JP4555158B2 - Electrolytic solution for electrolytic capacitor and electrolytic capacitor - Google Patents
Electrolytic solution for electrolytic capacitor and electrolytic capacitor Download PDFInfo
- Publication number
- JP4555158B2 JP4555158B2 JP2005158674A JP2005158674A JP4555158B2 JP 4555158 B2 JP4555158 B2 JP 4555158B2 JP 2005158674 A JP2005158674 A JP 2005158674A JP 2005158674 A JP2005158674 A JP 2005158674A JP 4555158 B2 JP4555158 B2 JP 4555158B2
- Authority
- JP
- Japan
- Prior art keywords
- acid
- leuconic
- electrolytic
- electrolytic capacitor
- electrolytic solution
- 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.)
- Expired - Fee Related
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- 239000003990 capacitor Substances 0.000 title claims description 15
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- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 229960001367 tartaric acid Drugs 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- 235000019303 thiodipropionic acid Nutrition 0.000 description 1
- SEACXNRNJAXIBM-UHFFFAOYSA-N triethyl(methyl)azanium Chemical compound CC[N+](C)(CC)CC SEACXNRNJAXIBM-UHFFFAOYSA-N 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
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- Electric Double-Layer Capacitors Or The Like (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
本発明は、電解コンデンサの駆動用電解液（以下、電解液と称す）および電解コンデンサの改良に関するものであり、特に耐電圧を改善した電解液に関するものである。 The present invention relates to an electrolytic solution for driving an electrolytic capacitor (hereinafter referred to as an electrolytic solution) and an electrolytic capacitor, and more particularly to an electrolytic solution with improved withstand voltage.
従来、中高圧用アルミニウム電解コンデンサ用の電解液としては、エチレングリコール等の溶媒に、高級二塩基酸またはそのアンモニウム塩、ホウ酸またはそのアンモニウム塩、およびマンニトール等の多価アルコール類を配合したものが用いられており、この種の電解液では、ホウ酸と多価アルコール類がエステル化合物を形成し、その構造的な特性により電解液の耐電圧が向上することが知られている。さらに他の多価アルコールとして、合成高分子であるポリビニルアルコールを溶解することにより耐電圧の向上を図ることが提案されている（例えば、特許文献１〜３参照）。
しかしながら、主鎖の炭素数が６程度であるマンニトール、ソルビトール等は配合量を増加させても電解液の耐電圧の向上が緩慢であるため、耐電圧を大幅に向上させるには大量に配合する必要があり、その結果、比抵抗の顕著な上昇を伴う。一方、ポリビニルアルコールはマンニトールより少量の添加で電解液の耐電圧向上が図れるが、エチレングリコールを主成分とする溶媒に対して溶解性が著しく低いため、十分な量を添加できず、かつ、電解液を調製する際、長時間の加熱と攪拌が必要であるという問題点がある。 However, mannitol, sorbitol, etc., having about 6 carbon atoms in the main chain, are slow to improve the withstand voltage of the electrolyte even if the blending amount is increased, so a large amount is blended to greatly improve the withstand voltage. With the consequent increase in resistivity. Polyvinyl alcohol, on the other hand, can improve the withstand voltage of the electrolyte solution by adding a smaller amount than mannitol, but it is extremely low in solubility in a solvent containing ethylene glycol as a main component. When preparing a liquid, there exists a problem that heating and stirring for a long time are required.
上記問題点に鑑みて、本発明の課題は、比抵抗上昇を抑えながら耐電圧の上昇を図ることができ、かつ、調製も効率よく行うことのできるアルミニウム電解コンデンサ用の駆動用電解液、およびこの駆動用電解液を用いたアルミニウム電解コンデンサを提供することにある。 In view of the above problems, an object of the present invention is to provide a driving electrolyte solution for an aluminum electrolytic capacitor that can increase a withstand voltage while suppressing an increase in specific resistance, and can be efficiently prepared, and An object of the present invention is to provide an aluminum electrolytic capacitor using this driving electrolyte.
本発明は、上記の課題を解決するため各種検討した結果、見出されたものであり、ロイコン酸が環状の多価アルコールであって、かつ、エチレングリコールを主成分とする溶媒への溶解性が極めて良好であることに着目し、さらに、その構造的な効果により電解液と電極箔との化学反応を抑制することにより、耐電圧の向上を図るものである。 The present invention has been found as a result of various studies to solve the above-mentioned problems, and was found to be soluble in a solvent in which leuconic acid is a cyclic polyhydric alcohol and contains ethylene glycol as a main component. In view of this, the withstand voltage is improved and the withstand voltage is improved by suppressing the chemical reaction between the electrolytic solution and the electrode foil by the structural effect.
すなわち、本発明のアルミニウム電解コンデンサでは、エチレングリコールを主成分とする溶媒中に、少なくとも、カルボン酸またはその塩と、以下の化学式（１）で示す無水ロイコン酸、化学式（２）で示す含水ロイコン酸、および化学式（１）、（２）で示す各状態の中間状態にある含水ロイコン酸のうちの少なくとも一つのロイコン酸とを含む駆動用電解液を用いたことを特徴とする。 That is, in the aluminum electrolytic capacitor of the present invention, at least a carboxylic acid or a salt thereof, a leuconic anhydride represented by the following chemical formula (1), and a hydrous leucon represented by the chemical formula (2) in a solvent mainly composed of ethylene glycol. A driving electrolyte solution containing an acid and at least one leuconic acid among hydrous leuconic acids in an intermediate state between the states represented by the chemical formulas (1) and (2) is used.
また、本発明のアルミニウム電解コンデンサでは、エチレングリコールを主成分とする溶媒中に、少なくとも、カルボン酸またはその塩と、上記の化学式（１）で示す無水ロイコン酸とを配合してなる駆動用電解液を用いたことを特徴とする。この場合には、電解液に無水ロイコン酸を配合したときでも、駆動用電解液中の水分によって、その一部があるいは全部が上記の化学式（２）で示す含水ロイコン酸、あるいは上記の化学式（１）（２）で示す各状態の中間状態にある含水ロイコン酸になっていると考えられる。 Further, in the aluminum electrolytic capacitor of the present invention, the electrolysis for driving formed by blending at least carboxylic acid or a salt thereof and leuconic anhydride represented by the above chemical formula (1) in a solvent mainly composed of ethylene glycol. It is characterized by using a liquid. In this case, even when leuconic anhydride is blended in the electrolytic solution, a part or all of the hydrous leuconic acid represented by the above chemical formula (2) or the above chemical formula ( 1) It is thought that it is the hydrous leuconic acid in the intermediate state of each state shown by (2).
本発明において、ロイコン酸（無水ロイコン酸あるいは含水ロイコン酸）の配合量は、電解液全体に対して０．１〜５．０ｗｔ％であることが好ましい。
ここで、無水ロイコン酸および含水ロイコン酸の双方が添加されている場合、これらのロイコン酸の含有量の総和が０．１〜５．０ｗｔ％であることが好ましい。
In this invention, it is preferable that the compounding quantity of leuconic acid (an anhydrous leuconic acid or hydrous leuconic acid) is 0.1-5.0 wt% with respect to the whole electrolyte solution.
Here, when both leuconic anhydride and hydrous leuconic acid are added, the total content of these leuconic acids is preferably 0.1 to 5.0 wt%.
本発明において、カルボン酸としては、ポリカルボン酸であるアゼライン酸、２−メチルアゼライン酸、セバシン酸、１，６−デカンジカルボン酸、５，６−デカンジカルボン酸、７−ビニルヘキサデセン−１，１６−ジカルボン酸、シュウ酸、マロン酸、コハク酸、グルタル酸、アジピン酸、ピメリン酸、スベリン酸、マレイン酸、フマル酸、イタコン酸、フタル酸、イソフタル酸、テレフタル酸、トリメリット酸、ピロメリット酸、チオジプロピオン酸などや、オキシカルボン酸である、グリコール酸、乳酸、酒石酸、サリチル酸、マンデル酸など。モノカルボン酸として、ギ酸、酢酸、プロピオン酸、酪酸、イソ酪酸、吉草酸、カプロン酸、エナント酸、カプリル酸、ペラルゴン酸、ラウリル酸、ミリスチン酸、ステアリン酸、ベヘン酸、アクリル酸、メタクリル酸、オレイン酸、安息香酸、ｐ−ニトロ安息香酸、アニス酸、クミン酸、ケイ皮酸、ナフトエ酸などがあり、その他に、ボロジシュウ酸、ボロジグリコール酸、ボロジサリチル酸、エチレングリコールホウ酸エステルなどを例示することができる。 In the present invention, examples of the carboxylic acid include azelaic acid, 2-methylazeleic acid, sebacic acid, 1,6-decanedicarboxylic acid, 5,6-decanedicarboxylic acid, and 7-vinylhexadecene-1,16 which are polycarboxylic acids. -Dicarboxylic acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, maleic acid, fumaric acid, itaconic acid, phthalic acid, isophthalic acid, terephthalic acid, trimellitic acid, pyromellitic acid Thiodipropionic acid and the like, and oxycarboxylic acids such as glycolic acid, lactic acid, tartaric acid, salicylic acid, and mandelic acid. Monocarboxylic acids include formic acid, acetic acid, propionic acid, butyric acid, isobutyric acid, valeric acid, caproic acid, enanthic acid, caprylic acid, pelargonic acid, lauric acid, myristic acid, stearic acid, behenic acid, acrylic acid, methacrylic acid, There are oleic acid, benzoic acid, p-nitrobenzoic acid, anisic acid, cumic acid, cinnamic acid, naphthoic acid, etc. In addition, borodisoxalic acid, borodiglycolic acid, borodisalicylic acid, ethylene glycol borate ester, etc. It can be illustrated.
カルボン酸の塩としては、アンモニウム塩の他、メチルアミン、エチルアミン、ｔ−ブチルアミン等の一級アミン塩、ジメチルアミン、エチルメチルアミン、ジエチルアミン等の二級アミン塩、トリメチルアミン、ジエチルメチルアミン、エチルジメチルアミン、トリエチルアミンＮ，Ｎ−ジメチル−Ｎ−（２−メトキシエチル）アミン等の三級アミン塩、テトラメチルアンモニウム、トリエチルメチルアンモニウム、テトラエチルアンモニウム等の四級アンモニウム塩、イミダゾリニウム塩等の溶融塩を例示することができる。 Carboxylic acid salts include ammonium salts, primary amine salts such as methylamine, ethylamine, and t-butylamine, secondary amine salts such as dimethylamine, ethylmethylamine, and diethylamine, trimethylamine, diethylmethylamine, and ethyldimethylamine. A tertiary amine salt such as triethylamine N, N-dimethyl-N- (2-methoxyethyl) amine, a quaternary ammonium salt such as tetramethylammonium, triethylmethylammonium and tetraethylammonium, and a molten salt such as an imidazolinium salt. It can be illustrated.
エチレングリコールに混合する副溶媒としては、プロピレングリコール等のグリコール類、γ−ブチロラクトン、Ｎ−メチル−２−ピロリドン等のラクトン類、Ｎ−メチルホルムアミド、Ｎ，Ｎ−ジメチルホルムアミド、Ｎ−エチルホルムアミド、Ｎ，Ｎ−ジエチルホルムアミド、Ｎ−メチルアセトアミド、Ｎ，Ｎ−ジメチルアセトアミド、Ｎ−エチルアセトアミド、Ｎ，Ｎ−ジエチルアセトアミド、ヘキサメチルホスホリックアミド等のアミド類、エチレンカーボネート、プロピレンカーボネート、イソブチレンカーボネート等の炭酸類、アセトニトリル等のニトリル類、ジメチルスルホキシド等のオキシド類、エーテル類、ケトン類、エステル類、スルホラン、スルホラン誘導体、水等を例示することができる。これらの溶媒は一種類だけでなく、二種類以上を混合して使用することができる。 As a co-solvent mixed with ethylene glycol, glycols such as propylene glycol, lactones such as γ-butyrolactone and N-methyl-2-pyrrolidone, N-methylformamide, N, N-dimethylformamide, N-ethylformamide, Amides such as N, N-diethylformamide, N-methylacetamide, N, N-dimethylacetamide, N-ethylacetamide, N, N-diethylacetamide, hexamethylphosphoricamide, ethylene carbonate, propylene carbonate, isobutylene carbonate, etc. Examples thereof include carbonic acids, nitriles such as acetonitrile, oxides such as dimethyl sulfoxide, ethers, ketones, esters, sulfolane, sulfolane derivatives, water and the like. These solvents can be used by mixing not only one type but also two or more types.
上記の電解液には、漏れ電流の低減、耐電圧向上、ガス吸収等の目的で種々の添加剤を加えることができる。添加剤の例としては、リン酸化合物、ホウ酸化合物、多価アルコール類、ポリビニルアルコール、ポリエチレングリコール、ポリプロピレングリコール、ポリオキシエチレンポリオキシプロピレングリコールのランダム共重合体およびブロック共重合体に代表される高分子化合物、ニトロ化合物等が挙げられる。 Various additives can be added to the electrolytic solution for the purpose of reducing leakage current, improving withstand voltage, and absorbing gas. Examples of additives include phosphoric acid compounds, boric acid compounds, polyhydric alcohols, polyvinyl alcohol, polyethylene glycol, polypropylene glycol, and polyoxyethylene polyoxypropylene glycol random copolymers and block copolymers. Examples thereof include a polymer compound and a nitro compound.
本発明において、ロイコン酸は、無水状態では、上記の化学式(１)の状態であるが、水分存在化では、上記の化学式（２）を示す含水ロイコン酸となる。また、水分量によっては、上記の化学式（１）、（２）で示す各状態の中間状態にあることも考えられる。
ここで、高圧用電解液中においては、水分を全く添加しない場合においても素子中に予め含まれている水分や、溶質や添加剤のエステル化反応により生じる縮合水が含まれている。従って、本発明による電解液をコンデンサに含浸した際には、ロイコン酸は、化学式（１）に示す無水の状態で配合しても、化学式（２）などで示す含水ロイコン酸の状態で溶解していることとなる。
In the present invention, leuconic acid is in the state of the above chemical formula (1) in the anhydrous state, but becomes water-containing leuconic acid having the above chemical formula (2) in the presence of water. Further, depending on the amount of water, it may be in an intermediate state between the states represented by the chemical formulas (1) and (2).
Here, in the high-pressure electrolyte, even when no moisture is added, moisture contained in the element in advance or condensed water generated by the esterification reaction of solutes and additives is contained. Accordingly, when the capacitor is impregnated with the electrolytic solution according to the present invention, leuconic acid dissolves in the state of hydrous leuconic acid represented by chemical formula (2) or the like even if blended in the anhydrous state represented by chemical formula (1). Will be.
この含水ロイコン酸は、従来の直鎖型の多価アルコール類とは異なり、環状のシクロペンタン環の周囲にヒドロキシル基が配置された構造になっているため、面構造により耐電圧向上に寄与する。このため、従来使用されてきた直鎖型の多価アルコールに比べ大幅な耐電圧向上効果が得られる。 Unlike conventional straight-chain polyhydric alcohols, this hydrous leuconic acid has a structure in which hydroxyl groups are arranged around a cyclic cyclopentane ring, which contributes to improved withstand voltage due to the surface structure. . For this reason, compared with the linear polyhydric alcohol conventionally used, the significant withstand voltage improvement effect is acquired.
また、含水ロイコン酸は、耐電圧向上剤として従来、使用されてきたマンニトールやソルビトールと同程度の分子量だが、それら以上の耐電圧向上効果が得られる。
さらに、ポリビニルアルコールなどの高分子系多価アルコールに比べ溶媒への溶解性が良好であるため、所定の量を配合できる。
それ故、比抵抗の上昇を抑制しながら耐電圧の向上を図ることができるとともに、熱的安定性にも優れるため、高温下での製品の信頼性を高めることができる。しかも、ロイコン酸は、ポリビニルアルコールなどの高分子系多価アルコールに比べ溶媒への溶解性が良好であるため、電解液の調製を効率よく行うことができる。
Hydrous leuconic acid has a molecular weight similar to that of mannitol and sorbitol, which have been conventionally used as a withstand voltage improver, but can provide a higher withstand voltage improvement effect.
Furthermore, since the solubility in a solvent is better than that of a polymeric polyhydric alcohol such as polyvinyl alcohol, a predetermined amount can be blended.
Therefore, the withstand voltage can be improved while suppressing an increase in specific resistance, and the thermal stability is excellent, so that the reliability of the product at high temperature can be enhanced. Moreover, leuconic acid has better solubility in a solvent than high molecular weight polyhydric alcohols such as polyvinyl alcohol, so that the electrolytic solution can be prepared efficiently.
エチレングリコールを主溶媒とし、溶質としてカルボン酸またはその塩を含有する電解液に、無水ロイコン酸を０．１〜５．０ｗｔ％溶解させて駆動用電解液を作製する。このような電解液において、ロイコン酸は、上記の化学式（２）を示す含水ロイコン酸、あるいは、上記の化学式（１）、（２）で示す各状態の中間状態にある。
このような駆動用電解液をアルミニウム電解コンデンサに用いると、耐電圧が向上し、かつ、高温下での製品の信頼性を高めることができる。
また、ロイコン酸は、ポリビニルアルコールなどの高分子系多価アルコールに比べ溶媒への溶解性が良好であるため、電解液の調製を効率よく行うことができる。
A driving electrolyte solution is prepared by dissolving 0.1 to 5.0 wt% of leuconic anhydride in an electrolyte solution containing ethylene glycol as a main solvent and carboxylic acid or a salt thereof as a solute. In such an electrolytic solution, leuconic acid is in an intermediate state between the hydrated leuconic acid represented by the chemical formula (2) or the states represented by the chemical formulas (1) and (2).
When such a driving electrolyte is used for an aluminum electrolytic capacitor, the withstand voltage is improved and the reliability of the product at high temperatures can be improved.
In addition, leuconic acid has better solubility in a solvent than high molecular weight polyhydric alcohols such as polyvinyl alcohol, so that the electrolytic solution can be prepared efficiently.
以下、本発明を実施例に基づき、より具体的に説明する。まず、表１および表２に示す組成で電解液を調合し、３０℃における電解液の比抵抗と８５℃における火花発生電圧（電解液の耐電圧）を測定し、表１および表２に示す結果を得た。なお、表１中、成分Ａは、無水ロイコン酸を示す。 Hereinafter, the present invention will be described more specifically based on examples. First, an electrolyte solution was prepared with the composition shown in Tables 1 and 2, and the specific resistance of the electrolyte solution at 30 ° C. and the spark generation voltage (withstand voltage of the electrolyte solution) at 85 ° C. were measured. The result was obtained. In Table 1, Component A represents leuconic anhydride.
表１より分かるように、アジピン酸およびセバシン酸を用いた電解液において、無水ロイコン酸を添加した実施例１、２、３、４、５に係る電解液はいずれも、従来例１より耐電圧が向上している。また、無水ロイコン酸を添加した実施例２、３、４に係る電解液は、耐電圧向上剤であるポリビニルアルコールを添加した従来例２より比抵抗が低く、耐電圧が高い。 As can be seen from Table 1, in the electrolytic solution using adipic acid and sebacic acid, all of the electrolytic solutions according to Examples 1, 2, 3, 4, and 5 to which leuconic anhydride was added had a higher withstand voltage than Conventional Example 1. Has improved. In addition, the electrolytic solutions according to Examples 2, 3, and 4 to which leuconic anhydride was added have lower specific resistance and higher withstand voltage than those of Conventional Example 2 to which polyvinyl alcohol as a withstand voltage improver is added.
ここで、無水ロイコン酸の配合量は０．１ｗｔ％未満（実施例１）では耐電圧向上の効果が十分でなく、５．０ｗｔ％を超える（実施例５）と比抵抗が高くなり、低比抵抗用途に不向きとなる。よって、無水ロイコン酸の溶解量は、０．１〜５．００ｗｔ％の範囲が好ましい。 Here, if the blending amount of leuconic anhydride is less than 0.1 wt% (Example 1), the effect of improving the withstand voltage is not sufficient, and if it exceeds 5.0 wt% (Example 5), the specific resistance becomes high and low. Unsuitable for specific resistance applications. Therefore, the dissolution amount of leuconic anhydride is preferably in the range of 0.1 to 5.00 wt%.
なお、本発明は実施例に限定されるものではなく、表２に示すように、先に例示した各種溶質を単独または複数溶解した電解液や、その他添加剤を加えた電解液、副溶媒を混合した電解液でも実施例と同等の効果があった。 In addition, this invention is not limited to an Example, As shown in Table 2, the electrolytic solution which melt | dissolved various solutes illustrated previously individually or severally, the electrolyte solution which added the other additive, and a subsolvent The mixed electrolyte solution had the same effect as the example.
また、上記形態では、電解液の調製時、ロイコン酸として無水ロイコン酸を添加したが、その一部あるいは全体を含水ロイコン酸として添加してもよい。 Moreover, in the said form, at the time of preparation of electrolyte solution, although leuconic anhydride was added as leuconic acid, you may add the one part or the whole as hydrous leuconic acid.
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| JPH09508487A (en) * | 1993-09-07 | 1997-08-26 | イーシーアール エレクトロ−ケミカル リサーチ リミテッド | Solid state electrochemical battery |
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