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Preparation method of high-purity tetraethylammonium chloride

A tetraethylammonium chloride, high-purity technology, applied in the preparation of amino compounds, organic compounds, chemical instruments and methods, etc., can solve the problems of low product purity, low production efficiency of tetraethylammonium chloride, reaction Long time and other problems, to achieve the effect of high purity and yield, conducive to dispersion, and simple steps

Inactive Publication Date: 2018-09-28
盐城泛安化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production efficiency of the tetraethylammonium chloride preparation method adopted in this patent is low, the reaction time is long, and the purity of the product is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) 45g ethyl chloride is dissolved in 300g dimethylbenzene, stand-by;

[0025] (2) Add 10g of triethylamine, 50g of ether, and 150g of xylene into the autoclave, and add 250g of ethyl chloride-xylene solution dropwise into the autoclave at 70°C. After 1 hour, feed gas to keep the pressure in the autoclave at 3MPa, and after reacting at 120°C for 12 hours, stop the ventilation, slowly open the vent valve, and cool down to room temperature;

[0026] (3) Filter the reaction solution obtained in step (2) to obtain 58.3g of filter cake A as the crude product of tetraethylammonium chloride, add the crude product of tetraethylammonium chloride to 100g of water, and stir at 45°C until most of the crude product dissolves , filtered while hot, 20.2g of filtrate was added to 80g of acetonitrile, 120g of pentylene glycol mixed solvent, stirred and left for half an hour, filtered, and the filter cake B was dried to obtain 15.9g of tetraethylammonium chloride, with a purity of 99.7%...

Embodiment 2

[0028] (1) 60g ethyl chloride is dissolved in 300g dimethylbenzene, stand-by;

[0029] (2) Add 10g of triethylamine, 44g of ether, and 176g of xylene into the autoclave, and add 200g of ethyl chloride-xylene solution dropwise into the autoclave at 75°C. After one hour, feed gas to keep the pressure in the autoclave at 1.5MPa, and after reacting at 150°C for 28 hours, stop the ventilation, slowly open the vent valve, and cool down to room temperature;

[0030] (3) Filter the reaction solution obtained in step (2) to obtain 60.7g of filter cake A as the crude product of tetraethylammonium chloride, add the crude product of tetraethylammonium chloride to 100g of water, and stir at 40°C until most of the crude product dissolves , filtered while hot, to get 22.5g of filtrate, add 113g of acetonitrile, 169g of pentylene glycol mixed solvent, stir and let it stand for half an hour, filter, and dry the filter cake B to get 16.6g of tetraethylammonium chloride, the purity is 99.6% , t...

Embodiment 3

[0032] (1) 54g ethyl chloride is dissolved in 300g dimethylbenzene, stand-by;

[0033] (2) Add 10g of triethylamine, 42g of ether, and 208g of xylene into the autoclave. At 80°C, add the ethyl chloride-xylene solution dropwise into the autoclave. After the addition is complete, keep the temperature for half an hour. Finally, feed gas to keep the pressure in the autoclave at 2MPa, and after reacting at 130°C for 18 hours, stop the ventilation, slowly open the vent valve, and cool down to room temperature;

[0034] (3) Filter the reaction solution obtained in step (2) to obtain 59.0 g of filter cake A as the crude product of tetraethylammonium chloride, add the crude product of tetraethylammonium chloride to 100 g of water, and stir at 50 ° C until most of the crude product dissolves , filtered while hot, 18.2g of filtrate was added to 110g of acetonitrile, 164g of pentylene glycol mixed solvent, stirred and left for half an hour, filtered, and the filter cake B was dried to obt...

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PUM

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Abstract

The invention provides a preparation method of high-purity tetraethylammonium chloride, which includes the steps of: 1) preparing a chloroethane-xylene solution; 2) adding triethylamine and a solventto a high-pressure reaction kettle, dropwise adding the chloroethane-xylene solution to the high-pressure reaction kettle at 70-80 DEG C, after the solution is added, performing a heat preservative reaction for 30 min, feeding gas to maintain the pressure in the kettle under 1.5-3 MPa, and performing a reaction for 12-28 h at 120-150 DEG C, stopping feeding the gas, slowly opening an exhaust valveand cooling the system to room temperature; 3) filtering the reaction liquid to obtain a filter cake A being a tetraethylammonium chloride crude product, adding the crude product to water, stirring the liquid at 40-50 DEG C for dissolution, and filtering the liquid while hot, adding a filtrate to a mixed solvent of acetonitrile and pentanediol, stirring the solution, allowing the solution to stand, filtering the solution to obtain a filter cake B, and drying the filter cake B to prepare the high-purity tetraethylammonium chloride. The preparation method has simple steps and high production efficiency, is high in purity and yield of product, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of high-purity tetraethylammonium chloride. Background technique [0002] Tetraethylammonium chloride is a kind of quaternary ammonium salt, which can form micelles of various shapes, and is widely used in organic synthesis, zeolite molecular sieve template, cellulose dissolution and regeneration, asymmetric catalysis, asymmetric alkane of aniline reactions such as radicalization and polymerization. [0003] Patent CN1347872A relates to the preparation method of tetraethylammonium chloride, and its preparation method is: surfactant, non-ionic solvent and triethylamine are placed in a closed container, after sealing, replace the air in the container with inert gas to oxygen After the content volume percentage is lower than 1%, then introduce ethyl chloride, react at a temperature of 50~120°C for 12~96 hours, cool down, and separate the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/12C07C209/84C07C211/63
CPCC07C209/12C07C209/84C07C211/63
Inventor 郭晓坚沈加春姚林钢李佳明
Owner 盐城泛安化学有限公司
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