CN115148500B - Preparation method of aluminum capacitor electrolyte - Google Patents

Preparation method of aluminum capacitor electrolyte Download PDF

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CN115148500B
CN115148500B CN202110340637.5A CN202110340637A CN115148500B CN 115148500 B CN115148500 B CN 115148500B CN 202110340637 A CN202110340637 A CN 202110340637A CN 115148500 B CN115148500 B CN 115148500B
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electrolyte
chromaticity
aluminum capacitor
solute
stirring
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CN115148500A (en
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於浩然
何家齐
郭丽
程琦玮
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Nantong Capchem Electronic Materials Co ltd
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Nantong Capchem Electronic Materials Co ltd
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Abstract

The invention belongs to the technical field of aluminum electrolytic capacitors, and particularly relates to a preparation method of an aluminum capacitance electrolyte, which comprises the following steps: (1) Heating and stirring the solvent, the solute and the chromaticity improver uniformly; (2) Continuously heating and stirring, preserving heat, and cooling to obtain electrolyte; in the step (1), the heating and stirring temperature is 30-100 ℃. According to the preparation method of the aluminum capacitor electrolyte, the color deepening problem of the electrolyte is effectively inhibited by controlling the addition sequence and the addition temperature of the chromaticity improver, the color of an electrolyte product is colorless to pale yellow, the decoloring effect is obvious, the method is convenient and simple to operate, the input amount is small, and the effect is stable.

Description

Preparation method of aluminum capacitor electrolyte
Technical Field
The invention belongs to the technical field of aluminum electrolytic capacitors, and particularly relates to a preparation method of an aluminum capacitance electrolyte.
Background
In an aluminum electrolytic capacitor, the electrolyte plays an important role in providing oxygen ions and repairing an anodic oxide film, so that the improvement of the quality of the electrolyte is one of the keys for improving the performance of the capacitor.
In the process of preparing the electrolyte, organic acids, sugar alcohols and other solutes in the electrolyte and the prepared electrolyte are often brown to dark brown after long-time high-temperature cooking (chromaticity is more than 500Hazen, platinum cobalt standard colorimetric method), and the appearance and the electrolyte performance are directly influenced. The main flow of decoloring technology comprises active carbon adsorption, sol-gel flocculation, oxidant oxidation decoloring and the like, and the subsequent decoloring treatment scheme has complex operation, larger loss and insignificant chromaticity improvement, so that energy and resource waste is caused, and the subsequent performance degradation of electrolyte preparation and the harm to the environment are caused.
At present, an effective method for solving the problems of solute and electrolyte color change in the process of preparing the aluminum capacitance electrolyte is lacking. Therefore, it is necessary to develop a method which is simple to operate, low in cost and capable of remarkably improving the chromaticity of the electrolyte.
Disclosure of Invention
Aiming at the technical problems, the invention aims to provide a preparation method of the aluminum capacitor electrolyte, which has simple process and low cost and can obviously improve the chromaticity of the electrolyte.
The preparation method of the aluminum capacitor electrolyte comprises the following steps:
(1) Heating and stirring the solvent, the solute and the chromaticity improver uniformly;
(2) Continuously heating and stirring, preserving heat, and naturally cooling to obtain electrolyte;
In the step (1), the heating and stirring temperature is 30-100 ℃.
In the preparation method of the electrolyte, the addition sequence of the chromaticity modifier is required to be added before heat preservation, more specifically before the reaction (comprising esterification reaction, oxidation reaction and dehydration reaction) of all materials, and the addition proper temperature of the chromaticity modifier is 30-100 ℃. By controlling the addition sequence and the addition temperature, the color deepening of the solute and the electrolyte can be effectively inhibited.
Further, the mass ratio of the solvent to the solute is (0.5-1): 1.
Further, the solutes include organic acids and sugar alcohols; the organic acid comprises one or more of suberic acid, azelaic acid and dodecanedioic acid; the sugar alcohol comprises one or more of mannitol, sorbitol and xylitol. Specifically, the mixing mass ratio of the organic acid and the sugar alcohol in the solute composition is not limited.
Further, the solvent is one or two of ethylene glycol and gamma-butyrolactone.
Further, the chromaticity improver comprises one or more of hypophosphorous acid, ammonium hypophosphite and phosphite.
Further, the addition mass of the chromaticity improver accounts for 0.01-2% of the solute, more preferably 0.1-0.5%.
Further, the stirring temperature and the heat preservation temperature in the step (2) are 120-180 ℃, the heat preservation is carried out for 1-8 hours, more preferably 140-160 ℃, and the heat preservation time is 4-6 hours.
The preparation method of the aluminum capacitor electrolyte has the following beneficial effects:
(1) According to the preparation method of the aluminum capacitor electrolyte, the chroma modifier is added, the addition sequence and the addition temperature of the chroma modifier are limited, the deepening of the color of a solute and the color of the electrolyte can be effectively inhibited, the problem that the color of the electrolyte is deepened and blackened in the high-temperature cooking process is solved, the color of an electrolyte product is colorless to pale yellow, the decoloring effect is obvious, and meanwhile, the preparation method is simple in process and low in cost; compared with the subsequent decoloring treatment, the method provided by the invention has no harm to the subsequent synthetic electrolyte and environment.
(2) In the preparation method of the aluminum capacitance electrolyte, the addition amount of the chromaticity improver is small, but the effect is stable, and the aluminum capacitance electrolyte has no side effect on the subsequent synthesis of the electrolyte.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, but is apparent to those skilled in the art in view of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
Example 1
The material information of the aluminum capacitor electrolyte in this embodiment is as follows:
250g of ethylene glycol, 500g of suberic acid and 2.0g of hypophosphorous acid are respectively weighed into a flask, heated and stirred to 30 ℃, continuously heated to 140 ℃, stirred and kept for 4 hours, and naturally cooled to obtain an electrolyte, the chromaticity of which is measured by a platinum-cobalt colorimetric method, and the appearance color is observed, and the result is shown in table 1.
Example 2
The material information of the aluminum capacitor electrolyte in this embodiment is as follows:
500g of ethylene glycol, 500g of sorbitol and 1.0g of hypophosphorous acid are respectively weighed into a flask, heated and stirred to 50 ℃, continuously heated to 145 ℃, stirred and kept for 4.5 hours, and then naturally cooled to obtain an electrolyte, the chromaticity of which is measured by a platinum-cobalt colorimetric method, and the appearance color is observed, and the result is shown in table 1.
Example 3
The material information of the aluminum capacitor electrolyte in this embodiment is as follows:
300g of ethylene glycol, 200g of dodecanedioic acid, 200g of xylitol and 2.4g of phosphite ester are respectively weighed into a flask, heated and stirred to 70 ℃, continuously heated to 150 ℃, stirred and kept for 5 hours, and the chromaticity of the electrolyte obtained after natural cooling is measured by a platinum-cobalt colorimetric method, and the appearance color is observed, and the result is shown in table 1.
Example 4
The material information of the aluminum capacitor electrolyte in this embodiment is as follows:
550g of ethylene glycol, 200g of dodecanedioic acid, 200g of suberic acid, 100g of mannitol, 50g of xylitol, 1.1g of hypophosphorous acid and 1.1g of ammonium hypophosphite are respectively weighed, the mixture is heated to 90 ℃, the temperature is continuously increased to 155 ℃, the temperature is kept for 5.5 hours, the chromaticity of the electrolyte obtained after natural cooling is measured by a platinum-cobalt colorimetry, and the appearance color is observed, and the result is shown in table 1.
Example 5
The material information of the aluminum capacitor electrolyte in this embodiment is as follows:
600g of ethylene glycol, 100g of dodecanedioic acid, 200g of suberic acid, 100g of azelaic acid, 50g of mannitol, 50g of xylitol, 100g of sorbitol, 1.0g of hypophosphorous acid, 1.0g of ammonium hypophosphite and 1.0g of phosphite are respectively weighed into a flask, heated and stirred to 100 ℃, continuously heated to 160 ℃, stirred and kept for 6 hours, and then the chromaticity of the electrolyte obtained after natural cooling is measured by a platinum-cobalt colorimetric method, and the appearance color is observed, and the result is shown in table 1.
Comparative example 1
The material information of the aluminum capacitor electrolyte of this comparative example is as follows:
250g of ethylene glycol and 500g of suberic acid are weighed respectively, put into a flask, directly heated to 140 ℃, stirred and kept for 4 hours, and then naturally cooled, the obtained electrolyte is subjected to chromaticity measurement by a platinum-cobalt colorimetric method, and the appearance color is observed, and the result is shown in Table 1.
Comparative example 2
The material information of the aluminum capacitor electrolyte of this comparative example is as follows:
300g of ethylene glycol, 200g of dodecanedioic acid and 200g of xylitol are respectively weighed and placed in a flask, the temperature is directly raised to 155 ℃, the temperature is kept for 5.5 hours by stirring, the chromaticity of the electrolyte obtained after natural cooling is measured by a platinum-cobalt colorimetric method, the appearance color is observed, and the result is shown in table 1.
Comparative example 3
The material information of the aluminum capacitor electrolyte of this comparative example is as follows:
300g of ethylene glycol, 200g of dodecanedioic acid and 200g of xylitol are respectively weighed and placed in a flask, the temperature is directly raised to 120 ℃, 2.4g of phosphite ester is added, the temperature is continuously raised to 155 ℃, the temperature is kept for 5.5 hours after stirring, the chromaticity of the electrolyte obtained after natural cooling is measured by a platinum-cobalt colorimetric method, and the appearance color is observed, and the result is shown in table 1.
Comparative example 4
The material information of the aluminum capacitor electrolyte of this comparative example is as follows:
300g of ethylene glycol, 200g of dodecanedioic acid and 200g of xylitol are respectively weighed and placed in a flask, the temperature is directly raised to 155 ℃, the stirring and the heat preservation are carried out for 5.5 hours, 2.4g of phosphite ester is added, the stirring is uniform, the chromaticity of the electrolyte obtained after natural cooling is measured by a platinum-cobalt colorimetric method, the appearance color is observed, and the result is shown in a table 1.
TABLE 1 results of the colorimetric and appearance color tests of the electrolytes in examples 1 to 5 and comparative examples 1 to 4
Group of Chroma/Hazen Appearance color
Example 1 25 Colorless and colorless
Example 2 45 Colorless and colorless
Example 3 105 Pale yellow
Example 4 132 Pale yellow
Example 5 116 Yellow colour
Comparative example 1 >500 Brown color
Comparative example 2 >500 Dark brown
Comparative example 3 >500 Dark brown
Comparative example 4 >500 Dark brown
As can be seen from the test results of comparative examples 1 to 5 and comparative examples 1 to 4 in Table 1, the present invention can effectively suppress the problem of color deepening of the electrolyte by limiting the addition order and addition temperature of the chromaticity improver, and the electrolyte exhibits colorless or pale yellow.
Example 6
The material information of the aluminum capacitor electrolyte in this embodiment is as follows:
300g of ethylene glycol, 200g of dodecanedioic acid, 200g of xylitol and 0.04g of phosphite ester are respectively weighed into a flask, heated and stirred to 70 ℃, continuously heated to 150 ℃, stirred and kept at the temperature for 5 hours, and the chromaticity of the electrolyte obtained after natural cooling is measured by a platinum-cobalt colorimetric method, the appearance color is observed, and the result is shown in a table 2.
Example 7
The material information of the aluminum capacitor electrolyte in this embodiment is as follows:
300g of ethylene glycol, 200g of dodecanedioic acid, 200g of xylitol and 0.4g of phosphite ester are respectively weighed into a flask, heated and stirred to 70 ℃, continuously heated to 150 ℃, stirred and kept at the temperature for 5 hours, and the chromaticity of the electrolyte obtained after natural cooling is measured by a platinum-cobalt colorimetric method, the appearance color is observed, and the result is shown in a table 2.
Example 8
The material information of the aluminum capacitor electrolyte in this embodiment is as follows:
300g of ethylene glycol, 200g of dodecanedioic acid, 200g of xylitol and 1.2g of phosphite ester are respectively weighed into a flask, heated and stirred to 70 ℃, continuously heated to 150 ℃, stirred and kept at the temperature for 5 hours, and the chromaticity of the electrolyte obtained after natural cooling is measured by a platinum-cobalt colorimetric method, the appearance color is observed, and the result is shown in table 2.
Example 9
The material information of the aluminum capacitor electrolyte in this embodiment is as follows:
300g of ethylene glycol, 200g of dodecanedioic acid, 200g of xylitol and 2g of phosphite ester are respectively weighed into a flask, heated and stirred to 70 ℃, continuously heated to 150 ℃, stirred and kept for 5 hours, and naturally cooled to obtain an electrolyte, the chromaticity of which is measured by a platinum-cobalt colorimetric method, and the appearance color is observed, and the result is shown in Table 2.
Example 10
The material information of the aluminum capacitor electrolyte in this embodiment is as follows:
300g of ethylene glycol, 200g of dodecanedioic acid, 200g of xylitol and 4g of phosphite ester are respectively weighed into a flask, heated and stirred to 70 ℃, continuously heated to 150 ℃, stirred and kept for 5 hours, and naturally cooled to obtain an electrolyte, the chromaticity of which is measured by a platinum-cobalt colorimetric method, and the appearance color is observed, and the result is shown in Table 2.
Example 11
The material information of the aluminum capacitor electrolyte in this embodiment is as follows:
300g of ethylene glycol, 200g of dodecanedioic acid, 200g of xylitol and 6g of phosphite ester are respectively weighed into a flask, heated and stirred to 70 ℃, continuously heated to 150 ℃, stirred and kept for 5 hours, and the chromaticity of the electrolyte obtained after natural cooling is measured by a platinum-cobalt colorimetric method, and the appearance color is observed, and the result is shown in table 2.
Example 12
The material information of the aluminum capacitor electrolyte in this embodiment is as follows:
300g of ethylene glycol, 200g of dodecanedioic acid, 200g of xylitol and 8g of phosphite ester are respectively weighed into a flask, heated and stirred to 70 ℃, continuously heated to 150 ℃, stirred and kept for 5 hours, and naturally cooled to obtain an electrolyte, the chromaticity of which is measured by a platinum-cobalt colorimetric method, and the appearance color is observed, and the result is shown in Table 2.
TABLE 2 results of the chroma and appearance color tests of the electrolytes of examples 6 to 12
Group of Chroma/Hazen Appearance color
Example 6 241 Yellow colour
Example 7 168 Pale yellow
Example 8 109 Pale yellow
Example 9 73 Pale yellow
Example 10 43 Colorless and colorless
Example 11 28 Colorless and colorless
Example 12 31 Colorless and colorless
As can be seen from the test results of examples 6 to 12 in Table 2, the chromaticity of the electrolyte gradually decreases with the addition of the chromaticity improver, and the appearance color also tends to be colorless; however, the invention controls the addition amount of the chromaticity modifier to be 0.01-2%, more preferably 0.1-0.5% based on the performance requirement of the electrolyte, and the chromaticity modifier is not added too much and the color modifying effect is combined.
According to the preparation method of the aluminum capacitor electrolyte, the chroma modifier is added, the addition sequence and the addition temperature of the chroma modifier are limited, the deepening of the color of a solute and the electrolyte can be effectively inhibited, the problem that the color of the electrolyte is deepened and blackened in the high-temperature cooking process is solved, the color of an electrolyte product is colorless to pale yellow, and the decoloring effect is obvious.
The invention has been further described with reference to specific embodiments, but it should be understood that the detailed description is not to be construed as limiting the spirit and scope of the invention, but rather as providing those skilled in the art with the benefit of this disclosure with the benefit of their various modifications to the described embodiments.

Claims (5)

1. The preparation method of the aluminum capacitor electrolyte is characterized by comprising the following steps of:
(1) Heating and stirring the solvent, the solute and the chromaticity improver uniformly; the solute comprises organic acids and/or sugar alcohols, and the chromaticity improver comprises one or more of hypophosphorous acid, ammonium hypophosphite and phosphite;
(2) Continuously heating to 120-180 ℃ and stirring, preserving heat, and cooling to obtain electrolyte;
Heating and stirring at 30-90 ℃ in the step (1);
the addition mass of the chromaticity improver accounts for 0.01-2% of that of the solute;
the mass ratio of the solvent to the solute in the step (1) is (0.5-1): 1.
2. The method of preparing an aluminum capacitor electrolyte according to claim 1, wherein the organic acids include one or more of suberic acid, azelaic acid, and dodecanedioic acid; the sugar alcohol comprises one or more of mannitol, sorbitol and xylitol.
3. The method for preparing an aluminum capacitor electrolyte according to claim 1, wherein the solvent is ethylene glycol,One or two of butyrolactone.
4. The method for preparing an aluminum capacitor electrolyte according to claim 1, wherein the addition mass of the chromaticity improver is 0.1-0.5% of the solute.
5. The method of preparing an aluminum capacitor electrolyte according to claim 1, wherein the temperature of the heat preservation in the step (2) is 120-180 ℃ and the heat preservation time is 1-8h.
CN202110340637.5A 2021-03-30 Preparation method of aluminum capacitor electrolyte Active CN115148500B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1601799A (en) * 2003-09-28 2005-03-30 张家港市国泰华荣化工新材料有限公司 Method of stabilizing colour of non-aquous electrolyte and lowering HF content
CN102013325A (en) * 2010-09-22 2011-04-13 湖南省衡阳华高电子有限公司 Electrolyte of wide-temperature long-life patch aluminium electrolytic capacitor and preparation method thereof
CN105895954A (en) * 2016-05-05 2016-08-24 东莞市凯欣电池材料有限公司 High-stability power battery electrolyte
WO2020242015A1 (en) * 2019-05-31 2020-12-03 에스케이케미칼 주식회사 Electrolyte solution for secondary battery and secondary battery comprising same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1601799A (en) * 2003-09-28 2005-03-30 张家港市国泰华荣化工新材料有限公司 Method of stabilizing colour of non-aquous electrolyte and lowering HF content
CN102013325A (en) * 2010-09-22 2011-04-13 湖南省衡阳华高电子有限公司 Electrolyte of wide-temperature long-life patch aluminium electrolytic capacitor and preparation method thereof
CN105895954A (en) * 2016-05-05 2016-08-24 东莞市凯欣电池材料有限公司 High-stability power battery electrolyte
WO2020242015A1 (en) * 2019-05-31 2020-12-03 에스케이케미칼 주식회사 Electrolyte solution for secondary battery and secondary battery comprising same

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