CN111029153A - Electrolyte for ultralow-temperature aluminum electrolytic capacitor and preparation method thereof - Google Patents
Electrolyte for ultralow-temperature aluminum electrolytic capacitor and preparation method thereof Download PDFInfo
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- CN111029153A CN111029153A CN201911285038.7A CN201911285038A CN111029153A CN 111029153 A CN111029153 A CN 111029153A CN 201911285038 A CN201911285038 A CN 201911285038A CN 111029153 A CN111029153 A CN 111029153A
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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
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/035—Liquid electrolytes, e.g. impregnating materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
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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
- H01G9/004—Details
- H01G9/08—Housing; Encapsulation
Abstract
The invention belongs to the technical field of aluminum electrolytic capacitors, and particularly relates to an electrolyte for an ultralow-temperature aluminum electrolytic capacitor and a preparation method thereof. The electrolyte for the ultralow-temperature aluminum electrolytic capacitor comprises the following raw materials in percentage by mass, 40-50% of a first solvent, 20-30% of a second solvent, 5-10% of a third solvent, 1-15% of a solute and 0.5-5% of an additive, wherein the additive comprises one or more of a hydrogen scavenger and a high-temperature stabilizer, so that the ultralow-temperature aluminum electrolytic capacitor is not frozen at ultralow temperature, the resistivity change is small, the produced aluminum electrolytic capacitor can be normally used at-55-105 ℃, the aluminum electrolytic capacitor sealing rubber is not corroded, the sealing performance is good, the service life is more stable, extra materials and process cost are not required to be added, and the ultralow-temperature aluminum electrolytic capacitor is suitable for mass production and use.
Description
Technical Field
The invention belongs to the technical field of aluminum electrolytic capacitors, and particularly relates to an electrolyte for an ultralow-temperature aluminum electrolytic capacitor and a preparation method thereof.
Background
The capacitor is a common device on an electronic circuit, plays electric roles of filtering, bypassing, coupling, decoupling, phase inversion and the like, and the aluminum electrolytic capacitor is the most special and most key component of the capacitor, has wide application in electric appliances, and can be said that no aluminum electrolytic capacitor is used, so that the diversified and powerful functions of the electric appliances are not used.
Due to the wide range of applications of electrical appliances, especially the extremely low temperature in the winter in the north, severe demands are placed on the use of aluminum electrolytic capacitors, among which the liquid electrolyte (generally referred to as electrolyte in the art) is the dominant one. The aluminum electrolytic capacitor produced by the common electrolyte can only be applied to a working environment above minus 40 ℃, and the capacity of the capacitor is extremely low in an ultralow temperature environment below minus 40 ℃, particularly at about minus 55 ℃, mainly because the electrolyte in the aluminum electrolytic capacitor can be frozen in the ultralow temperature environment or because the resistance of the electrolyte becomes extremely high, the basic function of the capacitor is lost, and the electrical appliance cannot be started. The existing part of aluminum electrolytic capacitors adopt GBL system aluminum electrolyte, and the electrolyte has relatively high resistivity, so that the produced capacitor has poor performance at normal temperature; secondly, GBL has extremely strong corrosivity to rubber (can dissolve common rubber), and the basic sealing performance can be achieved only by special materials and manufacturing processes, so that the overall cost of the capacitor is increased; thirdly, the GBL system electrolyte has great difficulty in the manufacturing process and the like.
Disclosure of Invention
In order to solve the problems that the electrolyte for the aluminum electrolytic capacitor has large resistivity and small capacity of the aluminum electrolytic capacitor, the electrical appliance cannot be started, the performance of the aluminum electrolytic capacitor is poor under the normal temperature and the ultralow temperature conditions, sealing rubber is easy to corrode, the service life is seriously shortened, the cost is high, the process difficulty is extremely high and the like, the invention provides the electrolyte for the ultralow temperature aluminum electrolytic capacitor and the preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the electrolyte for the ultralow temperature aluminum electrolytic capacitor comprises the following raw materials, by mass, 40-50% of a first solvent, 20-30% of a second solvent, 5-10% of a third solvent, 1-15% of a solute and 0.5-5% of an additive, wherein the additive comprises one or more of a hydrogen scavenger and a high-temperature stabilizer.
Further, the first solvent includes ethylene glycol.
Further, the second solvent includes water.
Further, the third solvent comprises one or more of sulfolane, 1, 2-propylene glycol, ethylene glycol monomethyl ether, and N, N-dimethylacetamide.
Further, the solute comprises one or more of ammonium adipate, adipic acid, ammonium succinate and ammonium formate.
Further, the hydrogen eliminating agent comprises one or more of p-nitrobenzoic acid, p-nitroaniline ammonium formate and p-nitroanisole.
Further, the high temperature stabilizer includes one or more of mannitol, citric acid, phosphoric acid and salts thereof.
A method for preparing electrolyte for an ultralow temperature aluminum electrolytic capacitor,
s1: uniformly mixing the first solvent and the second solvent, heating to 40-65 ℃, and keeping the temperature for 5-15 min;
s2: adding a third solvent into the mixed solution in the S1, heating to 75-90 ℃, and keeping the temperature for 20-40 min;
s3: then adding a solute and a high-temperature stabilizer, heating to 110 ℃, and keeping the temperature for 50-70 min;
s4: cooling to 80-90 deg.C, adding hydrogen eliminating agent, and keeping the temperature for 25-35 min;
s5: and cooling to below 60 ℃ to obtain the ultralow temperature electrolyte.
Further, the mass percent of the high-temperature stabilizer is 0.5-2%.
Further, the mass percent of the hydrogen eliminating agent is 0.5-2.5%.
The invention provides an electrolyte for an ultralow temperature aluminum electrolytic capacitor, which comprises the following raw materials, by mass, 40-50% of a first solvent, 20-30% of a second solvent, 5-10% of a third solvent, 1-15% of a solute and 0.5-5% of an additive, wherein the additive comprises one or more of a hydrogen scavenger and a high-temperature stabilizer, so that the ultralow temperature electrolyte has the following advantages:
1. the material can be normally used at the temperature of between 55 ℃ below zero and 105 ℃, is not frozen, and has small resistivity change;
2. the ultralow-temperature electrolyte is applied to an aluminum electrolytic capacitor under the normal temperature condition, the performance of the aluminum electrolytic capacitor is excellent, the level of a high-frequency low-resistance product which is generally used in the prior art is reached, the loss angle or ESR reaches less than half of that of a GBL system electrolyte, the product generates less heat, and the self-consumption energy is less;
3. the sealing rubber has the advantages that the common rubber is not corroded, the sealing performance is good, the service life is more stable, and extra materials and process cost are not required to be increased;
4. the composition materials are common, and the cost is low; the preparation process is simple and is suitable for mass production and use.
Drawings
FIG. 1 is a flow chart of a method for preparing an electrolyte for an ultra-low temperature aluminum electrolytic capacitor.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments.
The electrolyte for the ultralow temperature aluminum electrolytic capacitor comprises the following raw materials, by mass, 40-50% of a first solvent, 20-30% of a second solvent, 5-10% of a third solvent, 1-15% of a solute and 0.5-5% of an additive, wherein the additive comprises one or more of a hydrogen scavenger and a high-temperature stabilizer.
The solvent is used for dissolving the electrolyte and ionizing the electrolyte, and has low steam pressure at the highest use temperature and does not freeze at the lowest use temperature; the electrolyte can still be ionized and conducted under the ultralow temperature condition. Therefore, for the selection of the solvent, the ultralow temperature electrolyte must be suitable for use and not frozen under the condition of-55 ℃, and the temperature exceeds the freezing point of most of the solvents in the prior art, such as the freezing point of a first solvent, namely ethylene glycol, is-12.6 ℃, the freezing point of a second solvent, namely water is 0 ℃, and the like, although the freezing point is obviously reduced after the two solvents are mixed, the ionization effect is also obviously reduced, namely the conductivity is obviously poor, and the target requirement cannot be met, so that a solvent with a lower freezing point must be added to achieve a solvent with stronger ionization capacity under the ultralow temperature condition, and a third solvent is selected from sulfolane, 1, 2-propylene glycol, ethylene glycol monomethyl ether or N, N-dimethylacetamide;
the solute is selected mainly from electrolytes suitable for ultralow temperature electrolyte, such as ammonium adipate, adipic acid, ammonium succinate, ammonium formate and the like, and has the main effects that the electrolytes can be easily ionized in a solvent and are less influenced by temperature, but the solutes need to be matched for use, otherwise, the problems of conductivity, service life, obvious increase of resistivity under ultralow temperature conditions, incapability of reaching the use under ultralow temperature conditions and the like easily occur.
For the selection of additives, the additives mainly comprise a hydrogen eliminating agent, a high-temperature stabilizer and the like, the performance of the hydrogen eliminating agent is single, and the types of the hydrogen eliminating agent are generally not too many, such as p-nitrobenzoic acid, p-nitrobenzoic ammonium formate, p-nitroanisole and the like; however, the high-temperature stabilizer has more types, the single use effect is not ideal, and most occasions are matched with various types of high-temperature stabilizers, wherein mannitol, citric acid, phosphoric acid and salts thereof are mainly selected from one or more types of high-temperature stabilizers.
Example one
As shown in fig. 1, in order to prepare the electrolyte for the ultra-low temperature aluminum electrolytic capacitor, the preparation method is as follows:
s1: uniformly mixing the first solvent and the second solvent, heating to 40-65 ℃, and keeping the temperature for 5-15 min;
s2: adding a third solvent into the mixed solution in the S1, heating to 75-90 ℃, and keeping the temperature for 20-40 min;
s3: then adding a solute and a high-temperature stabilizer, heating to 110 ℃, and keeping the temperature for 50-70 min;
s4: cooling to 80-90 deg.C, adding hydrogen eliminating agent, and keeping the temperature for 25-35 min;
s5: and cooling to below 60 ℃ to obtain the ultralow temperature electrolyte.
Mixing 40-50% ethylene glycol and 20-30% water, heating to 50 deg.C, and keeping the temperature for 10 min; then adding 5-10% sulfolane, continuing to heat to 85 ℃, and preserving heat for 30 min; adding 8-15% ammonium adipate, 1-3% adipic acid, 3-5% mannitol, 0.5-2% citric acid, 0.5-2% ammonium dihydrogen phosphate, 1-3% ammonium succinate, and 1-3% ammonium formate, heating to 105 deg.C, and maintaining the temperature for 60 min; then cooling to 85 ℃, adding 0.5-2.5% of p-nitrobenzoic acid, and preserving heat for 30 min; finally, continuously cooling to below 60 ℃ to obtain the ultralow temperature electrolyte A.
Preferably, 45% of ethylene glycol, 25% of water, 7% of sulfolane, 10% of ammonium adipate, 2.5% of adipic acid, 2% of mannitol, 1% of citric acid, 2% of ammonium dihydrogen phosphate, 2% of ammonium succinate, 1.5% of ammonium formate and 2% of p-nitrobenzoic acid.
Example two
Mixing 43% ethylene glycol and 22% water, heating to 50 deg.C, and keeping the temperature for 10 min; then adding 8 percent of 1, 2-propylene glycol, continuously heating to 85 ℃, and preserving heat for 30 min; adding 13% ammonium adipate, 2% adipic acid, 4% mannitol, 1% citric acid, 1.5% diammonium hydrogen phosphate, 2% ammonium succinate and 2% ammonium formate, heating to 105 deg.C, and maintaining the temperature for 60 min; then cooling to 85 ℃, adding 1.5% of ammonium p-nitrobenzoate, and preserving heat for 30 min; finally, continuously cooling to below 60 ℃ to obtain the ultralow temperature electrolyte B.
EXAMPLE III
Mixing 45% ethylene glycol and 25% water, heating to 50 deg.C, and keeping the temperature for 10 min; then adding 9% ethylene glycol monomethyl ether, continuously heating to 85 ℃, and keeping the temperature for 30 min; adding 8% ammonium adipate, 1.5% adipic acid, 3% mannitol, 1.5% citric acid, 2% diammonium hydrogen phosphate, 3% ammonium succinate and 2% ammonium formate, heating to 105 deg.C, and maintaining the temperature for 60 min; then cooling to 85 ℃, and preserving heat for 30 min; and finally, continuously cooling to below 60 ℃ to obtain the ultralow-temperature electrolyte C.
Example four
Mixing 48% of ethylene glycol and 26% of water, heating to 50 ℃, and keeping the temperature for 10 min; then adding 5% N, N-dimethylacetamide, continuously heating to 85 ℃, and keeping the temperature for 30 min; adding 8% ammonium adipate, 2% adipic acid, 3% mannitol, 1% citric acid, 1% phosphoric acid, 2% ammonium succinate and 1.5% ammonium formate, heating to 105 deg.C, and maintaining the temperature for 60 min; then cooling to 85 ℃, adding 2.5% of p-nitroanisole, and preserving heat for 30 min; and finally, continuously cooling to below 60 ℃ to obtain the ultralow-temperature electrolyte D.
EXAMPLE five
The performance test comparison of the ultralow-temperature electrolyte A, B, C, D obtained in the first to fourth embodiments and the electrolyte of the domestic famous factory is carried out, and the ultralow-temperature electrolyte is superior to the mature electrolyte of the domestic famous factory through comparison, and the main surfaces of the ultralow-temperature electrolyte are as follows: 1) the sparking voltage (withstand voltage) of the ultralow-temperature electrolyte is obviously higher; 2) the ultralow temperature electrolyte used in the aluminum electrolytic capacitor has excellent performance at the temperature of 55 ℃ below zero; the domestic comparative electrolyte can only reach the qualified performance of-40 ℃, and the product performance is deteriorated under the condition of ultralow temperature of-55 ℃, namely, the capacitor has larger impedance and smaller capacity, and the comparative parameters are shown in the following table:
EXAMPLE six
Manufacture of aluminium electrolytic capacitor
The ultralow temperature electrolyte A, B, C, D obtained in the first to fourth embodiments is made of the same material (except for the electrolyte) as the electrolyte of a domestic well-known factory, and the aluminum electrolytic capacitor is produced by the same manufacturing process according to the existing known technology, which is not described one by one, wherein the production specification of the aluminum electrolytic capacitor is as follows: 16V470 μ F, size 8 x 11; the main materials for producing the aluminum electrolytic capacitor and the specifications thereof are as follows: anode foil 21VF-69 μ F/cm2Cathode foil 2VF-270 muF/cm2Electrolytic paper S255-40, guide needle 12082-2823, rubber plug phi 7.3, aluminum shell 8 x 11.3, sleeve phi 8-PET and the five electrolytes;
performance testing of aluminum electrolytic capacitors
And (3) carrying out comparison measurement on the aluminum electrolytic capacitors manufactured by the 5 electrolytes under the same condition, and carrying out parameter measurement under the conditions of normal temperature and low temperature. Through measurement, the following results are obtained: the difference of the 5 electrolytes is not obvious at the impedance ratio of-40 ℃ to 20 ℃; however, under the condition of-55 ℃, the performance of the comparative electrolyte is rapidly deteriorated, the impedance ratio reaches about 23 times, and the capacity is also reduced by about 64 percent. The impedance ratio of the ultralow temperature electrolyte A, B, C, D at the temperature of between 55 ℃ below zero and 20 ℃ below zero is within the standard, the capacity change rate is much smaller, particularly, the impedance ratio of the electrolyte B and the electrolyte C at the temperature of between 55 ℃ below zero and 20 ℃ below zero has a certain space with the standard, and the capacity attenuation is about 20 percent (the national standard does not make a regulation on the capacity change, and only makes a requirement on the impedance ratio). Thus, the formulation of electrolyte B is best seen from the data, and the comparative data are shown in the following table (Z represents the impedance and C/C% represents the loss rate):
the electrolyte for the ultralow-temperature aluminum electrolytic capacitor is not frozen at the temperature of-55 ℃, has small resistivity change, does not corrode common rubber, has good sealing performance and more stable service life, does not need to add extra materials and process cost, and is suitable for mass production and use; the ultralow-temperature electrolyte is applied to an aluminum electrolytic capacitor under the normal temperature condition, the aluminum electrolytic capacitor has excellent performance, can be normally used at the temperature of-55-105 ℃, reaches the level of a high-frequency low-resistance product which is commonly used in the prior art, has a loss angle or ESR less than half of that of a GBL system electrolyte, and has less product heat generation and less self-consumption energy.
The above description is only a preferred embodiment of the present invention, but the design concept of the present invention is not limited thereto, and any insubstantial modifications made by using the design concept should fall within the scope of infringing on the protection scope of the present invention.
Claims (10)
1. The electrolyte for the ultralow-temperature aluminum electrolytic capacitor is characterized in that: the composite material comprises, by mass, 40-50% of a first solvent, 20-30% of a second solvent, 5-10% of a third solvent, 1-15% of a solute and 0.5-5% of an additive, wherein the additive comprises one or more of a dehydrogenation agent and a high-temperature stabilizer.
2. The electrolytic solution for an ultra-low temperature aluminum electrolytic capacitor according to claim 1, characterized in that: the first solvent includes ethylene glycol.
3. The electrolytic solution for an ultra-low temperature aluminum electrolytic capacitor according to claim 1, characterized in that: the second solvent includes water.
4. The electrolytic solution for an ultra-low temperature aluminum electrolytic capacitor according to claim 1, characterized in that: the third solvent comprises one or more of sulfolane, 1, 2-propylene glycol, ethylene glycol monomethyl ether, and N, N-dimethylacetamide.
5. The electrolytic solution for an ultra-low temperature aluminum electrolytic capacitor according to claim 1, characterized in that: the solute comprises one or more of ammonium adipate, adipic acid, ammonium succinate and ammonium formate.
6. The electrolytic solution for an ultra-low temperature aluminum electrolytic capacitor according to claim 1, characterized in that: the hydrogen eliminating agent comprises one or more of p-nitrobenzoic acid, p-nitroaniline ammonium formate and p-nitroanisole.
7. The electrolytic solution for an ultra-low temperature aluminum electrolytic capacitor according to claim 1, characterized in that: the high temperature stabilizer comprises one or more of mannitol, citric acid, phosphoric acid and salts thereof.
8. A preparation method of electrolyte for an ultralow temperature aluminum electrolytic capacitor is characterized by comprising the following steps:
s1: uniformly mixing the first solvent and the second solvent, heating to 40-65 ℃, and keeping the temperature for 5-15 min;
s2: adding a third solvent into the mixed solution in the S1, heating to 75-90 ℃, and keeping the temperature for 20-40 min;
s3: then adding a solute and a high-temperature stabilizer, heating to 110 ℃, and keeping the temperature for 50-70 min;
s4: cooling to 80-90 deg.C, adding hydrogen eliminating agent, and keeping the temperature for 25-35 min;
s5: and cooling to below 60 ℃ to obtain the ultralow temperature electrolyte.
9. The method for preparing an electrolyte for an ultra-low temperature aluminum electrolytic capacitor as set forth in claim 8, wherein: the mass percentage of the high-temperature stabilizer is 0.5-2%.
10. The method for preparing an electrolyte for an ultra-low temperature aluminum electrolytic capacitor as set forth in claim 8, wherein: the mass percentage of the dehydrogenation agent is 0.5-2.5%.
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| CN112670089A (en) * | 2020-12-09 | 2021-04-16 | 珠海格力新元电子有限公司 | High-voltage aluminum electrolytic capacitor and preparation method thereof |
| CN112687472A (en) * | 2020-12-03 | 2021-04-20 | 盐城星晨科技有限公司 | High-frequency electrolyte and preparation method thereof |
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