A kind of purification method of quaternary ammonium salt

A purification method and quaternary ammonium salt technology, which are applied in the purification/separation of amino compounds, organic chemistry, etc., can solve the problems of product indicators failing to reach electronic-grade standards, and achieve low processing costs, mild reaction conditions, and reduction of quaternary ammonium salts. The effect of decomposition

Active Publication Date: 2021-07-09
HUIZHOU CAPCHEM CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, in the synthesis of the quaternary ammonium salt at home and abroad, due to the use of quaternary ammonium base as raw material, sodium, potassium, iron and other metals are inevitably brought into the product, causing the product index to fail to meet the electronic grade standard

Method used

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  • A kind of purification method of quaternary ammonium salt
  • A kind of purification method of quaternary ammonium salt
  • A kind of purification method of quaternary ammonium salt

Examples

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Effect test

Embodiment 1

[0056] This embodiment is used to illustrate the quaternary ammonium salt purification method disclosed by the present invention, comprising the following steps:

[0057] 1) Precipitation of impurities:

[0058] Tetramethylammonium tetrafluoroborate and pure water were mixed and dissolved in a weight ratio of 1.7:1, that is, tetramethylammonium tetrafluoroborate was 200.2kg, and pure water was 120.1kg. The pure water was prepared by ion exchange resin, After dissolving, heat to 70°C, add ammonia water to adjust the pH value to 7.01, stir for 1 hour to form impurity precipitates, and control the temperature of the quaternary ammonium salt aqueous solution to 70°C to filter out the impurity precipitates, and retain the quaternary ammonium salt filtrate;

[0059] 2) Concentration of the filtrate:

[0060] The quaternary ammonium salt filtrate in step 1 was concentrated under reduced pressure at a vacuum degree of -0.085MPa and a temperature of 66°C to a saturated aqueous solutio...

Embodiment 2

[0066] This embodiment is used to illustrate the quaternary ammonium salt purification method disclosed by the present invention, comprising the following steps:

[0067] 1) Precipitation of impurities:

[0068] Tetraethylammonium hexafluorophosphate and pure water are mixed and dissolved in a weight ratio of 2.0:1, that is, tetraethylammonium hexafluorophosphate is 700.5kg, and pure water is 350.4kg. The pure water is prepared by a distiller and dissolved After heating to 73°C, add sodium hydroxide solution to adjust the pH value to 6.8, stir for 1.5 hours to form impurity precipitates, and control the temperature of the quaternary ammonium salt aqueous solution within the range of 73°C to filter out the impurity precipitates, and retain the quaternary ammonium salt filtrate;

[0069] 2) Concentration of the filtrate:

[0070] The quaternary ammonium salt filtrate in step 1 was concentrated under reduced pressure at a vacuum degree of -0.1MPa and a temperature of 59°C to a s...

Embodiment 3

[0076] This embodiment is used to illustrate the quaternary ammonium salt purification method disclosed by the present invention, comprising the following steps:

[0077] 1) Precipitation of impurities:

[0078] Tetramethylammonium hexafluorophosphate and pure water are mixed and dissolved in a weight ratio of 1.8:1, that is, tetraethylammonium hexafluorophosphate is 700.5kg, and pure water is 350.4kg. The pure water is prepared by a distiller and dissolved After heating to 72°C, add ammonia solution to adjust the pH value to 6.9, stir for 1.0 hour to form impurity precipitates, and control the temperature of the quaternary ammonium salt aqueous solution at 72°C to filter out the impurity precipitates, and retain the quaternary ammonium salt filtrate;

[0079] 2) Concentration of the filtrate:

[0080] The quaternary ammonium salt filtrate in step 1 was concentrated under reduced pressure at a vacuum degree of -0.09MPa and a temperature of 63°C to a saturated aqueous solution...

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Abstract

The invention discloses a method for purifying a quaternary ammonium salt, which comprises the following processing steps: step 1, impurity precipitation; mixing and dissolving the quaternary ammonium salt and water in a weight ratio of 1.6 to 2.1, heating to 70°C to 75°C, and feeding the quaternary ammonium salt The ammonium salt aqueous solution is added with an alkaline solution to adjust the pH value to 6.5-7.5, and impurity precipitates are generated, and the impurity precipitates are removed by filtration, and the quaternary ammonium salt filtrate is retained; step 2, the filtrate is concentrated; the quaternary ammonium salt filtrate is concentrated under reduced pressure to the mass of water. Content is the quaternary ammonium salt saturated aqueous solution of 15%~25%; Step 3, recrystallization; According to the mass ratio of the water quality of the quaternary ammonium salt saturated aqueous solution obtained by concentration and the non-benign solvent, be 1:10~1:50, Recrystallize after adding a non-virtuous solvent, and filter to obtain quaternary ammonium salt crystals; Step 4, drying; drying the quaternary ammonium salt crystals in Step 3 at 75°C to 80°C to obtain the finished product. The invention has the advantages of high purification rate, high recovery rate, safety and environmental protection, low processing cost, easy realization of industrialized batch processing, and the like.

Description

technical field [0001] The invention relates to the technical field of electrolyte purification, in particular to a method for purifying a quaternary ammonium salt. Background technique [0002] Supercapacitors have excellent properties such as safety, high energy density, wide applicable temperature range, and environmental protection. The development of high-voltage and high-temperature-resistant electrolytes is currently a key research direction at home and abroad to improve the performance of supercapacitors. The quaternary ammonium salt, as the electrolyte salt of the electrolyte of the electric double layer capacitor, has the characteristics of high melting point, stable chemical structure, wide electrochemical window range, good solubility and high electrochemical decomposition voltage, and the electrolyte temperature adaptability of the electrolyte is good. , with high electrical conductivity, the formed electric double layer is stable and good, and the leakage curre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/84C07C211/63
CPCC07C209/84C07C211/63
Inventor 杨婷元曹英杰陈群
Owner HUIZHOU CAPCHEM CHEM CO LTD
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