CN112687470A - Electrolyte for accelerating aging rate of aluminum electrolytic capacitor product and preparation method thereof - Google Patents

Electrolyte for accelerating aging rate of aluminum electrolytic capacitor product and preparation method thereof Download PDF

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Publication number
CN112687470A
CN112687470A CN202011392957.7A CN202011392957A CN112687470A CN 112687470 A CN112687470 A CN 112687470A CN 202011392957 A CN202011392957 A CN 202011392957A CN 112687470 A CN112687470 A CN 112687470A
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parts
electrolyte
ammonium
electrolytic capacitor
aluminum electrolytic
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李志刚
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Yancheng Xingchen Technology Co ltd
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Yancheng Xingchen Technology Co ltd
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Abstract

The invention discloses an electrolyte for accelerating the aging rate of an aluminum electrolytic capacitor product, which is prepared from the following components in parts by weight: 20-30 parts of ethylene glycol, 30-40 parts of MH-35 dispersant, 5-10 parts of carboxylate, 2-3 parts of mannitol, 3-6 parts of polyethylene glycol 1000, 1-3 parts of boric acid, 2-4 parts of ammonium dodecanedioate, 8-10 parts of ammonium hydrogen azelate aqueous solution, 0.3-0.5 part of ammonium hypophosphite, 0.1-0.3 part of o-nitroacetophenone and 0.2-0.5 part of m-nitroanisole, wherein the MH-35 dispersant comprises ammonium butyl suberate and hydroxyl salt in a mass ratio. The electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product effectively reduces the oxidation aging time of the electrolytic capacitor product, shortens the aging time by about 50 percent in the traditional process, has high product qualification rate, completely reaches 125 ℃ for 2500 hours in the verification of the service life of the electrolytic capacitor product, and greatly reduces the production cost and the resource waste.

Description

Electrolyte for accelerating aging rate of aluminum electrolytic capacitor product and preparation method thereof
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to an electrolyte for accelerating the aging rate of an aluminum electrolytic capacitor product and a preparation method thereof.
Background
The electrolyte is used as a core component of the aluminum electrolytic capacitor, and the quality of the electrolyte directly influences the service performance and the service life of the capacitor. The aluminum electrolytic capacitor needs to be aged in the production process, and aims to remove defective products and repair an oxide film, because the cut part of the positive foil in the cutting process has no oxide film, and some local damages of the foil in the manufacturing process need to be repaired, the oxide film with the corresponding thickness is achieved. In the production process of the aluminum electrolytic capacitor, the control of the aging process and the aging time determine the service life of the aluminum electrolytic capacitor. In the existing traditional process, 400v ox horn products are aged for more than 18 hours, so that the production efficiency of an aluminum electrolytic capacitor and the product repair efficiency in the aging process are strictly limited; meanwhile, the aluminum electrolytic capacitor is restricted by the characteristics of the electrolyte in the aging process, and products aged at normal temperature and high temperature can generate heat, if the oxidation efficiency of the aluminum foil is poor, the single product can generate heat seriously after the boosting time is long, and even the valve is opened to lose efficacy.
Disclosure of Invention
In order to overcome some problems and defects in the prior art, the invention provides an electrolyte for accelerating the aging rate of an aluminum electrolytic capacitor product and a preparation method thereof.
The invention is realized by the following technical scheme.
An electrolyte for accelerating the aging rate of an aluminum electrolytic capacitor product is prepared from the following components in parts by weight:
20-30 parts of ethylene glycol, 30-40 parts of MH-35 dispersant, 5-10 parts of carboxylate, 2-3 parts of mannitol, 3-6 parts of polyethylene glycol 1000, 1-3 parts of boric acid, 2-4 parts of ammonium dodecanedioate, 8-10 parts of ammonium hydrogen azelate aqueous solution, 0.3-0.5 part of ammonium hypophosphite, 0.1-0.3 part of o-nitroacetophenone and 0.2-0.5 part of m-nitroanisole, wherein the MH-35 dispersant comprises ammonium butyl suberate and hydroxyl salt in a mass ratio.
Preferably, the electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product is prepared from the following components in parts by weight:
22-25 parts of ethylene glycol, 33-37 parts of MH-35 dispersant, 6-8 parts of carboxylate, 2-3 parts of mannitol, 4-6 parts of polyethylene glycol 1000, 2-3 parts of boric acid, 2-3 parts of ammonium dodecanedioate, 8-9 parts of ammonium hydrogen azelate aqueous solution, 0.4-0.5 part of ammonium hypophosphite, 0.2-0.3 part of o-nitroacetophenone and 0.3-0.5 part of m-nitroanisole, wherein the MH-35 dispersant comprises ammonium butyl suberate and hydroxyl salt in equal mass ratio.
Preferably, the electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product is prepared from the following components in parts by weight:
25 parts of ethylene glycol, 35 parts of MH-35 dispersing agent, 8 parts of carboxylate, 2 parts of mannitol, 3-6 parts of polyethylene glycol 1000, 2 parts of boric acid, 3 parts of ammonium dodecanedioate, 9 parts of ammonium hydrogen azelate aqueous solution, 0.4 part of ammonium hypophosphite, 0.2 part of o-nitroacetophenone and 0.3 part of m-nitroanisole, wherein the MH-35 dispersing agent is composed of ammonium butyl suberate and hydroxyl salt in equal mass ratio.
Specifically, the mass fraction of the ammonium hydrogen azelate aqueous solution is 10-15%.
The invention also provides a preparation method of the electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product, which comprises the following operation steps:
(1) firstly, setting the temperature of an electrolyte stirrer to be 125-135 ℃, adding ethylene glycol and one third of MH-35 dispersant, and then turning on a temperature switch to start heating;
(2) when the temperature in the electrolyte stirrer rises to above 65 ℃, sequentially adding mannitol, polyethylene glycol 1000 and ammonium dodecanedioate, and closing a cylinder cover of the electrolyte stirrer after the addition is finished;
(3) after the temperature in the electrolyte stirrer rises to 125-135 ℃, carrying out heat preservation treatment for half an hour, and then closing a temperature switch to start heating and cooling;
(4) when the temperature in the electrolyte stirrer is reduced to 95-105 ℃, opening a cylinder cover, adding boric acid, the residual MH-35 dispersant and the ammonium hydrogen azelate aqueous solution, and continuously stirring for 25-35 min;
(5) and continuously adding ammonium phosphite, o-nitroacetophenone and m-nitroanisole into the electrolyte, continuously stirring until the temperature in the electrolyte stirrer is reduced to 60-70 ℃, and finally, continuously stirring for 12-18min to obtain the electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product.
Specifically, in the step (3), the cooling water of the electrolyte mixer is started when the temperature is reduced, and the cooling water is closed when the temperature in the electrolyte mixer is reduced to 95-105 ℃ and the cylinder cover is opened.
According to the technical scheme, the beneficial effects of the invention are as follows:
1) the electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product effectively reduces the oxidation aging time of the electrolytic capacitor product, shortens the aging time by about 50 percent in the traditional process, has high product qualification rate, completely reaches the service life verification of the electrolytic capacitor product of 125 ℃ for 2500 hours, and greatly reduces the production cost and the resource waste;
2) the electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product improves the aluminum foil oxidation efficiency of the aluminum electrolytic capacitor product in the aging process, avoids overhigh temperature rise in normal-temperature aging, reduces the gas production number of the aluminum electrolytic capacitor in high-temperature aging, and improves the oxidation efficiency.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
An electrolyte for accelerating the aging rate of an aluminum electrolytic capacitor product is prepared from the following components in parts by weight:
20 parts of ethylene glycol, 30 parts of MH-35 dispersing agent, 5 parts of carboxylate, 2 parts of mannitol, 3 parts of polyethylene glycol 1000, 1 part of boric acid, 2 parts of ammonium dodecaduplex, 8 parts of ammonium hydrogen azelate aqueous solution with the mass fraction of 10%, 0.3 part of ammonium hypophosphite, 0.1 part of o-nitroacetophenone and 0.2 part of m-nitroanisole, wherein the MH-35 dispersing agent is composed of ammonium butyl suberate and hydroxyl salt in equal mass proportion.
The embodiment also provides a preparation method of the electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product, which comprises the following operation steps:
(1) firstly, setting the temperature of an electrolyte stirrer to be 125 ℃, adding ethylene glycol and one third of MH-35 dispersant, and then turning on a temperature switch to start heating;
(2) when the temperature in the electrolyte stirrer rises to above 65 ℃, sequentially adding mannitol, polyethylene glycol 1000 and ammonium dodecanedioate, and closing a cylinder cover of the electrolyte stirrer after the addition is finished;
(3) after the temperature in the electrolyte stirrer rises to 125 ℃, carrying out heat preservation treatment for half an hour, then closing a temperature switch to start heating and start cooling, wherein cooling water of the electrolyte stirrer is started when the temperature is reduced to 95 ℃, and cooling water is closed when a cylinder cover is opened when the temperature in the electrolyte stirrer is reduced to 95 ℃;
(4) when the temperature in the electrolyte stirrer is reduced to 95 ℃, opening a cylinder cover, adding boric acid, the residual MH-35 dispersant and the ammonium hydrogen azelate aqueous solution, and continuously stirring for 25 min;
(5) and continuously adding ammonium phosphite, o-nitroacetophenone and m-nitroanisole into the electrolyte, continuously stirring until the temperature in the electrolyte stirrer is reduced to 60 ℃, and finally, continuously stirring for 12min to obtain the electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product.
Example 2
An electrolyte for accelerating the aging rate of an aluminum electrolytic capacitor product is prepared from the following components in parts by weight:
30 parts of ethylene glycol, 40 parts of MH-35 dispersing agent, 10 parts of carboxylate, 3 parts of mannitol, 6 parts of polyethylene glycol 1000, 3 parts of boric acid, 4 parts of ammonium dodecaduplex, 10 parts of ammonium hydrogen azelate aqueous solution with the mass fraction of 15%, 0.5 part of ammonium hypophosphite, 0.3 part of o-nitroacetophenone and 0.5 part of m-nitroanisole, wherein the MH-35 dispersing agent is composed of ammonium butyl octanedioate, hydroxyl salt and the like in mass proportion.
The embodiment also provides a preparation method of the electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product, which comprises the following operation steps:
(1) firstly, setting the temperature of an electrolyte stirrer to 135 ℃, adding ethylene glycol and one third of MH-35 dispersant, and then turning on a temperature switch to start heating;
(2) when the temperature in the electrolyte stirrer rises to above 65 ℃, sequentially adding mannitol, polyethylene glycol 1000 and ammonium dodecanedioate, and closing a cylinder cover of the electrolyte stirrer after the addition is finished;
(3) after the temperature in the electrolyte stirrer rises to 135 ℃, carrying out heat preservation treatment for half an hour, then closing a temperature switch to start heating and start cooling, wherein cooling water of the electrolyte stirrer is started when the temperature is reduced to 105 ℃, and cooling water is closed when a cylinder cover is opened when the temperature in the electrolyte stirrer is reduced to 105 ℃;
(4) when the temperature in the electrolyte stirrer is reduced to 105 ℃, opening a cylinder cover, adding boric acid, the residual MH-35 dispersant and the ammonium hydrogen azelate aqueous solution, and continuously stirring for 35 min;
(5) and continuously adding ammonium phosphite, o-nitroacetophenone and m-nitroanisole into the electrolyte, continuously stirring until the temperature in the electrolyte stirrer is reduced to 70 ℃, and finally, continuously stirring for 18min to obtain the electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product.
Comparative example 1
An electrolyte for accelerating the aging rate of an aluminum electrolytic capacitor product is prepared from the following components in parts by weight:
30 parts of ethylene glycol, 40 parts of MH-35 dispersing agent, 10 parts of carboxylate, 3 parts of mannitol, 6 parts of polyethylene glycol 1000, 3 parts of boric acid and 4 parts of ammonium dodecanedioate, wherein the MH-35 dispersing agent comprises ammonium butyl octanedioate, hydroxyl salt and the like in mass proportion. The remaining procedure was exactly the same as in example 2.
The electrolyte is prepared by the methods of each embodiment and each comparative example, and then the performances of the electrolyte are tested by methods of detecting the content of chloride ions by a conductivity tester, a flash firing voltage tester and a silver nitrate titration method, wherein the temperature of the electrolyte is 30 ℃ during the test, and the test results are as follows:
item Sparking voltage, v Conductance,. mu.s/cm2 pH value Chloride ion content 400v ox horn product aging time, h
Example 1 530 2.2 6.6 No abnormal condition after titration of silver nitrate 8
Example 2 540 2.0 6.7 No abnormal condition after titration of silver nitrate 8
Comparative example 1 500 1.7 6.5 No abnormal condition after titration of silver nitrate 17
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims (6)

1. The electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product is characterized by being prepared from the following components in parts by weight:
20-30 parts of ethylene glycol, 30-40 parts of MH-35 dispersant, 5-10 parts of carboxylate, 2-3 parts of mannitol, 3-6 parts of polyethylene glycol 1000, 1-3 parts of boric acid, 2-4 parts of ammonium dodecanedioate, 8-10 parts of ammonium hydrogen azelate aqueous solution, 0.3-0.5 part of ammonium hypophosphite, 0.1-0.3 part of o-nitroacetophenone and 0.2-0.5 part of m-nitroanisole, wherein the MH-35 dispersant comprises ammonium butyl suberate and hydroxyl salt in a mass ratio.
2. The electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product according to claim 1, which is prepared from the following components in parts by weight:
22-25 parts of ethylene glycol, 33-37 parts of MH-35 dispersant, 6-8 parts of carboxylate, 2-3 parts of mannitol, 4-6 parts of polyethylene glycol 1000, 2-3 parts of boric acid, 2-3 parts of ammonium dodecanedioate, 8-9 parts of ammonium hydrogen azelate aqueous solution, 0.4-0.5 part of ammonium hypophosphite, 0.2-0.3 part of o-nitroacetophenone and 0.3-0.5 part of m-nitroanisole, wherein the MH-35 dispersant comprises ammonium butyl suberate and hydroxyl salt in equal mass ratio.
3. The electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product according to claim 1, which is prepared from the following components in parts by weight:
25 parts of ethylene glycol, 35 parts of MH-35 dispersing agent, 8 parts of carboxylate, 2 parts of mannitol, 3-6 parts of polyethylene glycol 1000, 2 parts of boric acid, 3 parts of ammonium dodecanedioate, 9 parts of ammonium hydrogen azelate aqueous solution, 0.4 part of ammonium hypophosphite, 0.2 part of o-nitroacetophenone and 0.3 part of m-nitroanisole, wherein the MH-35 dispersing agent is composed of ammonium butyl suberate and hydroxyl salt in equal mass ratio.
4. The electrolyte for accelerating the aging rate of aluminum electrolytic capacitor products as recited in claim 1, wherein the mass fraction of the aqueous ammonium azelate solution is 10-15%.
5. The method for preparing the electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product according to claim 1, comprising the following steps:
(1) firstly, setting the temperature of an electrolyte stirrer to be 125-135 ℃, adding ethylene glycol and one third of MH-35 dispersant, and then turning on a temperature switch to start heating;
(2) when the temperature in the electrolyte stirrer rises to above 65 ℃, sequentially adding mannitol, polyethylene glycol 1000 and ammonium dodecanedioate, and closing a cylinder cover of the electrolyte stirrer after the addition is finished;
(3) after the temperature in the electrolyte stirrer rises to 125-135 ℃, carrying out heat preservation treatment for half an hour, and then closing a temperature switch to start heating and cooling;
(4) when the temperature in the electrolyte stirrer is reduced to 95-105 ℃, opening a cylinder cover, adding boric acid, the residual MH-35 dispersant and the ammonium hydrogen azelate aqueous solution, and continuously stirring for 25-35 min;
(5) and continuously adding ammonium phosphite, o-nitroacetophenone and m-nitroanisole into the electrolyte, continuously stirring until the temperature in the electrolyte stirrer is reduced to 60-70 ℃, and finally, continuously stirring for 12-18min to obtain the electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product.
6. The method for preparing the electrolyte for accelerating the aging rate of the aluminum electrolytic capacitor product as recited in claim 5, wherein in the step (3), the cooling water of the electrolyte mixer is turned on when the temperature is reduced, and the cooling water is turned off when the temperature in the electrolyte mixer is reduced to 95-105 ℃ and the cylinder cover is opened.
CN202011392957.7A 2020-12-03 2020-12-03 Electrolyte for accelerating aging rate of aluminum electrolytic capacitor product and preparation method thereof Pending CN112687470A (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63301514A (en) * 1987-06-01 1988-12-08 Nichicon Corp Electrolyte for driving aluminum electrolytic capacitor
JPS6481307A (en) * 1987-09-24 1989-03-27 Hitachi Condenser Electrolyte for aluminum electrolytic capacitor
JPH05152165A (en) * 1991-11-29 1993-06-18 Hitachi Aic Inc Electrolyte for electrolytic capacitor
JP2004193436A (en) * 2002-12-12 2004-07-08 Nippon Chemicon Corp Electrolyte for electrolytic capacitor
JP2008042042A (en) * 2006-08-09 2008-02-21 Sanyo Chem Ind Ltd Electrolyte for electrochemical capacitor, and electrochemical capacitor
JP2011222956A (en) * 2010-03-26 2011-11-04 Sanyo Chem Ind Ltd Electrolyte for electrolytic capacitor and electrolytic capacitor using the same
CN104934225A (en) * 2015-04-30 2015-09-23 南通理工学院 Electrolyte and preparation method thereof
CN105280386A (en) * 2015-11-06 2016-01-27 广东风华高新科技股份有限公司 Aluminium electrolytic capacitor and electrolyte and preparation method thereof, and charging and aging method of aluminium electrolytic capacitor
CN106098379A (en) * 2016-08-08 2016-11-09 深圳市智胜新电子技术有限公司 Electrolyte, the preparation method of electrolyte and aluminium electrolutic capacitor

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63301514A (en) * 1987-06-01 1988-12-08 Nichicon Corp Electrolyte for driving aluminum electrolytic capacitor
JPS6481307A (en) * 1987-09-24 1989-03-27 Hitachi Condenser Electrolyte for aluminum electrolytic capacitor
JPH05152165A (en) * 1991-11-29 1993-06-18 Hitachi Aic Inc Electrolyte for electrolytic capacitor
JP2004193436A (en) * 2002-12-12 2004-07-08 Nippon Chemicon Corp Electrolyte for electrolytic capacitor
JP2008042042A (en) * 2006-08-09 2008-02-21 Sanyo Chem Ind Ltd Electrolyte for electrochemical capacitor, and electrochemical capacitor
JP2011222956A (en) * 2010-03-26 2011-11-04 Sanyo Chem Ind Ltd Electrolyte for electrolytic capacitor and electrolytic capacitor using the same
CN104934225A (en) * 2015-04-30 2015-09-23 南通理工学院 Electrolyte and preparation method thereof
CN105280386A (en) * 2015-11-06 2016-01-27 广东风华高新科技股份有限公司 Aluminium electrolytic capacitor and electrolyte and preparation method thereof, and charging and aging method of aluminium electrolytic capacitor
CN106098379A (en) * 2016-08-08 2016-11-09 深圳市智胜新电子技术有限公司 Electrolyte, the preparation method of electrolyte and aluminium electrolutic capacitor

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