KR19990049637A - Low Pressure Electrolyte for Electrolytic Capacitors - Google Patents
Low Pressure Electrolyte for Electrolytic Capacitors Download PDFInfo
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Abstract
본 발명은 전해 콘덴서용 저압용 전해액에 관한 것으로,The present invention relates to a low pressure electrolyte for an electrolytic capacitor,
전체 조성물의 중량을 기준으로, GBL(γ-부티로락톤) 55-71중량%과 에틸렌 글리콜 25-14중량%로된 혼합 용매,A mixed solvent of 55-71 wt% of GBL (γ-butyrolactone) and 25-14 wt% of ethylene glycol, based on the weight of the total composition,
프탈산 또는 말레산 5-13중량% 및 트리에틸아민 9-7중량%로된 용질 및Solute of 5-13% by weight of phthalic acid or maleic acid and 9-7% by weight of triethylamine, and
p-니트로벤조산 및/또는 아인산을 0.1-2중량% 첨가한 저압용 전해액이 제공된다.There is provided a low pressure electrolyte solution containing 0.1-2% by weight of p-nitrobenzoic acid and / or phosphorous acid.
본 발명에 의하면, GBL(γ-부티로락톤) 용매를 사용하여 사용 온도 범위를 확대할 뿐만 아니라 NMF계의 약품 위해성을 동시에 개선할 수 있다.According to the present invention, GBL (γ-butyrolactone) solvent can be used to not only expand the use temperature range, but also to improve the chemical risk of the NMF system at the same time.
Description
본 발명은 전해 콘덴서용 저압용 전해액에 관한 것으로, 보다 상세하게는 기존의 NMF계 대체 용매로서 GBR(γ-부티로락톤)을 사용하여 약품 위해성을 줄이고 광온 역대의 특성을 발현시키는 전해 콘덴서용 저압용 전해액에 관한 것이다.The present invention relates to a low pressure electrolytic solution for an electrolytic capacitor, and more particularly, a low pressure for an electrolytic capacitor which reduces chemical risks and expresses characteristics of a wide temperature range by using GBR (γ-butyrolactone) as an existing NMF-based alternative solvent. It relates to a solution electrolyte.
종래의 EG(에틸렌글리콜)계 전해액은 에틸렌 글리콜을 주용매로 사용하여 주 전해질로는 암모늄 아디페이트와 아디프산을 사용하고 첨가제로는 p-니트로벤조산과 디암모늄 하이드로겐 포스페이트를 사용하여 왔다.Conventional EG (ethylene glycol) -based electrolytes have been used ethylene glycol as the main solvent, ammonium adipate and adipic acid as the main electrolyte, and p-nitrobenzoic acid and diammonium hydrogen phosphate as additives.
상기 EG계 전해액은 일반적으로 에틸렌 글리콜 70%와 물 10%를 넣고 온도를 올려 70℃에서 용질로써 암모늄 아디페이트와 아디프산을 18.5중량% 첨가하고 첨가제로써 p-니트로벤조산과 디암모늄 하이드로겐 포스페이트를 1.5중량% 첨가하여 온도를 100℃까지 상승시키고 120분간 교반시켜 제조된다.The EG-based electrolyte is generally 70% ethylene glycol and 10% water, and the temperature is raised to 18.5% by weight of ammonium adipate and adipic acid as a solute at 70 ° C, and p-nitrobenzoic acid and diammonium hydrogen phosphate as additives. It is prepared by adding 1.5% by weight to raise the temperature to 100 ℃ and stirred for 120 minutes.
그러나 이 방법에 의하면, 물의 과다 사용으로 말미암아 105℃ 제품에는 사용하기 어려우며 용질량이 많고 교반 시간이 길어 제품의 손실각이 상승함으로 인해 우수한 품질의 제품을 제조하기 어렵다.However, according to this method, due to the excessive use of water, it is difficult to use the product at 105 ° C, and the mass of the product and the stirring time are long.
따라서 저압용에서 온도 범위를 확대하여 사용하는 제품 특성이 요구됨으로 인하여 NMF(메틸 포름아미드)계 전해액을 사용하게 되었다.Therefore, NMF (methyl formamide) type electrolyte was used due to the demand for product characteristics that extend the temperature range in low pressure.
상기 NMF계 전해액은 NMF를 주용매로 사용하고 용질로써 말레산, 트리에틸아민 등을 첨가하여 제조한다.The NMF electrolyte is prepared by using NMF as a main solvent and adding maleic acid, triethylamine, etc. as a solute.
그 사용비는 NMF 70-85중량%에 부틸산(BA) 5-11중량%, 말레산(MA) 1-5중량%, 트리에틸아민(TEA) 1-5중량% 그리고 첨가제로서 p-니트로벤조산 0.1-3중량%를 사용하여 왔다.The use ratio is 70-85% by weight of NMF, 5-11% by weight of butyric acid (BA), 1-5% by weight of maleic acid (MA), 1-5% by weight of triethylamine (TEA) and p-nitro as an additive. 0.1-3% by weight of benzoic acid has been used.
그러나 이 경우에는 105℃ 제품에는 사용가능하나, NMF 용매 자체의 약품 위해성으로 인한 규제 및 사용 온도 확대에 따른 특성이 미비한 문제가 있다.However, in this case, although it can be used in 105 ℃ products, there is a problem that the characteristics due to regulation and extended use temperature due to the chemical risk of the NMF solvent itself.
이에 본 발명의 목적은 사용 온도 범위를 확대할 뿐만 아니라 NMF계의 약품 위해성을 동시에 개선하는 GBL 용매를 사용한 전해 콘덴서용 저압용 전해액을 제공하고자 한다.Accordingly, an object of the present invention is to provide a low pressure electrolyte solution for an electrolytic capacitor using a GBL solvent that not only expands the use temperature range but also simultaneously improves the chemical hazards of the NMF system.
본 발명에 의하면,According to the invention,
전체 조성물의 중량을 기준으로, GBL(γ-부티로락톤) 55-71중량%과 에틸렌 글리콜 25-14중량%로된 혼합 용매,A mixed solvent of 55-71 wt% of GBL (γ-butyrolactone) and 25-14 wt% of ethylene glycol, based on the weight of the total composition,
프탈산 또는 말레산 5-13중량% 및 트리에틸아민 9-7중량%로된 용질 및Solute of 5-13% by weight of phthalic acid or maleic acid and 9-7% by weight of triethylamine, and
p-니트로벤조산 혹은 아인산을 0.1-2중량% 첨가한0.1-2% by weight of p-nitrobenzoic acid or phosphorous acid
전해 콘덴서용 저압용 전해액이 제공된다.A low pressure electrolyte for an electrolytic capacitor is provided.
이하, 본 발명에 대하여 상세히 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.
본 발명자들은 주용매로서 반응성이 낮고 용해성이 우수한 GBL(γ-니트로벤조산)과 에틸렌 글리콜의 혼합 용매를 사용하면 약품 위해성의 위험없이 광역 온도 범위에서 사용할 수 있다는데 착안하고 본 발명을 완성하기에 이르렀다.The present inventors have realized that the use of a mixed solvent of GBL (γ-nitrobenzoic acid) and ethylene glycol having low reactivity and excellent solubility as a main solvent can be used in a wide range of temperature ranges without the risk of chemical hazards, and has completed the present invention.
본 발명은 γ-부티로락톤 및 에틸렌 글리콜의 혼합 용매, 프탈산 또는 말레산 및 트리에틸아민로된 용질 및 가스 흡수제로써 p-니트로벤조산으로 이루어진 저압용 전해액을 제조한다.The present invention provides a low pressure electrolytic solution composed of p-nitrobenzoic acid as a solute and gas absorber consisting of a mixed solvent of γ-butyrolactone and ethylene glycol, phthalic acid or maleic acid and triethylamine.
γ-부티로락톤 및 에틸렌 글리콜의 혼합 용매는 프로톤계 및 비프로톤계 용매로 구성된 혼합 용매로써, 에틸렌 글리콜의 비점이 낮아 사용 온도 범위가 -40∼85℃로 한정되던 것을 γ-부티로락톤을 사용하여 전해액 조성물의 비점을 상승시킴으로써 105℃ 제품에 사용가능할 뿐만 아니라, 상온에서 적당한 점도를 유지시켜 함침율을 향상시킴으로써 함침 시간을 단축시킨다.The mixed solvent of γ-butyrolactone and ethylene glycol is a mixed solvent composed of a proton-based and aprotic-based solvent, and has a low boiling point of ethylene glycol, thus limiting the operating temperature range to -40 to 85 ° C. Not only can it be used for a 105 degreeC product by raising the boiling point of electrolyte composition, but it also shortens an impregnation time by maintaining an appropriate viscosity at normal temperature and improving an impregnation rate.
상기 혼합 용매의 사용량은 γ-부티로락톤 55-71중량%에 에틸렌 글리콜 25-14중량%으로 총량 80중량%가 바람직하다.The amount of the mixed solvent used is preferably 55-71% by weight of γ-butyrolactone, 25-14% by weight of ethylene glycol, and 80% by weight in total.
여기에 용질로써 프탈산 또는 말레산에 트리에틸아민을 첨가하면 프탈산이나 말레산의 말단 COOH기에 NH4 +염을 형성하여 전도도를 높이는 효과를 보이므로 비저항 특성을 유지시킨다.When triethylamine is added to phthalic acid or maleic acid as a solute, NH 4 + salts are formed in the terminal COOH group of phthalic acid or maleic acid to increase conductivity, thereby maintaining the resistivity characteristics.
상기 효과를 위해서는, 상기 프탈산 또는 말레산 5-13중량%에 트리에틸아민을 9-7중량% 첨가하는 것이 바람직하다. 상기 용질을 13중량% 이상 첨가하는 경우에는 용질이 석출되어 비저항값이 커짐으로써 전도도가 불량해지는 문제가 있으며, 5중량% 미만으로 첨가하는 경우에는 전해액 조성물의 점도가 너무 묽어져 제품의 제특성이 불량해지며, 상기 트리에틸아민을 첨가하는 효과또한 저하된다.For the above effects, it is preferable to add 9-7% by weight of triethylamine to 5-13% by weight of the phthalic acid or maleic acid. When the solute is added in an amount of 13% by weight or more, there is a problem in that conductivity is poor due to precipitation of solutes and a large resistivity value.In the case where the solute is added in an amount less than 5% by weight, the viscosity of the electrolyte composition is so diluted that the product characteristics are poor It becomes poor, and the effect of adding the triethylamine is also reduced.
또한 여기에 가스 흡수제로써 작용하도록 p-니트로벤조산 또는 아인산을 0.1-2중량% 첨가한다. 2중량%를 초과하면, 가스 흡수 효과가 더 이상 개선되지 않으며, 0.1중량% 미만으로 첨가되는 경우에는 가스 흡수제로서 작용하지 못한다.Also, 0.1-2% by weight of p-nitrobenzoic acid or phosphorous acid is added thereto to act as a gas absorbent. If it exceeds 2% by weight, the gas absorption effect is no longer improved, and when added below 0.1% by weight, it does not act as a gas absorbent.
상기한 바와 같이, 전체 조성물의 중량을 기준으로, γ-부티로락톤 55-71중량%과 에틸렌 글리콜 25-14중량%의 혼합 용매에 프탈산 또는 말레산 5-13중량% 및 트리에틸아민 9-7중량%로된 용질 및 가스 흡수제로써 p-니트로벤조산 혹은 아인산을 0.1-2중량% 첨가하여 제조한 저압용 전해액은 비저항, 내전압(SPV) 및 pH가 효과적으로 개선된다.As described above, 5-13% by weight of phthalic acid or maleic acid and triethylamine 9- in a mixed solvent of 55-71% by weight of γ-butyrolactone and 25-14% by weight of ethylene glycol based on the weight of the total composition. The low-pressure electrolyte prepared by adding 0.1-2% by weight of p-nitrobenzoic acid or phosphorous acid as a solute and gas absorbent of 7% by weight can effectively improve specific resistance, breakdown voltage (SPV) and pH.
이하, 본 발명의 실시예를 통하여 설명한다.Hereinafter, an embodiment of the present invention will be described.
실시예 1Example 1
전해 조성물 제조Electrolytic Composition Preparation
본 발명의 방법에 의해 상온에서 하기표 1에 기재된 바와 같은 조성으로 혼합 용매로써 에틸렌글리콜과 γ-부틸로락톤을 첨가하고 여기에 용질로써 o-프탈산을 첨가한 다음 트리에틸아민을 가하고 p-니트로벤조산 및/또는 아인산을 첨가하여 전해액 조성물을 제조하였다.By the method of the present invention, ethylene glycol and γ-butyrolactone are added as a mixed solvent in a composition as shown in Table 1 at room temperature, and o-phthalic acid is added thereto as a solute, followed by triethylamine, and p-nitro. Electrolyte composition was prepared by adding benzoic acid and / or phosphorous acid.
상기 전해액 조성물을 90℃까지 가열하고 90분간 유지시킨 다음 자연 냉각시켰다.The electrolyte composition was heated to 90 ° C., held for 90 minutes and then naturally cooled.
상기 전해액 조성물을 90℃까지 가열하고 90분간 유지시킨 다음 자연 냉각시켰다.The electrolyte composition was heated to 90 ° C., held for 90 minutes and then naturally cooled.
각 제조된 전해액 조성물로 부터 비저항과 내전압 그리고 pH를 측정하고 그 결과를 하기표 2에 나타내었다.Specific resistance, breakdown voltage and pH were measured from the prepared electrolyte compositions, and the results are shown in Table 2 below.
상기 표 2에서 보듯이, 본 발명에 의해 제조한 전해액 조성물(실시예)은 비저항이 개선되었으며, 내전압도 최소 95이상이고 pH도 보다 약알칼리성에 가까워 콘덴서 제품 제조시 부식 및 전기적 특성에 미치는 악영향을 개선함을 알 수 있다.As shown in Table 2, the electrolytic solution composition (Example) prepared by the present invention has improved specific resistance, withstand voltage at least 95, and pH is less alkaline than the pH, which has a negative effect on the corrosion and electrical properties in the production of capacitor products It can be seen that the improvement.
상기한 바에 따르면, GBL(γ-부틸로락톤) 용매를 사용하여 사용 온도 범위를 확대할 뿐만 아니라 NMF계의 약품 위해성을 동시에 개선할 수 있다.According to the above, the GBL (γ-butylolactone) solvent can be used to not only expand the use temperature range but also to improve the chemical risk of the NMF system at the same time.
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