JP4612430B2 - Electrolytic solution for electrolytic capacitor drive - Google Patents
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Description
本発明は、特に中高圧用アルミニウム電解コンデンサの駆動用電解液に関する。 The present invention particularly relates to an electrolytic solution for driving a medium-high voltage aluminum electrolytic capacitor.
従来、中高圧用アルミニウム電解コンデンサの駆動用電解液としては、 一般にエチレングリコールを主溶媒に、ほう酸又はその塩類を加えた電解液が使用されてきた。しかしながら、ほう酸は１０５℃以上の高温に於いて主溶媒であるエチレングリコールと容易にエステル化反応を起こし多量の水を生じる。この為、誘電体であるアルミニウム酸化皮膜を著しく水和劣化させ、また、その蒸気圧の高さから、防爆弁の開弁及び外装ケ−スの変形等を引き起こし、使用環境１０５℃以上でコンデンサの寿命を短くする原因となっていた。 Conventionally, as an electrolyte for driving an aluminum electrolytic capacitor for medium to high pressure, an electrolyte obtained by adding boric acid or a salt thereof to ethylene glycol as a main solvent has been used. However, boric acid easily undergoes an esterification reaction with ethylene glycol, which is the main solvent, at a high temperature of 105 ° C. or higher to produce a large amount of water. For this reason, the aluminum oxide film, which is a dielectric material, is significantly hydrated and deteriorated, and the high vapor pressure causes the explosion-proof valve to open and the outer case to be deformed. It was a cause to shorten the life of the.
そこでアゼライン酸、セバシン酸等のジカルボン酸またはその塩、２-ブチルオクタン二酸、２-メチルアゼライン酸等の側鎖にアルキル基を有するジカルボン酸あるいはその塩を含む電解液が使用されてきた(特許文献１および２)。 Therefore, an electrolytic solution containing a dicarboxylic acid such as azelaic acid or sebacic acid or a salt thereof, 2-butyloctanedioic acid, 2-methyl azelaic acid or the like, or a dicarboxylic acid having an alkyl group in the side chain or a salt thereof has been used ( Patent Documents 1 and 2).
しかし、アゼライン酸、セバシン酸等の側鎖を有しないジカルボン酸は主溶媒であるエチレングリコールに対する溶解性に乏しいため、電解液への添加量を低く抑えなければならなくなる。その結果比抵抗が増大し、満足するコンデンサ特性が得られない。またこれらの電解液は高圧コンデンサ駆動用電解としては耐電圧性が十分とは言えず、ポリビニルアルコール等の高分子化合物を添加して使用される。その結果電解液の粘性が増大し電解液のコンデンサへの含浸工程にかかる時間が長くなるためコンデンサの生産性に影響を及ぼす。 However, since dicarboxylic acids having no side chain such as azelaic acid and sebacic acid have poor solubility in ethylene glycol, which is the main solvent, the amount added to the electrolyte must be kept low. As a result, the specific resistance increases and satisfactory capacitor characteristics cannot be obtained. In addition, these electrolytic solutions cannot be said to have sufficient withstand voltage for electrolysis for driving a high-voltage capacitor, and are used by adding a polymer compound such as polyvinyl alcohol. As a result, the viscosity of the electrolytic solution increases and the time required for the step of impregnating the electrolytic solution into the capacitor becomes longer, which affects the productivity of the capacitor.
一方、２-ブチルオクタン二酸等の側鎖にアルキル基を有するジカルボン酸は、主溶媒であるエチレングリコールに対する溶解性こそ高いものの、耐電圧性は未だ十分とは言えず、前述のように高分子化合物を添加しなければ耐電圧性が確保できない問題が指摘される。
本発明は、かかる従来技術の有する欠点を解消し、電導性が高く、火花発生電圧が高く、かつ製品耐電圧が高く、且つ、優れた広範囲温度特性及び高温寿命特性に優れた新規な電解コンデンサ駆動用電解液を提供することを目的とする。 The present invention eliminates the disadvantages of the prior art, has a high electrical conductivity, a high spark generation voltage, a high product withstand voltage, and a novel electrolytic capacitor excellent in a wide range of temperature characteristics and high temperature life characteristics. An object is to provide a driving electrolyte.
本発明者は、上記課題を解決する為に種々の電解液について検討した結果、式（Ｉ）で示される化合物を有機溶媒に溶解して成る電解液をコンデンサ素子に含浸し電解コンデンサとしたところ、電導性を損なわず、火花発生電圧を高め、製品耐電圧を向上でき、且つ、優れた広範囲温度特性及び高温寿命特性耐電圧性が得られることを見いだし、本発明を完成するに至った。 As a result of studying various electrolytic solutions in order to solve the above problems, the present inventor has impregnated a capacitor element with an electrolytic solution obtained by dissolving a compound represented by the formula (I) in an organic solvent to obtain an electrolytic capacitor. The inventors have found that the spark generation voltage can be increased, the product withstand voltage can be improved without impairing electrical conductivity, and that excellent wide-range temperature characteristics and high-temperature life characteristics withstand voltage can be obtained, and the present invention has been completed.
かくして、本発明は以下の要旨からなる。
１．下記の式（Ｉ）で表される化合物が有機溶媒中に０．１〜２０重量％溶解されていることを特徴とする電解コンデンサ駆動用電解液。但し、式中Ｒ1、Ｒ2、Ｒ3はそれぞれ独立して、２価の有機基を表す。
Ｍ1、Ｍ2、Ｍ3は それぞれ独立して、水素原子、アンモニウム、第１級、第２級、第３級若しくは第４級アンモニウム、アルカリ金属原子を表す。
Thus, the present invention comprises the following gist.
1. An electrolytic solution for driving an electrolytic capacitor, wherein a compound represented by the following formula (I) is dissolved in an organic solvent in an amount of 0.1 to 20% by weight . However, in the formula, R 1 , R 2 and R 3 each independently represents a divalent organic group.
M 1 , M 2 and M 3 each independently represent a hydrogen atom, ammonium, primary, secondary, tertiary or quaternary ammonium or an alkali metal atom.
３.式(Ｉ)で表される化合物が、トリス(３-カルボキシプロピル)イソシアヌレート若しくはその塩、又はトリス(４-カルボキシブチル)イソシアヌレート若しくはその塩である上記１又は２に記載の電解コンデンサ駆動用電解液。
４.前記その塩がアンモニウム塩、又は第１級、第２級、第３級若しくは第４級アンモニウム塩である上記３に記載の電解コンデンサ駆動用電解液。
５.有機溶媒が、多価アルコール又は多価アルコールのモノ若しくはジアルキルエーテルである上記１〜４のいずれかに記載の電解コンデンサ駆動用電解液。
６.式（Ｉ）で表される化合物が２〜１０重量％溶解されている上記１〜５のいずれかに記載の電解コンデンサ駆動用電解液。
3. The electrolytic capacitor according to 1 or 2 above, wherein the compound represented by the formula (I) is tris (3-carboxypropyl) isocyanurate or a salt thereof, or tris (4-carboxybutyl) isocyanurate or a salt thereof. Electrolytic solution for driving.
4. The electrolytic solution for driving an electrolytic capacitor as described in 3 above, wherein the salt is an ammonium salt or a primary, secondary, tertiary or quaternary ammonium salt.
5. The electrolytic solution for driving an electrolytic capacitor as described in any one of 1 to 4 above , wherein the organic solvent is a polyhydric alcohol or a mono- or dialkyl ether of a polyhydric alcohol.
6. The electrolytic solution for driving an electrolytic capacitor according to any one of 1 to 5 above, wherein 2 to 10 % by weight of the compound represented by the formula (I) is dissolved .
本発明によれば、電導性が高く、火花発生電圧が高く、かつ製品耐電圧が高く、且つ、優れた広範囲温度特性及び高温寿命特性耐電圧性に優れた新規な電解コンデンサ駆動用電解液が提供される。 According to the present invention, there is provided a novel electrolytic solution for driving an electrolytic capacitor having high conductivity, high spark generation voltage, high product withstand voltage, and excellent wide temperature characteristics and high temperature life characteristics. Provided.
本発明の電解コンデンサ駆動用電解液は、上記した式（Ｉ）で示される化合物を溶質として有機溶媒に溶解してなるものである。式（Ｉ）におけるＲ1、Ｒ2、Ｒ3は、上記で定義したとおりであるが、なかでも、それぞれ独立して、炭素数が好ましくは１〜６、特には２〜４の２価の炭化水素基が好適である。炭化水素基は、直鎖型もしくは分枝型であってもよく、また、一部に酸素原子または硫黄原子が含んでいてもよい。特に、Ｒ1、Ｒ2、Ｒ3は、炭素数１〜６、好ましくは２〜４の直鎖型もしくは分枝型のアルキレン基が好適である。かかるアルキレン基の好ましい例は、エチレン、プロピレン、イソプロピレン、ブチレンなどが挙げられる。なかでも、プロピレン、ブチレンが好ましい。 The electrolytic solution for driving an electrolytic capacitor of the present invention is obtained by dissolving the compound represented by the above formula (I) as an solute in an organic solvent. R 1 , R 2 and R 3 in the formula (I) are as defined above, and among them, each independently preferably has 1 to 6 carbon atoms, particularly 2 to 4 divalent divalents. Hydrocarbon groups are preferred. The hydrocarbon group may be linear or branched, and may partially contain an oxygen atom or a sulfur atom. In particular, R 1 , R 2 , and R 3 are preferably a linear or branched alkylene group having 1 to 6 carbon atoms, preferably 2 to 4 carbon atoms. Preferable examples of such an alkylene group include ethylene, propylene, isopropylene, butylene and the like. Of these, propylene and butylene are preferable.
また、式(Ｉ)における、Ｍ1、Ｍ2、Ｍ3は上記に定義したとおりである。第１級、第２級又は第３級アンモニウムの好ましい例としては、モノエチルアンモニウム、ジエチルアンモニウム、ジメチルエチルアンモニウム、トリエチルアンモニウム、トリブチルアンモニウム、トリエタノールアンモニウムなどの１〜３級のアルキルアンモニウムが挙げられる。また、第４級アンモニウムの好ましい例としては、テトラメチルアンモニウム、トリメチルエチルアンモニウム、エチルメチルイミダゾリニウムなどの第４級アンモニウムが挙げられる。アルカリ金属原子としては、ナトリウム、カリウムが例示される。なかでも、Ｍ1、Ｍ2、Ｍ3はそれぞれ独立して、水素原子、アンモニウム、又は第１級、第２級、第３級若しくは第４級アンモニウムが好ましい。 In the formula (I), M 1 , M 2 and M 3 are as defined above. Preferable examples of primary, secondary or tertiary ammonium include primary to tertiary alkyl ammonium such as monoethylammonium, diethylammonium, dimethylethylammonium, triethylammonium, tributylammonium and triethanolammonium. . In addition, preferred examples of the quaternary ammonium include quaternary ammonium such as tetramethylammonium, trimethylethylammonium, and ethylmethylimidazolinium. Examples of the alkali metal atom include sodium and potassium. Among these, M 1 , M 2 , and M 3 are each independently preferably a hydrogen atom, ammonium, or primary, secondary, tertiary, or quaternary ammonium.
上記した式（Ｉ）で示される化合物の好ましい具体例としては、トリス(３-カルボキシプロピル)イソシアヌレート若しくはその塩、又はトリス(４-カルボキシブチル)イソシアヌレート若しくはその塩が挙げられる。かかる塩としては、上記したアンモニウム、又は第１級、第２級、第３級若しくは第４級アンモニウム、又はアルカリ金属原子である。なかでも、アンモニウム塩、又は第１級、第２級、第３級若しくは第４級アンモニウム塩が好ましい。 Preferable specific examples of the compound represented by the above formula (I) include tris (3-carboxypropyl) isocyanurate or a salt thereof, or tris (4-carboxybutyl) isocyanurate or a salt thereof. Such a salt is the above-mentioned ammonium, primary, secondary, tertiary or quaternary ammonium, or an alkali metal atom. Of these, ammonium salts or primary, secondary, tertiary or quaternary ammonium salts are preferred.
本発明のコンデンサ駆動用電解液の有機溶媒としては、上記式（Ｉ）で表される電解質を溶解するものが使用できる。該有機溶媒の例としては、メタノール、エタノール等のアルコール、エチレングリコール、ジエチレングリコール、１、４‐ブタンジオール、ポリエチレングリコール等の多価アルコール、ジエチレングリコールモノメチルエーテル、ジエチレングリコールモノエチルエーテル、ポリエチレングリコールモノメチルエーテル、ポリエチレングリコールモノエチルエーテル、ポリエチレングリコールジメチルエーテル、トリエチレングリコールモノメチルエーテル、トリエチレングリコールジメチルエーテル等の多価アルコールのモノ或いはジアルキルエーテル、Ｎ―メチルホルムアミド、ＮＮ―ジメチルホルムアミド等のアミド類、アセトニトリル、ブチロニトリルなどのニトリル類、又はγ―ブチロラクトン、γ―バレロラクトン等の環状エステルなどが挙げられる。有機溶媒としては、これらを１種又は２種以上使用することができる。有機溶媒は、必要に応じて水を含有させることも可能であるが高温度対応用とする場合、好ましくは５重量％以下、特には３重量％以下とすることが望ましい。 As the organic solvent for the electrolytic solution for driving a capacitor of the present invention, those capable of dissolving the electrolyte represented by the above formula (I) can be used. Examples of the organic solvent include alcohols such as methanol and ethanol, polyhydric alcohols such as ethylene glycol, diethylene glycol, 1,4-butanediol, and polyethylene glycol, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, polyethylene glycol monomethyl ether, and polyethylene. Mono- or dialkyl ethers of polyhydric alcohols such as glycol monoethyl ether, polyethylene glycol dimethyl ether, triethylene glycol monomethyl ether and triethylene glycol dimethyl ether, amides such as N-methylformamide and NN-dimethylformamide, nitriles such as acetonitrile and butyronitrile Or cyclic ethers such as γ-butyrolactone, γ-valerolactone, etc. Examples include stealth. These organic solvents can be used alone or in combination of two or more. The organic solvent can contain water as required, but when it is used for high temperatures, it is preferably 5% by weight or less, particularly 3% by weight or less.
本発明で使用される有機溶媒としては、なかでも、多価アルコール又は多価アルコールのモノ若しくはジアルキルエーテルを好ましくは５０重量％以上、特には７０重量％以上含有するものが好適である。多価アルコールとしては、エチレングリコール、ジエチレングリコール、ポリエチレングリコールが好ましい。また、多価アルコールのモノ若しくはジアルキルエーテルとしては、ジエチレングリコールモノメチルエーテル、ジエチレングリコールジメチルエーテルが好ましい。 As the organic solvent used in the present invention, those containing a polyhydric alcohol or a mono- or dialkyl ether of a polyhydric alcohol are preferably 50% by weight or more, particularly 70% by weight or more. As the polyhydric alcohol, ethylene glycol, diethylene glycol, and polyethylene glycol are preferable. Further, as the mono- or dialkyl ether of the polyhydric alcohol, diethylene glycol monomethyl ether and diethylene glycol dimethyl ether are preferable.
本発明のコンデンサ駆動用電解液は、式（Ｉ）で表される化合物を予め調製し、該化合物を上記有機溶媒に溶解することにより得られるが、上記の有機溶媒中で式（Ｉ）で表される化合物を形成する原材料又は前駆体成分を有機溶媒中へ同時に又は順次添加することにより得ることもできる。例えば、式（Ｉ）で表される遊離酸型の化合物とアンモニア又はアミン化合物を有機溶媒中に添加して目的とする式（Ｉ）で表されるアンモニウム塩、又は第１級、第２級、第３級若しくは第４級アンモニウム塩を溶解する本発明の電解液を得ることができる。また、本発明のコンデンサ駆動用電解液を得るに際しては、必要に応じて、加温、攪拌などの溶解を促進し、また均一な溶液を得るための手段を施すことができる。 The electrolytic solution for driving a capacitor of the present invention is obtained by preparing a compound represented by the formula (I) in advance and dissolving the compound in the organic solvent. In the organic solvent, the electrolytic solution for formula (I) It can also be obtained by simultaneously or sequentially adding raw materials or precursor components that form the compounds represented to the organic solvent. For example, a desired ammonium salt represented by the formula (I) by adding a free acid type compound represented by the formula (I) and ammonia or an amine compound into an organic solvent, or a primary or secondary class The electrolytic solution of the present invention that dissolves the tertiary or quaternary ammonium salt can be obtained. Moreover, when obtaining the electrolytic solution for driving a capacitor of the present invention, means for accelerating dissolution such as heating and stirring and obtaining a uniform solution can be applied as necessary.
本発明のコンデンサ駆動用電解液には、式（Ｉ）で表される化合物が、０．１〜２０重量％溶解されている。溶解量が０．１重量％未満では、電導性を損なうことなく、使用耐電圧を高め、しかも広範囲の使用温度に耐え、高温での長寿命を有するアルミニウム電解コンデンサ駆動用電解液を提供し難い。一方、溶解量が２０重量％を越えた場合にも本発明の目的を達成し難い。なかでも、好ましい溶解量は１〜１５重量％、特には２〜１０重量％が好ましい。
The capacitor driving electrolyte of the present invention is a compound represented by the formula (I) is 0. 1 to 20% by weight is dissolved. If the dissolution amount is less than 0.1% by weight, it is difficult to provide an electrolytic solution for driving an aluminum electrolytic capacitor that increases the withstand voltage, withstands a wide range of operating temperatures, and has a long life at high temperatures without impairing electrical conductivity. . On the other hand, it is difficult to achieve the object of the present invention even when the dissolution amount exceeds 20% by weight. Of these, good preferable dissolution amount 1-15% by weight, particularly preferably from 2 to 10 wt%.
本発明のコンデンサ駆動用電解液には、式（Ｉ）で表される化合物の溶質に加えて、コンデンサ駆動用電解液に使用されている既知の電解質が併用できる。かかる電解質の例としては、アジピン酸、アゼライン酸、セバシン酸等の直鎖ジカルボン酸若しくはその塩；２−ブチルオクタン二酸、３−メチルアジピン酸、２−メチルアゼライン酸等の側鎖ジカルボン酸若しくはその塩；ギ酸、酢酸、ノナン酸、ヘプタン酸等のモノカルボン酸もしくはその塩；安息香酸、フタル酸等の芳香族モノ若しくはジカルボン酸、又はその塩類が挙げられる。 In addition to the solute of the compound represented by the formula (I), a known electrolyte used in a capacitor driving electrolyte can be used in combination with the capacitor driving electrolyte of the present invention. Examples of such electrolytes include linear dicarboxylic acids such as adipic acid, azelaic acid, sebacic acid or salts thereof; side chain dicarboxylic acids such as 2-butyloctanedioic acid, 3-methyladipic acid, 2-methylazeleic acid, or the like. Examples thereof include monocarboxylic acids such as formic acid, acetic acid, nonanoic acid and heptanoic acid or salts thereof; aromatic mono- or dicarboxylic acids such as benzoic acid and phthalic acid; and salts thereof.
また、本発明の電解液には、必要に応じて種々添加剤を添加して、更なる特性向上を図ることができる。該添加剤の例として、硼酸、無水硼酸、メタ硼酸等の含ホウ素化合物；正リン酸、亜リン酸、ジ亜リン酸等の含リン化合物；o‐ニトロアニソール、ｍ‐ニトロアセトフェノン等のニトロ化合物；タングステン酸、リンタングステン酸等の金属酸化物等が挙げられる。
本発明のコンデンサ駆動用電解液は、種々の電解コンデンサに使用できるが、なかでも、定格電圧が３５０ボルト以上の高圧用アルミニウム電解コンデンサの駆動液として有用である。
In addition, various additives can be added to the electrolytic solution of the present invention as necessary to further improve the characteristics. Examples of the additive include boron-containing compounds such as boric acid, boric anhydride and metaboric acid; phosphorus-containing compounds such as orthophosphoric acid, phosphorous acid and diphosphorous acid; nitro such as o-nitroanisole and m-nitroacetophenone Compound: Metal oxides such as tungstic acid and phosphotungstic acid are exemplified.
The electrolytic solution for driving a capacitor of the present invention can be used for various electrolytic capacitors, and is particularly useful as a driving fluid for a high-voltage aluminum electrolytic capacitor having a rated voltage of 350 volts or more.
以下、本発明を実施例に基づいて具体的に説明するが、本発明の解釈はかかる実施例に限定されるものではない。 EXAMPLES Hereinafter, although this invention is demonstrated concretely based on an Example, the interpretation of this invention is not limited to this Example.
表１に、本発明の実施例における電解液の組成、比抵抗（Ω・ｃｍ）及び火花発生電圧（Ｖ）を示し、また、比較例の電解液の組成、比抵抗（Ω・ｃｍ）及び火花発生電圧（Ｖ）を示した。更に表１の組成に基づく電解液を密封容器に入れて１０５℃の温度雰囲気中に置き、一定時間経過毎に比抵抗（Ω・ｃｍ）を測定し、電解液の熱安定性を評価した結果を表２に示した。尚、表２中の（ ）内の数値は、初期値に対する比率を示す。 Table 1 shows the composition, specific resistance (Ω · cm) and spark generation voltage (V) of the electrolytic solution in the examples of the present invention, and the composition, specific resistance (Ω · cm) and the electrolytic solution of the comparative example. The spark generation voltage (V) is shown. Furthermore, the electrolytic solution based on the composition shown in Table 1 was put in a sealed container and placed in a temperature atmosphere of 105 ° C., and the specific resistance (Ω · cm) was measured every time a predetermined time passed, and the thermal stability of the electrolytic solution was evaluated. Are shown in Table 2. In Table 2, numerical values in parentheses indicate ratios relative to initial values.
更に、表１の組成の電解液を、定格電圧４５０ＷＶ、定格容量４００μＦの電解コンデンサ素子に含浸しコンデンサとしたものについて、１０５℃における定格電圧印加試験を実施し、その結果を表３に示した。 Further, a rated voltage application test at 105 ° C. was performed on an electrolytic capacitor element having a rated voltage of 450 WV and a rated capacity of 400 μF impregnated with an electrolytic solution having the composition shown in Table 1, and the results are shown in Table 3. .
上記表１からわかるように、本発明の実施例の駆動用電解液は、比較例１、２の電解液に比較すると、比抵抗は、若干大きいものの、火花発生電圧が著しく大きい。また、比較例３の電解液に比較すると、火花発生電圧は同等にも係わらず、比抵抗が著しく小さいことがわかる。 As can be seen from Table 1 above, the driving electrolytic solution of the example of the present invention has a slightly larger spark resistance than the electrolytic solutions of Comparative Examples 1 and 2, although the specific resistance is slightly larger. Moreover, when compared with the electrolyte solution of Comparative Example 3, it can be seen that the specific resistance is extremely small although the spark generation voltage is the same.
上記表２からは、本発明の実施例の駆動用電解液は、比較例のいずれの電解液に比較しても、高温下における経時変化が小さく安定性に優れることがわかる。 From Table 2 above, it can be seen that the driving electrolytic solution of the example of the present invention has a small change with time at high temperature and excellent stability compared to any electrolytic solution of the comparative example.
上記表３からは、本発明の実施例の駆動用電解液を使用したアルミニウム電解コンデンサ、なかでも、小型化、高密度実装化、超寿命化、高信頼性化が要求される、中高圧のアルミニウム電解コンデンサに適しており、電子機器に広く使用され、産業上に寄与するところが大である。 From Table 3 above, an aluminum electrolytic capacitor using the driving electrolyte according to the embodiment of the present invention, among which medium size and high pressure is required, which requires miniaturization, high density mounting, long life, and high reliability. It is suitable for aluminum electrolytic capacitors, is widely used in electronic equipment, and contributes to the industry.
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