carbon material include carbon black and graphite.
  • Examples of carbon black include furnace black, channel black, acetylene black, thermal black and Ketjen black.
  • the positive electrode active material 15 contains shrinkage fibers 18, an excellent utilization rate of the positive electrode active material can be obtained.
  • the reason for this is that the shrinkage fibers 18 adhere more strongly to the positive electrode current collector during aging and drying of the positive electrode plate than fibers having a small shrinkage rate (fibers that do not shrink relatively).
  • the present inventors speculate that this is because the electron conduction and the transfer of the electrolytic solution are preferably maintained by making the growth direction of PbSO 4 more uniform.
  • the lead-acid battery 1 described above includes, for example, a negative electrode plate manufacturing step for manufacturing a negative electrode plate, a positive electrode plate manufacturing step for manufacturing a positive electrode plate, and an assembly step for assembling the lead-acid battery 1 including the negative electrode plate and the positive electrode plate.
  • a negative electrode plate manufacturing step for manufacturing a negative electrode plate for manufacturing a negative electrode plate
  • a positive electrode plate manufacturing step for manufacturing a positive electrode plate for manufacturing a positive electrode plate
  • an assembly step for assembling the lead-acid battery 1 including the negative electrode plate and the positive electrode plate.
  • Manufactured by a manufacturing method The order of the negative electrode plate manufacturing process and the positive electrode plate manufacturing process is arbitrary.
  • the negative electrode current collector 12 holds the negative electrode active material 13. Specifically, first, the negative electrode current collector 12 holds the negative electrode active material paste, and the negative electrode active material paste is aged and dried to obtain an unchemicald negative electrode active material, and then the unchemicald negative electrode active material is obtained. To be formed.
  • the negative electrode active material paste contains, for example, lead powder, additives, solvent (for example, water or organic solvent) and sulfuric acid (for example, dilute sulfuric acid).
  • solvent for example, water or organic solvent
  • sulfuric acid for example, dilute sulfuric acid.
  • the negative electrode active material paste is obtained, for example, by mixing a lead powder and an additive to obtain a mixture, and then adding a solvent and sulfuric acid to the mixture and kneading the mixture.
  • the lead powder includes, for example, lead powder produced by a ball mill type lead powder manufacturing machine or a barton pot type lead powder manufacturing machine (in a ball mill type lead powder manufacturing machine, a mixture of powder of the main component PbO and scaly metal lead). ).
  • Aging may be carried out for 15 to 60 hours in an atmosphere having a temperature of 35 to 85 ° C. and a humidity of 50 to 98 RH%. Drying may be carried out at a temperature of 45 to 80 ° C. for 15 to 30 hours.
  • the positive electrode current collector 14 holds the positive electrode active material 15. Specifically, first, the positive electrode current collector 14 holds the positive electrode active material paste, and the positive electrode active material paste is aged and dried under the same conditions as in the negative electrode plate manufacturing process to obtain an unchemicald positive electrode active material. After obtaining, a non-chemical positive electrode active material is formed.
  • the positive electrode active material paste is, for example, the same lead powder as that used for the negative electrode active material paste, the above-mentioned shrink fibers, additives added as necessary, a solvent (for example, water or an organic solvent), and sulfuric acid (for example, rare). Sulfuric acid) is contained.
  • the positive electrode active material paste may further contain lead tan (Pb 3 O 4 ) from the viewpoint of shortening the chemical conversion time.
  • the negative electrode plate obtained in the negative electrode plate manufacturing process and the positive electrode plate obtained in the positive electrode plate manufacturing process are laminated via the separator 11, and the current collector of the electrode plates having the same polarity. Is welded with a strap to obtain a group of electrodes. This group of electrodes is arranged in an electric tank to produce an unchemical lead-acid battery. Next, dilute sulfuric acid is put into a non-chemical lead-acid battery, and a direct current is applied to form an electric tank. Subsequently, the lead storage battery 1 is obtained by adjusting the specific gravity (20 ° C.) of the sulfuric acid after chemical conversion to an appropriate specific gravity of the electrolytic solution.
  • the specific gravity (20 ° C.) of sulfuric acid used for chemical conversion may be 1.15 to 1.25.
  • the specific gravity (20 ° C.) of sulfuric acid after chemical conversion is preferably 1.25 to 1.33, more preferably 1.26 to 1.30.
  • the chemical conversion conditions and the specific gravity of sulfuric acid can be adjusted according to the size of the electrode plate.
  • the chemical conversion treatment may be carried out in the assembly process, or may be carried out in each of the negative electrode plate manufacturing process and the positive electrode plate manufacturing process (tank chemical conversion).
  • Example 1> Manufacturing of positive electrode plate
  • To 100 parts by mass of lead powder 2.2 parts by mass of acrylic fiber (shrinking fiber) having a shrinkage rate of 45% was added and mixed by a dry method.
  • 3 parts by mass of water was added to 100 parts by mass of the mixture composed of lead powder and shrink fibers, and 9 parts by mass of dilute sulfuric acid (specific gravity 1.28) was added stepwise and kneaded for 1 hour to activate the positive electrode.
  • a material paste was prepared.
  • An expanded positive electrode current collector produced by expanding a rolled sheet made of a lead alloy was filled with a positive electrode active material paste and then aged in an atmosphere of a temperature of 50 ° C. and a humidity of 98% for 24 hours. Then, it was dried at a temperature of 50 degreeC for 16 hours to obtain an unchemical positive electrode plate.
  • the expanded negative electrode current collector produced by expanding a rolled sheet made of a lead alloy was filled with this negative electrode active material paste and then aged in an atmosphere of a temperature of 50 ° C. and a humidity of 98% for 24 hours. Then, it was dried at a temperature of 50 degreeC for 16 hours to obtain an unchemical negative electrode plate.
  • Examples 2 to 5 and Comparative Example 1 In the production of the positive electrode plate, the positive electrode plate and the negative electrode plate were obtained in the same manner as in Example 1 except that the acrylic fibers having the shrinkage rate shown in Table 1 were used instead of the acrylic fibers (shrinkage fibers) having a shrinkage rate of 45%. And assembled the lead storage battery.
  • the theoretical capacity of the positive electrode active material is determined by "weight of lead oxide in the positive electrode (g) x 0.22 (Ah / g)".
  • 1 lead-acid battery, 9 ... negative electrode plate, 10 ... positive electrode plate, 11 ... separator, 12 ... negative electrode current collector, 13 ... negative electrode active material, 14 ... positive electrode current collector, 15 ... positive electrode active material.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

Un aspect de la présente invention est une plaque d'électrode positive pour une batterie de stockage au plomb. La plaque d'électrode positive comporte un collecteur d'électrode positive et un matériau actif d'électrode positive maintenu par le collecteur d'électrode positive. Le matériau actif d'électrode positive contient une fibre qui est rétractée irrégulièrement, le rapport de rétraction représenté par la formule (1) étant de 45 % ou plus.　(1) : Rapport de rétrécissement (%) = (y - x)/y × 100 (où x représente la plus petite distance à partir d'une extrémité à l'autre extrémité d'une fibre, et y représente la longueur de la fibre le long de la direction longitudinale).
PCT/JP2019/039529 2019-10-07 2019-10-07 Plaque d'électrode positive, batterie de stockage au plomb et procédé de fabrication associé WO2021070230A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2021550961A JP7223870B2 (ja) 2019-10-07 2019-10-07 正極板、鉛蓄電池及びそれらの製造方法
PCT/JP2019/039529 WO2021070230A1 (fr) 2019-10-07 2019-10-07 Plaque d'électrode positive, batterie de stockage au plomb et procédé de fabrication associé

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Application Number Priority Date Filing Date Title
PCT/JP2019/039529 WO2021070230A1 (fr) 2019-10-07 2019-10-07 Plaque d'électrode positive, batterie de stockage au plomb et procédé de fabrication associé

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4611223B1 (fr) * 1967-10-28 1971-03-22
JPS5253236A (en) * 1975-10-28 1977-04-28 Shin Kobe Electric Machinery Clad battery plate
JP2014049221A (ja) * 2012-08-30 2014-03-17 Gs Yuasa Corp 鉛蓄電池用極板及び鉛蓄電池

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4611223B1 (fr) * 1967-10-28 1971-03-22
JPS5253236A (en) * 1975-10-28 1977-04-28 Shin Kobe Electric Machinery Clad battery plate
JP2014049221A (ja) * 2012-08-30 2014-03-17 Gs Yuasa Corp 鉛蓄電池用極板及び鉛蓄電池

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JPWO2021070230A1 (fr) 2021-04-15
JP7223870B2 (ja) 2023-02-16

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