Purification method of quaternary ammonium salt

A purification method and quaternary ammonium salt technology, which is applied in the purification/separation of amino compounds, organic chemistry, etc., can solve the problems that product indicators fail to meet electronic grade standards, achieve low processing costs, reduce the decomposition of quaternary ammonium salts, and improve reaction conditions mild effect

Active Publication Date: 2019-01-04
HUIZHOU CAPCHEM CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Purification method of quaternary ammonium salt
  • Purification method of quaternary ammonium salt
  • Purification method of quaternary ammonium salt

Examples

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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 purification method of quaternary ammonium salt. The purification method comprises the steps as follows: step 1, impurity precipitates: mixing quaternary ammonium salt and water in the weight ratio being 1.6-2.1 for dissolution, heating the solution to 70-75 DEG C, adding an alkaline solution to the quaternary ammonium salt aqueous solution to adjust the pH value to 6.5-7.5 to produce impurity precipitates, removing the impurity precipitates through filtration, and reserving quaternary ammonium salt filtrate; step 2, filtrate concentration: concentrating the quaternary ammonium salt filtrate under reduced pressure into saturated quaternary ammonium salt aqueous solution with the mass percentage of water being 15%-25%; step 3, recrystallization: adding a non-benignsolvent for recrystallization according to the mass ratio of water of the concentrated saturated quaternary ammonium salt aqueous solution to the non-benign solvent of (1:10):(1:50), and performing filtration to obtain saturated quaternary ammonium salt crystals; step 4, drying: drying the saturated quaternary ammonium salt crystals in step 3 at 75-80 DEG C to obtain a finished product. The method has the advantages of being high in purification rate, high in recovery rate, safe, environmentally friendly, low in treatment cost, prone to industrial mass treatment 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 Applications(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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