JP2006196191A - Lead acid battery - Google Patents
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- JP2006196191A JP2006196191A JP2005003283A JP2005003283A JP2006196191A JP 2006196191 A JP2006196191 A JP 2006196191A JP 2005003283 A JP2005003283 A JP 2005003283A JP 2005003283 A JP2005003283 A JP 2005003283A JP 2006196191 A JP2006196191 A JP 2006196191A
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- 239000002253 acid Substances 0.000 title claims abstract description 10
- 229920005610 lignin Polymers 0.000 claims abstract description 39
- 239000006229 carbon black Substances 0.000 claims abstract description 9
- 239000007773 negative electrode material Substances 0.000 claims abstract description 7
- 229930185605 Bisphenol Natural products 0.000 claims abstract description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims abstract description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000295 fuel oil Substances 0.000 claims abstract description 3
- 229920000642 polymer Polymers 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- 239000000654 additive Substances 0.000 claims description 8
- 230000000996 additive effect Effects 0.000 claims description 5
- 239000011149 active material Substances 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 3
- ZAJAQTYSTDTMCU-UHFFFAOYSA-N 3-aminobenzenesulfonic acid Chemical compound NC1=CC=CC(S(O)(=O)=O)=C1 ZAJAQTYSTDTMCU-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- -1 acetylene black Chemical compound 0.000 description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- UYTPUPDQBNUYGX-UHFFFAOYSA-N guanine Chemical compound O=C1NC(N)=NC2=C1N=CN2 UYTPUPDQBNUYGX-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000002003 electrode paste Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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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- Battery Electrode And Active Subsutance (AREA)
Abstract
【課題】頻繁なエンジン始動と停止が繰り返されるような使用形態でも充電性が不足する事態が発生することのない自動車用液式鉛蓄電池を作製する。
【解決手段】鉛蓄電池の負極活物質に、分子量約１.７〜２.０万の合成リグニン（ビスフェノールスルホン酸ポリマー縮合物）を活物質量に対して０.２〜０.６wt％と、比表面積が１５０〜３００m2／gの重油を原料としたカーボンブラックを活物質量に対して０.２２〜１.２８wt％同時に添加する。
【選択図】図２A liquid lead-acid battery for an automobile that does not cause a situation in which chargeability is insufficient even when the engine is frequently started and stopped is produced.
SOLUTION: A synthetic lignin (bisphenol sulfonic acid polymer condensate) having a molecular weight of about 1.7 to 2 million is added to a negative electrode active material of a lead-acid battery in an amount of 0.2 to 0.6 wt% based on the amount of the active material. Carbon black using heavy oil having a specific surface area of 150 to 300 m 2 / g as a raw material is simultaneously added in an amount of 0.22 to 1.28 wt% based on the amount of active material.
[Selection] Figure 2
Description
本発明は鉛蓄電池の充電受入れ性向上に関するものである。 The present invention relates to an improvement in charge acceptance of a lead storage battery.
従来、鉛蓄電池の負極活物質には数種類の添加剤が添付されている。これらは錬合時に負極ペーストに添加され、リグニンは防縮剤として硫酸バリウムと併用して０.１〜０.４ｗｔ％程度添加されており、これらが負極活物質の凝集を抑えており、充放電の繰り返しによる性能の低下を抑制する。また、それ以外にもカーボンが０.１〜０.３wt％程度添加されており、充電時に電流効率を向上させている。リグニンは負極のサイクル寿命を向上させる効果があり、特許文献１に示されるような添加形態が提案されている。 Conventionally, several types of additives are attached to the negative electrode active material of a lead storage battery. These are added to the negative electrode paste at the time of smelting, and lignin is used in combination with barium sulfate as an anti-shrink agent, and is added in an amount of about 0.1 to 0.4 wt%, which suppresses the aggregation of the negative electrode active material, and is charged and discharged. Suppressing performance degradation due to repetition of. In addition, about 0.1 to 0.3 wt% of carbon is added to improve current efficiency during charging. Lignin has the effect of improving the cycle life of the negative electrode, and an additive form as shown in Patent Document 1 has been proposed.
天然物であるリグニンはその構造に複数の単位構造が複雑に結合した多種多様の構造を有しているため、上記リグニンは、通常カルボニル基等の酸化還元されやすい部分が存在する。そして、鉛蓄電池における充放電に際して、上記の部位は酸化又は還元され、ここにおいてリグニンは分解される。その結果、添加の効果が充放電の繰り返しにより低下する。負極添加剤として、従来使用されていたリグニンに代えて、構造的に類似した合成リグニンであるフェノール類・アミノベンゼンスルホン酸・ホルムアルデヒド縮合物を用いるものがあり、これは充放電で分解しにくく効果が長期間継続する。しかしながら合成リグニンも従来から使用されているカーボン、例えばアセチレンブラックとの組み合わせであると、近年普及してきたエンジン始動と停止が繰り返されるようないわゆるアイドリングストップ車（ISS車）のような使用形態では充電性が不足する事態が発生する。 Since lignin, which is a natural product, has a wide variety of structures in which a plurality of unit structures are complexly bonded to the structure, the lignin usually has a portion that is easily oxidized and reduced, such as a carbonyl group. And in the charge / discharge in a lead acid battery, said site | part is oxidized or reduced and lignin is decomposed | disassembled here. As a result, the effect of addition is reduced by repeated charge and discharge. Some negative electrode additives use structurally similar synthetic lignins, such as phenols, aminobenzenesulfonic acid, and formaldehyde condensates, instead of the conventionally used lignin. Continues for a long time. However, if synthetic lignin is also used in combination with conventional carbon, such as acetylene black, it is charged in the usage form such as the so-called idling stop car (ISS car) that has been repeatedly started and stopped in recent years. A situation that lacks gender occurs.
上記に示すような課題を解決するため本発明においては鉛蓄電池の負極活物質の添加剤に分子量約２万の合成リグニンを負極添加剤として、従来使用されていたリグニンに代えて、構造的に類似した合成重合物であるフェノール類・アミノベンゼンスルホン酸・ホルムアルデヒド縮合物と、比表面積が１５０〜３００m2／gのカーボンブラックを添加する。これにより従来の鉛蓄電池に比べて添加剤の効果が長期間維持され、なおかつ充電受入れ性の優れた鉛蓄電池を提供することができる。 In order to solve the problems as described above, in the present invention, synthetic lignin having a molecular weight of about 20,000 is used as the negative electrode additive in the negative electrode active material additive of the lead storage battery, instead of the conventionally used lignin, A similar synthetic polymer such as phenols, aminobenzenesulfonic acid and formaldehyde condensate, and carbon black having a specific surface area of 150 to 300 m 2 / g are added. Thereby, compared with the conventional lead acid battery, the effect of an additive can be maintained for a long time, and the lead acid battery excellent in charge acceptance can be provided.
本発明により鉛蓄電池の充電受入れ性が向上し、その結果、鉛蓄電池の寿命性能が向上する。 By this invention, the charge acceptance property of lead acid battery improves, As a result, the lifetime performance of lead acid battery improves.
以下、本発明の具体例について説明する。 Hereinafter, specific examples of the present invention will be described.
合成リグニンの分子量とカーボンの比表面積に着目して検討した。分子量が異なる各種リグニン（リグニンA、リグニンB、リグニンC、リグニンD）と各種カーボン（カーボンａ、ｂ、ｃ、ｄ、ｅ）の組み合わせによる充電受入れ性を評価した。なお、リグニンAは分子量約１.５万の合成リグニンであり、リグニンBは分子量が１.６万の合成リグニンであり、リグニンCは分子量約１.７万の合成リグニンであリ、グニンDは分子量約２万の合成リグニンである。なお、現在商業ベースで入手可能な合成リグニンの分子量の上限は約２万であるため、このリグニンが上限となる。 We examined the molecular weight of synthetic lignin and the specific surface area of carbon. The charge acceptability was evaluated by combining various lignins having different molecular weights (lignin A, lignin B, lignin C, lignin D) and various carbons (carbon a, b, c, d, e). Note that lignin A is a synthetic lignin having a molecular weight of about 15,000, lignin B is a synthetic lignin having a molecular weight of 16,000, lignin C is a synthetic lignin having a molecular weight of about 17,000, and guanine D. Is a synthetic lignin having a molecular weight of about 20,000. In addition, since the upper limit of the molecular weight of the synthetic lignin currently available on a commercial basis is about 20,000, this lignin is the upper limit.
カーボンaは比表面積が１３０ｇ／ｍ2であり、カーボンｂは比表面積が１５０ｇ／ｍ2であり、カーボンｃは比表面積が２３０ｇ／ｍ2であり、カーボンｄは比表面積が３００ｇ／ｍ2であり、カーボンeは比表面積が３３０ｇ／ｍ2である。なお、カーボンはそれぞれかさ密度が異なるので、体積一定として添加した。 Carbon a has a specific surface area of 130 g / m 2 , carbon b has a specific surface area of 150 g / m 2 , carbon c has a specific surface area of 230 g / m 2 , and carbon d has a specific surface area of 300 g / m 2 . The carbon e has a specific surface area of 330 g / m 2 . Since carbon has a different bulk density, carbon was added at a constant volume.
評価用電池としてＪＩＳ５５B２４サイズ相当の単電池（２V）を作成した。鉛粉１ｋｇを上記添加剤と乾式混合してペーストを厚さ０.９ｍｍのエキスパンド格子体（Ｃａ：０.０５％、Ｓｎ：０.５％、残部：Pb）に充填して通常の方法に従い、熟成、乾燥して負極板を得た。また、同じようにして正極板を作製した。これらの負極板、正極板およびポリエチレン多孔膜の通常のセパレータを用い、自動車用液式電池を作成した。この電池に通常の方法により比重１.２００の希硫酸を適量注入し、２５℃の水槽に静置した状態で７.２Aで４０時間通電後、比重を１.２８に調整して充電済みの電池とした。 A single cell (2 V) corresponding to JIS55B24 size was prepared as an evaluation battery. 1 kg of lead powder is dry-mixed with the above additives, and the paste is filled in an expanded lattice (Ca: 0.05%, Sn: 0.5%, balance: Pb) with a thickness of 0.9 mm, according to the usual method. Aged and dried to obtain a negative electrode plate. A positive electrode plate was produced in the same manner. Using these negative electrode plates, positive electrode plates, and ordinary separators of polyethylene porous membranes, liquid batteries for automobiles were prepared. A proper amount of diluted sulfuric acid with a specific gravity of 1.200 was injected into this battery by a normal method, and after charging for 40 hours at 7.2 A while standing in a water bath at 25 ° C., the specific gravity was adjusted to 1.28 and charged. A battery was obtained.
試験方法は以下の通りである。作成した電池を２５℃の空気中に６時間放置した後０.２Cで１時間定電流放電し、充電状態８０%に調整した。その後、電源を用いて３Cの定電流充電して充電開始後５秒目の端子電圧で評価した。なお、３Cの電流値は１８Aであり、この時の温度は２５℃である。充電受入れ５秒目電圧とは３C電流で充電を開始してから5秒目の電圧値を指し、この電圧値が低いほど充電電流が入りやすく、充電受入れ性が良いと言える。また、添加量は合成リグニンが０.４wt％、カーボンブラックが０.７ wt％である。 The test method is as follows. The prepared battery was left in air at 25 ° C. for 6 hours and then discharged at a constant current of 0.2 C for 1 hour to adjust the charged state to 80%. Thereafter, the battery was charged with a constant current of 3 C using a power source, and the terminal voltage at 5 seconds after the start of charging was evaluated. The current value of 3C is 18A, and the temperature at this time is 25 ° C. The charge acceptance 5 second voltage refers to the voltage value at 5 seconds after the start of charging at 3 C current. The lower this voltage value, the easier the charge current can enter and the better the charge acceptance. The addition amounts are 0.4 wt% for synthetic lignin and 0.7 wt% for carbon black.
図１に結果を示す。５秒目電圧の最も低い組み合わせの分子量が１.７万〜２.０万の合成リグニンと比表面積が１５０〜３００ｇ／ｍ2のカーボンブラックであり、従来から使用されているアセチレン熱分解によるアセチレンブラックと従来からよく使用されている天然リグニン（分子量７０００〜１万）よりも低かった。 The results are shown in FIG. Synthetic lignin with a molecular weight of 17,000 to 20000 and carbon black with a specific surface area of 150 to 300 g / m 2 , and the acetylene obtained by thermal decomposition of acetylene that has been used in the past. It was lower than the natural lignin (molecular weight 7,000 to 10,000) that has been used well with black.
この結果から、１.７万〜２.０万の分子量範囲内にある分子量が２万の合成リグニン（ビスフェノールスルホン酸ポリマー縮合物）と、比表面積が、１５０〜３００m2／gの範囲内にある比表面積が２６０m2／gである重油を原料としたカーボンブラックを用いて添加量について詳細検討した。 From this result, a synthetic lignin (bisphenol sulfonic acid polymer condensate) having a molecular weight of 20,000 in the molecular weight range of 17,000 to 20000 and a specific surface area in the range of 150 to 300 m 2 / g. The addition amount was examined in detail using carbon black made from heavy oil having a specific surface area of 260 m 2 / g.
図2にその結果を示す。リグニン添加量が０.１〜０.６wt%、カーボン量が０.２２〜１．２８wt%で５秒目電圧が低く、充電受入れ性向上に効果があることがわかる。 Figure 2 shows the results. It can be seen that the lignin addition amount is 0.1 to 0.6 wt%, the carbon amount is 0.22 to 1.28 wt%, and the voltage at the fifth second is low, which is effective in improving the charge acceptance.
また、図３にリグニン量を変化させた際のJIS低温高率放電試験（−１５℃、３００A放電）結果を示す。図３から合成リグニンの添加量は０.２wt%未満では低温での高率放電性能が劣るため、添加量は０.２wt%以上必要なことがわかる。 FIG. 3 shows the results of a JIS low-temperature high-rate discharge test (−15 ° C., 300 A discharge) when the amount of lignin was changed. As can be seen from FIG. 3, when the amount of synthetic lignin added is less than 0.2 wt%, the high rate discharge performance at low temperatures is inferior, so that the amount added must be 0.2 wt% or more.
またカーボン量が１.３wt%以上では、充電受入れ性が低下するが、これは化成後の活物質の構造が脆弱となり化成後に活物質の脱落が発生するためである。 In addition, when the amount of carbon is 1.3 wt% or more, the charge acceptability is lowered. This is because the structure of the active material after chemical conversion becomes fragile and the active material falls off after chemical conversion.
以上の結果より合成リグニン０.２〜０.６wt%、カーボンブラック０.２２〜１.２８wt%が最も良い添加量と考えられる。 From the above results, 0.2 to 0.6 wt% of synthetic lignin and 0.22 to 1.28 wt% of carbon black are considered to be the best addition amounts.
本電池は充電受入れ性に優れており、通常の始動用電池として高性能であり、ISS車用電池としても最適である。 This battery has excellent charge acceptability, has high performance as a normal starting battery, and is optimal as a battery for ISS cars.
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Cited By (32)
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| JP2008140645A (en) * | 2006-12-01 | 2008-06-19 | Matsushita Electric Ind Co Ltd | Lead acid battery |
| JP2008152955A (en) * | 2006-12-14 | 2008-07-03 | Shin Kobe Electric Mach Co Ltd | Lead acid battery |
| JP2008277244A (en) * | 2007-04-06 | 2008-11-13 | Shin Kobe Electric Mach Co Ltd | Lead acid battery |
| WO2011108175A1 (en) | 2010-03-02 | 2011-09-09 | 新神戸電機株式会社 | Lead storage battery |
| WO2011142072A1 (en) | 2010-05-10 | 2011-11-17 | 新神戸電機株式会社 | Lead storage battery |
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| WO2014070693A1 (en) | 2012-10-31 | 2014-05-08 | Exide Technologies | A composition that enhances deep cycle performance of valve- regulated lead-acid batteries filled with gel electrolyte |
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| WO2015181865A1 (en) * | 2014-05-26 | 2015-12-03 | 株式会社Ｇｓユアサ | Lead storage cell |
| JP2015534709A (en) * | 2012-09-28 | 2015-12-03 | キャボット コーポレイションＣａｂｏｔ Ｃｏｒｐｏｒａｔｉｏｎ | Active material composition comprising high surface area carbon material |
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