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Method for preparing tetraethyl ammonium hydroxide

A technology of tetraethylammonium hydroxide and tetraethylammonium bromide, which is applied in the preparation of amino compounds from amines, etc., can solve the problems of long reaction time and low product yield, so as to speed up the reaction time and increase the product yield , Improve the effect of economic and social benefits

Inactive Publication Date: 2011-04-27
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a kind of preparation method of tetraethylammonium hydroxide in order to overcome the defect that prior art reaction time is long, product yield is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) 80 grams of potassium hydroxide and 100 grams of methanol are mixed to obtain a mixed solution;

[0017] (2) in a reactor with 1000 milliliters of electric stirring, thermometer, water circulation condenser, drop into 200 gram tetraethylammonium bromide, 400 gram solvent methanol, stir and add step (1) gained mixed solution fast, Continue to stir until all the precipitates are precipitated, and react for 2 hours;

[0018] (3) Precipitation is filtered under reduced pressure, and the light yellow liquid of gained is tetraethylammonium hydroxide crude product;

[0019] (4) in a 1000 milliliter distiller with heating device, thermometer, water circulation condenser, drop into tetraethylammonium hydroxide crude product, 450 grams of deionized water, be heated to reflux, temperature remains on 35-50 ℃, Vacuum degree is controlled at 30-35mmHg column, constant temperature is reacted for 3 hours, cooled and crystallized, and the obtained white crystal is the finished prod...

Embodiment 2

[0021] (1) 90 grams of potassium hydroxide and 100 grams of methanol are mixed to obtain a mixed solution;

[0022] (2) in a reactor with 1000 milliliters of electric stirring, thermometer, water circulation condenser, drop into 200 gram tetraethylammonium bromide, 400 gram solvent methanol, stir and add step (1) gained mixed solution fast, Continue to stir until all the precipitates are precipitated, and react for 2 hours;

[0023] (3) Precipitation is filtered under reduced pressure, and the light yellow liquid of gained is tetraethylammonium hydroxide crude product;

[0024] (4) in a 1000 milliliter distiller with heating device, thermometer, water circulation condenser, drop into tetraethylammonium hydroxide crude product, 450 grams of deionized water, be heated to reflux, temperature remains on 35-50 ℃, Vacuum degree is controlled at 30-35mmHg column, constant temperature is reacted for 3 hours, cooled and crystallized, and the obtained white crystal is the finished prod...

Embodiment 3

[0026] (1) 100 grams of potassium hydroxide and 100 grams of methanol are mixed to obtain a mixed solution;

[0027] (2) in a reactor with 1000 milliliters of electric stirring, thermometer, water circulation condenser, drop into 200 gram tetraethylammonium bromide, 400 gram solvent methanol, stir and add step (1) gained mixed solution fast, Continue to stir until all the precipitates are precipitated, and react for 2 hours;

[0028] (3) Precipitation is filtered under reduced pressure, and the light yellow liquid of gained is tetraethylammonium hydroxide crude product;

[0029] (4) in a 1000 milliliter distiller with heating device, thermometer, water circulation condenser, drop into tetraethylammonium hydroxide crude product, 450 grams of deionized water, be heated to reflux, temperature remains on 35-50 ℃, Vacuum degree is controlled at 30-35mmHg column, constant temperature is reacted for 3 hours, cooled and crystallized, and the obtained white crystal is the finished pro...

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PUM

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Abstract

The invention relates to a method for preparing tetraethyl ammonium hydroxide, which is characterized in that potassium hydroxide and methanol are added to the mixing solution of the tetraethyl ammonium hydroxide and the methanol to prepare the finished product of the tetraethyl ammonium hydroxide through reaction, pressure reduction, filtration, precipitation, heating reflux, refrigeration and crystallization. The method has the advantages that the reaction speed is accelerated; the yield of the product is enhanced; the requirements in the market are satisfied; and the economic benefit and the social benefit of enterprises are enhanced.

Description

technical field [0001] The invention relates to the field of preparation methods of organic compounds, in particular to a preparation method of tetraethylammonium hydroxide. Background technique [0002] Tetraethylammonium hydroxide is a common chemical product in the market, and it is a chemical reagent with a wide range of uses. The main purpose is to determine lithium, magnesium, potassium, sodium polarographic analysis reagents, chemical reagents and acetylation of nucleosides Wait. The preparation method of existing tetraethylammonium hydroxide is (1) acetone and triethylamine are added in an airtight container, replace air with inert gas, then introduce ethyl chloride; (2) heat and continue to stir more than 150 hours , then, cooling, separation of tetraethylammonium chloride; (3) washing with water, carrying out ion exchange with efficient basic resin, to obtain tetraethylammonium hydroxide crude product; (4) concentrating under reduced pressure to obtain tetraethyla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/63C07C209/68
Inventor 徐博刚
Owner TIANJIN CHEM REAGENT RES INST