JP2004199950A - Manufacturing method of positive electrode plate for lead-acid storage battery - Google Patents

Manufacturing method of positive electrode plate for lead-acid storage battery Download PDF

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Publication number
JP2004199950A
JP2004199950A JP2002365437A JP2002365437A JP2004199950A JP 2004199950 A JP2004199950 A JP 2004199950A JP 2002365437 A JP2002365437 A JP 2002365437A JP 2002365437 A JP2002365437 A JP 2002365437A JP 2004199950 A JP2004199950 A JP 2004199950A
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Prior art keywords
lead
positive electrode
electrode plate
slurry
paste
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JP2002365437A
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Japanese (ja)
Inventor
Keiichi Wada
圭一 和田
Takafumi Kondo
隆文 近藤
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Resonac Corp
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Shin Kobe Electric Machinery Co Ltd
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Priority to JP2002365437A priority Critical patent/JP2004199950A/en
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    • 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

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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method of manufacturing a positive electrode plate for a lead storage battery without damaging chemical conversion efficiency and battery characteristics although a red lead is used. <P>SOLUTION: A positive electrode paste is manufactured by supplying the red lead and diluted sulfuric acid in a kneading mixer, and manufacturing a red lead slurry containing lead dioxide by kneading the red lead and the sulfuric acid, and drying the red lead slurry, and supplying the red lead slurry to the paste kneading device together with lead powder and kneading them. <P>COPYRIGHT: (C)2004,JPO&NCIPI

Description

【０００１】
【発明の属する技術分野】
本発明は、鉛丹を用いた鉛蓄電池用正極板の製造方法に関するものである。
【０００２】
【従来の技術】
鉛丹を用いた正極板の製造では、鉛丹と希硫酸を混合した鉛丹スラリーを鉛粉と共にペースト練合機に供給し、該ペースト練合機で作られた正極ペーストが用いられていた（例えば、特許文献１参照。）。
【０００３】
【特許文献１】
特開平５−１３０７４号公報
【０００４】
【発明が解決しようとする課題】
しかしながら、ペースト練合機中で鉛丹スラリーと鉛粉が接触すると、鉛丹スラリー中にある硫酸鉛と鉛粉が反応して三塩基性硫酸鉛の皮膜が鉛丹スラリーの周囲に形成される。このことにより直径約１ｍｍ以上の鉛丹スラリーの凝集粒子が正極ペースト中に存在することになる。この正極ペーストを用いて未化成正極板を完成させると、未化成活物質中に凝集した鉛丹スラリーが局部的に存在し、鉛丹スラリーの分布が不均一な未化成正極板ができあがる。このことは化成効率、電池製造に悪影響を及ぼす問題点がある。
【０００５】
従来の鉛丹を用いた正極板の製造方法では、化成効率、電池性能を損なうことなく製造するのは難しかった。
【０００６】
本発明の目的は、鉛丹を用いているにも拘らず、化成効率、電池性能を損なわないで製造できる鉛蓄電池用正極板の製造方法を提供することにある。
【０００７】
【課題を解決するための手段】
上記の目的を達成するため本発明は、正極ペーストを格子体に充填し、熟成、乾燥して製造する鉛蓄電池用正極板の製造方法において、
正極ペーストの製造は、鉛丹及び希硫酸を混練ミキサーに供給し、両者を混合して二酸化鉛を含む鉛丹スラリーを製造し、該鉛丹スラリーを乾燥させ、その後、鉛粉と共にペースト練合機に供給し、混練して行うことを特徴とする。
【０００８】
本発明では、鉛丹スラリーの製造後、この鉛丹スラリーを乾燥することで、鉛粉との接触時に三塩基性硫酸鉛の皮膜を形成しないようにする。このことにより、従来のように凝集した鉛丹スラリーが局部的に存在することがなくなり、正極未化成活物質中の鉛丹スラリーの分散を均一にすることができる。
【０００９】
鉛丹スラリーが均一に分散した正極板は、充電が均一にはいるため、より効率よく充電が完成する。また、鉛丹スラリー中の鉛丹が均一に分散するため、鉛丹の特徴である充放電サイクル中の活物質の脱落の影響を最小限に抑え、寿命サイクルに強い正極板を得ることができる。
【００１０】
【発明の実施の形態】
以下、本発明の実施の形態の各例を比較例と共に説明する。
【００１１】
（比較例１）
比較例１の鉛蓄電池は、次のようにして製造した。
【００１２】
正極板を、次のようにして作った。まず、鉛丹１５ｋｇと希硫酸（比重１．２６：２０℃）１１０Ｌ（リットル）を混練ミキサー中に投入し、鉛丹スラリーを作った。この鉛丹スラリーと鉛粉８５０ｋｇをペースト練合機に投入し、１００Ｌの水とを混練して正極活物質ペーストを作った。次に、この正極活物質ペースト１００ｇをカルシウム合金の格子体からなる集電体に充填してから、温度５０℃、湿度９５％中に１８時間放置して熟成した後に、温度１１０℃中に２時間放置して乾燥して未化成正極板を作った。
【００１３】
次に、負極板を、次のようにして作った。まず、鉛粉と、該鉛粉に対して１５質量％の希硫酸（比重１．２６：２０℃）と、該鉛粉に対して１２質量％の水とを混練して負極活物質ペーストを作った。次に、この負極活物質ペースト８０ｇをカルシウム合金の格子体からなる集電体に充填してから、温度５０℃、湿度９５％中に１８時間放置して熟成した後に、湿度１１０℃中に２時間放置して乾燥して未化成負極板を作った。
【００１４】
次に、未化成負極板８枚と未化成正極板７枚とをセパレータを介して交互に積層して各極板群を作った。
【００１５】
次に化成を、次のようにして行った。２５℃の雰囲気で２２．５Ａ、１２時間の定電流で充電を行った。充電に用いた硫酸の比重はｓ．ｇ．１．２４０とし、各セルに７００ｍｌ注入した。
【００１６】
以上の手順により、定格電圧１２Ｖ、定格容量（５時間率容量）５５Ａｈである、比較例１の自動車用鉛蓄電池８０Ｄ２６（ＪＩＳＤ５３０１記載）を完成した。
【００１７】
（実施の形態１）
実施の形態１の鉛蓄電池は、次のようにして製造した。
【００１８】
正極板を、次のようにして作った。まず、鉛丹１５ｋｇと希硫酸（比重１．２６：２０℃）１１０Ｌを混練ミキサー中に投入し、鉛丹スラリーを作った。この鉛丹スラリーを１１０℃の雰囲気に６時間放置し、水分を飛ばした。乾燥した鉛丹スラリーと鉛粉８５０ｋｇをペースト練合機に投入し、２００Ｌの水とを混練して正極活物質ペーストを作った。次に、この正極活物質ペースト１００ｇをカルシウム合金からなる格子体に充填してから、温度５０℃、湿度９５％中に１８時間放置して熟成した後に、温度１１０℃中に２時間放置して乾燥して未化成正極板を作った。
【００１９】
次に負極板を、次のようにして作った。まず、鉛粉と、該鉛粉に対して１５質量％の希硫酸（比重１．２６：２０℃）と、該鉛粉に対して１２質量％の水とを混練して負極活物質ペーストを作った。次に、この負極活物質ペースト８０ｇをカルシウム合金の格子体からなる集電体に充填してから、温度５０℃、湿度９５％中に１８時間放置して熟成した後に、温度１１０℃中に２時間放置して乾燥して未化成負極板を作った。
【００２０】
次に、未化成負極板８枚と未化成正極板７枚とをセパレータを介して交互に積層して各極板群を作った。
【００２１】
次に化成を、次のようにして行った。２５℃の雰囲気で２２．５Ａ、９時間の定電流で充電を行った。充電に用いた硫酸の比重はｓ．ｇ．１．２５０とし、各セルに７００ｍｌ注入した。
【００２２】
以上の手順により、定格電圧１２Ｖ、定格容量（５時間率容量）５５Ａｈである、実施の形態１の自動車用鉛蓄電池８０Ｄ２６（ＪＩＳＤ５３０１記載）を完成した。
【００２３】
図１は、比較例１と実施の形態１の充電時間を変えたときの正極活物質中に存在する残存硫酸鉛量の変化を示した。
【００２４】
比較例１は、約１２時間以上で残存硫酸鉛量の変化がなくなり、充電が完了したと言える。このことから比較例１は、上記に示したように充電時間を１２時間とした。
【００２５】
実施の形態１は、約９時間以上で残存硫酸鉛量の変化がなくなり、充電が完了したと言える。このことから実施の形態１は、上記に示したように充電時間を９時間とした。
【００２６】
図１から分かるように実施の形態１は鉛丹の分散性が均一であることから、比較例１に比べ充電性が良く、充電時間を短くすることができた。
【００２７】
図２は、重負荷寿命試験のサイクル容量変化を示した。試験条件は、４０℃の周囲温度で２０Ａ、１時間放電した後に、５Ａで５時間充電する充放電を１サイクルとして充放電を繰り返し、２５サイクル毎に２０Ａで端子電圧が１０．２Ｖになるまで連続放電を行い、放電持続時間を測定した。寿命サイクル数は、容量が５時間率容量の半分、即ち２２．５Ａｈとなる回数とした。
【００２８】
比較例１に比べ実施の形態１は、サイクル後半の容量低下が少なく、寿命判定容量を切るまでのサイクル数が多かった。このことからサイクル特性についても実施の形態１は大きな効果が得られた。
【００２９】
【発明の効果】
本発明に係る鉛蓄電池用正極板の製造方法では、鉛丹スラリーの製造後、この鉛丹スラリーを乾燥することで、鉛粉との接触時に三塩基性硫酸鉛の皮膜を形成しないようにし、このことにより正極未化成活物質中の鉛丹スラリーの分散を均一にすることができる。
【００３０】
鉛丹スラリーが均一に分散した正極板は、充電が均一にはいるため、より効率よく充電が完成する。また、鉛丹スラリー中の鉛丹が均一に分散するため、鉛丹の特徴である充放電サイクル中の活物質の脱落の影響を最小限に抑え、寿命サイクルに強い正極板を得ることができる。
【図面の簡単な説明】
【図１】比較例１と実施の形態１の鉛蓄電池の充電時間と残存硫酸鉛量の変化を示す図である。
【図２】比較例１と実施の形態１の鉛蓄電池の重負荷寿命試験における容量変化を示す図である。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method for manufacturing a positive electrode plate for a lead storage battery using lead tin.
[0002]
[Prior art]
In the production of a positive electrode plate using lead ginseng, a lead grit mixed with lead ginseng and dilute sulfuric acid was supplied to a paste kneading machine together with lead powder, and a positive electrode paste produced by the paste kneading machine was used. (For example, refer to Patent Document 1).
[0003]
[Patent Document 1]
JP-A-5-13074
[Problems to be solved by the invention]
However, when the lead-tan slurry and the lead powder come into contact in the paste kneading machine, the lead sulfate and lead powder in the lead-tan slurry react with each other to form a tribasic lead sulfate film around the lead-tan slurry. . As a result, agglomerated particles of the lead tin slurry having a diameter of about 1 mm or more are present in the positive electrode paste. When a non-chemically formed positive electrode plate is completed using this positive electrode paste, a non-chemically formed positive electrode plate is obtained in which the lead-iron slurry is locally present in the non-chemically-formed active material and the distribution of the lead-iron slurry is not uniform. This has a problem of adversely affecting the formation efficiency and battery production.
[0005]
With the conventional method of manufacturing a positive electrode plate using lead tin, it has been difficult to manufacture without impairing the chemical conversion efficiency and battery performance.
[0006]
An object of the present invention is to provide a method for producing a positive electrode plate for a lead-acid battery, which can be produced without impairing the chemical conversion efficiency and the battery performance despite using lead tin.
[0007]
[Means for Solving the Problems]
In order to achieve the above object, the present invention provides a method for producing a positive electrode plate for a lead-acid battery, which is prepared by filling a grid body with a positive electrode paste, aging, and drying.
In the production of the positive electrode paste, leadtan and dilute sulfuric acid are supplied to a kneading mixer, the two are mixed to produce a leadtan slurry containing lead dioxide, the leadtan slurry is dried, and then paste kneading with lead powder is performed. It is supplied to a kneader and kneaded.
[0008]
In the present invention, the lead-tan slurry is dried after production of the lead-tan slurry, so that a tribasic lead sulfate film is not formed at the time of contact with the lead powder. This eliminates the local presence of the agglomerated lead-tan slurry as in the prior art, making it possible to make the dispersion of the lead-tan slurry in the positive electrode unformed active material uniform.
[0009]
The positive electrode plate in which the lead-tin slurry is uniformly dispersed allows charging to be completed more efficiently because charging is uniform. In addition, since the red lead in the red lead slurry is uniformly dispersed, the effect of the active material falling off during the charge / discharge cycle, which is a characteristic of lead red, can be minimized, and a positive electrode plate that is strong in the life cycle can be obtained. .
[0010]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, examples of the embodiment of the present invention will be described together with comparative examples.
[0011]
(Comparative Example 1)
The lead storage battery of Comparative Example 1 was manufactured as follows.
[0012]
A positive electrode plate was made as follows. First, 15 kg of red lead and 110 L (liter) of dilute sulfuric acid (specific gravity 1.26: 20 ° C.) were charged into a kneading mixer to prepare a lead red slurry. This lead-tan slurry and 850 kg of lead powder were put into a paste kneading machine, and kneaded with 100 L of water to prepare a positive electrode active material paste. Next, 100 g of this positive electrode active material paste was filled in a current collector made of a lattice of calcium alloy, left to stand at a temperature of 50 ° C. and a humidity of 95% for 18 hours, and aged at 110 ° C. It was left to dry for a period of time to produce an unformed positive electrode plate.
[0013]
Next, a negative electrode plate was produced as follows. First, lead powder, 15% by mass of dilute sulfuric acid (specific gravity 1.26: 20 ° C.) with respect to the lead powder, and 12% by mass of water with respect to the lead powder are kneaded to form a negative electrode active material paste. Had made. Next, 80 g of the negative electrode active material paste was filled in a current collector made of a lattice of calcium alloy, left to stand at a temperature of 50 ° C. and a humidity of 95% for 18 hours, and then aged at 110 ° C. It was left to dry for a period of time to produce an unformed negative electrode plate.
[0014]
Next, eight unformed negative electrode plates and seven unformed positive electrode plates were alternately laminated with a separator interposed therebetween to form each electrode group.
[0015]
Next, chemical conversion was performed as follows. The battery was charged in a 25 ° C. atmosphere at a constant current of 22.5 A for 12 hours. The specific gravity of the sulfuric acid used for charging is s. g. It was 1.240, and 700 ml was injected into each cell.
[0016]
According to the above procedure, a lead-acid battery 80D26 (described in JISD5301) for a vehicle of Comparative Example 1 having a rated voltage of 12 V and a rated capacity (5 hour capacity) of 55 Ah was completed.
[0017]
(Embodiment 1)
The lead storage battery of the first embodiment was manufactured as follows.
[0018]
A positive electrode plate was made as follows. First, 15 kg of lead red and 110 L of dilute sulfuric acid (specific gravity: 1.26: 20 ° C.) were charged into a kneading mixer to prepare a lead red slurry. This lead-tan slurry was left in an atmosphere of 110 ° C. for 6 hours to remove moisture. The dried lead red slurry and 850 kg of lead powder were put into a paste kneading machine and kneaded with 200 L of water to prepare a positive electrode active material paste. Next, 100 g of this positive electrode active material paste was filled in a lattice made of a calcium alloy, left to age at 50 ° C. and 95% humidity for 18 hours, and then left at 110 ° C. for 2 hours. It dried and the unformed positive electrode plate was produced.
[0019]
Next, a negative electrode plate was produced as follows. First, lead powder, 15% by mass of dilute sulfuric acid (specific gravity 1.26: 20 ° C.) with respect to the lead powder, and 12% by mass of water with respect to the lead powder are kneaded to form a negative electrode active material paste. Had made. Next, 80 g of the negative electrode active material paste was filled in a current collector made of a lattice of calcium alloy, left to stand at a temperature of 50 ° C. and a humidity of 95% for 18 hours, and aged at 110 ° C. It was left to dry for a period of time to produce an unformed negative electrode plate.
[0020]
Next, eight unformed negative electrode plates and seven unformed positive electrode plates were alternately laminated with a separator interposed therebetween to form each electrode group.
[0021]
Next, chemical conversion was performed as follows. The battery was charged at a constant current of 22.5 A and 9 hours in an atmosphere of 25 ° C. The specific gravity of the sulfuric acid used for charging is s. g. It was set to 1.250, and 700 ml was injected into each cell.
[0022]
By the above procedure, the lead-acid battery 80D26 (described in JISD5301) for the vehicle of Embodiment 1 having a rated voltage of 12 V and a rated capacity (5 hour rate capacity) of 55 Ah was completed.
[0023]
FIG. 1 shows a change in the amount of residual lead sulfate present in the positive electrode active material when the charging time of Comparative Example 1 and Embodiment 1 was changed.
[0024]
In Comparative Example 1, there was no change in the amount of residual lead sulfate after about 12 hours or more, and it can be said that charging was completed. For this reason, in Comparative Example 1, the charging time was set to 12 hours as described above.
[0025]
In the first embodiment, it can be said that the charge has been completed since the change in the amount of residual lead sulfate disappeared in about 9 hours or more. For this reason, Embodiment 1 sets the charging time to 9 hours as described above.
[0026]
As can be seen from FIG. 1, in the first embodiment, since the dispersibility of the red lead was uniform, the chargeability was better and the charge time was shorter than in Comparative Example 1.
[0027]
FIG. 2 shows the cycle capacity change of the heavy load life test. The test conditions are as follows: charge and discharge are repeated at a cycle of charging and discharging at 20 A at an ambient temperature of 40 ° C. and discharging at 20 A for 1 hour and then charging at 5 A for 5 hours until the terminal voltage becomes 10.2 V at 20 A every 25 cycles. Continuous discharge was performed, and the discharge duration was measured. The number of life cycles was the number of times when the capacity was half of the 5-hour rate capacity, that is, 22.5 Ah.
[0028]
In the first embodiment, compared to Comparative Example 1, the capacity decrease in the latter half of the cycle was small, and the number of cycles until the life determination capacity was cut off was large. From this, the first embodiment also has a great effect on the cycle characteristics.
[0029]
【The invention's effect】
In the method for manufacturing a positive electrode plate for a lead storage battery according to the present invention, after manufacturing the lead-tan slurry, by drying the lead-tan slurry, a tribasic lead sulfate film is not formed at the time of contact with lead powder, This makes it possible to make the dispersion of the lead tin slurry in the positive electrode unformed active material uniform.
[0030]
The positive electrode plate in which the lead-tin slurry is uniformly dispersed allows charging to be completed more efficiently because charging is uniform. In addition, since the red lead in the red lead slurry is uniformly dispersed, the effect of the active material falling off during the charge / discharge cycle, which is a characteristic of lead red, can be minimized, and a positive electrode plate that is strong in the life cycle can be obtained. .
[Brief description of the drawings]
FIG. 1 is a diagram showing changes in the charging time and the amount of residual lead sulfate of the lead storage batteries of Comparative Example 1 and Embodiment 1.
FIG. 2 is a diagram showing a change in capacity in a heavy load life test of the lead storage batteries of Comparative Example 1 and Embodiment 1.

Claims (1)

正極ペーストを格子体に充填し、熟成、乾燥して製造する鉛蓄電池用正極板の製造方法において、
前記正極ペーストの製造は、鉛丹及び希硫酸を混練ミキサーに供給し、両者を混合して二酸化鉛を含む鉛丹スラリーを製造し、該鉛丹スラリーを乾燥させ、その後、鉛粉と共にペースト練合機に供給し、混練して行うことを特徴とする鉛蓄電池用正極板の製造方法。Filling the grid with the positive electrode paste, aging, in a method of manufacturing a positive electrode plate for a lead storage battery manufactured by drying,
In the production of the positive electrode paste, lead red and dilute sulfuric acid are supplied to a kneading mixer, the two are mixed to produce a lead red slurry containing lead dioxide, the lead red slurry is dried, and thereafter, the paste is kneaded with lead powder. A method for producing a positive electrode plate for a lead-acid battery, wherein the positive electrode plate is supplied to a joint machine and kneaded.
JP2002365437A 2002-12-17 2002-12-17 Manufacturing method of positive electrode plate for lead-acid storage battery Pending JP2004199950A (en)

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