CN119274981B - Electrolyte for aluminum electrolytic capacitor, aluminum electrolytic capacitor and preparation method of aluminum electrolytic capacitor - Google Patents
Electrolyte for aluminum electrolytic capacitor, aluminum electrolytic capacitor and preparation method of aluminum electrolytic capacitor Download PDFInfo
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- 239000003990 capacitor Substances 0.000 title claims abstract description 116
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 109
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 239000003792 electrolyte Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000011888 foil Substances 0.000 claims abstract description 34
- 239000002253 acid Substances 0.000 claims abstract description 29
- -1 carboxylic acid ammonium salt Chemical class 0.000 claims abstract description 26
- 239000002904 solvent Substances 0.000 claims abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 11
- 239000001257 hydrogen Substances 0.000 claims abstract description 11
- 239000006096 absorbing agent Substances 0.000 claims abstract description 8
- 239000003112 inhibitor Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 229910052708 sodium Inorganic materials 0.000 claims description 12
- 239000011734 sodium Substances 0.000 claims description 12
- WUODKTLXJOOQEJ-UHFFFAOYSA-N 4-hydroxycyclohexane-1-sulfonic acid Chemical compound OC1CCC(S(O)(=O)=O)CC1 WUODKTLXJOOQEJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 238000004804 winding Methods 0.000 claims description 7
- OTLNPYWUJOZPPA-UHFFFAOYSA-N 4-nitrobenzoic acid Chemical compound OC(=O)C1=CC=C([N+]([O-])=O)C=C1 OTLNPYWUJOZPPA-UHFFFAOYSA-N 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- 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 6
- 229930195725 Mannitol Natural products 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- SATJMZAWJRWBRX-UHFFFAOYSA-N azane;decanedioic acid Chemical compound [NH4+].[NH4+].[O-]C(=O)CCCCCCCCC([O-])=O SATJMZAWJRWBRX-UHFFFAOYSA-N 0.000 claims description 6
- 229940067597 azelate Drugs 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims description 6
- 239000000594 mannitol Substances 0.000 claims description 6
- 235000010355 mannitol Nutrition 0.000 claims description 6
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims description 6
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims description 3
- JKTYGPATCNUWKN-UHFFFAOYSA-N 4-nitrobenzyl alcohol Chemical compound OCC1=CC=C([N+]([O-])=O)C=C1 JKTYGPATCNUWKN-UHFFFAOYSA-N 0.000 claims description 2
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- YQCOSBVAJQCSEA-UHFFFAOYSA-N decanedioic acid;n-ethylethanamine Chemical compound CCNCC.OC(=O)CCCCCCCCC(O)=O YQCOSBVAJQCSEA-UHFFFAOYSA-N 0.000 claims 1
- 239000008151 electrolyte solution Substances 0.000 claims 1
- 230000007797 corrosion Effects 0.000 abstract description 25
- 238000005260 corrosion Methods 0.000 abstract description 25
- 239000003623 enhancer Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 16
- 239000000123 paper Substances 0.000 description 13
- 125000000542 sulfonic acid group Chemical group 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 230000002829 reductive effect Effects 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 239000010410 layer Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000012467 final product Substances 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- 230000008439 repair process Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 2
- VSSAZBXXNIABDN-UHFFFAOYSA-N cyclohexylmethanol Chemical compound OCC1CCCCC1 VSSAZBXXNIABDN-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000004901 spalling Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 206010060904 Freezing phenomenon Diseases 0.000 description 1
- 240000000907 Musa textilis Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010407 anodic oxide Substances 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002655 kraft paper Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- KSCKTBJJRVPGKM-UHFFFAOYSA-N octan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCCCCCC[O-].CCCCCCCC[O-].CCCCCCCC[O-].CCCCCCCC[O-] KSCKTBJJRVPGKM-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 150000005837 radical ions Chemical class 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
- H01G9/045—Electrodes or formation of dielectric layers thereon characterised by the material based on aluminium
-
- 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
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
-
- 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
- H01G9/145—Liquid electrolytic capacitors
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
本发明涉及电容器技术领域，尤其涉及一种铝电解电容器用电解液、铝电解电容器及其制备方法。该铝电解电容器由阳极铝箔、电解纸、阴极铝箔以及电解液所组成；其中电解液包括以下重量份的原料：溶剂60~90份、改性多元羧酸1~5份、有机羧酸铵盐5~20份、阻化剂1~4份、闪火电压提升剂2~15份以及吸氢剂1~3份。本发明还提供了其制备方法。与现有技术相比，本发明制备的铝电解电容器具备较高的静电容量以及良好的耐腐蚀性，同时还表现出优异的低温性能。The present invention relates to the technical field of capacitors, and in particular to an electrolyte for aluminum electrolytic capacitors, an aluminum electrolytic capacitor and a preparation method thereof. The aluminum electrolytic capacitor is composed of an anode aluminum foil, an electrolytic paper, a cathode aluminum foil and an electrolyte; wherein the electrolyte comprises the following raw materials in parts by weight: 60 to 90 parts of a solvent, 1 to 5 parts of a modified polycarboxylic acid, 5 to 20 parts of an organic carboxylic acid ammonium salt, 1 to 4 parts of an inhibitor, 2 to 15 parts of a flash voltage enhancer and 1 to 3 parts of a hydrogen absorber. The present invention also provides a preparation method thereof. Compared with the prior art, the aluminum electrolytic capacitor prepared by the present invention has a higher electrostatic capacitance and good corrosion resistance, and also exhibits excellent low temperature performance.
Description
Technical Field
The invention relates to the technical field of capacitors, in particular to electrolyte for an aluminum electrolytic capacitor, the aluminum electrolytic capacitor and a preparation method of the aluminum electrolytic capacitor.
Background
The aluminum electrolytic capacitor is a capacitor, the anode of which is composed of aluminum foil, and the cathode of which is composed of paper immersed with electrolyte and aluminum foil. The aluminum electrolytic capacitor has the main characteristics of large capacity, and has a larger capacitance value due to the special structural design and the special process manufacturing technology. This is mainly because the oxide film (Al 2O3) formed on the surface of the anode aluminum foil is very thin and dense, and this oxide film has a high dielectric constant as a dielectric, and can effectively store charges. In addition, the electrochemical etching process of the aluminum foil increases the surface area, thereby increasing the capacitance value. Aluminum electrolytic capacitors generally employ a structural design in which a flat plate capacitor is wound, which allows an increase in the surface area of the electrode in a relatively small space, thereby increasing the capacity of the capacitor. The positive and negative polarities are that the aluminum electrolytic capacitor has definite positive and negative polarities, and the correct connection of the positive and negative poles must be paid attention to when in use. If the capacitor is connected reversely, the capacitor cannot work normally, and the capacitor can generate heat due to overlarge leakage current, damage an oxide film and even explode. This phenomenon is called "valve effect" and is a cause of the polarity of the aluminum electrolytic capacitor. Pressure resistance limitation the pressure resistance of aluminum electrolytic capacitors is mainly limited by the thickness of the aluminum oxide film and the unevenness of the aluminum foil surface. The thickness of the aluminum oxide film is proportional to the withstand voltage, but an excessively thick oxide film easily becomes brittle and cracks on the rough porous surface of the aluminum foil, causing cracks and causing electric leakage. The unevenness of the surface of the aluminum foil also affects the withstand voltage of the capacitor, because the unevenness may cause local voltage concentration, and thus may cause breakdown. The self-repairing function of the oxide film is that the aluminum oxide film is gradually thickened in the working process of the aluminum electrolytic capacitor to form a protective layer to prevent aluminum from being dissolved in the electrolyte. When the inside of the capacitor fails, the capacitor can automatically start a self-repairing function, and the aluminum oxide film is reformed and thickened through a thermal effect and an ion diffusion effect, so that the normal working state of the capacitor is finally recovered.
CN112927938a discloses an electrolyte of an aluminum electrolytic capacitor, the aluminum electrolytic capacitor and an electronic device, and relates to the technical field of electrochemistry. The electrolyte of the aluminum electrolytic capacitor comprises an alcohol solvent, an auxiliary solvent, a solute, a spark voltage booster, a corrosion inhibitor and a novel hydrogen eliminator. The electrolyte of the aluminum electrolytic capacitor provided by the invention can inhibit the esterification reaction of the electrolyte at high temperature by introducing the solute with a long carbon chain and a branched chain, reduce the generation of moisture and improve the high-temperature stability of products, and can keep the internal air pressure of the aluminum electrolytic capacitor within a stable range by the synergistic effect of the auxiliary solvent and the novel hydrogen eliminator, so that the electrolyte is safe and stable, the bulge of the aluminum electrolytic capacitor is prevented, and the service life of the aluminum electrolytic capacitor is prolonged.
CN107910183a discloses a high-voltage aluminium electrolytic capacitor resistant to low temperature of-40 ℃, which comprises a shell and a cover body, wherein a core pack is arranged in the shell, the core pack is immersed with electrolyte, the conductivity of the electrolyte at-40 ℃ is more than 1.4ms/cm, the core pack is formed by overlapping and winding anode foil, cathode foil and electrolytic paper, the same sides of the cathode foil and the anode foil are respectively provided with the electrolytic paper serving as a substrate, the electrolytic paper comprises inner-layer electrolytic paper and outer-layer electrolytic paper, and the inner-layer electrolytic paper is made of manila hemp and kraft paper. The outer electrolytic paper is made of plant fibers which are not subjected to coating treatment and bleaching treatment. According to the invention, through improvement of process steps and conditions, the electrostatic capacity of the high-voltage aluminum electrolytic capacitor at the low temperature of-40 ℃ is improved to 65% -80% of that at the low temperature of 20 ℃, so that the low temperature resistance of the high-voltage aluminum electrolytic capacitor is effectively improved, the cost can be reduced, the volume of the capacitor is reduced, and the technical requirements of the current tightened electronic design are better met.
The aluminum electrolytic capacitor is widely applied to occasions such as power supply filtering, decoupling, signal coupling, time constant setting and the like, and has the advantages of large capacitance per unit volume and low cost, but has the disadvantages of large dielectric loss and capacity error and poor low temperature resistance and corrosion resistance. In general, electrolyte precipitation or electrolyte freezing phenomenon is easy to occur below-25 ℃, so that the capacity of the capacitor is rapidly attenuated, and when the low-temperature capacity attenuation exceeds a certain value, the whole machine can not be started. And the anode corrosion phenomenon of the electrolytic capacitor can greatly reduce the service life of the electrolytic capacitor.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention provides an electrolyte for an aluminum electrolytic capacitor, an aluminum electrolytic capacitor and a method for preparing the same.
The electrolyte in the aluminum electrolytic capacitor is a key component, and is closely related to the performance of the aluminum electrolytic capacitor, so that the electrolyte serves as an actual cathode of the aluminum electrolytic capacitor and plays an important role in providing oxygen ions and repairing an aluminum anodic oxide film. The common liquid aluminum electrolytic capacitor in the market at present has the problems that the electrolyte in the working electrolyte is mostly linear polycarboxylic acid, so that the electrolyte has low flash power, poor low-temperature performance, poor thermal stability and the like, and the performance of the aluminum electrolytic capacitor is greatly limited. The electrolyte significantly affects the electrostatic capacity, charge-discharge rate, long-term reliability and temperature characteristics of the capacitor through its conductivity, dielectric constant, chemical stability, amount, additives and solvent chemical characteristics, and thus, the selection of an appropriate electrolyte is critical to optimize the overall performance of the capacitor. The invention provides a modified polycarboxylic acid and organic carboxylic acid ammonium salt which are used as electrolyte in electrolyte, wherein the modified polycarboxylic acid has a ring structure, a nonpolar group and a sulfonic acid group, so that the modified polycarboxylic acid has more stable low-temperature electric performance and higher electrostatic capacity, and the sulfonic acid group has higher chemical stability and acidity, and can form a stable adsorption layer with the surface of metal, thereby inhibiting the corrosion of the metal, so that the sulfonic acid group can be used as a part of corrosion inhibitor in the electrolyte of an aluminum electrolytic capacitor, and can reduce the pitting and surface corrosion spalling phenomena of the aluminum foil in the corrosion process by acting with the surface of the aluminum foil, improve the distribution of surface tunnel holes and improve the performance and service life of the capacitor.
The invention provides an aluminum electrolytic capacitor, which comprises, by weight, 60-90 parts of a solvent, 1-5 parts of a modified polycarboxylic acid, 5-20 parts of an organic carboxylic acid ammonium salt, 1-4 parts of a stopping agent, 2-15 parts of a sparking voltage lifting agent and 1-3 parts of a hydrogen absorbing agent.
Obviously, the invention also synchronously provides an electrolyte for the aluminum electrolytic capacitor, which comprises the following raw materials, by weight, 60-90 parts of a solvent, 1-5 parts of modified polycarboxylic acid, 5-20 parts of an organic carboxylic acid ammonium salt, 1-4 parts of a stopping agent, 2-15 parts of a sparking voltage lifting agent and 1-3 parts of a hydrogen absorbing agent.
The preparation method of the modified polycarboxylic acid comprises the following steps:
X1, mixing 4-hydroxycyclohexane-1-sulfonic acid with sodium and anhydrous tetrahydrofuran in an inert atmosphere, wherein the molar ratio of the 4-hydroxycyclohexane-1-sulfonic acid to the sodium is 1:1-1.5, heating to 40-50 ℃, stirring for 6-10 hours, filtering, and concentrating to obtain a residue for the next step;
And X2, adding the product of the last step into ethylene glycol, adding 2-bromotetradecyl ethyl carbonate, heating to 70-80 ℃, stirring for 4-8 hours, adding a sodium hydroxide aqueous solution, stirring and hydrolyzing, and adding phosphoric acid to adjust the pH to be acidic, wherein the molar ratio of the product of the last step to the 2-bromotetradecyl ethyl carbonate to the sodium hydroxide is 1:1-2:1-2.
Further, the solvent is one or two of ethylene glycol and gamma-butyrolactone.
Further, the organic carboxylic acid ammonium salt comprises one or more of diethyl sebacate, ammonium sebacate and ammonium azelate.
Further, the inhibitor is one of phosphoric acid, phosphorous acid or hypophosphorous acid.
Further, the sparking voltage booster is one of mannitol, polyvinyl alcohol borate or polymerized fatty acid and ammonium salt.
Further, the hydrogen absorbing agent is one of p-nitrobenzoic acid, p-nitrobenzyl alcohol or p-nitrophenol.
The preparation method of the electrolyte for the aluminum electrolytic capacitor comprises the following steps:
Heating a solvent to 100-120 ℃, adding modified polycarboxylic acid, heating to 130-150 ℃, preserving heat for 1-2 hours, cooling to 100-120 ℃, adding organic carboxylic acid ammonium salt, continuously cooling to 80-90 ℃, adding a stopping agent, a sparking voltage lifting agent and a hydrogen absorbing agent, uniformly mixing, and cooling to room temperature to obtain the electrolyte for the aluminum electrolytic capacitor.
The invention also provides a preparation method of the aluminum electrolytic capacitor, which comprises the following steps:
winding the anode aluminum foil, the electrolytic paper and the cathode aluminum foil into a core package, immersing the core package in the electrolyte, pressurizing and immersing, and charging and aging to obtain the cathode aluminum foil.
Further, the pressurization is 3 to 5 atmospheres.
The invention has the beneficial effects that:
The invention provides a modified polycarboxylic acid and organic carboxylic acid ammonium salt which are used as electrolyte in electrolyte, wherein the modified polycarboxylic acid has a ring structure, a nonpolar group and a sulfonic acid group, so that the modified polycarboxylic acid has more stable low-temperature electric performance and higher electrostatic capacity, and the sulfonic acid group has higher chemical stability and acidity, and can form a stable adsorption layer with the surface of metal, thereby inhibiting the corrosion of the metal, so that the sulfonic acid group can be used as a part of corrosion inhibitor in the electrolyte of an aluminum electrolytic capacitor, and can reduce the pitting and surface corrosion spalling phenomena of the aluminum foil in the corrosion process by acting with the surface of the aluminum foil, improve the distribution of surface tunnel holes and improve the performance and service life of the capacitor.
Detailed Description
4-Hydroxycyclohexane-1-sulfonic acid, 4-hydroxycyclohexane-1-sulfonic acid, CAS number 58730-94-2.
Example 1
A preparation method of an aluminum electrolytic capacitor comprises the following steps:
Winding anode aluminum foil, electrolytic paper and cathode aluminum foil into a core package, immersing the core package in electrolyte, pressurizing to 5 atm for immersion, selecting specification and size of 400V,500 muF, phi 35 multiplied by 50mm for the capacitor core package, and charging and aging to obtain the final product.
The preparation method of the electrolyte for the aluminum electrolytic capacitor comprises the following steps of:
60 parts of ethylene glycol and 15 parts of gamma-butyrolactone are heated to 120 ℃,4 parts of modified polycarboxylic acid is added, the temperature is raised to 140 ℃, the heat is preserved for 1 hour, 8 parts of ammonium sebacate and 8 parts of ammonium azelate are added after the temperature is reduced to 120 ℃,2 parts of phosphorous acid, 9 parts of mannitol and 1 part of p-nitrobenzoic acid are added after the temperature is continuously reduced to 85 ℃, the mixture is uniformly mixed, and the mixture is cooled to room temperature, so that the electrolyte for the aluminum electrolytic capacitor is obtained;
Wherein the preparation method of the modified polycarboxylic acid comprises the following steps:
X1, mixing 4-hydroxycyclohexane-1-sulfonic acid with sodium and anhydrous tetrahydrofuran under an inert atmosphere, wherein the molar ratio of the 4-hydroxycyclohexane-1-sulfonic acid to the sodium is 1:1, heating to 45 ℃, stirring for 8 hours, filtering, and concentrating to obtain a residue for the next step;
And X2, adding the product of the last step into ethylene glycol, adding 2-bromotetradecyl ethyl carbonate, heating to 80 ℃, stirring for 6 hours, adding 1mol/L sodium hydroxide aqueous solution, stirring and hydrolyzing, and adding phosphoric acid to adjust the pH to be 6, wherein the mol ratio of the product of the last step to the 2-bromotetradecyl ethyl carbonate to the sodium hydroxide is 1:1:1.5.
Example 2
Substantially the same as in example 1, except that the amount of the modified polycarboxylic acid was 2 parts.
Example 3
Substantially the same as in example 1, except that the amount of the modified polycarboxylic acid was 3 parts.
Example 4
Substantially the same as in example 1, except that the amount of the modified polycarboxylic acid was 5 parts.
Comparative example 1
A preparation method of an aluminum electrolytic capacitor comprises the following steps:
Winding anode aluminum foil, electrolytic paper and cathode aluminum foil into a core package, immersing the core package in electrolyte, pressurizing to 5 atm for immersion, selecting specification and size of 400V,500 muF, phi 35 multiplied by 50mm for the capacitor core package, and charging and aging to obtain the final product.
The preparation method of the electrolyte for the aluminum electrolytic capacitor comprises the following steps of:
60 parts of ethylene glycol and 15 parts of gamma-butyrolactone are heated to 120 ℃,10 parts of ammonium sebacate and 10 parts of ammonium azelate are added, after the temperature is continuously reduced to 85 ℃,2 parts of phosphorous acid, 9 parts of mannitol and 1 part of p-nitrobenzoic acid are added, the mixture is uniformly mixed, and the mixture is cooled to room temperature, thus obtaining the electrolyte for the aluminum electrolytic capacitor.
Comparative example 2
A preparation method of an aluminum electrolytic capacitor comprises the following steps:
Winding anode aluminum foil, electrolytic paper and cathode aluminum foil into a core package, immersing the core package in electrolyte, pressurizing to 5 atm for immersion, selecting specification and size of 400V,500 muF, phi 35 multiplied by 50mm for the capacitor core package, and charging and aging to obtain the final product.
The preparation method of the electrolyte for the aluminum electrolytic capacitor comprises the following steps of:
60 parts of ethylene glycol and 15 parts of gamma-butyrolactone are heated to 120 ℃,4 parts of modified polycarboxylic acid is added, the temperature is raised to 140 ℃, the heat is preserved for 1 hour, 8 parts of ammonium sebacate and 8 parts of ammonium azelate are added after the temperature is reduced to 120 ℃,2 parts of phosphorous acid, 9 parts of mannitol and 1 part of p-nitrobenzoic acid are added after the temperature is continuously reduced to 85 ℃, the mixture is uniformly mixed, and the mixture is cooled to room temperature, so that the electrolyte for the aluminum electrolytic capacitor is obtained;
Wherein the preparation method of the modified polycarboxylic acid comprises the following steps:
X1, mixing cyclohexanol, sodium and anhydrous tetrahydrofuran in an inert atmosphere, wherein the molar ratio of cyclohexanol to sodium is 1:1, heating to 45 ℃, stirring for 8 hours, filtering, and concentrating to obtain a residue for the next step;
And X2, adding the product of the last step into ethylene glycol, adding 2-bromotetradecyl ethyl carbonate, heating to 80 ℃, stirring for 6 hours, adding 1mol/L sodium hydroxide aqueous solution, stirring and hydrolyzing, and adding phosphoric acid to adjust the pH to be 6, wherein the mol ratio of the product of the last step to the 2-bromotetradecyl ethyl carbonate to the sodium hydroxide is 1:1:1.5.
Comparative example 3
A preparation method of an aluminum electrolytic capacitor comprises the following steps:
Winding anode aluminum foil, electrolytic paper and cathode aluminum foil into a core package, immersing the core package in electrolyte, pressurizing to 5 atm for immersion, selecting specification and size of 400V,500 muF, phi 35 multiplied by 50mm for the capacitor core package, and charging and aging to obtain the final product.
The preparation method of the electrolyte for the aluminum electrolytic capacitor comprises the following steps of:
60 parts of ethylene glycol and 15 parts of gamma-butyrolactone are heated to 120 ℃,4 parts of modified polycarboxylic acid is added, the temperature is raised to 140 ℃, the heat is preserved for 1 hour, 8 parts of ammonium sebacate and 8 parts of ammonium azelate are added after the temperature is reduced to 120 ℃,2 parts of phosphorous acid, 9 parts of mannitol and 1 part of p-nitrobenzoic acid are added after the temperature is continuously reduced to 85 ℃, the mixture is uniformly mixed, and the mixture is cooled to room temperature, so that the electrolyte for the aluminum electrolytic capacitor is obtained;
Wherein the preparation method of the modified polycarboxylic acid comprises the following steps:
x1, mixing cyclohexyl methanol with sodium and anhydrous tetrahydrofuran in an inert atmosphere, wherein the molar ratio of the cyclohexyl methanol to the sodium is 1:1, heating to 45 ℃, stirring for 8 hours, filtering, and concentrating to obtain a residue for the next step;
And X2, adding the product of the last step into ethylene glycol, adding 2-bromotetradecyl ethyl carbonate, heating to 80 ℃, stirring for 6 hours, adding 1mol/L sodium hydroxide aqueous solution, stirring and hydrolyzing, and adding phosphoric acid to adjust the pH to be 6, wherein the mol ratio of the product of the last step to the 2-bromotetradecyl ethyl carbonate to the sodium hydroxide is 1:1:1.5.
Test example 1
The aluminum electrolytic capacitors prepared in examples and comparative examples were tested for electrostatic capacity at normal temperature, equivalent Series Resistance (ESR) value, conductivity, and sparking voltage, and specific data are shown in table 1.
TABLE 1 electrical properties of aluminum electrolytic capacitors
Capacitance and equivalent series resistance are two important parameters of a capacitor that describe the behavior of the capacitor in a circuit. Electrostatic capacitance is the ability of a capacitor to store charge, the size of the capacitor determining how much charge it can store, and the ability to store these charges at a given voltage. The equivalent series resistance refers to the equivalent resistance of the capacitor in the ac circuit due to leakage, dielectric loss, conductor resistance, and the like. ESR describes the effect of these non-idealities on capacitor performance. ESR has an important influence on the charge-discharge speed, ripple current bearing capacity and heat loss of the capacitor. The lower the ESR, the higher the charge-discharge efficiency of the capacitor, the stronger the ripple current carrying capacity and the smaller the heat loss. As can be seen from the test data in Table 1, the aluminum electrolytic capacitors prepared by the invention have higher electrostatic capacity and lower equivalent series resistance. Conductivity refers to an indicator of the conductivity of a capacitor, which indicates the ability of a current per unit length or per unit area to pass through the capacitor. The higher the conductivity, the more conductive the capacitor. The sparking voltage refers to the voltage at which sparking (i.e., electrical breakdown) occurs in the capacitor working electrolyte. The sparking voltage is an important parameter for measuring the insulating properties of the capacitor, and is related to the conductivity and the water content of the electrolyte. As can be seen from the data in table 1, the aluminum electrolytic capacitors of examples and comparative examples 2 to 3 have higher conductivity and sparking voltage than comparative example 1, probably because the modified polycarboxylic acids of examples and comparative examples 2 to 3 have not only alkane branches but also cyclic structures and nonpolar groups, and the ring tension of the cyclic structures results in more stable ionic movement rate in solution, thus having better electrical properties. However, in example 1, compared with other examples, the electrolyte was used as a key repair factor for repairing the anode foil oxide film in the electrolyte, and when the content of the repair factor was low, the repair capability in the electrolyte was insufficient and could not counter balance the discharge capability of the oxygen anions, thus making the electrical performance poor. Conversely, if the electrolyte content is too high, the acidity of the electrolyte increases, with a consequent increase in the concentration of oxyacid radical ions, which increases the probability of discharge of oxyanions, which in turn leads to a decrease in the flashover voltage. The aluminum electrolytic capacitor in example 1 thus exhibits the best electrical performance.
Test example 2
The aluminum electrolytic capacitors prepared in examples and comparative examples were subjected to durability test at low temperature, applied with 450V voltage and 1.33A ripple current, subjected to durability test (120 Hz) at-50, -25, 20 ℃ for 2000 hours, and tested for capacity loss, and leakage current, see in particular table 2.
TABLE 2 Low temperature electrical durability of aluminum electrolytic capacitors
As can be seen from the data in table 2, the aluminum electrolytic capacitor prepared in other examples of the present invention has good low temperature performance compared to comparative example 1, probably because the electrolyte used in other examples has not only branched carboxylic acid ammonium salt but also modified polycarboxylic acid, which contains nonpolar groups such as ether bond, the alkyl group can hinder the generation of oxyanion while the potential is higher, and the ring tension of the ring structure also ensures that the ion movement rate in the solution is more stable, thus maintaining good electrical performance even at low temperature.
Test example 3
The life test was performed on 20 samples of each of the aluminum electrolytic capacitors of each example and comparative example in a convection oven at a constant temperature of 105 ℃, and the corrosion was observed, and the shortest life time and the number of corrosions were recorded, as shown in Table 3.
TABLE 3 Corrosion resistance of aluminum electrolytic capacitors
| Experimental protocol | Duration of life/h | Number of corrosions/number of corrosions |
| Example 1 | 6000 | 0 |
| Example 2 | 6000 | 0 |
| Example 3 | 6000 | 0 |
| Example 4 | 5500 | 0 |
| Comparative example 1 | 2500 | 16 |
| Comparative example 2 | 3500 | 14 |
| Comparative example 3 | 3500 | 15 |
As can be seen from the corrosion resistance test, the aluminum electrolytic capacitor prepared in the examples has better corrosion resistance than the comparative example, probably because the modified polycarboxylic acid prepared in the examples has an additional sulfonic acid group, and the sulfonic acid group has higher chemical stability and acidity, and is capable of forming a stable adsorption layer with the metal surface, thereby inhibiting corrosion of the metal. In the electrolyte of the aluminum electrolytic capacitor, the sulfonic acid group can be used as a part of a corrosion inhibitor, and can act with the surface of the aluminum foil to reduce pitting corrosion and surface corrosion peeling phenomena of the aluminum foil in the corrosion process, improve the distribution of surface tunnel holes and improve the performance and service life of the capacitor. In comparative example 1, however, the modified polycarboxylic acids of comparative examples 2 to 3 have no sulfonic acid group, and thus have poor corrosion resistance.
The foregoing describes in detail preferred embodiments of the present invention. It should be understood that numerous modifications and variations can be made in accordance with the concepts of the invention by one of ordinary skill in the art without undue burden. Therefore, all technical solutions which can be obtained by logic analysis, reasoning or limited experiments based on the prior art by the person skilled in the art according to the inventive concept shall be within the scope of protection defined by the claims.
Claims (9)
1. The aluminum electrolytic capacitor is characterized by comprising, by weight, 60-90 parts of a solvent, 1-5 parts of a modified polycarboxylic acid, 5-20 parts of an organic carboxylic acid ammonium salt, 1-4 parts of a stopping agent, 2-15 parts of a spark voltage lifting agent and 1-3 parts of a hydrogen absorber, wherein the electrolyte comprises the following raw materials:
X1, mixing 4-hydroxycyclohexane-1-sulfonic acid with sodium and anhydrous tetrahydrofuran in an inert atmosphere, wherein the molar ratio of the 4-hydroxycyclohexane-1-sulfonic acid to the sodium is 1:1-1.5, heating to 40-50 ℃, stirring for 6-10 hours, filtering, and concentrating to obtain a residue for the next step;
And X2, adding the product of the last step into ethylene glycol, adding 2-bromotetradecyl ethyl carbonate, heating to 70-80 ℃, stirring for 4-8 hours, adding a sodium hydroxide aqueous solution, stirring and hydrolyzing, and adding phosphoric acid to adjust the pH to be acidic, wherein the molar ratio of the product of the last step to the 2-bromotetradecyl ethyl carbonate to the sodium hydroxide is 1:1-2:1-2.
2. The aluminum electrolytic capacitor as recited in claim 1, wherein the solvent is one or both of ethylene glycol and γ -butyrolactone.
3. The aluminum electrolytic capacitor as recited in claim 1, wherein the organic carboxylic acid ammonium salt comprises one or a mixture of a plurality of diethylamine sebacate, ammonium sebacate and ammonium azelate.
4. The aluminum electrolytic capacitor as recited in claim 1, wherein the inhibitor is one of phosphoric acid, phosphorous acid or hypophosphorous acid.
5. The aluminum electrolytic capacitor as recited in claim 1 wherein the sparking voltage booster is one of mannitol, polyvinyl alcohol borate or polymerized fatty acid and ammonium salt.
6. The aluminum electrolytic capacitor as recited in claim 1, wherein the hydrogen getter is one of p-nitrobenzoic acid, p-nitrobenzyl alcohol or p-nitrophenol.
7. The aluminum electrolytic capacitor as recited in claim 1, wherein the method for preparing the electrolytic solution comprises the steps of:
Heating a solvent to 100-120 ℃, adding modified polycarboxylic acid, heating to 130-150 ℃, preserving heat for 1-2 h, cooling to 100-120 ℃, adding organic carboxylic acid ammonium salt, continuously cooling to 80-90 ℃, adding a stopping agent, a sparking voltage lifting agent and a hydrogen absorbing agent, uniformly mixing, and cooling to room temperature to obtain the electrolyte.
8. A method of manufacturing the aluminum electrolytic capacitor as recited in any one of claims 1 to 7, comprising the steps of:
winding the anode aluminum foil, the electrolytic paper and the cathode aluminum foil into a core package, immersing the core package in the electrolyte, pressurizing and immersing, and charging and aging to obtain the cathode aluminum foil.
9. The electrolyte for the aluminum electrolytic capacitor is characterized by comprising, by weight, 60-90 parts of a solvent, 1-5 parts of modified polycarboxylic acid, 5-20 parts of an organic carboxylic acid ammonium salt, 1-4 parts of a stopping agent, 2-15 parts of a sparking voltage lifting agent and 1-3 parts of a hydrogen absorbing agent;
the preparation method of the modified polycarboxylic acid comprises the following steps:
X1, mixing 4-hydroxycyclohexane-1-sulfonic acid with sodium and anhydrous tetrahydrofuran in an inert atmosphere, wherein the molar ratio of the 4-hydroxycyclohexane-1-sulfonic acid to the sodium is 1:1-1.5, heating to 40-50 ℃, stirring for 6-10 hours, filtering, and concentrating to obtain a residue for the next step;
And X2, adding the product of the last step into ethylene glycol, adding 2-bromotetradecyl ethyl carbonate, heating to 70-80 ℃, stirring for 4-8 hours, adding a sodium hydroxide aqueous solution, stirring and hydrolyzing, and adding phosphoric acid to adjust the pH to be acidic, wherein the molar ratio of the product of the last step to the 2-bromotetradecyl ethyl carbonate to the sodium hydroxide is 1:1-2:1-2.
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