CN117476368B - Aluminum electrolytic capacitor with high stability and long service life - Google Patents

Aluminum electrolytic capacitor with high stability and long service life Download PDF

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CN117476368B
CN117476368B CN202311582018.2A CN202311582018A CN117476368B CN 117476368 B CN117476368 B CN 117476368B CN 202311582018 A CN202311582018 A CN 202311582018A CN 117476368 B CN117476368 B CN 117476368B
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CN117476368A (en
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苏镇顺
苏志鹏
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Shenzhen Donglianfa Technology Co ltd
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    • 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
    • H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
    • H01G13/006—Apparatus or processes for applying terminals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
    • H01G13/02—Machines for winding capacitors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
    • H01G13/04—Drying; Impregnating
    • 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
    • H01G9/008—Terminals
    • 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
    • H01G9/08—Housing; Encapsulation
    • 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

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Abstract

The invention discloses an aluminum electrolytic capacitor with high stability and long service life, which comprises anode foil, cathode foil, electrolytic paper and electrolyte; wherein the electrolyte consists of the following components in parts by weight: 90-120 parts of ethylene glycol, 10-25 parts of long-chain carboxylic acid, 10-25 parts of branched polycarboxylic acid, 5-15 parts of polyethylene glycol, 4-6 parts of pure water, 0.5-2 parts of nano silicon dioxide, 0.5-1 part of waterproof agent, 0.5-2 parts of hydrogen eliminating agent, 0.5-1 part of boric acid and 2-5 parts of flame retardant. According to the invention, by adjusting the composition of the electrolyte of the aluminum electrolytic capacitor, the aluminum electrolytic capacitor has good heat and cold resistance stability, high flash power and long service life.

Description

Aluminum electrolytic capacitor with high stability and long service life
Technical Field
The invention relates to the technical field of aluminum electrolytic capacitors, in particular to an aluminum electrolytic capacitor with high stability and long service life.
Background
Aluminum electrolytic capacitors generally comprise an aluminum foil, an electrolyte and electrodes, the working principle of which is based on ion conduction in the electrolyte. Aluminum electrolytic capacitors are a very important basic electronic component and have been widely used in consumer electronics, communication products, computers and peripheral products, instrumentation, automation control, automotive industry, photovoltaic products, high-speed rail and aviation and military equipment, etc. The aluminum electrolytic capacitor has large capacitance per unit volume and low cost, because the constituent materials of the electrolytic capacitor are common industrial materials, and the production cost is relatively low. The aluminum electrolytic capacitor has the characteristic of self-healing in the working process, has very high rated electrostatic capacity and can bear high electric field intensity. However, in practical application, the aluminum electrolytic capacitor is greatly affected by temperature, the electrolyte of the aluminum electrolytic capacitor is in a liquid state, the core heats or the electrolyte is volatilized due to higher ambient temperature, the electrolyte can be even dried and disabled for a long time, and the service life of the aluminum electrolytic capacitor can be shortened when the temperature is increased by 10 degrees in working. In addition, aluminum electrolytic capacitors may suffer from reduced performance under extreme temperature conditions, which can be a problem for some special applications, such as automotive electronics and military equipment.
Therefore, there is a need to develop an aluminum electrolytic capacitor having high stability and long life.
Disclosure of Invention
Based on the problems existing in the background technology, the invention provides the aluminum electrolytic capacitor with high stability and long service life, and the composition of the electrolyte of the aluminum electrolytic capacitor is adjusted, so that the aluminum electrolytic capacitor has good heat and cold resistance, high flash power and long service life.
The invention is implemented by the following technical scheme:
An aluminum electrolytic capacitor with high stability and long service life comprises anode foil, cathode foil, electrolytic paper and electrolyte;
Wherein the electrolyte consists of the following components in parts by weight: 90-120 parts of ethylene glycol, 10-25 parts of long-chain carboxylic acid, 10-25 parts of branched polycarboxylic acid, 5-15 parts of polyethylene glycol, 3-5 parts of pure water, 0.5-2 parts of nano silicon dioxide, 0.5-1 part of waterproof agent, 0.5-2 parts of hydrogen eliminating agent, 0.5-1 part of boric acid and 2-5 parts of flame retardant.
Further, the method for producing a long-chain carboxylic acid comprises the steps of:
S1, adding 1, 5-diphenyl pentan-1, 4-diene-3-ketone and 2-ketoglutaric acid into a high-temperature high-pressure kettle, adding 3-benzyl-5- (2-hydroxyethyl) -4-methylthiazolium chloride, ethanol and triethylamine serving as catalysts, introducing argon to perform gas replacement on a reaction system, and heating for reaction for 9-11h;
s2, removing the solvent by rotary evaporation after the reaction of the S1 is finished, adding ethyl acetate and pure water, washing off the catalyst in the system, collecting the organic phase, removing the solvent by rotary evaporation, adding absolute methanol, and dropwise adding sodium hydroxide solution until the pH value of the solution is 9.5-10; transferring the mixture into a reflux condenser tube, and reacting for 6 hours at 60 ℃;
S3, removing the solvent by rotary evaporation after the reaction of the S2 is finished, adding ethyl acetate and pure water for extraction, collecting the water phase, dropwise adding a phosphoric acid solution until the pH value of the solution is 2-2.5, adding the ethyl acetate solution, dissolving out a product, extracting and separating the solution, collecting the organic phase, removing the solvent by rotary evaporation, and drying the product to obtain the long-chain carboxylic acid.
Further, the preparation method of the branched polycarboxylic acid comprises the following steps:
S1, taking methanol as a solvent, regulating the pH value of a reaction solution to 2-3 under the catalysis of ferrous sulfate by using 1,4 cyclohexanedione and hydrogen peroxide, and controlling the reaction temperature to-5-10 ℃ to open the loop of the 1,4 cyclohexanedione to obtain a solution A;
S2, adding methyl acrylate into the solution A, reacting for 1-2 hours at 50-60 ℃, adding ethylene glycol, distilling, and collecting fractions at 125-135 ℃;
S3, adding the fraction collected in the S2 into 50% sodium hydroxide solution, reacting for 3-4 hours at 80-85 ℃, cooling to room temperature after the reaction is finished, adding phosphoric acid solution to adjust the pH value to 2-2.5, standing for 2 hours, filtering, collecting precipitate, washing with pure water, and drying to obtain the branched polycarboxylic acid.
Further, the waterproof agent is monoammonium phosphate or ammonium hypophosphite.
Further, the hydrogen eliminating agent is one or more of p-nitrobenzoic acid, p-nitrobenzyl alcohol or p-nitrophenol.
Further, the flame retardant is diethyl phosphite.
Further, the preparation method of the electrolyte comprises the following steps:
S1, adding long-chain carboxylic acid and branched polycarboxylic acid into ethylene glycol, stirring and mixing uniformly, and introducing ammonia gas until the pH value of the solution reaches 7.5-8 to obtain a carboxylic acid ammonium salt-ethylene glycol solution;
S2, heating the ammonium carboxylate-glycol solution to 110-130 ℃, adding polyethylene glycol and a hydrogen eliminating agent, preserving heat, stirring for 10-30min, cooling to 50 ℃, adding nano silicon dioxide, pure water, a waterproof agent, boric acid and a flame retardant, stirring until the nano silicon dioxide, the pure water, the waterproof agent, the boric acid and the flame retardant are completely dissolved, and cooling to room temperature to obtain the electrolyte.
Further, when ammonia gas is introduced in the step S1, the ventilation rate of the mixed solution of each liter of long-chain carboxylic acid, branched-chain polycarboxylic acid and ethylene glycol is 0.2-0.4m 3/min.
Further, the aluminum electrolytic capacitor further comprises an extraction bar, a cover plate and an aluminum shell.
Further, the preparation method of the aluminum electrolytic capacitor comprises the following steps:
(1) Cutting the anode foil, the cathode foil, the electrolytic paper and the leading-out strip into specified sizes for standby;
(2) Riveting the leading-out strip on a corresponding aluminum foil, inserting electrolytic paper between the anode foil and the cathode foil of rivet over, and winding into a cylinder to obtain a prime;
(3) Immersing the wound element into electrolyte;
(4) Assembling an aluminum shell outside the aluminum electrolytic capacitor with a prime body, sealing the aluminum shell with a black rubber leather head, and blocking volatilization and leakage of an aluminum electrolyte;
(5) And (3) applying direct-current voltage to repair the damaged oxide film on the surface of the aluminum foil, thus obtaining the aluminum electrolytic capacitor.
The invention has the beneficial effects that:
(1) According to the invention, the composition of the electrolyte of the aluminum electrolytic capacitor is regulated, long-chain ammonium carboxylate and branched-chain ammonium polycarboxylic acid are mixed to be used as effective solutes of the electrolyte, the water content in the electrolyte and the composition of other additives are controlled, and the conductivity and sparking voltage of the electrolyte are effectively improved; the aluminum electrolytic capacitor prepared by the electrolyte has higher temperature resistance and stability, and the service life of the aluminum electrolytic capacitor is prolonged.
(2) The long-chain carboxylic acid prepared by the method increases the length of a carbon chain, reduces the polarity of the long-chain carboxylic acid, and simultaneously increases the polarity of the long-chain carboxylic acid by introducing a plurality of carbonyl groups, compared with the straight-chain carboxylic acid, the long-chain carboxylic acid prepared by the method has better solubility in ethylene glycol; compared with the traditional straight-chain carboxylic acid, the electrolyte prepared from the long-chain carboxylic acid has better performance.
(3) The branched polycarboxylic acid prepared by the method adopts 1,4 cyclohexanedione as a raw material, and is synthesized by a cyclohexanone Fenton method, so that chain growth of the branched polycarboxylic acid is realized, meanwhile, one more carbonyl group in the structure of the branched polycarboxylic acid increases the polarity of the branched polycarboxylic acid, the solubility of the branched polycarboxylic acid in glycol is improved, and the electrolyte prepared by the branched polycarboxylic acid prepared by the method has better performance.
Detailed Description
The technical scheme of the present invention will be further described in detail with reference to the following specific examples, but the scope of the present invention is not limited to the following examples.
Example 1
The aluminum electrolytic capacitor electrolyte consists of the following components in parts by weight: 110 parts of ethylene glycol, 15 parts of long-chain carboxylic acid, 15 parts of branched polycarboxylic acid, 10 parts of polyethylene glycol, 4 parts of pure water, 1 part of nano silicon dioxide, 0.8 part of waterproof agent ammonium hypophosphite, 1 part of hydrogen-eliminating agent p-nitrobenzoic acid, 0.8 part of boric acid and 4 parts of flame retardant diethyl phosphite.
Wherein, the preparation method of the long-chain carboxylic acid comprises the following steps:
S1, adding 2mmol of 1, 5-diphenylpentan-1, 4-diene-3-one and 5mmol of 2-ketoglutaric acid into a high-temperature high-pressure kettle, adding 0.4mmol of catalyst 3-benzyl-5- (2-hydroxyethyl) -4-methylthiazolium chloride, 15mL of ethanol and 5mmol of triethylamine, introducing argon gas to perform gas replacement on the reaction system, and heating at 120 ℃ for reaction for 9h;
s2, removing the solvent by rotary evaporation after the reaction of the S1 is finished, adding ethyl acetate and pure water, washing off the catalyst in the system, collecting the organic phase, removing the solvent by rotary evaporation, adding absolute methanol, and dropwise adding 50% sodium hydroxide solution until the pH value of the solution is 10; transferring the mixture into a reflux condenser tube, and reacting for 6 hours at 60 ℃;
s3, removing the solvent by rotary evaporation after the reaction of the S2 is finished, adding ethyl acetate and pure water for extraction, collecting the water phase, dropwise adding a phosphoric acid solution until the pH value of the solution is 2.5, adding the ethyl acetate solution, dissolving out a product, extracting and separating liquid, collecting an organic phase, removing the solvent by rotary evaporation, and drying the product to obtain the long-chain carboxylic acid.
The preparation method of the branched polycarboxylic acid comprises the following steps:
s1, taking 50mL of methanol as a solvent, regulating the pH value of a reaction solution to 2.5 under the catalysis of 0.025mol of ferrous sulfate by 0.05mol of 1,4 cyclohexanedione and 0.025mol of hydrogen peroxide, controlling the reaction temperature to 0 ℃, and reacting for 6 hours to open the loop of the 1,4 cyclohexanedione to obtain a solution A;
S2, adding 0.04mol of methyl acrylate into the solution A, reacting for 2 hours at 50 ℃, adding glycol, distilling, and collecting fractions at 125-135 ℃;
S3, adding the fraction collected in the S2 into 30mL of 50% sodium hydroxide solution, reacting for 3 hours at 85 ℃, cooling to room temperature after the reaction is finished, adding phosphoric acid solution to adjust the pH value to 2.5, standing for 2 hours, filtering, collecting precipitate, washing with pure water, and drying to obtain the branched polycarboxylic acid.
The preparation method of the electrolyte comprises the following steps:
S1, adding long-chain carboxylic acid and branched polycarboxylic acid into ethylene glycol, stirring and mixing uniformly, and introducing ammonia gas until the pH value of the solution reaches 7.5-8 to obtain a carboxylic acid ammonium salt-ethylene glycol solution; wherein the ventilation rate of the mixed solution of each liter of long-chain carboxylic acid, branched-chain polycarboxylic acid and glycol is 0.3m 3/min;
S2, heating the ammonium carboxylate-glycol solution to 120 ℃, adding polyethylene glycol and a hydrogen eliminating agent, preserving heat, stirring for 20min, cooling to 50 ℃, adding nano silicon dioxide, pure water, a waterproof agent, boric acid and a flame retardant, stirring until the nano silicon dioxide, the pure water, the waterproof agent, the boric acid and the flame retardant are completely dissolved, and cooling to room temperature to obtain the electrolyte.
Example 2
The aluminum electrolytic capacitor electrolyte consists of the following components in parts by weight: 110 parts of ethylene glycol, 10 parts of long-chain carboxylic acid, 20 parts of branched polycarboxylic acid, 10 parts of polyethylene glycol, 4 parts of pure water, 1 part of nano silicon dioxide, 0.8 part of waterproof agent ammonium hypophosphite, 1 part of hydrogen-eliminating agent p-nitrobenzoic acid, 0.8 part of boric acid and 4 parts of flame retardant diethyl phosphite.
The procedure was as in example 1.
Example 3
The aluminum electrolytic capacitor electrolyte consists of the following components in parts by weight: 110 parts of ethylene glycol, 20 parts of long-chain carboxylic acid, 10 parts of branched polycarboxylic acid, 10 parts of polyethylene glycol, 4 parts of pure water, 1 part of nano silicon dioxide, 0.8 part of waterproof agent ammonium hypophosphite, 1 part of hydrogen-eliminating agent p-nitrobenzoic acid, 0.8 part of boric acid and 4 parts of flame retardant diethyl phosphite.
The procedure was as in example 1.
Example 4
The aluminum electrolytic capacitor electrolyte consists of the following components in parts by weight: 120 parts of ethylene glycol, 20 parts of long-chain carboxylic acid, 20 parts of branched polycarboxylic acid, 10 parts of polyethylene glycol, 6 parts of pure water, 1 part of nano silicon dioxide, 0.8 part of waterproof agent ammonium hypophosphite, 1 part of hydrogen-eliminating agent p-nitrobenzoic acid, 0.8 part of boric acid and 4 parts of flame retardant diethyl phosphite.
The procedure was as in example 1.
Comparative example 1
The aluminum electrolytic capacitor electrolyte consists of the following components in parts by weight: 110 parts of ethylene glycol, 30 parts of branched polycarboxylic acid, 10 parts of polyethylene glycol, 4 parts of pure water, 1 part of nano silicon dioxide, 0.8 part of waterproof agent ammonium hypophosphite, 1 part of hydrogen eliminator p-nitrobenzoic acid, 0.8 part of boric acid and 4 parts of flame retardant diethyl phosphite.
The branched polycarboxylic acid was prepared in the same manner as in example 1.
The preparation method of the electrolyte comprises the following steps:
s1, adding branched polycarboxylic acid into ethylene glycol, stirring and mixing uniformly, and introducing ammonia gas until the pH value of the solution reaches 7.5-8 to obtain a carboxylic acid ammonium salt-ethylene glycol solution; wherein the ventilation rate of the mixed solution of each liter of long-chain carboxylic acid, branched-chain polycarboxylic acid and glycol is 0.3m 3/min;
S2, heating the ammonium carboxylate-glycol solution to 120 ℃, adding polyethylene glycol and a hydrogen eliminating agent, preserving heat, stirring for 20min, cooling to 50 ℃, adding nano silicon dioxide, pure water, a waterproof agent, boric acid and a flame retardant, stirring until the nano silicon dioxide, the pure water, the waterproof agent, the boric acid and the flame retardant are completely dissolved, and cooling to room temperature to obtain the electrolyte.
Comparative example 2
The aluminum electrolytic capacitor electrolyte consists of the following components in parts by weight: 110 parts of ethylene glycol, 30 parts of long-chain carboxylic acid, 10 parts of polyethylene glycol, 4 parts of pure water, 1 part of nano silicon dioxide, 0.8 part of waterproof agent ammonium hypophosphite, 1 part of hydrogen eliminator p-nitrobenzoic acid, 0.8 part of boric acid and 4 parts of flame retardant diethyl phosphite.
The preparation of the long-chain carboxylic acid was the same as in example 1.
The preparation method of the electrolyte comprises the following steps:
S1, adding long-chain carboxylic acid into glycol, stirring and mixing uniformly, and introducing ammonia gas until the pH value of the solution reaches 7.5-8 to obtain a carboxylic acid ammonium salt-glycol solution; wherein the ventilation rate of the mixed solution of each liter of long-chain carboxylic acid, branched-chain polycarboxylic acid and glycol is 0.3m 3/min;
S2, heating the ammonium carboxylate-glycol solution to 120 ℃, adding polyethylene glycol and a hydrogen eliminating agent, preserving heat, stirring for 20min, cooling to 50 ℃, adding nano silicon dioxide, pure water, a waterproof agent, boric acid and a flame retardant, stirring until the nano silicon dioxide, the pure water, the waterproof agent, the boric acid and the flame retardant are completely dissolved, and cooling to room temperature to obtain the electrolyte.
Comparative example 3
The aluminum electrolytic capacitor electrolyte consists of the following components in parts by weight: 110 parts of ethylene glycol, 15 parts of ammonium sebacate, 15 parts of branched polycarboxylic acid, 10 parts of polyethylene glycol, 4 parts of pure water, 1 part of nano silicon dioxide, 0.8 part of waterproof agent ammonium hypophosphite, 1 part of hydrogen-eliminating agent p-nitrobenzoic acid, 0.8 part of boric acid and 4 parts of flame retardant diethyl phosphite.
The branched polycarboxylic acid was prepared in the same manner as in example 1.
The preparation method of the electrolyte comprises the following steps:
s1, adding branched polycarboxylic acid into ethylene glycol, stirring and mixing uniformly, and introducing ammonia gas until the pH value of the solution reaches 7.5-8 to obtain a carboxylic acid ammonium salt-ethylene glycol solution; wherein the ventilation rate of the mixed solution of each liter of long-chain carboxylic acid, branched-chain polycarboxylic acid and glycol is 0.3m 3/min;
s2, heating the ammonium carboxylate-glycol solution to 120 ℃, adding ammonium sebacate, polyethylene glycol and a hydrogen eliminating agent, preserving heat and stirring for 20min, cooling to 50 ℃, adding nano silicon dioxide, pure water, a waterproof agent, boric acid and a flame retardant, stirring until the nano silicon dioxide, the pure water, the waterproof agent, the boric acid and the flame retardant are completely dissolved, and cooling to room temperature to obtain the electrolyte.
Comparative example 4
The aluminum electrolytic capacitor electrolyte consists of the following components in parts by weight: 110 parts of ethylene glycol, 15 parts of long-chain carboxylic acid, 15 parts of branched polycarboxylic acid, 10 parts of polyethylene glycol, 2 parts of pure water, 1 part of nano silicon dioxide, 0.8 part of waterproof agent ammonium hypophosphite, 1 part of hydrogen-eliminating agent p-nitrobenzoic acid, 0.8 part of boric acid and 4 parts of flame retardant diethyl phosphite.
The preparation of long-chain carboxylic acids and branched polycarboxylic acids was carried out in the same manner as in example 1.
The preparation method of the electrolyte comprises the following steps:
S1, adding long-chain carboxylic acid and branched polycarboxylic acid into ethylene glycol, stirring and mixing uniformly, and introducing ammonia gas until the pH value of the solution reaches 7.5-8 to obtain a carboxylic acid ammonium salt-ethylene glycol solution; wherein the ventilation rate of the mixed solution of each liter of long-chain carboxylic acid, branched-chain polycarboxylic acid and glycol is 0.3m 3/min;
s2, heating the ammonium carboxylate-glycol solution to 120 ℃, adding polyethylene glycol and a hydrogen eliminating agent, preserving heat, stirring for 20min, cooling to 50 ℃, adding nano silicon dioxide, a waterproof agent, boric acid and a flame retardant, stirring until the nano silicon dioxide, the waterproof agent, the boric acid and the flame retardant are completely dissolved, and cooling to room temperature to obtain the electrolyte.
Comparative example 5
The aluminum electrolytic capacitor electrolyte consists of the following components in parts by weight: 110 parts of ethylene glycol, 15 parts of long-chain carboxylic acid, 15 parts of branched polycarboxylic acid, 10 parts of polyethylene glycol, 10 parts of pure water, 1 part of nano silicon dioxide, 0.8 part of waterproof agent ammonium hypophosphite, 1 part of hydrogen-eliminating agent p-nitrobenzoic acid, 0.8 part of boric acid and 4 parts of flame retardant diethyl phosphite.
The preparation procedure was the same as in comparative example 4.
Example 5
An aluminum electrolytic capacitor having a specification of 450v,470 μf (phi=35 mm×50 mm) was produced using the electrolytes in examples 1 to 4 and comparative examples 1 to 5, and the aluminum electrolytic capacitor was produced by a method comprising the steps of:
(1) Cutting the anode foil, the cathode foil, the electrolytic paper and the drawing strip into specified sizes for standby;
(2) Riveting the leading-out strip on a corresponding aluminum foil, inserting electrolytic paper between the anode foil and the cathode foil of rivet over, and winding into a cylinder to obtain a prime;
(3) Immersing the wound element into electrolyte;
(4) Assembling an aluminum shell outside the aluminum electrolytic capacitor with a prime body, sealing the aluminum shell with a black rubber leather head, and blocking volatilization and leakage of an aluminum electrolyte;
(5) And (3) applying direct-current voltage to repair the damaged oxide film on the surface of the aluminum foil, thus obtaining the aluminum electrolytic capacitor.
Test example 1
Adopting a conductivity meter to test the conductivity of the electrolyte with the temperature of 30 ℃; the sparking voltage of the electrolyte with the temperature of 30 ℃ was measured under the condition of constant current by using a TV tester, and the test results are shown in Table 1.
TABLE 1
Group of Conductivity (mS/cm) Sparking voltage (V)
Example 1 2.34 559
Example 2 2.42 519
Example 3 2.21 528
Example 4 2.38 563
Comparative example 1 2.31 491
Comparative example 2 1.95 505
Comparative example 3 2.34 503
Comparative example 4 1.75 520
Comparative example 5 2.57 437
As can be seen from the data in Table 1, the electrolyte prepared in the examples 1-4 of the invention has higher conductivity and sparking voltage, and the sparking voltage of the electrolyte is reduced when the ammonium carboxylate-glycol solution is prepared from branched polycarboxylic acid and glycol in the comparative example 1; in comparative example 2, a carboxylic acid ammonium salt-ethylene glycol solution is prepared from long-chain carboxylic acid and ethylene glycol, and the conductivity of the electrolyte is reduced; in comparative example 3, the linear carboxylate sebacate ammonium is adopted to replace the long-chain carboxylate ammonium salt, and the prepared electrolyte has small conductivity change, but the sparking voltage is reduced; the pure water content in the electrolyte was adjusted in comparative examples 4 and 5, and it was found that when the pure water content in the electrolyte was low, the conductivity of the electrolyte was significantly reduced, and as the pure water content was increased, the conductivity of the electrolyte became large, but the sparking voltage was reduced, and at the same time, the water content was increased, the sparking voltage of the electrolyte was unstable, and the pressure drop was increased.
Test example two
The aluminum electrolytic capacitor prepared in example 5 was subjected to performance tests at normal temperature (25 ℃) and low temperature (-40 ℃) and tested for capacitance, dissipation factor loss angle and impedance according to the CD261X type fixed aluminum electrolytic capacitor, which is a detailed specification for electronic components; in each example, 10 aluminum electrolytic capacitors were produced and tested in the same manner as in the comparative example, and the average value was obtained, and the specific results are shown in table 2.
TABLE 2
Note that: the percent reduction of C is calculated by dividing the difference between the performance at-40 ℃ and the performance at 25 ℃ by the performance at 25 ℃; DF and Z rise times are calculated as the ratio of-40 ℃ performance to 20 ℃.
As is clear from the results of Table 2, the aluminum electrolytic capacitors prepared from the electrolytes of examples 1 to 4 were in acceptable ranges in terms of capacitance, dissipation factor loss angle and impedance value at-40 ℃.
Test example three
The aluminum electrolytic capacitor prepared in example 5 was subjected to a +105℃ C high-temperature load reliability life test according to the standard of CD261X type fixed aluminum electrolytic capacitor, which is a specification for electronic components, and the specific results are shown in Table 3.
TABLE 3 Table 3
As can be seen from the results of Table 3, the aluminum electrolytic capacitors prepared by the electrolytes of examples 1 to 4 of the present invention have a small loss rate of capacitance and stable performance after long-term use at a high temperature of 105 ℃. The aluminum electrolytic capacitor has better high-temperature reliability service life.
Finally, it should be noted that: the above examples merely illustrate several embodiments of the present invention and are not intended to limit the invention, and any modifications, equivalent substitutions, improvements, etc. made by those skilled in the art without departing from the spirit of the present invention are intended to be included in the scope of the present invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (8)

1. An aluminum electrolytic capacitor with high stability and long service life is characterized by comprising anode foil, cathode foil, electrolytic paper and electrolyte;
Wherein the electrolyte consists of the following components in parts by weight: 90-120 parts of ethylene glycol, 10-25 parts of long-chain carboxylic acid, 10-25 parts of branched polycarboxylic acid, 5-15 parts of polyethylene glycol, 4-6 parts of pure water, 0.5-2 parts of nano silicon dioxide, 0.5-1 part of waterproof mixture, 0.5-2 parts of hydrogen eliminating agent, 0.5-1 part of boric acid and 2-5 parts of flame retardant; the preparation method of the long-chain carboxylic acid comprises the following steps:
S1, adding 1, 5-diphenyl pentan-1, 4-diene-3-ketone and 2-ketoglutaric acid into a high-temperature high-pressure kettle, adding 3-benzyl-5- (2-hydroxyethyl) -4-methylthiazolium chloride, ethanol and triethylamine serving as catalysts, introducing argon to perform gas replacement on a reaction system, and heating for reaction for 9-11h;
s2, removing the solvent by rotary evaporation after the reaction of the S1 is finished, adding ethyl acetate and pure water, washing off the catalyst in the system, collecting the organic phase, removing the solvent by rotary evaporation, adding absolute methanol, and dropwise adding sodium hydroxide solution until the pH value of the solution is 9.5-10; transferring the mixture into a reflux condenser tube, and reacting for 6 hours at 60 ℃;
S3, removing the solvent by rotary evaporation after the reaction of the S2 is finished, adding ethyl acetate and pure water for extraction, collecting a water phase, dropwise adding a phosphoric acid solution until the pH value of the solution is 2-2.5, adding the ethyl acetate solution, dissolving out a product, extracting and separating liquid, collecting an organic phase, removing the solvent by rotary evaporation, and drying the product to obtain long-chain carboxylic acid; the preparation method of the branched polycarboxylic acid comprises the following steps:
S1, taking methanol as a solvent, regulating the pH value of a reaction solution to 2-3 under the catalysis of ferrous sulfate by using 1,4 cyclohexanedione and hydrogen peroxide, and controlling the reaction temperature to-5-10 ℃ to open the loop of the 1,4 cyclohexanedione to obtain a solution A;
S2, adding methyl acrylate into the solution A, reacting for 1-2 hours at 50-60 ℃, adding ethylene glycol, distilling, and collecting fractions at 125-135 ℃;
S3, adding the fraction collected in the S2 into 50% sodium hydroxide solution, reacting for 3-4 hours at 80-85 ℃, cooling to room temperature after the reaction is finished, adding phosphoric acid solution to adjust the pH value to 2-2.5, standing for 2 hours, filtering, collecting precipitate, washing with pure water, and drying to obtain the branched polycarboxylic acid.
2. The aluminum electrolytic capacitor according to claim 1, wherein the water-repellent agent is monoammonium phosphate or ammonium hypophosphite.
3. The aluminum electrolytic capacitor as recited in claim 1, wherein the hydrogen scavenger is one or more of p-nitrobenzoic acid, p-nitrobenzyl alcohol or p-nitrophenol.
4. The aluminum electrolytic capacitor as recited in claim 1, wherein the flame retardant is diethyl phosphite.
5. The aluminum electrolytic capacitor as recited in claim 1, wherein the method for preparing the electrolytic solution comprises the steps of:
S1, adding long-chain carboxylic acid and branched polycarboxylic acid into ethylene glycol, stirring and mixing uniformly, and introducing ammonia gas until the pH value of the solution reaches 7.5-8 to obtain a carboxylic acid ammonium salt-ethylene glycol solution;
S2, heating the ammonium carboxylate-glycol solution to 110-130 ℃, adding polyethylene glycol and a hydrogen eliminating agent, preserving heat, stirring for 10-30min, cooling to 50 ℃, adding nano silicon dioxide, pure water, a waterproof agent, boric acid and a flame retardant, stirring until the nano silicon dioxide, the pure water, the waterproof agent, the boric acid and the flame retardant are completely dissolved, and cooling to room temperature to obtain the electrolyte.
6. The aluminum electrolytic capacitor as recited in claim 5, wherein the aeration rate per liter of the mixed solution of the long-chain carboxylic acid, the branched polycarboxylic acid and the ethylene glycol is 0.2 to 0.4m 3/min when the ammonia gas is introduced in the step S1.
7. The aluminum electrolytic capacitor as recited in claim 1, further comprising a lead-out bar, a cover plate, and an aluminum case.
8. The aluminum electrolytic capacitor as recited in claim 1, wherein the method for manufacturing the aluminum electrolytic capacitor comprises the steps of:
(1) Cutting the anode foil, the cathode foil, the electrolytic paper and the leading-out strip into specified sizes for standby;
(2) Riveting the leading-out strip on a corresponding aluminum foil, inserting electrolytic paper between the anode foil and the cathode foil of rivet over, and winding into a cylinder to obtain a prime;
(3) Immersing the wound element into electrolyte;
(4) Assembling an aluminum shell outside the aluminum electrolytic capacitor with a prime body, sealing the aluminum shell with a black rubber leather head, and blocking volatilization and leakage of an aluminum electrolyte;
(5) And (3) applying direct-current voltage to repair the damaged oxide film on the surface of the aluminum foil, thus obtaining the aluminum electrolytic capacitor.
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WO2021149739A1 (en) * 2020-01-22 2021-07-29 日本ケミコン株式会社 Solid electrolytic capacitor

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US4860169A (en) * 1988-12-14 1989-08-22 North American Philips Corporation Long chain carboxylic acids for very high voltage aluminum electrolytic capacitors
JP2007126611A (en) * 2005-11-07 2007-05-24 Okamura Seiyu Kk Long chain dibasic acid
CN101840785B (en) * 2010-04-23 2012-08-22 福建云星电子有限公司 Novel electrolyte
JP2013211372A (en) * 2012-03-30 2013-10-10 Hitachi Aic Inc Electrolyte for electrolytic capacitor
CN105469991B (en) * 2015-12-22 2018-11-13 东莞市久制电子有限公司 A kind of high scintillation long life aluminum electrolytic capacitor electrolyte and preparation method thereof
CN105938760A (en) * 2016-06-01 2016-09-14 广东黄宝石电子科技有限公司 Electrolytic capacitor high voltage electrolyte and preparation method thereof
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WO2021149739A1 (en) * 2020-01-22 2021-07-29 日本ケミコン株式会社 Solid electrolytic capacitor

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