CN113539688B - Electrolyte for aluminum electrolytic capacitor with working voltage of 300-500V and aluminum electrolytic capacitor - Google Patents
Electrolyte for aluminum electrolytic capacitor with working voltage of 300-500V and aluminum electrolytic capacitor Download PDFInfo
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- CN113539688B CN113539688B CN202010275478.0A CN202010275478A CN113539688B CN 113539688 B CN113539688 B CN 113539688B CN 202010275478 A CN202010275478 A CN 202010275478A CN 113539688 B CN113539688 B CN 113539688B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/145—Liquid electrolytic capacitors
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
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- H01G9/022—Electrolytes; Absorbents
- H01G9/035—Liquid electrolytes, e.g. impregnating materials
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Abstract
In order to solve the problems of poor wide temperature performance, large leakage current return rise and short service life of a capacitor in the high-voltage application of the electrolyte for the aluminum electrolytic capacitor in the prior art, the invention provides the electrolyte for the aluminum electrolytic capacitor with the working voltage of 300-500V, which comprises a main solvent, a main solute and water, wherein the main solute comprises m-diazacyclopentene cations and organic carboxylic acid anions, the main solvent selects lactone compounds, and the content of the water is 0.01-2 percent based on the total weight of the electrolyte as 100 percent. The invention also provides an aluminum electrolytic capacitor, which comprises the electrolyte for the aluminum electrolytic capacitor with the working voltage of 300-500V. The electrolyte for the aluminum electrolytic capacitor with the working voltage of 300-500V has the advantages of excellent high voltage resistance, wide use temperature, low leakage current rising value and long service life of the capacitor.
Description
Technical Field
The invention belongs to the field of electrolyte for capacitors, and particularly relates to electrolyte for an aluminum electrolytic capacitor with a working voltage of 300-500V and an aluminum electrolytic capacitor.
Background
The aluminum electrolytic capacitor has wide application range, and particularly relates to the fields of household appliances, industry, agriculture, aerospace and the like. Aluminum electrolytic capacitors have the effects of tuning, filtering, coupling, bypassing, and energy conversion in the circuit and are inexpensive, which are not alternatives to other capacitors. At present, the traditional aluminum electrolytic capacitor with the high-voltage section voltage of 300-500V mainly uses ethylene glycol as a main solvent. Ethylene glycol is the electrolyte of the main solvent system, and is easy to fail due to capacity fading, dissipation factors (Dissipation Factor, DF) and other parameter degradation at the low temperature of-40 ℃. Moreover, as the market has gradually widened the demand for aluminum electrolytic capacitors, the wide temperature performance requirements for aluminum electrolytic capacitor electrolytes have also gradually become higher. This results in an electrolyte product with ethylene glycol as the main solvent system which cannot meet the market requirements, and development of a novel system electrolyte for aluminum electrolytic capacitors is very necessary.
The lactone solvent is mainly used in low-voltage section aluminum electrolyte with the voltage of less than 100V at present. The electrolyte of the lactone solvent system has excellent wide temperature performance, and all parameters can be kept within the qualified parameter range under the condition of low temperature of-55 ℃.
However, in the use of the high-voltage aluminum electrolytic capacitor with the working voltage of 300-500V, a more compact and stable aluminum oxide film needs to be formed on the surface of the positive foil, and the electrolyte with the lactone as a main solvent has limited capability of providing oxygen anions and limited capability of dissolving high-voltage solutes, so that the problems of poor high-voltage resistance, large leakage current return and short service life of the aluminum electrolytic capacitor using the electrolyte are caused.
Disclosure of Invention
The invention aims to solve the technical problems of poor high voltage resistance, large leakage current return rise and short service life of a capacitor of an electrolyte for an aluminum electrolytic capacitor in the prior art, and provides the electrolyte for the aluminum electrolytic capacitor with the working voltage of 300-500V and the aluminum electrolytic capacitor.
The technical scheme adopted by the invention for solving the problems is as follows:
in one aspect, the invention provides an electrolyte for an aluminum electrolytic capacitor with the working voltage of 300-500V, which comprises the following components:
a primary solvent, a primary solute and water, wherein the primary solvent comprises a lactone compound, and the primary solute comprises a meta-diazacyclopentene cation and an organic carboxylic acid anion; the content of the water is 0.01-2% based on 100% of the total weight of the electrolyte.
Optionally, the content of the main solvent is 55% -97% and the content of the main solute is 0.5% -12% based on 100% of the total weight of the electrolyte.
Optionally, the lactone compound comprises gamma-butyrolactone and/or gamma-valerolactone.
Optionally, the m-diazapentene cation comprises one or more of 1-ethyl-3-methyl-m-diazapentene cation, 1-ethyl-2, 3-dimethyl-m-diazapentene cation, 1,2,3, 4-tetramethyl-m-diazapentene cation, 1, 3-dimethyl-m-diazapentene cation, 1,2, 3-trimethyl-m-diazapentene cation, 2-methyl-m-diazapentene cation, 2-phenyl-m-diazapentene cation, and 2-propyl-2-m-diazapentene cation;
the organic carboxylic acid is selected from benzoic acid or a compound shown in a structural formula I:
wherein, P is selected from a main carbon chain with 1-20 carbon atoms, R 1 、R 2 、R 3 、R 4 Each independently selected from hydrogen, benzene ring, hydrocarbyl benzene ring, nitrobenzene ring, straight carbon chain with 1-8 carbon atoms, carbon chain with 1-8 branched carbon atoms or carboxyl, and R 1 、R 2 、R 3 、R 4 One or both of which are selected from carboxyl groups.
Optionally, the electrolyte further comprises an auxiliary solvent, wherein the auxiliary solvent comprises one or more of ethylene glycol, diethylene glycol, methoxypropanediol, dimethyl sulfoxide, propylene glycol, glycerol, N-butanol, N-octanol, sulfolane, N-methylformamide, N-dimethylformamide and N, N-diethylformamide, and the content of the auxiliary solvent is 4-20% based on the total weight of the electrolyte being 100%.
Optionally, the electrolyte further comprises auxiliary solutes, wherein the auxiliary solutes comprise one or more of dimethylamine, diethylamine, triethylamine, diethylamine azelate, dimethylamine azelate, triethylamine azelate, diethylamine sebacate, triethylamine sebacate and organic carboxylic acid with 5-15 carbon atoms and ammonium salt, and the content of the auxiliary solutes is 0.1-5% based on 100% of the total weight of the electrolyte.
Optionally, the electrolyte further comprises a waterproof agent, wherein the waterproof agent comprises one or more of mannitol, xylitol, alkyl phosphate, boric acid, ammonium pentaborate, hypophosphorous acid and ammonium salt, phosphoric acid and ammonium salt, phosphate ester, phosphorous acid and ammonium salt, phosphotungstic acid and ammonium salt, phosphomolybdic acid and ammonium salt, polyphosphoric acid and ammonium salt, and the content of the waterproof agent is 0.05% -3.5% based on the total weight of the electrolyte being 100%.
Optionally, the electrolyte further comprises a sparking lifting agent, wherein the sparking lifting agent comprises one or more of polyvinyl alcohol borate, polyvinyl alcohol with the polymerization degree of 200-5000, polyglycerol with the polymerization degree of 100-5000, polyacrylate with the polymerization degree of 200-5000, a silane coupling agent, polypropylene oxide ether, polymerized fatty acid and ammonium salt, nano silicon dioxide, organic silicon and ammonium polyacrylate, and the content of the sparking lifting agent is 3-12% based on the total weight of the electrolyte being 100%.
Optionally, the electrolyte further comprises a hydrogen eliminator, wherein the hydrogen eliminator comprises one or more of hydroquinone, resorcinol, p-nitrobenzyl alcohol, m-nitroacetophenone, p-nitrobenzoic acid, ammonium p-nitrobenzoate, p-nitrophenol, m-nitrophenol, o-nitrophenol, p-nitroacetophenone and o-nitroanisole, and the content of the hydrogen eliminator is 0.1-1.5% based on 100% of the total weight of the electrolyte.
On the other hand, the invention also provides an aluminum electrolytic capacitor, which comprises a positive foil, a negative foil, electrolytic paper and the electrolyte of any one of the above.
The electrolyte for the aluminum electrolytic capacitor with the working voltage of 300-500V provided by the invention takes lactone compounds as main solvents through optimizing the formula, and adds main solutes comprising m-diazacyclopentene cations and organic carboxylic acid anions and water; because the high-voltage aluminum electrolytic capacitor needs a compact and stable aluminum oxide film on the surface of the positive foil to ensure the insulation voltage endurance capability in the work, and the electrolyte with lactone as the main solvent has limited capability of providing oxygen anions, the aluminum electrolytic capacitor has insufficient voltage endurance, large leakage current return and short service life. The invention provides sufficient oxygen anions by adding a certain amount of water, so that the electrolyte has excellent high-voltage resistance, wide use temperature range, small rise value of low leakage current and long service life of the capacitor.
Drawings
Fig. 1 is a diagram of a test method for testing sparking voltage provided by the invention.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects solved by the invention more clear, the invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The invention provides electrolyte for a 300-500V aluminum electrolytic capacitor, which comprises the following components:
a primary solvent, a primary solute and water, wherein the primary solvent comprises a lactone compound, and the primary solute is composed of a meta-diazacyclopentene cation and an organic carboxylic acid; the content of water is 0.01% -2% based on 100% of the total weight of the electrolyte.
The aluminum electrolytic capacitor has the advantages of improving the withstand voltage of the capacitor, reducing leakage current and prolonging the service life of the capacitor product by improving the insulating capability of the positive foil. While improving the insulating ability of the positive foil, it is necessary to form a dense and stable aluminum oxide film on the surface thereof, and thus it is also necessary that the electrolyte provide sufficient oxygen anions. The oxygen anions form alumina with aluminum ions on the surface of the aluminum foil, and insulating repair is carried out on the place where the surface of the positive foil is damaged. The better the insulation of the positive foil is, the higher the withstand voltage is, and the smaller the leakage current in the placing process is; meanwhile, under the high-voltage condition, the oxygen anions repair the damaged oxide film in time, so that the breakdown failure condition of the capacitor in the use process can be prevented. The electrolyte using lactone compound as main solvent has very limited capability of providing oxygen anions, so that the electrolyte of the system has larger defects in the aspects of voltage resistance and leakage current rise, and the service life of the capacitor is easily shortened, and the leakage current rise is large. In order to provide enough oxygen anions, the invention adds 0.01 to 2 percent of water, and the content of the water in the range ionizes to generate oxygen anions which are enough to provide the oxygen anions needed for repairing the oxide film, so that the product of the system has the characteristics of excellent high pressure resistance, low leakage current value and service life.
If the added moisture content of the electrolyte is more than 2%, firstly, excessive moisture reacts with the aluminum oxide film to form aluminum hydroxide, so that the compactness of the oxide film on the surface of the positive foil is affected, and the problems of poor wide-temperature performance of the high-voltage section of the electrolyte for the capacitor, large leakage current rise and shortened service life of the capacitor are caused. Second, a large amount of moisture can electrolytically generate gas, causing severe capacitor over-solder bump.
The electrolyte provided by the invention takes lactone compounds with optimized formulas as main solvents, and adds main solutes comprising meta-diazacyclopentene cations and organic carboxylic acid anions and water, because oxygen anions are needed for forming compact and stable aluminum oxide films on the surface of positive foil of the aluminum electrolytic capacitor and the capacity of providing oxygen anions by the lactone main solvents is limited, the high-voltage resistance performance of the aluminum electrolytic capacitor is poor, the leakage current is increased and the service life is short.
The lactone solvent system can be applied to high-voltage aluminum electrolytic capacitors with the working voltage of 300-500V.
In some embodiments of the present invention, the content of the main solvent is 55% to 97% and the content of the main solute is 0.5% to 12% based on 100% of the total weight of the electrolyte.
In some embodiments of the invention, the lactone compound includes gamma-butyrolactone and/or gamma-valerolactone.
Preferably, gamma-butyrolactone is used as the main solvent.
In some embodiments of the invention, the m-diazapentene cation comprises one or more of 1-ethyl-3-methyl-m-diazapentene cation, 1-ethyl-2, 3-dimethyl-m-diazapentene cation, 1,2,3, 4-tetramethyl-m-diazapentene cation, 1, 3-dimethyl-m-diazapentene cation, 1,2, 3-trimethyl-m-diazapentene cation, 2-methyl-m-diazapentene cation, 2-phenyl-m-diazapentene cation, and 2-propyl-2-m-diazapentene cation;
the organic carboxylic acid is selected from benzoic acid or a compound shown in a structural formula I:
wherein, P is selected from a main carbon chain with 1-20 carbon atoms, R 1 、R 2 、R 3 、R 4 Each independently selected from hydrogen, benzene ring, hydrocarbyl benzene ring, nitrobenzene ring, straight carbon chain with 1-8 carbon atoms, carbon chain with 1-8 branched carbon atoms or carboxyl, and R 1 、R 2 、R 3 、R 4 One or both of which are selected from carboxyl groups.
In some embodiments of the invention, the electrolyte further comprises an auxiliary solvent comprising one or more of ethylene glycol, diethylene glycol, methoxypropanediol, dimethyl sulfoxide, propylene glycol, glycerol, N-butanol, N-octanol, sulfolane, N-methylformamide, N-dimethylformamide, and N, N-diethylformamide.
Preferably, the auxiliary solvent is selected from the group consisting of ethylene glycol, a combination of ethylene glycol and sulfolane.
The content of the auxiliary solvent is 4-20% based on 100% of the total weight of the electrolyte.
When the main solvent is selected from lactone compounds, the invention often adds some additives in a preferred scheme, and because the additives are difficult to dissolve in the lactone compounds, auxiliary solvents are needed to aid the dissolution of the additives.
In some embodiments of the present invention, the electrolyte further comprises an auxiliary solute comprising one or more of dimethylamine, diethylamine, triethylamine, diethylamine azelate, dimethylamine azelate, triethylamine azelate, diethylamine sebacate, triethylamine sebacate, and an organic carboxylic acid having 5 to 15 carbon atoms and an ammonium salt, wherein the auxiliary solute is present in an amount of 0.1 to 5% based on 100% by weight of the total electrolyte.
The organic carboxylic acid and ammonium salt with 5-15 carbon atoms comprise adipic acid and ammonium salt, benzoic acid and ammonium salt, sebacic acid and ammonium salt and dodecadienoic acid ammonium salt.
In some embodiments of the present invention, the electrolyte further includes a waterproofing agent including one or more of mannitol, xylitol, alkyl phosphate, boric acid, ammonium pentaborate, hypophosphorous acid and ammonium salt, phosphoric acid and ammonium salt, phosphate ester, phosphorous acid and ammonium salt, phosphotungstic acid and ammonium salt, phosphomolybdic acid and ammonium salt, and polyphosphoric acid and ammonium salt, the waterproofing agent being present in an amount of 0.05% to 3.5% based on 100% by weight of the total electrolyte.
In the invention, the use of the waterproof mixture densifies the alumina film on the surface of the aluminum electrolytic capacitor, and further improves the high voltage resistance of the electrolyte and reduces the leakage current rise.
In some embodiments of the present invention, the electrolyte further comprises a flash-fire promoting agent comprising one or more of polyvinyl alcohol borate, polyvinyl alcohol having a polymerization degree of 200 to 5000, polyglycerol having a polymerization degree of 100 to 5000, polypropylene alcohol having a polymerization degree of 200 to 5000, a silane coupling agent, polypropylene oxide ether, polymerized fatty acid and ammonium salt, nano-silica, organic silicon and ammonium polyacrylate, the content of the flash-fire promoting agent being 3 to 12% based on 100% by weight of the total electrolyte.
The addition of the sparking enhancing agent has obvious sparking voltage effect on the electrolyte, has little influence on conductivity, can improve the service life and stability of the capacitor, and improves the leakage current rise.
In some embodiments of the invention, the electrolyte further comprises a hydrogen scavenger comprising one or more of hydroquinone, resorcinol, p-nitrobenzyl alcohol, m-nitroacetophenone, p-nitrobenzoic acid, ammonium p-nitrobenzoate, p-nitrophenol, m-nitrophenol, o-nitrophenol, p-nitroacetophenone, and o-nitroanisole, the hydrogen scavenger being present in an amount of 0.1% to 1.5% based on 100% total weight of the electrolyte.
The invention also provides an aluminum electrolytic capacitor, which comprises a positive foil, a negative foil, electrolytic paper and the electrolyte of any one of the above.
The invention is further illustrated by the following examples. It is to be understood that the present invention is not limited to the following embodiments, and the methods are regarded as conventional methods unless otherwise specified. Materials are commercially available from public sources unless otherwise indicated.
Example 1
This example is for illustrating the working voltage 300-500V electrolyte for aluminum electrolytic capacitor and the preparation method thereof.
Based on 100 percent of the total weight of the electrolyte, the electrolyte comprises the following components:
(1) Gamma-butyrolactone 86.0%
(2) 1.5% of 1-ethyl-3-methyl-m-diazepine cation
(3) 2-butyl-suberic acid 1.5%
(4) Organosilicon 10%
(5) P-nitrobenzyl alcohol 0.5%
(6) Water 0.5%
The preparation method comprises the following steps:
(1) According to the components, firstly, mixing 1-ethyl-3-methyl m-diazacyclopentene cation and 2-butyl-suberic acid to prepare a main solute;
(2) According to the components, gamma-butyrolactone, main solute, organic silicon, p-nitrobenzyl alcohol and water are uniformly mixed to prepare electrolyte, and the electrolyte is marked as S1.
Example 2
This example is for illustrating the working voltage 300-500V electrolyte for aluminum electrolytic capacitor and the preparation method thereof.
Based on 100 percent of the total weight of the electrolyte, the electrolyte comprises the following components:
(1) Gamma-butyrolactone 77.9%
(2) 5.5% of 1-ethyl-3-methyl-m-diazepine cation
(3) 2-butyl-suberic acid 5.5%
(4) Hypophosphorous acid and ammonium salt 0.1%
(5) Organosilicon 10%
(6) P-nitrobenzyl alcohol 0.5%
(7) Water 0.5%
The preparation method comprises the following steps:
(1) According to the components, firstly, mixing 1-ethyl-3-methyl m-diazacyclopentene cation and 2-butyl-suberic acid to prepare a main solute;
(2) According to the components, the gamma-butyrolactone, the main solute, the hypophosphorous acid and ammonium salt, the organic silicon, the p-nitrobenzyl alcohol and the water are uniformly mixed to prepare the electrolyte, and the electrolyte is marked as S2.
Example 3
This example is for illustrating the working voltage 300-500V electrolyte for aluminum electrolytic capacitor and the preparation method thereof.
Based on 100 percent of the total weight of the electrolyte, the electrolyte comprises the following components:
(1) Gamma-butyrolactone 74.5%
(2) 5.5% of 1-ethyl-3-methyl-m-diazepine cation
(3) 2-hexyl-adipic acid 5.5%
(4) Ethylene glycol 5%
(5) Hypophosphorous acid and ammonium salt 0.1%
(6) Inorganic nano silicon dioxide 8%
(7) P-nitrobenzyl alcohol 0.7%
(8) Water 0.7%
The preparation method comprises the following steps:
(1) According to the components, firstly, mixing 1-ethyl-3-methyl m-diazacyclopentene cation and 2-hexyl-adipic acid to prepare a main solute;
(2) According to the components, the gamma-butyrolactone, the main solute, the ethylene glycol, the hypophosphorous acid and ammonium salt, the inorganic nano silicon dioxide, the p-nitrobenzyl alcohol and the water are uniformly mixed to prepare the electrolyte, and the electrolyte is marked as S3.
Example 4
This example is for illustrating the working voltage 300-500V electrolyte for aluminum electrolytic capacitor and the preparation method thereof.
Based on 100 percent of the total weight of the electrolyte, the electrolyte comprises the following components:
(1) Gamma-butyrolactone 74.0%
(2) 7% of 1,2,3, 4-tetramethyl-m-diazacyclopentene cation
(3) 2-hexyl-adipic acid 7%
(4) 0.5% of ammonium sebacate
(5) 10% of inorganic nano silicon dioxide
(6) M-nitroacetophenone 0.5%
(7) Water 1.0%
The preparation method comprises the following steps:
(1) According to the components, firstly, mixing 1,2,3, 4-tetramethyl-m-diazacyclopentene cations and 2-hexyl-adipic acid to prepare a main solute;
(2) According to the components, the gamma-butyrolactone, the main solute, ammonium sebacate, inorganic nano silicon dioxide, organic silicon, m-nitroacetophenone and water are uniformly mixed to prepare the electrolyte, and the electrolyte is marked as S4.
Comparative example 1
This comparative example is used for comparative illustration of the electrolyte for an aluminum electrolytic capacitor with the working voltage of 300-500V and the preparation method thereof.
The comparative composition, based on 100% total weight of electrolyte, comprises the following components:
(1) Gamma-butyrolactone 80.5%
(2) 5.5% of 1,2,3, 4-tetramethyl-m-diazacyclopentene cation
(3) Benzoic acid 5.5%
(4) Organosilicon 8%
(5) P-nitrophenol 0.5%
The preparation method comprises the following steps:
(1) According to the components, firstly, mixing 1,2,3, 4-tetramethyl-m-diazacyclopentene cations and benzoic acid to prepare a main solute;
(2) According to the components, gamma-butyrolactone, main solute, organic silicon and p-nitrophenol are uniformly mixed to prepare the contrast electrolyte, and the contrast electrolyte is marked as D1.
Comparative example 2
This comparative example is used for comparative illustration of the electrolyte for an aluminum electrolytic capacitor with the working voltage of 300-500V and the preparation method thereof.
The comparative composition, based on 100% total weight of electrolyte, comprises the following components:
(1) Gamma-butyrolactone 86.5%
(2) 1.5% of 1-ethyl-3-methyl-m-diazepine cation
(3) 2-butyl-suberic acid 1.5%
(4) Organosilicon 10%
(5) P-nitrobenzyl alcohol 0.5%
The preparation method comprises the following steps:
(1) According to the components, firstly, mixing 1-ethyl-3-methyl m-diazacyclopentene cation and 2-butyl-suberic acid to prepare a main solute;
(2) According to the components, gamma-butyrolactone, main solute, organic silicon and p-nitrobenzyl alcohol are uniformly mixed to prepare the contrast electrolyte, which is marked as D2.
Comparative example 3
This comparative example is used for comparative illustration of the electrolyte for an aluminum electrolytic capacitor with the working voltage of 300-500V and the preparation method thereof.
The comparative composition, based on 100% total weight of electrolyte, comprises the following components:
(1) 86.5% of ethylene glycol
(2) 1.5% of 1-ethyl-3-methyl-m-diazepine cation
(3) 2-butyl-suberic acid 1.5%
(4) Organosilicon 10%
(5) P-nitrobenzyl alcohol 0.5%
The preparation method comprises the following steps:
(1) According to the components, firstly, mixing 1-ethyl-3-methyl m-diazacyclopentene cation and 2-butyl-suberic acid to prepare a main solute;
(2) According to the components, ethylene glycol, a main solute, organic silicon and p-nitrobenzyl alcohol are uniformly mixed to prepare a contrast electrolyte, and the contrast electrolyte is marked as D3.
Comparative example 4
This comparative example is used for comparative illustration of the electrolyte for an aluminum electrolytic capacitor with the working voltage of 300-500V and the preparation method thereof.
The comparative composition, based on 100% total weight of electrolyte, comprises the following components:
(1) Gamma-butyrolactone 84.0%
(2) 1.5% of 1-ethyl-3-methyl-m-diazepine cation
(3) 2-butyl-suberic acid 1.5%
(4) Organosilicon 10%
(5) P-nitrobenzyl alcohol 0.5%
(6) Water 2.5%
The preparation method comprises the following steps:
(1) According to the components, firstly, mixing 1-ethyl-3-methyl m-diazacyclopentene cation and 2-butyl-suberic acid to prepare a main solute;
(2) According to the components, gamma-butyrolactone, main solute, organic silicon, p-nitrobenzyl alcohol and water are uniformly mixed to prepare the electrolyte with the contrast, and the electrolyte is marked as D4.
Performance testing
And performing performance tests on the S1-S4 and the comparative samples D1-D4 obtained by the preparation.
1. And respectively carrying out conductivity tests and sparking voltage tests on the S1-S4 and the comparative samples D1-D4 obtained by the preparation.
(1) Conductivity of
Conductivity of the above prepared S1 to S4 and comparative samples D1 to D4 were respectively tested using a conductivity meter.
(2) Sparking voltage
The sparking voltages of the above prepared S1-S4 and comparative samples D1-D4 were tested using a test method shown in FIG. 1, wherein the test conditions are voltages: the voltage of the steel is 800V,
current flow: 20mA, temperature: 30 ℃.
The test results obtained are filled in Table 1.
TABLE 1
As is clear from Table 1, examples S1 to S4 have higher conductivity and sparking voltage than the case where the lactone type solvent is used as the main solvent than the case where the ethylene glycol is used as the main solvent, as compared with D3.
2. The prepared electrolytes S1-S4 and the comparative samples D1-D4 are respectively tested and calculated at 20 ℃ and-55 ℃ to obtain capacitance values (C), delta C (%), dissipation factor loss angles (DF), impedance (Z) and impedance ratios, wherein the specification and the size of the capacitor core pack are selected: 400V6.8. Mu.F, phi.10X12.
The test results obtained are filled in table 2.
TABLE 2
As can be seen from Table 2, in the examples S1 to S4 in which water was added, the various parameters at a low temperature of-55℃were satisfactory, whereas in the case of adding excessive water, the various parameters at a low temperature of-55℃were unsatisfactory.
3. Carrying out load tests on the S1-S4 and the comparative samples D1-D4 obtained by the preparation at the high temperature of 125 ℃ to test the capacitance value (Cap), dissipation factor loss angle (DF), leakage current rise value (LC), delta C (%) and gas production condition of the capacitor, wherein the specification and the size of the capacitor core package are selected: 400V6.8. Mu.F, phi.10X12.
The test results obtained are filled in Table 3.
TABLE 3 Table 3
As can be seen from Table 3, when the load life of the water-added examples S1 to S4 is 5000H at the high temperature of 125 ℃, the parameters are in the qualified range, and the service life requirement of 5000H at 125 ℃ can be met; in comparative examples D1 to D2, due to the lack of oxygen anions provided by water, damaged oxide films cannot be repaired in time in the load life process, the insulativity is reduced, and breakdown failure occurs before 2000H is taken way; d3 using ethylene glycol as a main solvent, wherein the pressure resistance is insufficient, the gas production is serious, and the convex bottom is opened, so that each parameter exceeds standard and fails; in comparative example D4, the oxide film was broken down by adding excessive water, and the insulation was lowered, resulting in breakdown failure before 2000H.
4. Storage tests are carried out on the S1-S4 and the comparative samples D1-D4 obtained by the preparation at the high temperature of 105 ℃ to test the capacitance value (Cap), dissipation factor loss angle (DF), leakage current rise value (LC) and delta C (%) of the capacitor, wherein the specification and the size of the capacitor core package are selected: 400V6.8. Mu.F, phi.10X12.
The test results obtained are filled in table 4.
TABLE 4 Table 4
As is clear from Table 4, the leakage current rise values of examples S1 to S4 were small, and the leakage current rise was severe as compared with comparative examples D1 to D4. From the analysis, it was found that comparative examples D1 to D3 lack oxygen anions, and cannot repair the aluminum oxide film in time, and the insulation of the aluminum oxide film is lowered, resulting in a rapid increase in leakage current, and comparative example D4, which added excessive water, damages the aluminum oxide film, and the insulation of the aluminum oxide film is lowered, resulting in a rapid increase in leakage current.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (9)
1. The electrolyte for the aluminum electrolytic capacitor with the working voltage of 300-500V is characterized by comprising the following components:
a primary solvent, a primary solute, and water;
wherein the main solvent comprises a lactone compound;
the primary solute comprises a meta-diazacyclopentene cation and an organic carboxylic acid anion;
the content of the water is 0.5% -2% based on 100% of the total weight of the electrolyte;
the m-diazapentene cation includes one or more of 1-ethyl-3-methyl-m-diazapentene cation, 1-ethyl-2, 3-dimethyl-m-diazapentene cation, 1,2, 3-trimethyl-m-diazapentene cation, 2-methyl-m-diazapentene cation, 2-phenyl-m-diazapentene cation and 2-propyl-2-m-diazapentene cation;
the organic carboxylic acid anion is selected from compounds shown in a structural formula I:
structural formula I
Wherein, P is selected from a main carbon chain with 5-20 carbon atoms, R 1 、R 2 、R 3 、R 4 Each independently selected from hydrogen, benzene ring, hydrocarbyl benzene ring, nitrobenzene ring, straight carbon chain with 1-8 carbon atoms, carbon chain with 1-8 branched carbon atoms or carboxyl, and R 1 、R 2 、R 3 、R 4 Is selected from carboxyl groups.
2. The electrolyte according to claim 1, wherein the content of the main solvent is 55% to 97% and the content of the main solute is 0.5% to 12% based on 100% of the total weight of the electrolyte.
3. Electrolyte according to claim 1, characterized in that the lactone-type compound comprises gamma-butyrolactone and/or gamma-valerolactone.
4. The electrolyte of claim 2, further comprising an auxiliary solvent, wherein the auxiliary solvent comprises one or more of ethylene glycol, diethylene glycol, methoxypropanediol, dimethyl sulfoxide, propylene glycol, glycerol, N-butanol, N-octanol, sulfolane, N-methylformamide, N-dimethylformamide and N, N-diethylformamide, and the auxiliary solvent is present in an amount of 4% to 20% based on 100% of the total weight of the electrolyte.
5. The electrolyte according to claim 2, further comprising an auxiliary solute comprising one or more of dimethylamine, diethylamine, triethylamine, diethylamine azelate, dimethylamine azelate, triethylamine azelate, diethylamine sebacate, triethylamine sebacate and an organic carboxylic acid having 5 to 15 carbon atoms and an ammonium salt, wherein the auxiliary solute is contained in an amount of 0.1 to 5% based on 100% by weight of the total electrolyte.
6. The electrolyte of claim 2, further comprising a water-repellent agent comprising one or more of mannitol, xylitol, alkyl phosphate, boric acid, ammonium pentaborate, hypophosphorous acid and ammonium salt, phosphoric acid and ammonium salt, phosphate ester, phosphorous acid and ammonium salt, phosphotungstic acid and ammonium salt, phosphomolybdic acid and ammonium salt, and polyphosphoric acid and ammonium salt, the water-repellent agent being present in an amount of 0.05% to 3.5% based on 100% by weight of the total electrolyte.
7. The electrolyte of claim 2 further comprising a flash fire booster comprising one or more of polyvinyl alcohol borate, polyvinyl alcohol having a degree of polymerization of 200 to 5000, polyglycerol having a degree of polymerization of 100 to 5000, polyacrylate having a degree of polymerization of 200 to 5000, silane coupling agent, polypropylene oxide ether, polymerized fatty acid and ammonium salt, nano silica, silicone and ammonium polyacrylate, the flash fire booster being present in an amount of 3% to 12% based on 100% by weight of the total electrolyte.
8. The electrolyte of claim 2, further comprising a hydrogen scavenger comprising one or more of hydroquinone, resorcinol, p-nitrobenzyl alcohol, m-nitroacetophenone, p-nitrobenzoic acid, ammonium p-nitrobenzoate, p-nitrophenol, m-nitrophenol, o-nitrophenol, p-nitroacetophenone, and o-nitroanisole, wherein the hydrogen scavenger is present in an amount of 0.1% to 1.5% based on 100% by weight of the total electrolyte.
9. An aluminum electrolytic capacitor comprising a positive foil, a negative foil, an electrolytic paper, and the electrolytic solution according to any one of claims 1 to 8.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1116785A (en) * | 1997-04-30 | 1999-01-22 | Nippon Chemicon Corp | Electrolytic solution for electrolytic capacitor |
| JP2011091282A (en) * | 2009-10-26 | 2011-05-06 | Sanyo Chem Ind Ltd | Electrolyte for aluminum electrolytic capacitor, and aluminum electrolytic capacitor using the same |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09148196A (en) * | 1995-11-27 | 1997-06-06 | Elna Co Ltd | Aluminium electrolytic capacitor and electrolyte for the aluminium electrolytic capacitor drive use |
| US8828261B2 (en) * | 2009-11-26 | 2014-09-09 | Panasonic Corporation | Electrolytic solution for aluminum electrolytic capacitor, and aluminum electrolytic capacitor using same |
| CN103843091B (en) * | 2011-10-14 | 2017-03-08 | 三洋化成工业株式会社 | Electrolyte for aluminum electrolytic capacitor and the aluminium electrolutic capacitor using this electrolyte |
| JP6422165B2 (en) * | 2014-01-28 | 2018-11-14 | 富山薬品工業株式会社 | Electrolytic solution for electrolytic capacitor drive |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1116785A (en) * | 1997-04-30 | 1999-01-22 | Nippon Chemicon Corp | Electrolytic solution for electrolytic capacitor |
| JP2011091282A (en) * | 2009-10-26 | 2011-05-06 | Sanyo Chem Ind Ltd | Electrolyte for aluminum electrolytic capacitor, and aluminum electrolytic capacitor using the same |
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