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Polycarboxylic acid for electrolyte as well as preparation method and application thereof

A polycarboxylic acid and polycarboxylic acid ester technology, which is applied in the preparation of carboxylate, electrical components, electrolytic capacitors, etc., can solve the problems of insufficient large-scale production, low electrolyte conductivity, and poor low temperature resistance. Achieve the effect of high yield, simple operation and high flash voltage

Active Publication Date: 2013-12-11
武汉海斯普林科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, they have the problems of low solubility in the solvent, low conductivity of the prepared electrolyte, low flashover voltage, poor low temperature resistance and short service life, which cannot meet the needs of the modern high-end capacitor industry, such as medium and high voltage aluminum electrolysis. Capacitor needs
[0003] In recent years, a large number of literature patents disclose such as: 2-butyl suberic acid (also known as 1,6-decane dicarboxylic acid) and its ammonium salt, 1,7-octane dicarboxylic acid and its ammonium salt and other substances The detailed application of these substances, and the electrical properties and service life of such substances have been significantly improved, but the existing technology about its preparation and purification methods is not enough to achieve large-scale production

Method used

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  • Polycarboxylic acid for electrolyte as well as preparation method and application thereof
  • Polycarboxylic acid for electrolyte as well as preparation method and application thereof
  • Polycarboxylic acid for electrolyte as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The preparation method of polyvalent carboxylic acid for electrolyte comprises the following steps:

[0048] a. Add 500 ml of anhydrous methanol and 49 g (0.5 mol) of cyclohexanone into a well-dried 1 L four-neck flask equipped with stirring, dropping funnel, and thermometer, and cool down to -5°C. Then, 3.0 g of concentrated sulfuric acid was slowly added dropwise from the dropping funnel. After completion, dropwise add 30% volume concentration of H 2 o 2 The solution was 57.8g, and the temperature was kept at about 8°C. After the completion, the stirring was continued for 15 minutes.

[0049] b. Add 79 g (0.5 mol) of dimethyl itaconate dissolved in methanol solvent dropwise into the reaction solution, keeping the temperature at -10-5°C. After completion, continue stirring for 15 min. 140g of FeSO 4 ·7H 2O was slowly added to the reaction solution, keeping the temperature below 5°C. After completion, continue stirring for 30 min. Add 100g of diethyl ether for e...

Embodiment 2

[0072] The preparation method of polyvalent carboxylic acid for electrolyte comprises the following steps:

[0073] a, step a with embodiment 1;

[0074] b. Add 158 g (1 mol) of dimethyl itaconate dissolved in methanol solvent dropwise into the reaction solution, keeping the temperature at -10-5°C. After completion, continue stirring for 15 min. 140g of FeSO 4 ·7H 2 O was slowly added to the reaction solution, keeping the temperature below 5°C. After completion, continue stirring for 30 min. Add 100g of diethyl ether for extraction, wash with water, and distill off the solvent to obtain the carboxylate product.

[0075] c. Add the above carboxylate product into 800 g of 10% sodium methoxide solution by weight, raise the temperature to 120° C., and react for 4 hours to obtain the sodium carboxylate product.

[0076] d. Acidify the obtained sodium carboxylic acid product with 150 g of 50% dilute sulfuric acid to obtain a total of 243.8 g of the carboxylic acid product.

...

Embodiment 3

[0080] The preparation method of polyvalent carboxylic acid for electrolyte comprises the following steps:

[0081] a, step a with embodiment 1;

[0082] b. Add 237 g (1.5 mol) of dimethyl itaconate dissolved in methanol solvent dropwise into the reaction solution, keeping the temperature at -10-5°C. After completion, continue stirring for 15 min. 140g of FeSO 4 ·7H 2 O was slowly added to the reaction solution, keeping the temperature below 5°C. After completion, continue stirring for 30 min. Add 100g of diethyl ether for extraction, wash with water, and distill off the solvent to obtain the carboxylate product.

[0083] c, adding the above-mentioned carboxylate product to 800g weight concentration is 20% Na 2 CO 3 In the solution, the temperature was raised to 100°C, and the reaction was carried out for 10 hours to obtain the sodium salt of carboxylic acid.

[0084] d. The obtained sodium salt was acidified with 150 g of dilute sulfuric acid with a weight concentrati...

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Abstract

The invention discloses a polycarboxylic acid for electrolyte as well as a preparation method and application thereof. The polycarboxylic acid for the electrolyte has a structural general formula, wherein R1, R2, R3 and R5 are hydrogen radicals and alkyl radicals; n is an integer from 2 to 12; m is an integer from 1 to 3; and R1, R2, R3 and R5 are same or different to each other. The ammonium salt of the polycarboxylic acid for the electrolyte has the advantages of high solubility in a menstruum, high conductivity, excellent high-low temperature resistance, long service life, and the like; and in addition, the invention has the advantages of simple preparation method, high yield, low foreign ion content and suitability for industrial large-scale production.

Description

technical field [0001] The invention belongs to the technical field of electrolyte synthesis for aluminum electrolytic capacitors, and specifically refers to a polycarboxylic acid for electrolyte, a preparation method and application thereof. Background technique [0002] At present, the acids and their ammonium salts commonly used in the electrolyte of aluminum electrolytic capacitors include ammonium borate, ammonium formate, ammonium adipate, ammonium succinate, ammonium maleate, ammonium phthalate, quaternary ammonium salt, and decane Ammonium diacid, ammonium azelate, ammonium benzoate, etc. The acid and its ammonium salt used in the above-mentioned working electrolyte have mature production technologies and have achieved large-scale production. However, they have the problems of low solubility in the solvent, low conductivity of the prepared electrolyte, low flashover voltage, poor low temperature resistance and short service life, which cannot meet the needs of the m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/24C07C55/22C07C51/02H01G9/035
Inventor 刘立周宜海
Owner 武汉海斯普林科技发展有限公司
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