CN113327770B - Working electrolyte of low-voltage electrolytic capacitor for high-temperature working and preparation method thereof - Google Patents
Working electrolyte of low-voltage electrolytic capacitor for high-temperature working and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a working electrolyte of a low-voltage electrolytic capacitor for high-temperature work and a preparation method thereof, and the working electrolyte comprises the following steps: (1) preparing raw materials: 5-15% of ethylene glycol, 30-50% of gamma-butyrolactone, 10-20% of sulfolane, 10-15% of benzene ring-containing organic carboxylic acid compound, 0.5-3% of acidic compound formed by atoms with unfilled valence shell, 5-8% of imidazole compound, 0.5-5% of phosphorus-containing heteropoly acid and 1-5% of silicon source; (2) heating ethylene glycol to a temperature of not higher than 70 ℃, adding an acidic compound formed by atoms with unfilled valence shell layers, stirring and dissolving, adding a silicon source, heating for reaction, cooling to a temperature of not higher than 70 ℃, adding the rest raw materials, and stirring while keeping the temperature until the mixture is clear to obtain the working electrolyte. The working electrolyte provided by the invention can enable a low-voltage electrolytic capacitor to have better durability at a high working temperature of 135-150 ℃.
Description
Technical Field
The invention relates to the technical field of electrolytic capacitors, in particular to a working electrolyte of a low-voltage electrolytic capacitor for high-temperature work and a preparation method thereof.
Background
The electrolytic capacitor is one of basic elements of electronic products, and with the development of automobile electronic control units and 5G communication base stations, the demand of the electrolytic capacitor with high temperature resistance, particularly the electrolytic capacitor with the temperature of 135-150 ℃ is increasing.
The electrolyte is the cathode of the aluminum electrolytic capacitor, can repair the defects and flaws of the anodic oxide film, and plays a decisive role in the service temperature range, the service life, the reliability and other electrical properties of the aluminum electrolytic capacitor. The quality and characteristics of the working electrolyte will directly affect the performance and application of the capacitor. The working electrolyte of the electrolytic capacitor is classified into a low-voltage working electrolyte and a medium-high voltage working electrolyte according to the working voltage used.
The working electrolyte used by the low-voltage aluminum electrolytic capacitor in the industry at present is generally a gamma-butyrolactone organic amine system, and the formula is as follows: 69g of gamma-butyrolactone, 26g of ammonium tetramethylsuccinate and 5g of pure water, the working electrolyte has a conductivity of 85 omega cm, and is applied to low-voltage products at 125 ℃ for 1000hr (Linchuqing, Hongsubao, aluminum electrolytic capacitor engineering technology [ M ]. 2002, page 126). The electrolyte with poor durability can not meet the requirement of the service life of the aluminum electrolytic capacitor at the working temperature of 135-150 ℃ because the steam pressure is higher and the capacitor is easy to swell and lose efficacy.
Disclosure of Invention
In order to solve the problem that the existing working electrolyte can not meet the durability of a low-voltage electrolytic capacitor at the working temperature of 135-150 ℃, the working electrolyte of the low-voltage electrolytic capacitor for high-temperature working and the preparation method thereof are provided. The working electrolyte provided by the invention can enable the low-voltage electrolytic capacitor to have better durability at a high working temperature of 135-150 ℃, and not only has better high-temperature resistance, but also has longer service life.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the preparation method of the working electrolyte of the low-voltage electrolytic capacitor for high-temperature work comprises the following steps:
(1) the working electrolyte comprises the following raw materials in percentage by weight: 5-15% of ethylene glycol, 30-50% of gamma-butyrolactone, 10-20% of sulfolane, 10-15% of benzene ring-containing organic carboxylic acid compound, 0.5-3% of acidic compound formed by atoms with unfilled valence shell, 5-8% of imidazole compound, 0.5-5% of phosphorus-containing heteropoly acid and 1-5% of silicon source;
(2) heating the ethylene glycol to a temperature not higher than 70 ℃, adding the acidic compound formed by the atoms with unfilled valence shell layers, stirring for dissolving, adding the silicon source, carrying out a heating reaction, cooling to a temperature not higher than 70 ℃, adding the rest raw materials, and stirring to clarify under heat preservation to obtain the low-voltage electrolytic capacitor working electrolyte for high-temperature work.
Further, the organic carboxylic acid compound containing a benzene ring is one or more of terephthalic acid, isophthalic acid, phthalic acid and trimesic acid. The organic carboxylic acid compound containing benzene ring is used as a main solute, and has extremely high stability at high temperature due to the large pi bond with the benzene ring structure, so that molecular cracking is not easy to occur. Preferably, the organic carboxylic acid compound containing a benzene ring is phthalic acid, which can rapidly react due to its high ionization degree.
Further, the imidazole compound is 1,2,3, 4-tetramethylimidazole.
Further, the acidic compound formed by the atoms which contain the unfilled valence shell layer is boric acid; the heteropoly acid containing phosphorus is one of heteropoly acid of phosphorus tungsten, heteropoly acid of phosphorus molybdenum and heteropoly acid of phosphorus tungsten molybdenum.
Further, the silicon source is tetraethoxysilane.
Further, the specific temperature of not higher than 70 ℃ in the step (2) is 60-65 ℃; the temperature of the heating reaction is 150-160 ℃, and the reaction time is 10-30 min.
Preferably, the working electrolyte comprises the following raw materials in percentage by weight: 12% of ethylene glycol, 42% of gamma-butyrolactone, 16% of sulfolane, 13% of organic carboxylic acid compound containing benzene ring, 2% of acidic compound formed by atoms with unfilled valence shell, 7% of imidazole compound, 5% of heteropoly acid containing phosphorus and 3% of silicon source.
On the other hand, the invention provides the working electrolyte of the low-voltage electrolytic capacitor for high-temperature work, which is obtained by the preparation method, can work at the high temperature of 135-150 ℃, is a high-temperature working electrolyte and is suitable for the low-voltage electrolytic capacitor.
In the above raw materials for preparing the working electrolyte, the solvent is ethylene glycol, γ -butyrolactone and sulfolane, the solute is an acidic compound formed by an organic carboxylic acid compound containing a benzene ring and atoms containing valence shell layer unfilled atoms, and the additive is a heteropoly acid containing phosphorus and a silicon source. During the preparation process, an acidic compound formed by atoms with unfilled valence shell, such as boric acid, has the characteristic of Lewis acid and can catalyze the esterification reaction of the acidic compound and ethylene glycol at a lower temperature, and the esterification reaction formula is B (OH)3 + 2HO-CH2-CH2-OH→H[B(O2C2H4)2] + 3H2O, producing a borate and water; subsequent addition of a silicon source such as tetraethyl orthosilicate in the water from the former reaction is hydrolyzed to ethanol and silicic acid (H)2SiO3) When the temperature of the temperature rise reaction reaches more than 150 ℃, on one hand, the boric acid ester generated by the boric acid ester continuously reacts with redundant ethylene glycol to form a ternary network type ester which is similar to a complex structure and has larger steric hindrance and can generate the electric field shielding effectInhibiting electron discharge, forming a ternary network type esterified substance and simultaneously enhancing acidity, on the other hand forming silica soluble nano particles by silicic acid under an acidic condition, and being beneficial to improving the dispersibility of the silica soluble nano particles after the acidity is enhanced, and finally adding the rest materials in the formula to obtain the working electrolyte.
The working electrolyte of the invention is used in a low-voltage electrolytic capacitor, and the working electrolyte finally formed in the preparation process contains highly dispersed nano silicon dioxide, hydroxyl contained on the surface of the anode foil can generate better adsorbability on the surface of a corrosion hole of the anode foil of the electrolytic capacitor, and modify and cover the defect point of the insulating oxide film on the surface of the anode foil, the formed ternary network type ester can generate electric field shielding effect due to larger steric hindrance so as to control electronic discharge, and the two elements can simultaneously improve and stabilize the sparking voltage of the electrolyte, the electrolytic capacitor has better high-voltage resistance after the sparking voltage of the working electrolyte is improved and stabilized, the continuous operation of 2000-3000h at 135-150 ℃ still has better functional parameters, and in addition, the working voltage of the low-voltage electrolytic capacitor can reach 100V level.
In addition, the solute in the obtained working electrolyte can stably exist at high temperature due to the large pi bond with a benzene ring structure, molecular cracking is not easy to occur, and the working electrolyte has high conductivity due to high ionization degree.
On the last hand, the added heteropoly acid containing phosphorus further carries out oxidation repair on the defect point of the insulating oxide film on the surface of the anode foil so as to further improve the high voltage resistance of the electrolytic capacitor; and when the phosphorus-containing heteropoly acid adsorbs the surface of the anode foil, the corrosion action of factors such as hydration for blocking water and the like on the surface of the anode foil can be inhibited, and further the leakage current of the electrolytic capacitor is reduced.
The beneficial technical effects are as follows:
the working electrolyte for the low-voltage electrolytic capacitor at the working temperature of 135-150 ℃ prepared by the method has good high-voltage resistance and high-voltage stability, so that the low-voltage electrolytic capacitor still can keep good performance at the working temperature of 135-150 ℃, and has long service life and good durability; and the working temperature range of the capacitor can be expanded to-55-150 ℃.
Drawings
FIG. 1 is a graph of the sparking voltage of a working electrolyte as a function of time; wherein (A) represents the working electrolyte prepared in comparative example 1, and (B) represents the working electrolyte prepared in example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. 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.
Unless specifically stated otherwise, the numerical values set forth in these examples do not limit the scope of the invention. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
Example 1
The preparation method of the working electrolyte of the low-voltage electrolytic capacitor for high-temperature work comprises the following steps:
(1) the working electrolyte comprises the following raw materials in percentage by weight: 12% of ethylene glycol, 42% of gamma-butyrolactone, 16% of sulfolane, 13% of phthalic acid, 2% of boric acid, 7% of 1,2,3, 4-tetramethylimidazole, 5% of phosphotungstic heteropoly acid and 3% of ethyl orthosilicate;
(2) heating ethylene glycol to 65 ℃, adding boric acid, stirring for dissolving, then adding tetraethoxysilane, stirring while heating to 160 ℃, reacting for 20min, then cooling to 60-65 ℃, adding the rest raw materials, and stirring for clarifying under heat preservation to obtain the low-voltage electrolytic capacitor working electrolyte for high-temperature work.
The electrolyte of the embodiment has the conductivity (30 ℃) of 5000-7000 mu S/cm and the sparking voltage (85 ℃) of 140-160V. The time-dependent change curve of the working electrolyte sparking voltage of the embodiment is shown in fig. 1 (B), and as can be seen from fig. 1 (B), the time-dependent change of the working electrolyte sparking voltage of the embodiment is relatively stable, and the voltage endurance is relatively good.
8 aluminum electrolytic capacitors (63V 1000, 16X 31.5 specification) were prepared under the same conditions using the working electrolyte prepared in this example, and the aluminum electrolytic capacitors were subjected to a durability test at 150 ℃ and 63VDC for 2000 hours, and the results are shown in Table 1.
Table 1 example 1 working electrolyte used in durability test of aluminum electrolytic capacitor (63V 1000, 16 × 31.5 gauge)
As can be seen from Table 1, the aluminum electrolytic capacitor (63V 1000, 16X 31.5 standard) after 2000h had no bottom bulge and the parameters were normal. It can be seen that the working electrolyte of the embodiment still has good performance and good durability after working at 150 ℃ for 2000 hours, and thus the working electrolyte of the embodiment has good pressure stability at high temperature.
10 aluminum electrolytic capacitors (100V 160, 12.5X 20 specification) were prepared under the same conditions using the working electrolyte prepared in this example, and durability test of the aluminum electrolytic capacitors was carried out at 135 ℃ and 100VDC for 3000 hours, and the results are shown in Table 2.
Table 2 example 2 working electrolyte used in durability test of aluminum electrolytic capacitor (100V 160, 12.5 × 20 gauge)
As can be seen from Table 2, after 3000 hours, no bulge occurred in the appearance of the aluminum electrolytic capacitor (100V 160, 12.5X 20 standard), and the parameters were normal. Therefore, the working electrolyte of the embodiment still has good performance and good durability after being operated at 130 ℃ for 3000 hours, and the working electrolyte of the embodiment has good pressure resistance stability at high temperature.
The working electrolyte of the embodiment is adopted to prepare 2 aluminum electrolytic capacitors with two specifications for normal temperature and low temperature-55 ℃ parameter test, and the data is shown in table 3.
TABLE 3 data change rate of two aluminum electrolytic capacitors with different specifications made from the working electrolyte of this example at normal and low temperatures
As can be seen from tables 1-3, the aluminum electrolytic capacitor made by using the working electrolyte of the embodiment can not only withstand long-term operation at higher temperature (135-. As can be seen from table 3, the working electrolyte of the present embodiment is an electrolyte that can be used at high temperature, and can be used to fabricate a 100V-class electrolytic capacitor.
Example 2
The preparation method of the working electrolyte of the low-voltage electrolytic capacitor for high-temperature work comprises the following steps:
(1) the working electrolyte comprises the following raw materials in percentage by weight: 15% of ethylene glycol, 38% of gamma-butyrolactone, 20% of sulfolane, 10% of phthalic acid, 3% of boric acid, 5% of 1,2,3, 4-tetramethylimidazole, 4% of phosphomolybdic acid and 5% of ethyl orthosilicate;
(2) heating ethylene glycol to 60 ℃, adding boric acid, stirring for dissolving, then adding tetraethoxysilane, stirring while heating to 150 ℃, reacting for 30min, then cooling to 60-65 ℃, adding the rest raw materials, and stirring for clarifying under heat preservation to obtain the low-voltage electrolytic capacitor working electrolyte for high-temperature work.
The electrolyte has the conductivity (30 ℃) of 5000-68000 mu S/cm, the sparking voltage (85 ℃) of 150-160V and small fluctuation of the sparking voltage, and is stable.
Example 3
The preparation method of the working electrolyte of the low-voltage electrolytic capacitor for high-temperature work comprises the following steps:
(1) the working electrolyte comprises the following raw materials in percentage by weight: 10% of ethylene glycol, 50% of gamma-butyrolactone, 10% of sulfolane, 15% of phthalic acid, 1% of boric acid, 8% of 1,2,3, 4-tetramethylimidazole, 3% of phosphotungstomolybdenum heteropoly acid and 3% of tetraethoxysilane;
(2) heating ethylene glycol to 65 ℃, adding boric acid, stirring for dissolving, then adding tetraethoxysilane, stirring while heating to 155 ℃, reacting for 20min, then cooling to 60-65 ℃, adding the rest raw materials, and stirring for clarifying under heat preservation to obtain the low-voltage electrolytic capacitor working electrolyte for high-temperature work.
The electrolyte has the conductivity of 6000-8000 mu S/cm at 30 ℃, the sparking voltage of 140-150V at 85 ℃, and the smaller fluctuation of the sparking voltage is stable.
Comparative example 1
The working electrolyte of this comparative example was prepared in the same manner as in example 1, except that the temperature of the temperature-raising reaction in step (2) was 135 ℃.
The electrolyte of the comparative example has the conductivity (30 ℃) of 4500-6500 mu S/cm, the sparking voltage (85 ℃) of 165-175V, large fluctuation of the sparking voltage and unstable performance, and the curve of the sparking voltage changing along with time is shown in (A) of figure 1. As can be seen from fig. 1 (a), the working electrolyte of the present comparative example can obtain a high initial sparking voltage, but gradually becomes unstable in the boosting process with time, and has a greater volatility than that of fig. 1 (B), and the working electrolyte of the present comparative example has a lower pressure resistance than that of the working electrolyte of example 1. The reason is that the boric acid ester and the ethylene glycol generated by the boric acid ester can not react at 135 ℃ to obtain the ternary network ester, so that the electron discharge can not be inhibited, and the phenomenon of unstable sparking voltage in the boosting process can be generated. That is, the reaction in the invention can generate ternary network type ester at higher temperature, namely more than 150 ℃, and the generation of the product can improve the pressure resistance stability of the working electrolyte. Even if the working electrolyte system is added with phosphotungstic heteropoly acid, silica sol and the like to improve the sparking voltage, if the ternary network type ester compound is not present to inhibit the electron discharge, the phenomenon of unstable voltage resistance, wherein the sparking voltage is changed with time and fluctuates greatly, can occur. In addition, the working electrolyte of the comparative example 1 is unstable in sparking voltage, and cannot be used for manufacturing 100V-class electrolytic capacitors.
As can be seen from the above, the principle of stabilizing and increasing the sparking voltage is: the invention generates the ternary network type ester to generate the electric field shielding effect to inhibit the electronic discharge and control the sparking voltage to generate smaller fluctuation in the boosting process; meanwhile, the silicon dioxide soluble nano particles generated in situ are distributed with more surface charges in a working system, so that the silicon dioxide soluble nano particles can be adsorbed on an anode foil (corrosion holes and surfaces) to a greater extent to cover defect points and the phosphotungstic heteropoly acid can further repair the defects, and the comprehensive effect can improve the sparking voltage of the low-voltage electrolytic capacitor and obtain more stable pressure resistance, so that the low-voltage electrolytic capacitor adopting the working electrolyte disclosed by the invention has better durability when working at a high temperature of 135-150 ℃.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. The preparation method of the working electrolyte of the low-voltage electrolytic capacitor for high-temperature work is characterized by comprising the following steps of:
(1) the working electrolyte comprises the following raw materials in percentage by weight: 5-15% of ethylene glycol, 30-50% of gamma-butyrolactone, 10-20% of sulfolane, 10-15% of benzene ring-containing organic carboxylic acid compound, 0.5-3% of acidic compound formed by atoms with unfilled valence shell, 5-8% of imidazole compound, 0.5-5% of phosphorus-containing heteropoly acid and 1-5% of silicon source;
(2) heating the ethylene glycol to a temperature not higher than 70 ℃, adding the acidic compound formed by the atoms with unfilled valence shell layers, stirring for dissolving, adding the silicon source, performing a heating reaction at a temperature of 150-160 ℃, cooling to a temperature not higher than 70 ℃, adding the rest raw materials, and stirring to clarify under heat preservation to obtain the low-voltage electrolytic capacitor working electrolyte for high-temperature work.
2. The method for preparing the working electrolyte of the low-voltage electrolytic capacitor for high-temperature working according to claim 1, wherein the organic carboxylic acid compound containing the benzene ring is one or more of terephthalic acid, isophthalic acid, phthalic acid and trimesic acid.
3. The method for preparing the working electrolyte of the low-voltage electrolytic capacitor for high-temperature work according to claim 1, wherein the imidazole compound is 1,2,3, 4-tetramethylimidazole.
4. The method for preparing a working electrolyte of a low-voltage electrolytic capacitor for high-temperature operation according to claim 1, wherein the acidic compound formed by the atoms with unfilled valence shell is boric acid; the heteropoly acid containing phosphorus is one of heteropoly acid of phosphorus tungsten, heteropoly acid of phosphorus molybdenum and heteropoly acid of phosphorus tungsten molybdenum.
5. The method for preparing a working electrolyte for a low-voltage electrolytic capacitor working at high temperature according to claim 1, wherein the silicon source is tetraethoxysilane.
6. The preparation method of the working electrolyte of the low-voltage electrolytic capacitor for high-temperature working according to claim 1, wherein the specific temperature of not higher than 70 ℃ in the step (2) is 60-65 ℃; the reaction time of the temperature rise reaction is 10-30 min.
7. The method for preparing the working electrolyte of the low-voltage electrolytic capacitor for high-temperature operation according to claim 1, wherein the working electrolyte comprises the following raw materials in percentage by weight: 12% of ethylene glycol, 42% of gamma-butyrolactone, 16% of sulfolane, 13% of organic carboxylic acid compound containing benzene ring, 2% of acidic compound formed by atoms with unfilled valence shell, 7% of imidazole compound, 5% of heteropoly acid containing phosphorus and 3% of silicon source.
8. A working electrolyte for a low-pressure electrolytic vessel for high-temperature operation, which is prepared by the preparation method according to any one of claims 1 to 7.
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