CN102074357B - Preparation method, product and application of electrolyte for high voltage aluminum electrolytic capacitor - Google Patents
Preparation method, product and application of electrolyte for high voltage aluminum electrolytic capacitor Download PDFInfo
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- CN102074357B CN102074357B CN2010106210965A CN201010621096A CN102074357B CN 102074357 B CN102074357 B CN 102074357B CN 2010106210965 A CN2010106210965 A CN 2010106210965A CN 201010621096 A CN201010621096 A CN 201010621096A CN 102074357 B CN102074357 B CN 102074357B
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Abstract
The invention provides a preparation method of an electrolyte for a high voltage aluminum electrolytic capacitor and the electrolyte obtained by the preparation method. The electrolyte comprises the following components by weight portion: 78-85 main solvent, 0.7 hydrogen absorber, 9-15 main solute, 0.3 waterproof combined additive, 2-6 auxiliary solute and 0-3 sparking voltage improving agent. The invention comprises the key technology that: high-molecular-weight aliphatic dicarboxylic acid with branched-chain alkyl is used as a main electrolyte, and an aromatic nitro compound cathode depolarizing agent is added, and an ammonium phosphorous acid is added to prevent an alumina membrane from hydration. The electrolyte provided by the invention can withstand more than 3,000 hours under the loads that the sparking voltage is greater than 470V and the temperature is 125 DEG C, has the advantages of high sparking voltage, high conductivity and high reliability, and can be applied to the manufacture of the high voltage electrolytic capacitor.
Description
Technical field
The present invention relates to the electrolyte technical field, relate to a kind of high-pressure aluminum electrolytic capacitor especially with electrolyte and be applied to prepare high-pressure aluminum electrolytic capacitor.
Background technology
Aluminium electrolytic capacitor is one of base components of electronic product.Along with improving constantly and the expansion of aluminium electrolytic capacitor range of application of electronic product quality, higher requirement is proposed its performance.Electronic product such as Switching Power Supply, electricity-saving lamp requires very high to the security performance of high-voltage electrolysis capacitor.In filter circuit, capacitor bears high voltage, high ripple current, if feed is unstable or apply overvoltage, can cause capacitor destruction, catch fire, accident such as burning.Aluminum electrolytic capacitor electrolyte is the actual negative electrode in the capacitor entire work process, and the performance of capacitor is had material impact, and wherein: serviceability temperature scope, working life, reliability, leakage current, loss, volume change etc. play a decisive role to electrical property.
Chinese patent 200910054661.1 (documents) is the approaching prior art of the present invention, and it discloses a kind of 600V superhigh pressure aluminum electrolytic capacitor electrolyte, and discloses its raw material group particularly, and itself and technical scheme of the present invention and its difference see the following form:
The solute that patent 200910054661.1 also discloses its electrolyte is selected from boric acid, ammonium borate, ammonium pentaborate, ammonium sebacate, 1,10 one dodecandioic acid ammonium, 1; The 7-ammonium sebacate; 1,6 one dodecandioic acid ammonium, C14; C 16; C 24, and the mixture of one or both in the aliphatic acid ammonium with single-ended side side chain or both end sides side chain of the aliphatic acid with single-ended side side chain or both end sides side chain of C 30, C14, C 16, C 24, C 30 is that with main key technology difference of the present invention master's solute of the present invention is an aliphat macromolecule binary acid ammonium; Selected aliphat macromolecule binary acid ammonium is a mixture, and this mixture is C13, C18, C23 any one or multiple and the band branched hydrocarbyl aliphat macromolecule binary acid, wherein, main component is C18.In addition, patent of the present invention has been got rid of ammonium borate, ammonium pentaborate electrolyte fully, makes the performance of capacitor be greatly improved.
Summary of the invention
The object of the invention is to provide a kind of high-pressure aluminum electrolytic capacitor to use electrolyte; Thereby solve current electrolysis liquid and be difficult to satisfy capacitor high frequencyization, Low ESR, low electric leakage, long-life requirement; When especially having solved employing ammonium borate class electrolyte bath; It and ethylene glycol can produce esterification and generate water, cause technical barriers such as condenser leakage current is big, storage weak point in useful life because of aquation.
The present invention is following for the technical scheme that solves above-mentioned technical barrier and provide:
A kind of high-pressure aluminum electrolytic capacitor comprises following processing step with the preparation method of electrolyte:
(1) takes by weighing ethylene glycol, ammonium sebacate, aliphat macromolecule binary acid ammonium salt, p-nitrophenyl methyl alcohol, 1,7 ammonium sebacate, ammonium hypophosphite, oxirane expoxy propane copolyether;
(2) ethylene glycol, aliphat macromolecule binary acid ammonium salt, ammonium sebacate, 1,7 ammonium sebacate, oxirane expoxy propane copolyether are added in the dosing still, stir, heat temperature raising when temperature reaches 105 ℃, stirs, insulation 50min;
(3) add p-nitrophenyl methyl alcohol and ammonium hypophosphite,, material is dissolved fully at 105 ℃ of stirring and dissolving 10-20min;
(4) logical cold water, when being cooled to 45 ℃, feeding ammonia adjusting PH is 6.8-7.0;
(5) discharging gets high-pressure aluminum electrolytic capacitor and uses electrolyte.
A kind of high-pressure aluminum electrolytic capacitor that makes according to above-mentioned preparation method is used electrolyte, comprises following raw material components weight portion proportioning:
| Main solvent: | 78～85 | Hydrogen absorber: | 0.7 |
| Main solute: | 9～15 | The methanol additive: | 0.7 |
| Auxiliary solute: | 2～6 | The flash over voltage improving agent: | 0～3 |
Said main solvent is an ethylene glycol;
Said main solute is an aliphat macromolecule binary acid ammonium;
Said auxiliary solute is any or two kinds of ammonium sebacate, 1,7 ammonium sebacate;
Said hydrogen absorber is a p-nitrophenyl methyl alcohol; Said methanol additive comprises ammonium hypophosphite;
Said flash over voltage improving agent is an oxirane expoxy propane copolyether.
Described aliphat macromolecule binary acid is the aliphat macromolecule binary acid of band branched hydrocarbyl, and its structural formula is:
HOOC-(CH
2)
3-Mn-(CH
2)
3-COOH formula I
Wherein, n representes the degree of polymerization among the formula I, and value is 1,2 or 3;
M representes that isoprene monomer carries out the chain link of sudden reaction, and its structure is with Formula Il, formula III, and formula IV, any that formula V is represented:
Formula II formula III
Formula IV formula V
Wherein, formula II, the n value is 1,2 or 3 in the formula III; Formula IV, the n value is 1 or 2 among the formula V.
Aforesaid aliphat macromolecule binary acid comprises C13, C18, and the aliphat macromolecule binary acid of C23 any one or multiple band branched hydrocarbyl wherein comprises a kind of C18 at least.
A kind of high-pressure aluminum electrolytic capacitor is used electrolyte, and it can select following prescription:
Prescription one:
| Ethylene glycol: | 79～81 | Ammonium sebacate: | 3 |
| Aliphat macromolecule binary acid ammonium salt: | 12～14 | P-nitrophenyl methyl alcohol: | 0.7 |
| 1,7 ammonium sebacate: | 3 | Ammonium hypophosphite: | 0.3 |
Prescription two:
| Ethylene glycol: | 81～83 | Ammonium sebacate: | 2 |
| Aliphat macromolecule binary acid ammonium salt: | 12～14 | P-nitrophenyl methyl alcohol: | 0.7 |
| 1,7 ammonium sebacate: | 2 | Ammonium hypophosphite: | 0.3 |
Prescription three:
| Ethylene glycol: | 84～85 | 1,7 ammonium sebacate: | 2 |
| Aliphat macromolecule binary acid ammonium salt: | 9～10 | P-nitrophenyl methyl alcohol: | 0.7 |
| Oxirane expoxy propane copolyether: | 3 | Ammonium hypophosphite: | 0.3 |
[0038]High-pressure aluminum electrolytic capacitor of the present invention is applied to the preparation of high-voltage electrolysis capacitor with electrolyte.
The beneficial effect of the invention
1, the electrolyte used of high-pressure aluminum electrolytic capacitor provided by the invention has the performance of high flash over voltage, high conductivity.At present, state's electrolyte inside adopts dicarboxylate as high-pressure electrolysis matter more.From the adipic acid to the dodecandioic acid, along with increasing carboxylate radical intrusion oxide-film ability, carbochain weakens, and flash over voltage increases and improves along with molecular weight.The dodecandioic acid ammonium can precipitate because solubility is low at normal temperatures separates out, and therefore uses to be restricted.It is main electrolyte that the present invention adopts the aliphat band side chain binary acid ammonium salt of macromolecule, is solvent with ethylene glycol.HOOC-(the CH that the present invention adopts
2)
3-Mn-(CH
2)
3-COOH is being superior to the dodecandioic acid ammonium with its macromolecule aspect the flash over voltage, again because of it is that the solubility property of branched acids in ethylene glycol is better, overcome the defective of dodecandioic acid ammonium dissolving difficulty.
2, security performance is high: electrolyte of the present invention does not adopt the electrolyte of boric acid series, does not produce the problem of water with ethylene glycol esterification reaction, and electrolyte was used in behind the product under severe environmental conditions, like high temperature, high capacity, big electric current, heat balance difficulty in the past.After producing more moisture content, leakage current can strengthen, and capacitor can play drum, and fatal inefficacy appears in lead-in wire fusing.Electrolyte of the present invention has improved the security performance and the useful life of capacitor greatly.
3, high-pressure aluminum electrolytic capacitor of the present invention reaches more than the 470V with the electrolyte flash over voltage, and its capacitor working is pressed in more than the 400V, and can bear 125 ℃ of loads more than 3000 hours.
4, high-pressure aluminum electrolytic capacitor provided by the invention is with the preparation method of electrolyte, and it is simple to operate, and process conditions are prone to control, are easy to realize industrialization production.
Below in conjunction with embodiment, the present invention is further specified.
Description of drawings: Fig. 1 is a dosing still sketch map.
Embodiment
Embodiment 1
Present embodiment provides the electrolyte of three prescriptions (seeing table 1-3) preparation, comprises the preparation and the Performance Detection thereof of electrolyte.
One, preparation electrolyte
A kind of high-pressure aluminum electrolytic capacitor comprises following processing step with the preparation method of electrolyte:
(1) weighing: three prescriptions according to table 1-3 take by weighing raw material respectively;
(2) ethylene glycol, aliphat macromolecule binary acid ammonium salt, ammonium sebacate, 1,7 ammonium sebacate, oxirane expoxy propane copolyether are added in the dosing still (as shown in Figure 1), cover kettle cover; Begin to stir; Heat temperature raising when temperature reaches 105 ℃, stirs; Insulation 50min has the steam outlet of small amount of water vapor from the kettle cover overflow (material and still wall adsorbed water) this moment;
(3) add p-nitrophenyl methyl alcohol, ammonium hypophosphite and other methanol agent from charge door,, dissolve fully until material at 105 ℃ of stirring and dissolving 10-20min;
(4) turn off heater and steam outlet, slowly feed cold water, when being cooled to 45 ℃, feeding ammonia adjusting PH is 6.8-7.0;
(5) discharging makes high-pressure aluminum electrolytic capacitor and uses electrolyte.
Two, the Performance Detection of electrolyte test
(1) detection is by the flash over voltage and the conductivity of the electrolyte of method for preparing, and the result sees table 10;
(2) be made into 5 in the capacitor of operating voltage 400V with the high-pressure aluminum electrolytic capacitor of above-mentioned preparation respectively with electrolyte, do 125 ℃ storage test, the result sees table 11.
Detect electrolyte property, its result satisfies operating voltage 400V, can load more than the delivery 3000h for 125 ℃.
Table 1
| Ethylene glycol: | 79 | Ammonium sebacate: | 3 |
| The GZS-1 ammonium salt: | 14 | P-nitrophenyl methyl alcohol: | 0.7 |
| 1,7 ammonium sebacate: | 3 | Ammonium hypophosphite: | 0.3 |
Table 2
| Ethylene glycol: | 81 | Ammonium sebacate: | 3 |
| The GZS-1 ammonium salt: | 12 | P-nitrophenyl methyl alcohol: | 0.7 |
| 1,7 ammonium sebacate: | 3 | Ammonium hypophosphite: | 0.3 |
Table 3
| Ethylene glycol: | 80 | Ammonium sebacate: | 3 |
| The GZS-1 ammonium salt: | 13 | P-nitrophenyl methyl alcohol: | 0.7 |
| 1,7 ammonium sebacate: | 3 | Ammonium hypophosphite: | 0.3 |
Embodiment 2
One, preparation electrolyte
The preparation method of present embodiment and embodiment 1 is basic identical, and its difference is that used raw material is formed and weight portion is different: see table 4-6.
Two, the Performance Detection of electrolyte
(1) detection is by the flash over voltage and the conductivity of the electrolyte of method for preparing, and the result sees table 10;
(2) be made into 5 in the capacitor of operating voltage 450V with the electrolyte of above-mentioned preparation, do 125 ℃ storage test, the result sees table 12.
In addition, the prescription according to table 4-6 prepares electrolyte respectively, and detects electrolyte property, and its result satisfies operating voltage 450V, can load more than the delivery 3000h for 125 ℃.
Table 4
| Ethylene glycol: | 81 | Ammonium sebacate: | 2 |
| The GZS-1 ammonium salt: | 14 | P-nitrophenyl methyl alcohol: | 0.7 |
| 1,7 ammonium sebacate: | 2 | Ammonium hypophosphite: | 0.3 |
Table 5
| Ethylene glycol: | 83 | Ammonium sebacate: | 2 |
| The GZS-1 ammonium salt: | 12 | P-nitrophenyl methyl alcohol: | 0.7 |
| 1,7 ammonium sebacate: | 2 | Ammonium hypophosphite: | 0.3 |
Table 6
| Ethylene glycol: | 82 | Ammonium sebacate: | 2 |
| The GZS-1 ammonium salt: | 13 | P-nitrophenyl methyl alcohol: | 0.7 |
| 1,7 ammonium sebacate: | 2 | Ammonium hypophosphite: | 0.3 |
Embodiment 3
One, preparation electrolyte
Present embodiment and embodiment are basic identical, and its difference is to prepare the raw material composition and the weight portion difference of electrolyte, and the raw material of present embodiment is formed and weight portion: see table 7-9.
Two, the Performance Detection of electrolyte
(1) detection is by the flash over voltage and the conductivity of the electrolyte of method for preparing, and the result sees table 10
(2) will be made into 5 in the capacitor of operating voltage 500V by the electrolyte that is prepared into, and do 125 ℃ storage test, the result sees table 13.
Detect electrolyte property, its result satisfies operating voltage 500V, can load more than the delivery 3000h for 125 ℃.
Table 7
| Ethylene glycol: | 84 | 1,7 ammonium sebacate: | 2 |
| The GZS-1 ammonium salt: | 10 | P-nitrophenyl methyl alcohol: | 0.7 |
| Oxirane expoxy propane copolyether: | 3 | Ammonium hypophosphite: | 0.3 |
Table 8
| Ethylene glycol: | 85 | 1,7 ammonium sebacate: | 2 |
| The GZS-1 ammonium salt: | 9 | P-nitrophenyl methyl alcohol: | 0.7 |
| Oxirane expoxy propane copolyether: | 3 | Ammonium hypophosphite: | 0.3 |
Table 9
| Ethylene glycol: | 84.5 | 1,7 ammonium sebacate: | 2 |
| The GZS-1 ammonium salt: | 9.5 | P-nitrophenyl methyl alcohol: | 0.7 |
| Oxirane expoxy propane copolyether: | 3 | Ammonium hypophosphite: | 0.3 |
Test result
The The performance test results table of each embodiment electrolyte of table 10
Can find out that from table 10 high-pressure aluminum electrolytic capacitor of the present invention reaches more than the 470V with the electrolyte flash over voltage, be fit to the capacitor of the above operating voltage of preparation 400V.Wherein the conductivity of embodiment 1 reaches 2.2ms/cm, has high than the conductivity of embodiment 2/3.Embodiment 1 is that with the difference of embodiment 2 content of solute 1,7 ammonium sebacate, ammonium sebacate is different, visible both to content be controlled at account for component be 3 o'clock higher than 2 conductivity, flash over voltage is all low.Therefore want to improve the content that conductivity can improve 1,7 ammonium sebacate, ammonium sebacate, flash over voltage can descend accordingly simultaneously; Want to have higher flash over voltage, can reduce the content of 1,7 ammonium sebacate, ammonium sebacate, can cause conductivity to descend simultaneously.The present invention adjusts the content of 1,7 ammonium sebacate, ammonium sebacate according to the performance demands of different capacitors voltage to electrolyte.
Embodiment 1,2,3 listed electrolyte are made into respectively process electrolytic capacitor: 400V, 450V, 500V also detect its performance index in different time sections down at 125 ℃, and its result sees table 11～13.
Each item The performance test results mean value of table 11 embodiment 1 prepared capacitor
Each item The performance test results mean value of table 12 embodiment 2 prepared capacitors
Each item The performance test results mean value of table 13 embodiment 3 prepared capacitors
Can find out from embodiment 1, embodiment 2, embodiment 3 that the present invention fills a prescription and all can bear 125 ℃ that 3000 hours load delivery has excellent shelf characteric and functional reliability.
The present invention is not limited to said embodiment, and every all execution modes that are equal to that can realize the object of the invention are all within protection scope of the present invention.
Claims (8)
1. a high-pressure aluminum electrolytic capacitor is characterized in that with the preparation method of electrolyte, comprises following processing step:
(1) takes by weighing raw material, comprising: ethylene glycol, ammonium sebacate, aliphat macromolecule binary acid ammonium salt, p-nitrophenyl methyl alcohol, 1,7 ammonium sebacate, ammonium hypophosphite, oxirane expoxy propane copolyether;
Described aliphat macromolecule binary acid is the aliphat macromolecule binary acid of band branched hydrocarbyl, and its structural formula is:
HOOC-(CH
2)
3-Mn-(CH
2)
3-COOH formula I
Wherein, n representes the degree of polymerization among the formula I, and value is 1,2 or 3;
M representes that isoprene monomer carries out the chain link of sudden reaction, and its structure is with Formula Il, formula III, and formula IV, any that formula V is represented:
Wherein, formula II, the n value is 1,2 or 3 in the formula III; Formula IV, the n value is 1 or 2 among the formula V;
(2) ethylene glycol, aliphat macromolecule binary acid ammonium salt, ammonium sebacate, 1,7 ammonium sebacate, oxirane expoxy propane copolyether are added in the dosing still, stir, heat temperature raising, when temperature reached 105 ℃, stirring is insulation 50min down;
(3) add p-nitrophenyl methyl alcohol and ammonium hypophosphite,, material is dissolved fully at 105 ℃ of following stirring and dissolving 10-20min;
(4) logical cold water when being cooled to 45 ℃, feeds ammonia, and adjusting PH is 6.8-7.0;
(5) discharging gets high-pressure aluminum electrolytic capacitor and uses electrolyte.
2. use electrolyte according to the said high-pressure aluminum electrolytic capacitor of claim 1 with the high-pressure aluminum electrolytic capacitor that the preparation method of electrolyte makes for one kind, it is characterized in that, comprise following raw material components weight portion proportioning:
Main solvent: 78～85 hydrogen absorbers: 0.7
Main solute: 9～15 methanol additives: 0.7
Auxiliary solute: 2～6 flash over voltage improving agents: 0～3
3. high-pressure aluminum electrolytic capacitor according to claim 2 is used electrolyte, it is characterized in that, said main solvent is an ethylene glycol; Said main solute is an aliphat macromolecule binary acid; Said auxiliary solute is any or two kinds of ammonium sebacate, 1,7 ammonium sebacate; Said hydrogen absorber is a p-nitrophenyl methyl alcohol; Said methanol additive comprises ammonium hypophosphite; Said flash over voltage improving agent is an oxirane expoxy propane copolyether.
4. high-pressure aluminum electrolytic capacitor according to claim 3 is used electrolyte, it is characterized in that, said aliphat macromolecule binary acid is the aliphat macromolecule binary acid of band branched hydrocarbyl, and its structural formula is:
HOOC-(CH
2)
3-Mn-(CH
2)
3-COOH formula I
Wherein, n representes the degree of polymerization among the formula I, and value is 1,2 or 3;
M representes that isoprene monomer carries out the chain link of sudden reaction, and its structure is with Formula Il, formula III, and formula IV, any that formula V is represented or two kinds:
Wherein, formula II, formula III, middle n value is 1,2 or 3; Formula IV, the n value is 1 or 2 among the formula V.
5. electrolyte for capacitor according to claim 3 is characterized in that, aliphat macromolecule binary acid comprises C13, C18, and the aliphat macromolecule binary acid of C23 any one or multiple band branched hydrocarbyl wherein comprises a kind of C18 at least.
6. high-pressure aluminum electrolytic capacitor according to claim 3 is used electrolyte, it is characterized in that, said high-pressure aluminum electrolytic capacitor is used electrolyte, comprises following raw material components weight portion proportioning:
Ethylene glycol: 79～81 ammonium sebacates: 3
Aliphat macromolecule binary acid ammonium salt: 12～14 p-nitrophenyl methyl alcohol: 0.7
1,7 ammonium sebacate: 3 ammonium hypophosphites: 0.3
7. high-pressure aluminum electrolytic capacitor according to claim 3 is used electrolyte, it is characterized in that, said high-pressure aluminum electrolytic capacitor is used electrolyte, comprises following raw material components weight portion proportioning:
Ethylene glycol: 81～83 ammonium sebacates: 2
Aliphat macromolecule binary acid ammonium salt: 12～14 p-nitrophenyl methyl alcohol: 0.7
1,7 ammonium sebacate: 2 ammonium hypophosphites: 0.3
8. high-pressure aluminum electrolytic capacitor according to claim 3 is used electrolyte, it is characterized in that, said high-pressure aluminum electrolytic capacitor is used electrolyte, comprises following raw material components weight portion proportioning:
Ethylene glycol: 84～85 1,7 ammonium sebacates: 2
Aliphat macromolecule binary acid ammonium salt: 9～10 p-nitrophenyl methyl alcohol: 0.7
Oxirane expoxy propane copolyether: 3 ammonium hypophosphites: 0.3.
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| CN103632851B (en) * | 2012-08-27 | 2016-08-17 | 深圳市金元电子技术有限公司 | High conductivity boron series-free working electrolyte and preparation method thereof |
| CN103632850B (en) * | 2012-08-27 | 2016-08-17 | 深圳市金元电子技术有限公司 | High flash over voltage boron series-free working electrolyte and preparation method thereof |
| CN104217858A (en) * | 2013-05-30 | 2014-12-17 | 南通一品机械电子有限公司 | High-voltage, high-conductivity and long-life electrolyte |
| CN105239128B (en) * | 2015-09-01 | 2018-03-30 | 广西贺州市桂东电子科技有限责任公司 | A kind of super-pressure Waste Acid From Hua Cheng Foil forms liquid and compound method |
| CN109448996B (en) * | 2018-12-29 | 2020-05-22 | 广州鸿葳科技股份有限公司 | High-voltage high-conductivity electrolyte and preparation method and application thereof |
| CN112885606A (en) * | 2021-01-11 | 2021-06-01 | 深圳市金富康电子有限公司 | Electrolyte additive, high-voltage high-conductivity electrolyte and preparation method thereof, and aluminum electrolytic capacitor and preparation method thereof |
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| CN1862728A (en) * | 2005-12-28 | 2006-11-15 | 横店集团东磁有限公司 | Flash lamp aluminum electrolytic capacitor and preparation method thereof |
| CN101483101A (en) * | 2008-12-25 | 2009-07-15 | 佛山市三水日明电子有限公司 | 125 DEG C high temperature long life aluminum electrolysis capacitor, production method thereof and special electrolysis liquid |
| CN101599367A (en) * | 2009-07-10 | 2009-12-09 | 南通江海电容器股份有限公司 | 600V ultrahigh voltage aluminum electrolytic capacitor working electrolyte and preparation and application thereof |
| CN101866751A (en) * | 2010-06-07 | 2010-10-20 | 广东风华高新科技股份有限公司 | Temperature-resistant electrolyte for aluminum electrolysis and application thereof |
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| CN1862728A (en) * | 2005-12-28 | 2006-11-15 | 横店集团东磁有限公司 | Flash lamp aluminum electrolytic capacitor and preparation method thereof |
| CN101483101A (en) * | 2008-12-25 | 2009-07-15 | 佛山市三水日明电子有限公司 | 125 DEG C high temperature long life aluminum electrolysis capacitor, production method thereof and special electrolysis liquid |
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