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Method for preparing tetrabutylammonium hydroxide

A technology of tetrabutylammonium hydroxide and tetrabutylammonium bromide, which is applied in the direction of preparing amino compounds from amines, can solve the problems of difficult raw material recovery, high price, and low product yield, so as to improve economic and social benefits, The effect of improving product yield

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

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Problems solved by technology

After comparison, it can be found that both the first method and the second method use an expensive raw material silver oxide and high-efficiency basic resin, and the recovery of these two raw materials is difficult. The third method is cheap and requires low equipment. , the process is simple and easy to learn. At present, without adding advanced equipment and increasing the technical requirements of operators, the yield of the synthesized product is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) 80 grams of potassium hydroxide and 100 grams of methanol are mixed to obtain a mixed solution, and in a 1000-milliliter reactor with electric stirring, a thermometer, and a water circulation condenser, drop 200 grams of tetrabutylammonium bromide, 400 gram of solvent methanol, stir and quickly add the mixed solution of potassium hydroxide and methanol, continue to stir until all the precipitates are precipitated, and react for 2 hours;

[0016] (2) Precipitation is filtered under reduced pressure, and the light yellow liquid of gained is the tetrabutylammonium hydroxide crude product;

[0017] (3) In a 1000 ml distiller with a heating device, a thermometer, and a water circulation condenser, put the crude product of tetrabutylammonium hydroxide and 450 grams of deionized water into it, heat to reflux, and keep the temperature at 35-50° C. Control the column at 30-35mmHg, react at constant temperature for 3 hours, cool and crystallize, and the white crystal obtained...

Embodiment 2

[0019] (1) 90 grams of potassium hydroxide and 100 grams of methanol are mixed to obtain a mixed solution. In a 1000-milliliter reactor with electric stirring, a thermometer, and a water circulation condenser, 200 grams of tetrabutylammonium bromide, 400 gram of solvent methanol, stir and quickly add the mixed solution of potassium hydroxide and methanol, continue to stir until all the precipitates are precipitated, and react for 2 hours;

[0020] (2) Precipitation is filtered under reduced pressure, and the light yellow liquid of gained is the tetrabutylammonium hydroxide crude product;

[0021] (3) In a 1000 ml distiller with a heating device, a thermometer, and a water circulation condenser, put the crude product of tetrabutylammonium hydroxide and 450 grams of deionized water into it, heat to reflux, and keep the temperature at 35-50° C. Control the column at 30-35mmHg, react at constant temperature for 3 hours, cool and crystallize, and the white crystal obtained is the f...

Embodiment 3

[0023] (1) 100 grams of potassium hydroxide and 100 grams of methanol are mixed to obtain a mixed solution, and in a 1000-milliliter reactor with electric stirring, a thermometer, and a water circulation condenser, drop 200 grams of tetrabutylammonium bromide, 400 gram of solvent methanol, stir and quickly add the mixed solution of potassium hydroxide and methanol, continue to stir until all the precipitates are precipitated, and react for 2 hours;

[0024] (2) Precipitation is filtered under reduced pressure, and the light yellow liquid of gained is the tetrabutylammonium hydroxide crude product;

[0025] (3) In a 1000 ml distiller with a heating device, a thermometer, and a water circulation condenser, put the crude product of tetrabutylammonium hydroxide and 450 grams of deionized water into it, heat to reflux, and keep the temperature at 35-50° C. Control the column at 30-35mmHg, react at constant temperature for 3 hours, cool and crystallize, and the white crystal obtaine...

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Abstract

The invention relates to a method for preparing tetrabutylammonium hydroxide, which is characterized by comprising the following steps of: blending potassium hydroxide and methanol, adding the mixture into mixed solution of tetrabutyl ammonium bromide and the methanol, filtering and precipitating under reduced pressure, and after heating and refluxing, cooling and crystallizing to obtain the finished product of the tetrabutylammonium hydroxide. By the method, the yield of the product is improved; the requirements of the market are met; and the economic benefit and the social benefit of an enterprise are improved.

Description

technical field [0001] The invention relates to the field of preparation methods of organic compounds, in particular to a preparation method of tetrabutylammonium hydroxide. Background technique [0002] As a chromatographic analysis agent, tetrabutylammonium hydroxide is widely used in industry and scientific research fields. The production methods of this product mainly include the following three methods: 1. Using tetrabutylammonium halide as raw material to react with silver oxide; 2. Using tetrabutylammonium halide as raw material to produce by ion exchange with high-efficiency basic resin; 3. It is produced by reacting tetrabutylammonium halide with potassium hydroxide. After comparison, it can be found that both the first method and the second method use an expensive raw material silver oxide and high-efficiency basic resin, and the recovery of these two raw materials is difficult. The third method is cheap and requires low equipment. , the process is simple and eas...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/68
Inventor 徐博刚
Owner TIANJIN CHEM REAGENT RES INST
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