CN101114544A - Working electrolyte for wide temperature high voltage aluminium electrolytic capacitor and method for making same thereof - Google Patents
Working electrolyte for wide temperature high voltage aluminium electrolytic capacitor and method for making same thereof Download PDFInfo
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Abstract
The invention discloses working electrolyte for the aluminum electrolytic capacitor with wide working temperature range and high voltage and the manufacturing method. The invention includes the following materials (calculating with weight percent): 60 percent to 80 percent glycol, 5 percent to 20 percent Gamma butyrolactone, 0 percent to 5 percent water, 2 percent to 5 percent ammonium sebacate, 5 percent to 10 percent isosebacic acid ammonium, 0 percent to 5 percent sebacic acid, 0.1 percent to 2 percent ammonium dihydrogen phosphate, 0.1 percent to 1 percent citric acid, 0.1 percent to 2 percent p-nitrobenzoic acid and 5 percent to 20 percent polyethylene glycol. The manufacturing method is as follows: (1) well-mixing the glycol, Gamma butyrolactone and water and heating to 60 DEG C through 90 DEG C; (2) adding the ammonium sebacate, sebacic acid, ammonium dihydrogen phosphate, citric acid, p-nitrobenzoic acid, polyethylene glycol to the mixed solvent and well-mixing; (3) after ample dissolution of the materials, keeping the temperature in the step (3) for five through thirty minutes; (4) adding the isosebacic acid ammonium to the mixture and keeping the temperature in the step (3) for five through thirty minutes, and stopping heating and natural cooling in the air, and obtaining the aluminum electrolytic capacitor with wide working temperature range and high voltage. The product increases the conductivity and the sparking voltage of the working electrolyte and reduces the production cost.
Description
(1) technical field:
The present invention relates to a kind of aluminium electrolytic capacitor Working electrolyte, particularly a kind of wide temperature high voltage aluminium electrolytic capacitor Working electrolyte; The invention still further relates to the preparation method of this wide temperature high voltage aluminium electrolytic capacitor with Working electrolyte.
(2) background technology:
The electronic devices and components industry is the basis of information industry, and capacitor is the chief component of electronic devices and components, accounts for 40% of electronic devices and components.Capacitor product mainly is a three major types at present: electrolytic capacitor, ceramic capacitor, organic film condenser, wherein aluminium electrolytic capacitor account for its 36.8%, because the characteristics (high specific capacity and very high applied electric field intensity) of aluminium electrolytic capacitor, make it to become the consumption maximum, one of electronic devices and components of still not replacing at present, especially high-pressure aluminum electrolytic capacitor has been widely used in automotive electronics, household electrical appliance, display, Switching Power Supply, electricity-saving lamp, in the electronic equipments such as electron rectifier, become an indispensable part in the complete electronic set system.Because mainly is that spent glycol is made solvent at the high-pressure aluminum electrolytic capacitor of current use with Working electrolyte, do solute with boric acid and ammonium salt thereof such as ammonium pentaborate, it is formulated to be aided with corresponding additive.The maximum operation (service) temperature of this system is 85 ℃, at high temperature boric acid is easy to generate a large amount of water with ethylene glycol generation esterification, thereby cause electrolyte vapour pressure when high temperature excessive, the easy bulging of capacitor even burst and lost efficacy, and boric acid is separated out easily when low temperature, therefore, the electrolyte of this system is difficult to satisfy the requirement of making wide temperature high voltage aluminium electrolytic capacitor.People used organic dicarboxylic acids of straight chain and ammonium salt thereof as electrolyte afterwards, but along with carbon number increases, the solubility of the organic dicarboxylic acids of straight chain in ethylene glycol diminishes gradually, cause in the electrolyte solutes content less, thereby its conductivity is diminished, and because the carbochain of the organic dicarboxylic acids of straight chain is longer, influenced by three-dimensional effect etc., the rate of pressure rise of electrolyte is slower, and oxidation efficiency is low, and is bigger with the loss tangent of the capacitor of its production.And it is relatively poor to do the electrolyte solution high-temperature stability with the organic dicarboxylic acids of straight chain separately.
(3) summary of the invention:
The present invention will disclose the wide temperature high voltage aluminium electrolytic capacitor work electrolyte prescription that a kind of cost is lower, high-temperature stability is good; The present invention also will be openly with the best preparation method of this wide temperature high voltage aluminium electrolytic capacitor of above-mentioned formulation with Working electrolyte.
Study repeatedly, test through the applicant, adopt ethylene glycol, gamma-butyrolacton, water to make mixed solvent, doing compound solute with the isosebacic acid ammonium, decanedioic acid, the ammonium sebacate that have side chain is the primary raw material of electrolytic capacitor with Working electrolyte, and with above-mentioned each raw material according to reacting under following formula rate and the process conditions, then can prepare the wide temperature high voltage aluminium electrolytic capacitor Working electrolyte that cost is lower, high-temperature stability is good.
Concrete prescription (each component is by percentage to the quality):
Ethylene glycol 60～80%; Gamma-butyrolacton 5～20%; Water 0～5%;
Ammonium sebacate 2～5%; Isosebacic acid ammonium 5～10%; Decanedioic acid 0～5%;
Ammonium dihydrogen phosphate 0.1～2%; Citric acid 0.1～1%; Paranitrobenzoic acid 0.1～2%;
Polyethylene glycol 5～20%.
The preparation method:
1) ethylene glycol, gamma-butyrolacton, water are mixed, be heated to 60～90 ℃, make fully reaction between each reactant, also can quicken the speed of raw material dissolving simultaneously;
2) in above-mentioned mixed solvent, add ammonium sebacate, decanedioic acid, ammonium dihydrogen phosphate, citric acid, paranitrobenzoic acid, polyethylene glycol, stir;
3) mixture of gained is heated to 110～150 ℃, treat that each raw material fully dissolves after, kept said temperature 5～30 minutes, the water that generates with ER; It mainly is to be fast reaction speed that mixture is heated to 110～150 ℃, and the water that reaction is generated can evaporate faster; Described blend heated preferred temperature is 110～140 ℃;
4) add the isosebacic acid ammonium in said mixture, kept the described temperature of step 3) 5～30 minutes, the water that ER generates stops heating then, treats its natural cooling in air, obtains the wide temperature high voltage aluminium electrolytic capacitor Working electrolyte.
Wide temperature high voltage aluminium electrolytic capacitor Working electrolyte with this method preparation, both can remedy the shortcoming of ethylene glycol to ammonium sebacate solvability difference, can guarantee the oxidation efficiency of electrolyte again, simultaneously the high-temperature behavior of electrolyte is improved greatly, can satisfy the requirement of wide temperature, high-voltage electrolysis capacitor well.
(4) embodiment:
Embodiment 1:
Each raw material proportioning sees Table 1.
Table 1 embodiment 1 each raw material components
| Title | Ethylene glycol | γ-butyrolactone | Ammonium sebacate | The isosebacic acid ammonium | Decanedioic acid | Citric acid | Paranitrobenzoic acid | Polyethylene glycol | Ammonium dihydrogen phosphate | Water |
| Mass percent % | 60 | 8 | 3 | 10 | 2 | 0.3 | 1 | 13 | 0.7 | 2 |
1) ethylene glycol, gamma-butyrolacton, water are mixed, be heated to 60 ℃;
2) in above-mentioned mixed solvent, add ammonium sebacate, decanedioic acid, ammonium dihydrogen phosphate, citric acid, paranitrobenzoic acid, polyethylene glycol, stir;
3) mixture of gained is heated to 110 ℃, treat that each raw material fully dissolves after, kept said temperature 30 minutes;
4) in said mixture, add the isosebacic acid ammonium, be incubated 15 minutes, stop heating then, in air, treat its natural cooling, obtain the wide temperature high voltage aluminium electrolytic capacitor Working electrolyte.
Embodiment 2:
Each raw material proportioning sees Table 2.
The component of table 2 embodiment 2 each raw material
| Title | Ethylene glycol | γ-butyrolactone | Ammonium sebacate | The isosebacic acid ammonium | Decanedioic acid | Citric acid | Paranitrobenzoic acid | Polyethylene glycol | Ammonium dihydrogen phosphate | Water |
| Quality compares % for hundred parts | 72 | 6 | 2 | 8 | 1 | 0.3 | 0.8 | 8 | 0.9 | 1 |
1) ethylene glycol, gamma-butyrolacton, water are mixed, be heated to 90 ℃;
2) in above-mentioned mixed solvent, add ammonium sebacate, decanedioic acid, ammonium dihydrogen phosphate, citric acid, paranitrobenzoic acid, polyethylene glycol, stir;
3) mixture of gained is heated to 120 ℃, treat that each raw material fully dissolves after, kept said temperature 30 minutes;
4) in said mixture, add the isosebacic acid ammonium, be incubated 10 minutes, stop heating then, in air, treat its natural cooling, obtain the wide temperature high voltage aluminium electrolytic capacitor Working electrolyte.
Embodiment 3
Each raw material proportioning sees Table 3.
The component of table 3 embodiment 3 each raw material
| Title | Ethylene glycol | γ-butyrolactone | Ammonium sebacate | The isosebacic acid ammonium | Citric acid | Paranitrobenzoic acid | Polyethylene glycol | Ammonium dihydrogen phosphate |
| Mass percent % | 68 | 8 | 4 | 8 | 0.5 | 0.5 | 10 | 1 |
1) ethylene glycol, gamma-butyrolacton are mixed, be heated to 90 ℃;
2) in above-mentioned mixed solvent, add ammonium sebacate, ammonium dihydrogen phosphate, citric acid, paranitrobenzoic acid, polyethylene glycol, stir;
3) mixture of gained is heated to 140 ℃, treat that each raw material fully dissolves after, kept said temperature 10 minutes;
4) in said mixture, add the isosebacic acid ammonium, be incubated 30 minutes, stop heating then, in air, treat its natural cooling, obtain the wide temperature high voltage aluminium electrolytic capacitor Working electrolyte.
Embodiment 4:
Each raw material sees Table 4.
Table 4 embodiment 4 each raw material components
| Title | Ethylene glycol | Gamma-butyrolacton | Ammonium sebacate | The isosebacic acid ammonium | Decanedioic acid | Citric acid | Paranitrobenzoic acid | Polyethylene glycol | Ammonium dihydrogen phosphate |
| Quality compares % for hundred parts | 72 | 6 | 2 | 9 | 1 | 0.3 | 0.8 | 8 | 0.9 |
1) ethylene glycol, gamma-butyrolacton are mixed, be heated to 90 ℃;
2) in above-mentioned mixed solvent, add ammonium sebacate, decanedioic acid, ammonium dihydrogen phosphate, citric acid, paranitrobenzoic acid, polyethylene glycol, stir;
3) treat that each raw material fully dissolves after, kept 90 ℃ of temperature 30 minutes;
4) in said mixture, add the isosebacic acid ammonium, kept 90 ℃ of temperature 20 minutes, stop heating then, in air, treat its natural cooling, obtain the wide temperature high voltage aluminium electrolytic capacitor Working electrolyte.
Embodiment 5:
Each raw material sees Table 5.
Table 5 embodiment 5 each raw material components
| Title | Ethylene glycol | Gamma-butyrolacton | Ammonium sebacate | The isosebacic acid ammonium | Citric acid | Paranitrobenzoic acid | Polyethylene glycol | Ammonium dihydrogen phosphate | Water |
| Quality compares % for hundred parts | 80 | 5 | 2 | 5 | 0.3 | 0.7 | 5 | 0.8 | 1.2 |
1) ethylene glycol, gamma-butyrolacton, water are mixed, be heated to 75 ℃;
2) in above-mentioned mixed solvent, add ammonium sebacate, ammonium dihydrogen phosphate, citric acid, paranitrobenzoic acid, polyethylene glycol, stir;
3) mixture of gained is heated to 150 ℃, treat that each raw material fully dissolves after, kept said temperature 5 minutes;
4) in said mixture, add the isosebacic acid ammonium, be incubated 10 minutes, stop heating then, in air, treat its natural cooling, obtain the wide temperature high voltage aluminium electrolytic capacitor Working electrolyte.
Embodiment 6:
Each raw material proportioning sees Table 6.
Table 6 embodiment 6 each raw material components
| Title | Ethylene glycol | γ-butyrolactone | Ammonium sebacate | The isosebacic acid ammonium | Citric acid | Paranitrobenzoic acid | Polyethylene glycol | Ammonium dihydrogen phosphate | Water |
| Mass percent % | 60 | 19 | 5 | 5 | 0.3 | 0.5 | 5 | 0.2 | 5 |
1) ethylene glycol, gamma-butyrolacton, water are mixed, be heated to 70 ℃;
2) in above-mentioned mixed solvent, add ammonium sebacate, ammonium dihydrogen phosphate, citric acid, paranitrobenzoic acid, polyethylene glycol, stir;
3) mixture of gained is heated to 150 ℃, treat that each raw material fully dissolves after, kept said temperature 30 minutes;
4) in said mixture, add the isosebacic acid ammonium, be incubated 20 minutes, stop heating then, in air, treat its natural cooling, obtain the wide temperature high voltage aluminium electrolytic capacitor Working electrolyte.
The electrolyte property of embodiment 1,2,3,4,5,6 gained sees Table 8.
Table 8 embodiment HTHP Working electrolyte performance
| Project | 25 ℃ of conductivity | 25 ℃ of flash over voltages | 25 ℃ of pH values |
| Embodiment 1 | 1.6ms.cm - | ≥480V | 6.2 |
| Embodiment 2 | 1.5ms.cm - | ≥480V | 6.0 |
| Embodiment 3 | 1.47ms.cm - | ≥480V | 6.3 |
| Embodiment 4 | 1.46ms.cm - | ≥480V | 6.2 |
| Embodiment 5 | 1.29ms.cm - | ≥480V | 6.0 |
| Embodiment 6 | 1.1ms.cm - | ≥480V | 6.0 |
Test example 1:
The electrolyte of embodiment 1 preparation is made the capacitor of CD293 type 400V22 μ F, and check its performance, the electric parameter of product sees Table 9.
Table 9 embodiment 1 aluminium electrolytic capacitor electric property parameter
| Project | Before the high-temperature storage | After the high-temperature storage | ||||||
| Capacity (μ F) | Loss | Leakage current (μ A) | Capacity (μ F) | Loss | Leakage current (μ A) | Visual examination | ||
| Mean value | The actual measurement national standard | 21.24 | 0.032 | 6 | 20.72 | 0.038 | 160 | Well |
| ≤±20％ | ≤0.24 | ≤264 | ≤±20％ | ≤0.48 | ≤528 | Well | ||
| The changing value actual measurement | -3.5％ | 0.032 | 6 | -6％ | 0.038 | 160 | Well | |
Test example 2:
The electrolyte of embodiment 2 preparations is made the capacitor of CD110 type 400V100 μ F, and check its performance, the electric parameter of product sees Table 10.
Table 10 embodiment 2 aluminium electrolytic capacitor electric property parameters
| Project | Before the high-temperature storage | After the high-temperature storage | ||||||
| Capacity (μ F) | Loss | Leakage current (μ A) | Capacity (μ F) | Loss | Leakage current (μ A) | Visual examination | ||
| Mean value | The actual measurement national standard | 95.57 | 0.054 | 26 | 93.33 | 0.049 | 665 | Well |
| ≤±20％ | ≤0.24 | ≤ 1200 | ≤±20％ | ≤0.48 | ≤2400 | Well | ||
| The changing value actual measurement | -4.4％ | 0.054 | 26 | -6.67％ | 0.049 | 665 | Well | |
Test example 3:
The electrolyte of embodiment 3 preparations is made the capacitor of CD110 type 400V22 μ F, and check its performance, the electric parameter of product sees Table 11.
Table 11 embodiment 3 aluminium electrolytic capacitor electric property parameters
| Project | Before the high-temperature storage | After the high-temperature storage | ||||||
| Capacity (μ F) | Loss | Leakage current (μ A) | Capacity (μ F) | Loss | Leakage current (μ A) | Visual examination | ||
| Mean value | The actual measurement national standard | 21.4 | 0.03 | 10 | 20.9 | 0.04 | 180 | Well |
| ≤±20％ | ≤0.24 | ≤264 | ≤±20％ | ≤0.48 | ≤528 | Well | ||
| The changing value actual measurement | -2.7％ | 0.03 | 10 | -5％ | 0.04 | 180 | Well | |
Test example 4:
The electrolyte of embodiment 4 preparations is made the capacitor of CD110 type 400V3.3 μ F, and check its performance, the electric parameter of product sees Table 12.
Table 12 embodiment 4 aluminium electrolytic capacitor electric property parameters
| Project | Before the high-temperature storage | After the high-temperature storage | ||||||
| Capacity (μ F) | Loss | Leakage current (μ A) | Capacity (μ F) | Loss | Leakage current (μ A) | Visual examination | ||
| Mean value | The actual measurement national standard | 3.2 | 0.05 | 7 | 3.1 | 0.07 | 52 | Well |
| ≤±20％ | ≤0.24 | ≤40 | ≤±20％ | ≤0.48 | ≤80 | Well | ||
| The changing value actual measurement | -3％ | 0.05 | 7 | -6.1％ | 0.07 | 52 | Well | |
Test example 5:
The electrolyte of embodiment 5 preparations is made the capacitor of CD110 type 400V3.3 μ F, and check its performance, the electric parameter of product sees Table 13.
Table 13 embodiment 5 aluminium electrolytic capacitor electric property parameters
| Project | Before the high-temperature storage | After the high-temperature storage | ||||||
| Capacity (μ F) | Loss | Leakage current (μ A) | Capacity (μ F) | Loss | Leakage current (μ A) | Visual examination | ||
| Mean value | The actual measurement national standard | 3.2 | 0.04 | 6 | 3.1 | 0.06 | 48 | Well |
| ≤±20％ | ≤0.24 | ≤40 | ≤±20％ | ≤0.48 | ≤80 | Well | ||
| The changing value actual measurement | -3％ | 0.04 | 6 | -6.1％ | 0.06 | 48 | Well | |
Test example 6:
The electrolyte of embodiment 6 preparations is made the capacitor of CD110 type 400V22 μ F, and check its performance, the electric parameter of product sees Table 14.
Table 14 embodiment 6 aluminium electrolytic capacitor electric property parameters
| Project | Before the high-temperature storage | After the high-temperature storage | ||||||
| Capacity (μ F) | Loss | Leakage current (μ A) | Capacity (μ F) | Loss | Leakage current (μ A) | Visual examination | ||
| Mean value | The actual measurement national standard | 21 | 0.03 | 11 | 20 | 0.04 | 220 | Well |
| ≤±20％ | ≤0.24 | ≤264 | ≤±20％ | ≤0.48 | ≤528 | Well | ||
| The changing value actual measurement | -4.5％ | 0.03 | 11 | -9％ | 0.04 | 220 | Well | |
Claims (3)
1. wide temperature high voltage aluminium electrolytic capacitor Working electrolyte comprises by following raw material by percentage to the quality:
Ethylene glycol 60～80%; Gamma-butyrolacton 5～20%; Water 0～5%;
Ammonium sebacate 2～5%; Isosebacic acid ammonium 5～10%; Decanedioic acid 0～5%;
Ammonium dihydrogen phosphate 0.1～2%; Citric acid 0.1～1%;
Paranitrobenzoic acid 0.1～2%; Polyethylene glycol 5～20%.
2. the described wide temperature high voltage aluminium electrolytic capacitor of claim 1 is with the preparation method of Working electrolyte, and its step is as follows:
1) ethylene glycol, gamma-butyrolacton, water are mixed, be heated to 60～90 ℃;
2) in above-mentioned mixed solvent, add ammonium sebacate, decanedioic acid, ammonium dihydrogen phosphate, citric acid, paranitrobenzoic acid, polyethylene glycol, stir;
3) mixture of gained is heated to 110～150 ℃, treat that each raw material fully dissolves after, kept said temperature 5～30 minutes;
4) in said mixture, add the isosebacic acid ammonium, kept the described temperature of step 3) 5～30 minutes, stop heating then, in air, treat its natural cooling, obtain the wide temperature high voltage aluminium electrolytic capacitor Working electrolyte.
3. wide temperature high voltage aluminium electrolytic capacitor according to claim 2 is characterized in that with the preparation method of Working electrolyte: in the step 3), the mixture of gained is heated to 110～140 ℃.
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| CN114420454B (en) * | 2021-12-25 | 2024-03-29 | 深圳奥凯普电容器有限公司 | Electrolyte for high-temperature-resistant capacitor and preparation method thereof |
| CN114284071A (en) * | 2021-12-29 | 2022-04-05 | 深圳奥凯普电容器有限公司 | Capacitor electrolyte with prolonged service life and preparation method thereof |
| CN114284071B (en) * | 2021-12-29 | 2024-09-17 | 深圳奥凯普电容器有限公司 | Electrolyte for capacitor with prolonged service life and preparation method thereof |
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