CN116364437A - Working electrolyte for medium-high voltage aluminum electrolytic capacitor and preparation method thereof - Google Patents
Working electrolyte for medium-high voltage aluminum electrolytic capacitor and preparation method thereof Download PDFInfo
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- CN116364437A CN116364437A CN202310294911.9A CN202310294911A CN116364437A CN 116364437 A CN116364437 A CN 116364437A CN 202310294911 A CN202310294911 A CN 202310294911A CN 116364437 A CN116364437 A CN 116364437A
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 83
- 239000003990 capacitor Substances 0.000 title claims abstract description 82
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 109
- 239000002904 solvent Substances 0.000 claims abstract description 69
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 60
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 59
- 229920000642 polymer Polymers 0.000 claims abstract description 42
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 41
- OTRAYOBSWCVTIN-UHFFFAOYSA-N OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N Chemical compound OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N OTRAYOBSWCVTIN-UHFFFAOYSA-N 0.000 claims abstract description 33
- VJCJAQSLASCYAW-UHFFFAOYSA-N azane;dodecanoic acid Chemical compound [NH4+].CCCCCCCCCCCC([O-])=O VJCJAQSLASCYAW-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229940067597 azelate Drugs 0.000 claims abstract description 31
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims abstract description 31
- SATJMZAWJRWBRX-UHFFFAOYSA-N azane;decanedioic acid Chemical compound [NH4+].[NH4+].[O-]C(=O)CCCCCCCCC([O-])=O SATJMZAWJRWBRX-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000654 additive Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- 229940116351 sebacate Drugs 0.000 claims abstract description 19
- 230000000996 additive effect Effects 0.000 claims abstract description 18
- 125000005210 alkyl ammonium group Chemical group 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims description 49
- 238000010438 heat treatment Methods 0.000 claims description 46
- 239000003795 chemical substances by application Substances 0.000 claims description 44
- 239000002202 Polyethylene glycol Substances 0.000 claims description 39
- 229920001223 polyethylene glycol Polymers 0.000 claims description 39
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 31
- 238000001816 cooling Methods 0.000 claims description 31
- 229910052739 hydrogen Inorganic materials 0.000 claims description 31
- 239000001257 hydrogen Substances 0.000 claims description 31
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 28
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 25
- 229930195725 Mannitol Natural products 0.000 claims description 25
- 239000000594 mannitol Substances 0.000 claims description 25
- 235000010355 mannitol Nutrition 0.000 claims description 25
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 24
- 239000012046 mixed solvent Substances 0.000 claims description 24
- 238000004090 dissolution Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 13
- OTLNPYWUJOZPPA-UHFFFAOYSA-N 4-nitrobenzoic acid Chemical group OC(=O)C1=CC=C([N+]([O-])=O)C=C1 OTLNPYWUJOZPPA-UHFFFAOYSA-N 0.000 claims description 12
- GJYJYFHBOBUTBY-UHFFFAOYSA-N alpha-camphorene Chemical group CC(C)=CCCC(=C)C1CCC(CCC=C(C)C)=CC1 GJYJYFHBOBUTBY-UHFFFAOYSA-N 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- -1 adding a main solute Substances 0.000 claims description 4
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002516 radical scavenger Substances 0.000 claims 1
- 238000010411 cooking Methods 0.000 abstract description 15
- 239000011888 foil Substances 0.000 abstract description 8
- 238000004321 preservation Methods 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 5
- 238000001179 sorption measurement Methods 0.000 abstract description 5
- 125000000524 functional group Chemical group 0.000 abstract description 4
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 49
- 230000000052 comparative effect Effects 0.000 description 17
- 125000000217 alkyl group Chemical group 0.000 description 9
- CXMXRPHRNRROMY-UHFFFAOYSA-L sebacate(2-) Chemical compound [O-]C(=O)CCCCCCCCC([O-])=O CXMXRPHRNRROMY-UHFFFAOYSA-L 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 4
- 229920005646 polycarboxylate Polymers 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- KWIPUXXIFQQMKN-UHFFFAOYSA-N 2-azaniumyl-3-(4-cyanophenyl)propanoate Chemical compound OC(=O)C(N)CC1=CC=C(C#N)C=C1 KWIPUXXIFQQMKN-UHFFFAOYSA-N 0.000 description 2
- 229940090948 ammonium benzoate Drugs 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- IUZSEJJESGRFMH-UHFFFAOYSA-N azane;decanedioic acid Chemical compound N.OC(=O)CCCCCCCCC(O)=O IUZSEJJESGRFMH-UHFFFAOYSA-N 0.000 description 1
- IKFMRFYLIRAXAJ-UHFFFAOYSA-N azane;nonanedioic acid Chemical compound N.OC(=O)CCCCCCCC(O)=O IKFMRFYLIRAXAJ-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical class OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000001734 carboxylic acid salts Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/0029—Processes of manufacture
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a working electrolyte for a medium-high voltage aluminum electrolytic capacitor and a preparation method thereof, belonging to the technical field of capacitor preparation. The working electrolyte takes ammonium sebacate as a main solute, alkyl ammonium sebacate as a secondary solute, polyvinyl alcohol and ethylene glycol as polymer additives, and at least one of ammonium azelate, ammonium dodecanoate and ammonium pentaborate as an auxiliary solute. Adding a high polymer in the preparation process, controlling the cooking temperature and the heat preservation time of the electrolyte, and enhancing the dissolving capacity of the high polymer by utilizing the reaction between the polymer additive and the solvent; the adsorption of polymers with different molecular chain lengths and polymer molecules containing different kinds of functional groups on the anode foil is utilized to enhance the repairing capability of the anode foil to anode surface defects in the working process of the capacitor. The invention improves the stability of the working electrolyte for the medium-high voltage aluminum electrolytic capacitor and improves the comprehensive performance of the capacitor mainly through adjusting the formula of the electrolyte and the cooking process.
Description
Technical Field
The invention belongs to the technical field of capacitor preparation, and particularly relates to a working electrolyte for a medium-high voltage aluminum electrolytic capacitor and a preparation method thereof.
Background
The medium-high voltage aluminum electrolytic capacitor is one of basic elements of electronic products and is widely used in the production of automobile electronics, frequency conversion technology, displays, chargers, electronic ballasts, switching power supplies and energy-saving lamps. In recent years, the rapid development of electronic technology and the further improvement of integration degree have put forward higher requirements on the comprehensive performance of the aluminum electrolytic capacitor, and the aluminum electrolytic capacitor is driven to develop towards high voltage, high capacity and long service life.
The aluminum electrolytic capacitor mainly comprises a capacitor core and working electrolyte, wherein the working electrolyte plays a key role in the performance of the aluminum electrolytic capacitor, and determines the working temperature range, rated voltage, loss factor, impedance, rated ripple current, the working life of the capacitor and the like of the electrolytic capacitor. In the preparation process, the formula of the electrolyte and the cooking process are critical, and in the preparation process, a series of complex chemical reactions such as acid ammonium decomposition, esterification and transesterification can occur among the components, so that the preparation process is required to be researched and determined through a large number of experiments.
At present, most of working electrolytes of medium-high voltage aluminum electrolytic capacitors are linear carboxylic acid ammonium salt, boric acid salt and ethylene glycol systems, the higher the number of carbon atoms in linear carboxylic acid salt is, the higher the sparking voltage is, but the solubility of the working electrolytes is drastically reduced along with the increase of molecular weight, for example, the solubility of ammonium sebacate in ethylene glycol which is usually used is not more than 5%, so that the impedance is increased, the crystallization is easy to separate out at low temperature, and the working temperature range of the capacitor is restricted. The branched chain polycarboxylate has relatively high solubility in a polybasic solvent, is not easy to crystallize at low temperature, has wide use temperature range and high electrolyte conductivity, and the prepared capacitor has strong voltage resistance and high ripple current resistance, but the branched chain polycarboxylate has the defect of high cost. In addition, the aluminum electrolytic capacitor prepared by the common working electrolyte has the defects of large leakage current, insufficient ripple resistance and the like. And other solutes which can be used as working electrolyte of the medium-high voltage aluminum electrolytic capacitor also comprise straight-chain carboxylate salts such as azelaic acid ammonium, sebacic acid ammonium, and dodecanoic acid ammonium, ammonium pentaborate, ammonium benzoate and the like, but each has certain disadvantages such as difficult availability of the dodecanoic acid ammonium, high conductivity of the ammonium pentaborate, unstable ammonium benzoate at high temperature and the like.
Disclosure of Invention
In order to solve the technical problems, the invention provides the working electrolyte for the medium-high voltage aluminum electrolytic capacitor and the preparation method thereof, and the stability of the working electrolyte for the aluminum electrolytic capacitor is improved and the comprehensive performance of the capacitor is improved by adjusting the formula of the electrolyte and the cooking process technology.
In order to achieve the above purpose, the present invention provides the following technical solutions:
one of the technical proposal is as follows:
the working electrolyte for the medium-high voltage aluminum electrolytic capacitor uses ammonium sebacate as a main solute, alkyl ammonium sebacate as a secondary solute, polyvinyl alcohol and ethylene glycol as high molecular additives, and at least one of ammonium azelate, ammonium dodecanoate and ammonium pentaborate as an auxiliary solute, wherein the polyvinyl alcohol consists of PVA with different molecular weights, and the ethylene glycol consists of PEG with different molecular weights.
Further, the working electrolyte for the medium-high voltage aluminum electrolytic capacitor comprises the following components in percentage by mass: 2-4% of auxiliary solvent, 5% of main solute, 2% of secondary solute, 2% of mannitol, 3% of ammonium pentaborate, 0.9% of ammonium azelate, 0.4% of ammonium dodecanoate, 0.4% of hydrogen eliminating agent, 0.4% of forming agent, 1.2-1.4% of polymer additive and the balance of main solvent.
Further, the main solvent is ethylene glycol, the auxiliary solvent is one or more of gamma-butyrolactone, glycerol and diglycol, the hydrogen eliminating agent is p-nitrobenzoic acid, and the forming agent is ammonium hypophosphite.
The invention selects polyvinyl alcohol with different molecular weights and ethylene glycol with different molecular weights to prepare according to a certain proportion as a high polymer additive of electrolyte. Firstly, the electrostatic and physical adsorption of different functional groups on different polymers on the surface of the anode foil is utilized, and secondly, the adsorption of molecular chains with different lengths on the surface of the anode foil is exerted by utilizing the difference of molecular weights of the polymers. Therefore, on one hand, different types of polymers are selected, and on the other hand, polymers with different molecular chain lengths are selected and prepared according to a certain proportion, so that the sparking voltage of working electrolyte is improved, the capability of the electrolyte for repairing the surface defects of a dielectric film of a capacitor is enhanced, the voltage resistance and other capabilities of an aluminum electrolytic capacitor are improved, and the leakage current of the capacitor is reduced.
Further, the mass ratio of the polyvinyl alcohol to the ethylene glycol in the polymer additive is 1:1.3-2.
Further, the polyvinyl alcohol is made of PVA 105 、PVA 117 And PVA 124 Is composed of two or more of triethylene glycol and PEG 200 、PEG 400 And PEG (polyethylene glycol) 600 Two or more of the above.
The working electrolyte of the invention is added with the ammonium pentaborate, the ammonium azelate and the ammonium dodecanoate, so that the conductivity of the electrolyte can be enhanced, and the problems of less dissolution of ammonium sebacate and insufficient conductivity of the electrolyte are solved; and secondly, branched alkyl ammonium sebacate is added as a secondary solute, and the branched polycarboxylate is utilized to have high solubility in a solvent, is not easy to crystallize at low temperature, improves the service temperature range of the electrolyte, and enhances the voltage resistance and the high ripple current resistance of the capacitor.
The second technical scheme is as follows:
the preparation method of the working electrolyte for the medium-high voltage aluminum electrolytic capacitor comprises the following steps:
(1) Weighing the components according to the mass percentage for standby;
(2) Mixing an auxiliary solvent with a main solvent to obtain a mixed solvent, adding main solute, mannitol, ammonium azelate hydrogen and ammonium dodecanoate into the solvent under heating, and dissolving to obtain a mixture A;
(3) Adding polyvinyl alcohol into the mixture A, heating, preserving heat, naturally cooling, then adding ammonium pentaborate and ethylene glycol, preserving heat and cooling to obtain a mixture B;
(4) And (3) carrying out heat preservation on the secondary solute, the hydrogen eliminating agent and the forming agent in the mixture B for a period of time, and cooling to room temperature to obtain the working electrolyte for the medium-high voltage aluminum electrolytic capacitor.
Further, the step (2) specifically comprises: mixing the auxiliary solvent with the main solvent to obtain a mixed solvent, heating the mixed solvent to 60 ℃, adding the main solute, heating to 80 ℃ after complete dissolution, adding mannitol, ammonium azelate and ammonium dodecanoate, and continuously heating to 130 ℃ to obtain a mixture A after complete dissolution.
Further, in the step (3), a high polymer polyvinyl alcohol is added in the cooking process, the temperature is heated to 145-160 ℃, the temperature is kept for 30min, the natural cooling is carried out to 130 ℃, ammonium pentaborate and ethylene glycol are added in, the temperature is kept for 35min at 130 ℃, and the cooling is carried out to 100 ℃.
Further, in the step (4), after adding the secondary solute, the hydrogen eliminating agent and the forming agent, the temperature is kept at 100 ℃ for 35min, and the mixture is cooled to room temperature.
In the preparation process of the working electrolyte for the medium-high voltage aluminum electrolytic capacitor, the addition time and the cooking temperature of secondary solute alkyl ammonium sebacate and a high polymer have great influence on the performance of the electrolyte.
The high polymer polyvinyl alcohol used in the working electrolyte has larger molecular weight, is difficult to dissolve in the solvent ethylene glycol at ordinary temperature, PVA can be completely dissolved by means of high temperature in the cooking process, and can be separated out again due to the reduced solubility at low temperature, so that the performances of the electrolyte and the aluminum electrolytic capacitor are affected. In the cooking process adopted by the invention, after the polyvinyl alcohol is added, the heating temperature of the electrolyte is not lower than 145 ℃, not higher than 160 ℃, the heat preservation time is longer, the high temperature and the control of the heat preservation time are adopted, and the polymer is utilized to carry out a certain degree of complex chemical reaction with the solvent under proper cooking conditions, especially at high temperature, so as to improve the solubility of the polymer, keep the stability of the polymer in the solvent and avoid precipitation at low temperature.
And the third technical scheme is as follows:
the working electrolyte for the medium-high voltage aluminum electrolytic capacitor is applied to the medium-high voltage aluminum electrolytic capacitor.
Compared with the prior art, the invention has the following advantages and technical effects:
the invention improves the stability of the working electrolyte for the aluminum electrolytic capacitor and the comprehensive performance of the capacitor by adjusting the formula of the electrolyte and the cooking process technology, and the overall performance of the working electrolyte for the medium-high voltage aluminum electrolytic capacitor is as follows: at 40 ℃, the pH is about 5.94, the conductivity exceeds 2200 mu S/cm, the sparking voltage reaches 500V, and the aluminum electrolytic capacitor (400V-6.8 uF) prepared by the method has good comprehensive electrochemical performance: the capacitor is 6.6-6.7 mu F, the leakage current is less than or equal to 12 mu A, the loss tan delta is about 0.05, the ripple resistance is good, and the service life is longer than 8kh at 105 ℃.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and/or materials in connection with which the documents are cited in the context of this specification in the event of conflict with any incorporated documents.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The invention provides a working electrolyte for a medium-high voltage aluminum electrolytic capacitor, which takes ammonium sebacate as a main solute, alkyl ammonium sebacate as a secondary solute, polyvinyl alcohol and ethylene glycol as a high molecular additive, and at least one of ammonium azelate, ammonium dodecanoate and ammonium pentaborate as an auxiliary solute, wherein the polyvinyl alcohol consists of PVA with different molecular weights, and the ethylene glycol consists of PEG with different molecular weights.
In some embodiments of the present invention, the working electrolyte comprises the following components in percentage by mass: 2-4% of auxiliary solvent, 5% of main solute, 2% of secondary solute, 2% of mannitol, 3% of ammonium pentaborate, 0.9% of ammonium azelate, 0.4% of ammonium dodecanoate, 0.4% of hydrogen eliminating agent, 0.4% of forming agent, 1.2-1.4% of polymer additive and the balance of main solvent.
In some embodiments of the present invention, the main solvent is ethylene glycol, the auxiliary solvent is one or more of γ -butyrolactone, glycerol, and diethylene glycol, the hydrogen eliminator is p-nitrobenzoic acid, and the forming agent is ammonium hypophosphite.
Based on the consideration that the ammonium sebacate is less dissolved in a solvent and can cause insufficient electric conduction of the electrolyte, in some preferred embodiments of the invention, on the one hand, ammonium pentaborate, ammonium azelate and ammonium dodecanoate are added into the working electrolyte, and as auxiliary solutes, the electric conduction of the electrolyte can be enhanced, and the problems of insufficient electric conduction of the electrolyte due to the less dissolution of the ammonium sebacate can be solved; on the other hand, branched alkyl ammonium sebacate is added as secondary solute, and branched polycarboxylate is utilized to have high solubility in solvent, difficult crystallization at low temperature, increase the use temperature range of electrolyte, and enhance the voltage and high ripple current resistance of capacitor.
In some embodiments of the invention, polyvinyl alcohols of different molecular weights are selected, and ethylene glycols of different molecular weights are added in a ratio of 1:1.3-2Is prepared as a polymer additive of electrolyte. Wherein the polyvinyl alcohol is formed by PVA 105 、PVA 117 And PVA 124 Is composed of two or more of triethylene glycol and PEG 200 、PEG 400 And PEG (polyethylene glycol) 600 Two or more of the above. Thus, the electrostatic and physical adsorption effect of different functional groups on different polymers on the surface of the anode foil and the adsorption effect of molecular chains with different lengths on the surface of the anode foil can be utilized to improve the sparking voltage of working electrolyte and enhance the repairing capability of the electrolyte to the surface defects of the dielectric film of the capacitor, improve the voltage resistance and other capabilities of the aluminum electrolytic capacitor and reduce the leakage current of the capacitor.
The invention also provides a preparation method of the working electrolyte for the medium-high voltage aluminum electrolytic capacitor, which comprises the following steps:
(1) Mixing an auxiliary solvent with a main solvent to obtain a mixed solvent, heating the mixed solvent to 60 ℃, adding a main solute, heating to 80 ℃ after complete dissolution, adding mannitol, ammonium azelate and ammonium dodecanoate, continuously heating to 130 ℃, and obtaining a mixture A after complete dissolution;
(2) The cooking process comprises the following steps: adding high molecular polymer polyvinyl alcohol into the mixture A, heating to 145-160 ℃, preserving heat for 30min, naturally cooling to 130 ℃, adding ammonium pentaborate and ethylene glycol, preserving heat for 35min at 130 ℃, and cooling to 100 ℃ to obtain a mixture B;
(3) And (3) adding secondary solute, hydrogen eliminating agent and forming agent into the mixture B, preserving heat at 100 ℃ for 35min, and cooling to room temperature to obtain the working electrolyte for the medium-high voltage aluminum electrolytic capacitor.
In the preparation process of the working electrolyte for the medium-high voltage aluminum electrolytic capacitor, the addition sequence and the boiling temperature of secondary solute alkyl ammonium sebacate have great influence on the performance of the electrolyte.
The high polymer polyvinyl alcohol used by the working electrolyte has larger molecular weight, is difficult to dissolve in the solvent ethylene glycol at ordinary temperature, PVA can be completely dissolved by means of high temperature in the cooking process, and can be separated out again due to the reduced solubility at low temperature, so that the performances of the electrolyte and the aluminum electrolytic capacitor are seriously affected. In the cooking process adopted by the invention, after the polyvinyl alcohol is added, the heating temperature of the electrolyte is not lower than 145 ℃, not higher than 160 ℃ and the heat preservation time is longer, and the polymer is utilized to generate a certain degree of complex chemical reaction between the functional group and the solvent under proper cooking conditions, especially longer-time high-temperature heat preservation, so that the solubility of the polymer is improved, the stability of the polymer in the solvent is maintained, and the polymer is not separated out at low temperature.
All the components used in the examples of the present invention are commercially available.
The technical scheme of the invention is further described by the following examples. The examples and comparative examples are merely to aid in the understanding of the present invention and should not be construed as a specific limitation of the present invention.
Example 1
(1) Weighing the following components in percentage by mass: 2.5 percent of auxiliary solvent (gamma-butyrolactone and diethylene glycol with the mass ratio of 1:1), 5 percent of main solute (ammonium sebacate), 2 percent of secondary solute (ammonium alkyl sebacate), 2 percent of mannitol, 3 percent of ammonium pentaborate, 0.9 percent of ammonium azelate, 0.4 percent of ammonium dodecanoate, 0.4 percent of hydrogen eliminator (p-nitrobenzoic acid), 0.4 percent of forming agent (ammonium hypophosphite) and 1.4 percent of macromolecule additive (PVA) 105 0.4％、PVA 117 0.2％，PEG 200 And PEG (polyethylene glycol) 400 0.4% each) with the balance being the main solvent (ethylene glycol).
(2) Mixing a main solvent and an auxiliary solvent to obtain a mixed solvent, heating the mixed solvent to 60 ℃, adding a main solute (ammonium sebacate), heating to 80 ℃ after complete dissolution, adding mannitol, ammonium azelate and ammonium dodecanoate, and continuously heating to 130 ℃ to obtain a mixture A;
(3) Adding polyvinyl alcohol into the mixture A, heating to 145 ℃, preserving heat for 30min, cooling to 130 ℃, adding ammonium pentaborate and ethylene glycol, preserving heat, and cooling to 100 ℃ to obtain a mixture B.
(4) Adding secondary solute, hydrogen eliminating agent and forming agent into the mixture B, preserving heat at 100 ℃ for 35min, and cooling to room temperature to obtain the working electrolyte for the medium-high voltage aluminum electrolytic capacitor.
Example 2
(1) Weighing the following components in percentage by mass: 2.5% of auxiliary solvent (gamma-butyrolactone and diethylene glycol in a mass ratio of 1:1), 5% of main solute (ammonium sebacate), 2% of secondary solute (ammonium alkyl sebacate), 2% of mannitol, 3% of ammonium pentaborate, 0.9% of ammonium azelate, 0.4% of ammonium dodecanoate, 0.4% of hydrogen eliminator (p-nitrobenzoic acid), 0.4% of forming agent (ammonium hypophosphite) and 1.2% of polymer additive (PVA) 105 0.2％、PVA 124 0.2％，PEG 200 And PEG (polyethylene glycol) 600 0.4% each) with the balance being the main solvent (ethylene glycol).
(2) Mixing a main solvent and an auxiliary solvent to obtain a mixed solvent, heating the mixed solvent to 60 ℃, adding a main solute (ammonium sebacate), heating to 80 ℃ after complete dissolution, adding mannitol, ammonium azelate and ammonium dodecanoate, and continuously heating to 130 ℃ to obtain a mixture A;
(3) Adding polyvinyl alcohol into the mixture A, heating to 160 ℃, preserving heat for 30min, cooling to 130 ℃, adding ammonium pentaborate and ethylene glycol, preserving heat, and cooling to 100 ℃ to obtain a mixture B.
(4) Adding secondary solute, hydrogen eliminating agent and forming agent into the mixture B, preserving heat for 35min, and cooling to room temperature to obtain the working electrolyte for the medium-high voltage aluminum electrolytic capacitor.
Comparative example 1 (omitting the addition of the secondary solvent alkyl ammonium sebacate):
the only difference from example 1 is that the addition of secondary solutes (ammonium alkyl sebacate) was omitted, in particular:
(1) 2.5% of auxiliary solvent (gamma-butyrolactone and diethylene glycol in mass ratio of 1:1), 5% of main solute (ammonium sebacate), 2% of secondary solute (ammonium alkyl sebacate), 2% of mannitol, 3% of ammonium pentaborate, 0.9% of ammonium azelate, 0.4% of ammonium dodecanoate, 0.4% of hydrogen eliminator (p-nitrobenzoic acid), 0.4% of forming agent (ammonium hypophosphite) and high concentrationMolecular additive 1.4% (PVA) 105 0.4％、PVA 117 0.2％，PEG 200 And PEG (polyethylene glycol) 400 0.4% each) with the remainder being the main solvent (ethylene glycol).
Weighing the following components in percentage by mass: 2.5% of auxiliary solvent (50% of gamma-butyrolactone and diethylene glycol respectively), 5% of main solute (ammonium sebacate), 2% of mannitol, 3% of ammonium pentaborate, 0.9% of ammonium azelate, 0.4% of ammonium dodecanoate, 0.4% of hydrogen eliminator (p-nitrobenzoic acid), 1.4% of forming agent (ammonium hypophosphite) and 1.4% of polymer additive (PVA) 105 0.4％、PVA 117 0.2％，PEG 200 And PEG (polyethylene glycol) 400 0.4% each) with the balance being the main solvent (ethylene glycol).
(2) Mixing a main solvent and an auxiliary solvent to obtain a mixed solvent, heating the mixed solvent to 60 ℃, adding a main solute (ammonium sebacate), heating to 80 ℃ after complete dissolution, adding mannitol, ammonium azelate and ammonium dodecanoate, and continuously heating to 130 ℃ to obtain a mixture A;
(3) Adding polyvinyl alcohol into the mixture A, heating to 145 ℃, preserving heat for 30min, cooling to 130 ℃, adding ammonium pentaborate and ethylene glycol, preserving heat, and cooling to 100 ℃ to obtain a mixture B.
(4) Adding a hydrogen eliminating agent and a forming agent into the mixture B, preserving heat for 35min, and cooling to room temperature to obtain the working electrolyte for the medium-high voltage aluminum electrolytic capacitor.
Comparative example 2 (high molecular Polymer type is a single polyvinyl alcohol)
As in example 2, the only difference is that the high molecular polymer is a single polyvinyl alcohol PVA 105 . The method comprises the following steps:
1) Weighing the following components in percentage by mass: 2.5 percent of auxiliary solvent (the mass ratio of gamma-butyrolactone and diglycol is 1:1), 5 percent of main solute (ammonium sebacate), 2 percent of secondary solute (ammonium alkyl sebacate), 2 percent of mannitol, 3 percent of ammonium pentaborate, 0.9 percent of ammonium azelate, 0.4 percent of ammonium dodecanoate, 0.4 percent of hydrogen eliminator (p-nitrobenzoic acid) and forming agent (ammonium hypophosphite), and PVA as a high molecular additive 105 1.2% and the balance of main solvent (ethylene glycol).
(2) Mixing a main solvent and an auxiliary solvent to obtain a mixed solvent, heating the mixed solvent to 60 ℃, adding a main solute (ammonium sebacate), heating to 80 ℃ after complete dissolution, adding mannitol, ammonium azelate and ammonium dodecanoate, and continuously heating to 130 ℃ to obtain a mixture A;
(3) Adding a polymer additive PVA into the mixture A 105 Heating to 160 ℃, preserving heat for 30min, cooling to 130 ℃, adding ammonium pentaborate, preserving heat, and cooling to 100 ℃ to obtain a mixture B.
(4) Adding secondary solute, hydrogen eliminating agent and forming agent into the mixture B, preserving heat for 35min, and cooling to room temperature to obtain the working electrolyte for the medium-high voltage aluminum electrolytic capacitor.
Comparative example 3 (changing the type of high molecular Polymer to Single ethylene glycol)
The difference is that the high molecular polymer is single PEG as in example 2 200 . The method comprises the following steps:
(1) Weighing the following components in percentage by mass: 2.5 percent of auxiliary solvent (the mass ratio of gamma-butyrolactone and diglycol is 1:1), 5 percent of main solute (ammonium sebacate), 2 percent of secondary solute (ammonium alkyl sebacate), 2 percent of mannitol, 3 percent of ammonium pentaborate, 0.9 percent of ammonium azelate, 0.4 percent of ammonium dodecanoate, 0.4 percent of hydrogen eliminator (p-nitrobenzoic acid) and forming agent (ammonium hypophosphite), and the high molecular additive is PEG 200 1.2% and the balance of main solvent (ethylene glycol).
(2) Mixing a main solvent and an auxiliary solvent to obtain a mixed solvent, heating the mixed solvent to 60 ℃, adding a main solute (ammonium sebacate), heating to 80 ℃ after complete dissolution, adding mannitol, ammonium azelate and ammonium dodecanoate, and continuously heating to 130 ℃ to obtain a mixture A;
(3) PEG is added to the mixture A 200 Ammonium pentaborate, incubating for 30min, and cooling to 100deg.C to obtain mixture B.
(4) Adding secondary solute, hydrogen eliminating agent and forming agent into the mixture B, preserving heat for 35min, and cooling to room temperature to obtain the working electrolyte for the medium-high voltage aluminum electrolytic capacitor.
Comparative example 4 (varying the addition time of the less solute alkyl ammonium sebacate)
The only difference from example 1 is that the secondary solute and the primary solute are added simultaneously. The method comprises the following steps:
(1) Weighing the following components in percentage by mass: 2.5% of auxiliary solvent (50% of gamma-butyrolactone and diethylene glycol respectively), 5% of main solute (ammonium sebacate), 2% of secondary solute (ammonium alkyl sebacate), 2% of mannitol, 3% of ammonium pentaborate, 0.9% of ammonium azelate, 0.4% of ammonium dodecanoate, 0.4% of hydrogen eliminator (p-nitrobenzoic acid) and forming agent (ammonium hypophosphite) respectively, 1.4% of polymer additive (PVA) 105 0.4％、PVA 117 0.2％，PEG 200 And PEG (polyethylene glycol) 400 0.4% each) with the balance being the main solvent (ethylene glycol);
(2) Mixing a main solvent and an auxiliary solvent to obtain a mixed solvent, heating the mixed solvent to 60 ℃, adding a main solute and a secondary solute, heating to 80 ℃ after complete dissolution, adding mannitol, ammonium azelate hydrogen and ammonium dodecanoate, and continuously heating to 130 ℃ to obtain a mixture A;
(3) Adding polyvinyl alcohol into the mixture A, heating to 150 ℃, preserving heat for 30min, cooling to 130 ℃, adding ammonium pentaborate and ethylene glycol, preserving heat, and cooling to 100 ℃ to obtain a mixture B.
(4) Adding a hydrogen eliminating agent and a forming agent into the mixture B, preserving heat for 35min, and cooling to room temperature to obtain the working electrolyte for the medium-high voltage aluminum electrolytic capacitor.
Comparative example 5 (changing the addition time and temperature of high molecular Polymer)
The difference is that the two types of polymer additives are added simultaneously and the electrolyte cooking temperatures are different as in example 1. The method comprises the following steps:
(1) Weighing the following components in percentage by mass: 2.5% of auxiliary solvent (50% of gamma-butyrolactone and diethylene glycol respectively), 5% of main solute (ammonium sebacate), 2% of secondary solute (ammonium alkyl sebacate), 2% of mannitol, 3% of ammonium pentaborate, 0.9% of ammonium azelate, 0.4% of ammonium dodecanoate, 0.4% of hydrogen eliminator (p-nitrobenzoic acid), 0.4% of forming agent (ammonium hypophosphite) and 1.4% of polymer additive (PVA) 105 0.4％、PVA 117 0.2％，PEG 200 And PEG (polyethylene glycol) 400 0.4% each) with the balance being the main solvent (ethylene glycol)；
(2) Mixing a main solvent and an auxiliary solvent to obtain a mixed solvent, heating the mixed solvent to 60 ℃, adding a main solute (ammonium sebacate), heating to 80 ℃ after complete dissolution, adding mannitol, ammonium azelate and ammonium dodecanoate, and continuously heating to 130 ℃ to obtain a mixture A;
(3) PVA was added to the mixture A 105 、PVA 117 、PEG 200 And PEG (polyethylene glycol) 400 Ammonium pentaborate, and after maintaining the temperature at 130 ℃, cooling to 100 ℃ to obtain a mixture B.
(4) Adding secondary solute, hydrogen eliminating agent and forming agent into the mixture B, preserving heat for 35min, and cooling to room temperature to obtain the working electrolyte for the medium-high voltage aluminum electrolytic capacitor.
Comparative example 6
The same as in example 1, except that no high molecular polymer was added, specifically:
(1) Weighing the following components in percentage by mass: 2.5 percent of auxiliary solvent (the mass ratio of gamma-butyrolactone to diglycol is 1:1), 5 percent of main solute (ammonium sebacate), 2 percent of secondary solute (ammonium alkyl sebacate), 2 percent of mannitol, 3 percent of ammonium pentaborate, 0.9 percent of ammonium azelate, 0.4 percent of ammonium dodecanoate, 0.4 percent of hydrogen eliminator (p-nitrobenzoic acid), 0.4 percent of forming agent (ammonium hypophosphite) and the balance of main solvent (ethylene glycol).
(2) Mixing a main solvent and an auxiliary solvent to obtain a mixed solvent, heating the mixed solvent to 60 ℃, adding a main solute (ammonium sebacate), heating to 80 ℃ after complete dissolution, adding mannitol, ammonium azelate and ammonium dodecanoate, and continuously heating to 130 ℃ to obtain a mixture A;
(3) Ammonium pentaborate is added to the mixture A for heat preservation, and then the mixture A is cooled to 100 ℃ to obtain a mixture B.
(4) Adding secondary solute, hydrogen eliminating agent and forming agent into the mixture B, preserving heat for 35min, and cooling to room temperature to obtain the working electrolyte for the medium-high voltage aluminum electrolytic capacitor.
Performance test: the prepared working electrolyte of the capacitor is used for measuring pH and conductivity sigma at a constant sealing temperature of 40 ℃, and the foil sparking voltage is measured by boosting the constant current (3 mA) of the anode foil. As a medium-high voltage aluminum electrolytic capacitor, the primary sparking voltage Us of the working electrolyte is more than or equal to 400V, and the sparking time is lower than 130s when reaching 500V, so that the oxidation efficiency requirement is met.
The electrolyte is used for preparing a capacitor with the specification of 400v-6.8 mu F, a durability test is carried out after aging, and the performance of the capacitor is measured by adopting a high-temperature (105 ℃) accelerated life test.
Table 1 shows the results of performance tests on the working electrolytes obtained in examples 1-2 and comparative examples 1-6, and Table 2 shows the electrochemical properties of each capacitor prepared with the electrolytes.
Table 1 results of performance tests of working electrolytes of examples and comparative examples
Table 2 electrochemical properties of working electrolytes for examples and comparative examples for preparing aluminum electrolytic capacitors
| Capacitance/. Mu.F | Leakage current/. Mu.A | Loss tan delta | |
| Example 1 | 6.73 | 11.6 | 0.047 |
| Example 2 | 6.69 | 12.0 | 0.049 |
| Comparative example 1 | 6.25 | 14.9 | 0.058 |
| Comparative example 2 | 6.19 | 15.4 | 0.061 |
| Comparative example 3 | 6.22 | 16.1 | 0.063 |
| Comparative example 4 | 6.65 | 13.3 | 0.056 |
| Comparative example 5 | 6.18 | 16.2 | 0.064 |
| Comparative example 6 | 6.15 | 16.7 | 0.067 |
As can be seen from tables 1 and 2, the working electrolyte prepared by the embodiment of the invention has good conductive performance, can meet the use requirement of an aluminum electrolytic capacitor, and the performance of the prepared capacitor is in a qualified range. Compared with the comparative example, the overvoltage resistance of the aluminum electrolytic capacitor is improved, and the leakage current of the capacitor is obviously reduced. The working electrolyte for the medium-high voltage aluminum electrolytic capacitor has the characteristics that the pH is about 5.94, the conductivity exceeds 2200 mu S/cm, the sparking voltage reaches 500V at 40 ℃, and the aluminum electrolytic capacitor (400V-6.8 uF) prepared by the method has good comprehensive electrochemical performance: the capacitance is 6.6-6.7 mu F, the leakage current is about 12 mu A, the loss tan delta is less than or equal to 0.05, and the composite performance is good. The capacitor has a service life of more than 8kh at 105 ℃.
The foregoing is merely a preferred embodiment of the present application, but the scope of the present application is not limited thereto, and any changes or substitutions easily conceivable by those skilled in the art within the technical scope of the present application should be covered in the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
Claims (10)
1. The working electrolyte for the medium-high voltage aluminum electrolytic capacitor is characterized in that ammonium sebacate is used as a main solute, alkyl ammonium sebacate is used as a secondary solute, polyvinyl alcohol and ethylene glycol are used as high molecular additives, at least one of ammonium azelate, ammonium dodecanoate and ammonium pentaborate is used as an auxiliary solute, the polyvinyl alcohol consists of PVA with different molecular weights, and the ethylene glycol consists of PEG with different molecular weights.
2. The working electrolyte for the medium-high voltage aluminum electrolytic capacitor according to claim 1, wherein the working electrolyte for the medium-high voltage aluminum electrolytic capacitor comprises the following components in percentage by mass: 2-4% of auxiliary solvent, 5% of main solute, 2% of secondary solute, 2% of mannitol, 3% of ammonium pentaborate, 0.9% of ammonium azelate, 0.4% of ammonium dodecanoate, 0.4% of hydrogen eliminating agent, 0.4% of forming agent, 1.2-1.4% of polymer additive and the balance of main solvent.
3. The working electrolyte for a medium-high voltage aluminum electrolytic capacitor according to claim 2, wherein the main solvent is ethylene glycol, the auxiliary solvent is one or more of γ -butyrolactone, glycerol and diethylene glycol, the hydrogen eliminator is p-nitrobenzoic acid, and the forming agent is ammonium hypophosphite.
4. The working electrolyte for a medium-high voltage aluminum electrolytic capacitor according to claim 1, wherein the mass ratio of the polyvinyl alcohol to the ethylene glycol in the polymer additive is 1:1.3-2.
5. The working electrolyte for a medium-high voltage aluminum electrolytic capacitor according to claim 1, wherein the polyvinyl alcohol is made of PVA 105 、PVA 117 And PVA 124 Is composed of two or more of triethylene glycol and PEG 200 、PEG 400 And PEG (polyethylene glycol) 600 Two or more of the above.
6. A method for producing the working electrolyte for a medium-high voltage aluminum electrolytic capacitor as recited in any one of claims 1 to 5, comprising the steps of:
(1) Weighing the components according to the mass percentage for standby;
(2) Mixing an auxiliary solvent with a main solvent to obtain a mixed solvent, adding a main solute, mannitol, ammonium azelate hydrogen and ammonium dodecanoate under a heating condition, and heating and dissolving to obtain a mixture A;
(3) Adding polyvinyl alcohol into the mixture A, heating, preserving heat, naturally cooling, then adding ammonium pentaborate and ethylene glycol, preserving heat and cooling to obtain a mixture B;
(4) Adding secondary solute, hydrogen eliminating agent and forming agent into the mixture B, preserving heat, and cooling to room temperature to obtain the working electrolyte for the medium-high voltage aluminum electrolytic capacitor.
7. The preparation method of claim 6, wherein the step (2) is specifically: mixing the auxiliary solvent with the main solvent to obtain a mixed solvent, heating the mixed solvent to 60 ℃, adding the main solute, heating to 80 ℃ after complete dissolution, adding mannitol, ammonium azelate and ammonium dodecanoate, and continuously heating to 130 ℃ to obtain a mixture A after complete dissolution.
8. The preparation method of claim 6, wherein in the step (3), polyvinyl alcohol is added to be heated to 145-160 ℃, the temperature is kept for 30min and cooled to 130 ℃, and ammonium pentaborate and ethylene glycol are added to be kept at the temperature.
9. The process according to claim 6, wherein in the step (4), the secondary solute, the hydrogen scavenger and the forming agent are added, and then the mixture is kept at 100℃for 35 minutes.
10. The use of the working electrolyte for a medium-high voltage aluminum electrolytic capacitor as claimed in any one of claims 1 to 5 in a medium-high voltage aluminum electrolytic capacitor.
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