CN104538183A - Electrolyte for medium and high voltage of electrolytic capacitor and preparation method of electrolyte - Google Patents

Electrolyte for medium and high voltage of electrolytic capacitor and preparation method of electrolyte Download PDF

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Publication number
CN104538183A
CN104538183A CN201410754203.XA CN201410754203A CN104538183A CN 104538183 A CN104538183 A CN 104538183A CN 201410754203 A CN201410754203 A CN 201410754203A CN 104538183 A CN104538183 A CN 104538183A
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China
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parts
electrolyte
electrolytic capacitor
maleic anhydride
preparation
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CN201410754203.XA
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Chinese (zh)
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薛瑄武
赵玉玲
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NANTONG REDA ELECTRONIC MATERIAL CO Ltd
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NANTONG REDA ELECTRONIC MATERIAL CO Ltd
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Abstract

The invention discloses an electrolyte for the medium and high voltage of an electrolytic capacitor and a preparation method of the electrolyte. The electrolyte includes, by weight, 5 to 10 parts of chloroactic acid, 2 to 4 parts of polyethylene glycol, 10 to 20 parts of ethanediol, 2 to 8 parts of isopropyl alcohol, 3 to 7 parts of maleic anhydride, 4 to 8 parts of azelaic acid, 2 to 5 parts of phthalic acid, 1 to 3 parts of potassium biphthalate, 1 to 5 parts of anhydride maleic, 2 to 5 parts of triethanolamine, 1 to 5 parts of sodium tetraborate decahydrate, 0.3 to 0.6 part of nitrophenol and 1 to 4 parts of diammonium hydrogen phosphate. The preparation method includes the steps that all constituents are mixed, so that mixed liquid is acquired, inert gas is blown into the mixed liquid, oxygen in the mixed liquid is exhausted, the mixed liquid is heated to conduct a reaction under the vacuum condition, and therefore the electrolyte for the medium and high voltage of the electrolytic capacitor is acquired. The electrolyte is good in electrical property, long in service life and suitable for the medium and high voltage conditions.

Description

A kind of electrolytic capacitor mesohigh electrolyte and preparation method thereof
Technical field
The invention belongs to electrolyte preparing technical field, be specifically related to a kind of electrolytic capacitor mesohigh electrolyte and preparation method thereof.
Background technology
The normal solvent used has dimethyl formamide, gamma-butyrolacton, ethylene glycol, glycerol, water etc. in the electrolytic solution.Dimethyl formamide is the solvent of a kind of army electricity container, and it has very wide operating temperature range.In Asia, gamma-butyrolacton uses also very popular as electrolytical solvent, is mainly used in low-voltage miniature capacitor, uses the capacitor that this solvent is main solvent to have lower ESR.Ethylene glycol is most popular solvent, secondary capacitor usually be the system that ethylene glycol adds that part water is solvent.Solute in electrolyte mainly be boric acid, borate, carboxylate and other a small amount of inorganic salts and depolarising disappear hydrogen agent, corrosion inhibiter, hydrolysis inhibitor etc.Be adding portion water for people general in low-voltage electrolysis liquid, improve the electric conductivity of electrolyte; Mesohigh electrolyte, normally used is anhydrous glycol system, also requires below 3% even if moisture.
Mesohigh main electrolyte development is roughly as follows:
(1) boric acid+glycol system: this system is the electrolyte of aluminium electrolytic capacitor early application.Such electrolyte from boric acid produce the crystallization water and between ethylene glycol and boric acid due to esterification generate a large amount of condensation water, cause that the moisture of electrolyte system inside raises, its result uses this electrolyte under the serviceability temperature condition more than 100 DEG C time, water in electrolyte will become steam and evaporate, in the assembly of electrochemical capacitor thereupon, voltage rise is high, the so-called destruction problem of unavoidable generation, this system cannot be applied in hot environment, is now substantially eliminated.
(2) linear carboxylate+glycol system: adopt straight chain type saturated dicarboxylic acid such as containing azelaic acid, decanedioic acid, dodecanedioic acid or its salt as electrolyte solution, this is current domestic widely used system, but linear carboxylate has the phenomenon of crystallization at low temperatures, have impact on the cryogenic property of capacitor, and the oxidation efficiency of straight-chain carboxylic acid's salt system is lower, these problems all govern the further raising of capacitor performance.
(3) branched carboxylic acids salt+glycol system: foreign vendor's many uses branched carboxylic acids salt is as main electrolyte.Compare in straight-chain carboxylic acid, the introducing of side-chain radical in branched carboxylic acids, its ability suppressing esterification is under the high temperature conditions strengthened, thus improves high-temperature stability; And due to the sterically hindered effect of group on side chain and the polarization of alkoxy grp, its solubility in ethylene glycol is increased, thus improve its cryogenic property, solubility and the thermal stability of branched carboxylic acids salt are all better than linear carboxylate, can produce the capacitor product that performance is more excellent.
The mesohigh electrolyte used at present, useful life is shorter, and electrolytical electric property is general simultaneously, therefore needs to be improved further.
Summary of the invention
The object of the invention is to provide a kind of electrolytic capacitor mesohigh electrolyte and preparation method thereof to overcome above the deficiencies in the prior art, improving electric property and the stability of electrolyte.
The present invention is realized by following technological means:
A kind of electrolytic capacitor mesohigh electrolyte, comprises in components by weight percent: monoxone 5-10 part, polyethylene glycol 2-4 part, ethylene glycol 10-20 part, isopropyl alcohol 2-8 part, maleic anhydride 3-7 part, azelaic acid 4-8 part, phthalic acid 2-5 part, Potassium Hydrogen Phthalate 1-3 part, maleic anhydride 1-5 part, triethanolamine 2-5 part, sodium tetraborate decahydrate 1-5 part, nitrophenol 0.3-0.6 part, diammonium hydrogen phosphate 1-4 part.
Described electrolytic capacitor mesohigh electrolyte, can preferably comprise in components by weight percent: monoxone 6-8 part, polyethylene glycol 2-3 part, ethylene glycol 15-18 part, isopropyl alcohol 6-8 part, maleic anhydride 4-6 part, azelaic acid 5-7 part, phthalic acid 2-4 part, Potassium Hydrogen Phthalate 2-3 part, maleic anhydride 3-5 part, triethanolamine 2-4 part, sodium tetraborate decahydrate 1-3 part, nitrophenol 0.4-0.6 part, diammonium hydrogen phosphate 1-3 part.
Above-described electrolytic capacitor mesohigh electrolyte, can more preferably comprise in components by weight percent: monoxone 7 parts, polyethylene glycol 3 parts, ethylene glycol 17 parts, isopropyl alcohol 7 parts, maleic anhydride 5 parts, azelaic acid 6 parts, phthalic acid 3 parts, Potassium Hydrogen Phthalate 2 parts, maleic anhydride 4 parts, triethanolamine 3 parts, sodium tetraborate decahydrate 2 parts, nitrophenol 0.5 part, diammonium hydrogen phosphate 2 parts.
The preparation method of the electrolytic capacitor mesohigh electrolyte described in above any one, comprises the following steps:
Step one, takes each component according to weight portion;
Step 2, each component is mixed, obtain mixed liquor, then in mixed liquor, inert gas is blasted, being got rid of by oxygen in mixed liquor, is then be warming up to 40-50 DEG C under the condition of 0.02-0.06MPa in vacuum degree, stirs 60-90 minute, naturally be down to room temperature, obtain electrolytic capacitor mesohigh electrolyte.
The preparation method of described electrolytic capacitor mesohigh electrolyte, in step 2, inert gas can be nitrogen or argon gas.
The preparation method of described electrolytic capacitor mesohigh electrolyte, the time blasting inert gas in step 2 can be 40-50 minute.
The preparation method of described electrolytic capacitor mesohigh electrolyte, the speed stirred in step 2 can be 70-80 rev/min.
Electrolytic capacitor mesohigh electrolyte provided by the invention is when sparking voltage is 400V, conductivity reaches more than 3.6ms/cm, reach voltage and reach 428-438V, under 125 DEG C of conditions, life test reaches more than 3700h, there is good conductivity and useful life, can better in the electrolysis of condition of high voltage.
Embodiment
Embodiment 1
A kind of electrolytic capacitor mesohigh electrolyte, comprises in components by weight percent: monoxone 5 parts, polyethylene glycol 2 parts, ethylene glycol 10 parts, isopropyl alcohol 2 parts, maleic anhydride 3 parts, azelaic acid 4 parts, phthalic acid 2 parts, Potassium Hydrogen Phthalate 1 part, maleic anhydride 1 part, triethanolamine 2 parts, sodium tetraborate decahydrate 1 part, nitrophenol 0.3 part, diammonium hydrogen phosphate 1 part.
The preparation method of described electrolytic capacitor mesohigh electrolyte, comprises the following steps:
Step one, takes each component according to weight portion;
Step 2, each component is mixed, obtain mixed liquor, then in mixed liquor, blast nitrogen, the time blasting gas is 40 minutes, oxygen in mixed liquor is got rid of, then be warming up to 40 DEG C under the condition of 0.02MPa in vacuum degree, stir 60 minutes, the speed of stirring is 70 revs/min, naturally be down to room temperature, obtain electrolytic capacitor mesohigh electrolyte.
Embodiment 2
A kind of electrolytic capacitor mesohigh electrolyte, comprises in components by weight percent: monoxone 6 parts, polyethylene glycol 2 parts, ethylene glycol 15 parts, isopropyl alcohol 6 parts, maleic anhydride 4 parts, azelaic acid 5 parts, phthalic acid 2 parts, Potassium Hydrogen Phthalate 2 parts, maleic anhydride 3 parts, triethanolamine 2 parts, sodium tetraborate decahydrate 1 part, nitrophenol 0.4 part, diammonium hydrogen phosphate 1 part.
The preparation method of described electrolytic capacitor mesohigh electrolyte, comprises the following steps:
Step one, takes each component according to weight portion;
Step 2, each component is mixed, obtain mixed liquor, then in mixed liquor, blast argon gas, the time blasting gas is 42 minutes, oxygen in mixed liquor is got rid of, then be warming up to 43 DEG C under the condition of 0.03MPa in vacuum degree, stir 65 minutes, the speed of stirring is 70 revs/min, naturally be down to room temperature, obtain electrolytic capacitor mesohigh electrolyte.
Embodiment 3
A kind of electrolytic capacitor mesohigh electrolyte, comprises in components by weight percent: monoxone 7 parts, polyethylene glycol 2 parts, ethylene glycol 16 parts, isopropyl alcohol 8 parts, maleic anhydride 5 parts, azelaic acid 5 parts, phthalic acid 4 parts, Potassium Hydrogen Phthalate 2 parts, maleic anhydride 5 parts, triethanolamine 2 parts, sodium tetraborate decahydrate 1 part, nitrophenol 0.4 part, diammonium hydrogen phosphate 2 parts.
The preparation method of described electrolytic capacitor mesohigh electrolyte, comprises the following steps:
Step one, takes each component according to weight portion;
Step 2, each component is mixed, obtain mixed liquor, then in mixed liquor, blast argon gas, the time blasting gas is 45 minutes, oxygen in mixed liquor is got rid of, then be warming up to 46 DEG C under the condition of 0.03MPa in vacuum degree, stir 75 minutes, the speed of stirring is 72 revs/min, naturally be down to room temperature, obtain electrolytic capacitor mesohigh electrolyte.
Embodiment 4
A kind of electrolytic capacitor mesohigh electrolyte, comprises in components by weight percent: monoxone 7 parts, polyethylene glycol 3 parts, ethylene glycol 17 parts, isopropyl alcohol 7 parts, maleic anhydride 5 parts, azelaic acid 6 parts, phthalic acid 3 parts, Potassium Hydrogen Phthalate 2 parts, maleic anhydride 4 parts, triethanolamine 3 parts, sodium tetraborate decahydrate 2 parts, nitrophenol 0.5 part, diammonium hydrogen phosphate 2 parts.
The preparation method of described electrolytic capacitor mesohigh electrolyte, comprises the following steps:
Step one, takes each component according to weight portion;
Step 2, each component is mixed, obtain mixed liquor, then in mixed liquor, blast nitrogen, the time blasting gas is 48 minutes, oxygen in mixed liquor is got rid of, then be warming up to 48 DEG C under the condition of 0.04MPa in vacuum degree, stir 80 minutes, the speed of stirring is 75 revs/min, naturally be down to room temperature, obtain electrolytic capacitor mesohigh electrolyte.
Embodiment 5
A kind of electrolytic capacitor mesohigh electrolyte, comprises in components by weight percent: monoxone 8 parts, polyethylene glycol 3 parts, ethylene glycol 18 parts, isopropyl alcohol 8 parts, maleic anhydride 6 parts, azelaic acid 7 parts, phthalic acid 4 parts, Potassium Hydrogen Phthalate 3 parts, maleic anhydride 5 parts, triethanolamine 4 parts, sodium tetraborate decahydrate 3 parts, nitrophenol 0.6 part, diammonium hydrogen phosphate 3 parts.
The preparation method of described electrolytic capacitor mesohigh electrolyte, comprises the following steps:
Step one, takes each component according to weight portion;
Step 2, each component is mixed, obtain mixed liquor, then in mixed liquor, blast nitrogen, the time blasting gas is 50 minutes, oxygen in mixed liquor is got rid of, then be warming up to 50 DEG C under the condition of 0.05MPa in vacuum degree, stir 85 minutes, the speed of stirring is 76 revs/min, naturally be down to room temperature, obtain electrolytic capacitor mesohigh electrolyte.
Embodiment 6
A kind of electrolytic capacitor mesohigh electrolyte, comprises in components by weight percent: monoxone 10 parts, polyethylene glycol 4 parts, ethylene glycol 20 parts, isopropyl alcohol 8 parts, maleic anhydride 7 parts, azelaic acid 8 parts, phthalic acid 5 parts, Potassium Hydrogen Phthalate 3 parts, maleic anhydride 5 parts, triethanolamine 5 parts, sodium tetraborate decahydrate 5 parts, nitrophenol 0.6 part, diammonium hydrogen phosphate 4 parts.
The preparation method of described electrolytic capacitor mesohigh electrolyte, comprises the following steps:
Step one, takes each component according to weight portion;
Step 2, each component is mixed, obtain mixed liquor, then in mixed liquor, blast nitrogen, the time blasting gas is 0 minute, oxygen in mixed liquor is got rid of, then be warming up to 50 DEG C under the condition of 0.06MPa in vacuum degree, stir 90 minutes, the speed of stirring is 80 revs/min, naturally be down to room temperature, obtain electrolytic capacitor mesohigh electrolyte.
Carry out performance test to the electrolytic capacitor mesohigh electrolyte that above embodiment prepares, result is as follows:
Project Sparking voltage/V Conductivity M/S 40℃ Reach voltage/V 125 DEG C of life tests
Embodiment 1 400 3.6ms/cm 428 3700h
Embodiment 2 400 3.8ms/cm 435 4200h
Embodiment 3 400 4.2ms/cm 435 4300h
Embodiment 4 400 4.5ms/cm 438 4500h
Embodiment 5 400 3.9ms/cm 430 4200h
Embodiment 6 400 3.4ms/cm 430 3950h
As can be seen from above result of the test, electrolytic capacitor mesohigh electrolyte provided by the invention is when sparking voltage is 400V, conductivity reaches more than 3.6ms/cm, reach voltage and reach 428-438V, under 125 DEG C of conditions, life test reaches more than 3700h, there is good conductivity and useful life, can better in the electrolysis of condition of high voltage.

Claims (7)

1. an electrolytic capacitor mesohigh electrolyte, is characterized in that, comprises in components by weight percent: monoxone 5-10 part, polyethylene glycol 2-4 part, ethylene glycol 10-20 part, isopropyl alcohol 2-8 part, maleic anhydride 3-7 part, azelaic acid 4-8 part, phthalic acid 2-5 part, Potassium Hydrogen Phthalate 1-3 part, maleic anhydride 1-5 part, triethanolamine 2-5 part, sodium tetraborate decahydrate 1-5 part, nitrophenol 0.3-0.6 part, diammonium hydrogen phosphate 1-4 part.
2. electrolytic capacitor mesohigh electrolyte according to claim 1, is characterized in that, comprise in components by weight percent: monoxone 6-8 part, polyethylene glycol 2-3 part, ethylene glycol 15-18 part, isopropyl alcohol 6-8 part, maleic anhydride 4-6 part, azelaic acid 5-7 part, phthalic acid 2-4 part, Potassium Hydrogen Phthalate 2-3 part, maleic anhydride 3-5 part, triethanolamine 2-4 part, sodium tetraborate decahydrate 1-3 part, nitrophenol 0.4-0.6 part, diammonium hydrogen phosphate 1-3 part.
3. electrolytic capacitor mesohigh electrolyte according to claim 1, is characterized in that, comprise in components by weight percent: monoxone 7 parts, polyethylene glycol 3 parts, ethylene glycol 17 parts, isopropyl alcohol 7 parts, maleic anhydride 5 parts, azelaic acid 6 parts, phthalic acid 3 parts, Potassium Hydrogen Phthalate 2 parts, maleic anhydride 4 parts, triethanolamine 3 parts, sodium tetraborate decahydrate 2 parts, nitrophenol 0.5 part, diammonium hydrogen phosphate 2 parts.
4. the preparation method of the electrolytic capacitor mesohigh electrolyte described in any one of claim 1-3, is characterized in that, comprise the following steps:
Step one, takes each component according to weight portion;
Step 2, each component is mixed, obtain mixed liquor, then in mixed liquor, inert gas is blasted, being got rid of by oxygen in mixed liquor, is then be warming up to 40-50 DEG C under the condition of 0.02-0.06MPa in vacuum degree, stirs 60-90 minute, naturally be down to room temperature, obtain electrolytic capacitor mesohigh electrolyte.
5. the preparation method of electrolytic capacitor mesohigh electrolyte according to claim 4, is characterized in that, in step 2, inert gas is nitrogen or argon gas.
6. the preparation method of electrolytic capacitor mesohigh electrolyte according to claim 4, is characterized in that, the time blasting inert gas in step 2 is 40-50 minute.
7. the preparation method of electrolytic capacitor mesohigh electrolyte according to claim 4, is characterized in that, the speed stirred in step 2 is 70-80 rev/min.
CN201410754203.XA 2014-12-10 2014-12-10 Electrolyte for medium and high voltage of electrolytic capacitor and preparation method of electrolyte Pending CN104538183A (en)

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CN105154952A (en) * 2015-09-01 2015-12-16 广西贺州市桂东电子科技有限责任公司 Formation method of ultrahigh-pressure electronic aluminum foil
CN109411237A (en) * 2018-12-26 2019-03-01 南通瑞达电子材料有限公司 A kind of electrolyte for electrolytic capacitor and preparation method thereof

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CN1467764A (en) * 2002-06-05 2004-01-14 松下电器产业株式会社 Electrolyte for driving electrolytic capacitor and electrolytic capacitor using the same electrolyte
CN1806068A (en) * 2003-06-17 2006-07-19 凯米特电子公司 Method of anodizing valve metal derived anode bodies and electrolyte therefor
CN1595711A (en) * 2003-09-09 2005-03-16 三洋电机株式会社 Non-aqueous solvent secondary battery
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Publication number Priority date Publication date Assignee Title
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CN109411237A (en) * 2018-12-26 2019-03-01 南通瑞达电子材料有限公司 A kind of electrolyte for electrolytic capacitor and preparation method thereof

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