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Crystallization refining method of tetrabutylammonium bromide

A technology of tetrabutylammonium bromide and refining method, which is applied in the direction of amino compound purification/separation, organic chemistry, etc., can solve the problems of low production efficiency and long time consumption, and achieve low impurity content, shortened time and high yield Effect

Pending Publication Date: 2022-02-08
安徽赛迪生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method takes too long, the crystallization time is as long as more than 3 days, and the production efficiency is extremely low

Method used

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  • Crystallization refining method of tetrabutylammonium bromide

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Effect test

Embodiment 1

[0021] A kind of crystallization refining method of tetrabutylammonium bromide, comprises the following steps:

[0022] S1. Add ethyl acetate into the reaction kettle, preheat to 33°C, then add molten crude tetrabutylammonium bromide under the condition of stirring at 100rpm, and ultrasonically treat it for 4min at the frequency of 40kHZ and the power of 150W to obtain Crystal stock solution, wherein the mass ratio of crude tetrabutylammonium bromide to ethyl acetate is 0.9:1;

[0023] S2. Cool the crystallization stock solution to 9°C at a cooling rate of 12°C / h, crystallize under the stirring condition of 100rpm for 2.5h, and then raise the temperature to 13°C at a heating rate of 4°C / h. Ultrasonic treatment for 8 minutes under the condition;

[0024] S3. Cool down to 5°C at a cooling rate of 4°C / h, crystallize under 100rpm stirring conditions for 4.5h, then raise the temperature to 9°C at a heating rate of 4°C / h, and ultrasonicate at a frequency of 40kHZ and a power of 550...

Embodiment 2

[0031] A kind of crystallization refining method of tetrabutylammonium bromide, comprises the following steps:

[0032] S1. Add ethyl acetate into the reaction kettle, preheat to 30°C, then add molten crude tetrabutylammonium bromide under the condition of stirring at 50rpm, and ultrasonically treat it for 3min under the condition of frequency 30kHZ and power 100W, to obtain Crystal stock solution, wherein the mass ratio of crude tetrabutylammonium bromide to ethyl acetate is 0.8:1;

[0033] S2. Cool the crystallization stock solution to 10°C at a cooling rate of 10°C / h, crystallize under the stirring condition of 50rpm for 2h, and then raise the temperature to 12°C at a heating rate of 3°C / h, under the conditions of frequency 30kHZ and power 100W Ultrasonic treatment for 5 minutes;

[0034] S3. Cool down to 5°C at a cooling rate of 3°C / h, crystallize under stirring conditions of 50rpm for 4h, then raise the temperature to 8°C at a heating rate of 3°C / h, and perform ultrasoni...

Embodiment 3

[0039] A kind of crystallization refining method of tetrabutylammonium bromide, comprises the following steps:

[0040] S1. Add ethyl acetate into the reaction kettle, preheat to 35°C, then add molten crude tetrabutylammonium bromide under the condition of stirring at 150rpm, and ultrasonically treat it for 5min under the condition of frequency 40kHZ and power 200W, to obtain Crystal stock solution, wherein the mass ratio of crude tetrabutylammonium bromide to ethyl acetate is 1:1;

[0041] S2. Cool the crystallization stock solution to 8°C at a cooling rate of 15°C / h, crystallize at a stirring condition of 150rpm for 3h, then raise the temperature to 15°C at a heating rate of 5°C / h, under the conditions of a frequency of 40kHZ and a power of 200W Ultrasonic treatment for 10 minutes;

[0042] S3. Cool down to 6°C at a cooling rate of 5°C / h, crystallize under stirring conditions of 150rpm for 5h, then raise the temperature to 10°C at a heating rate of 5°C / h, and perform ultras...

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Abstract

The invention discloses a crystallization refining method of tetrabutylammonium bromide, the method comprises the following steps: firstly, adding a molten tetrabutylammonium bromide crude product into a preheated solvent ethyl acetate, and then carrying out continuous crystallization by adopting a staged heating and cooling and ultrasonic coupling method. According to the method, the time required for crystallization and refining of tetrabutylammonium bromide can be greatly shortened, the yield is high, and the one-time crystallization rate can reach 99% or above.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for crystallization and purification of tetrabutylammonium bromide. Background technique [0002] The molecular formula of tetrabutylammonium bromide is C 16 h 36 BrN, which is a common organic synthesis intermediate and phase transfer catalyst, is widely used in chemical industry, new energy and anti-epidemic. At present, the synthetic method of tetrabutylammonium bromide is mainly based on tributylamine and bromobutane as raw materials, and is prepared by quaternization reaction. After solvent removal, the obtained tetrabutylammonium bromide crude product was melted, and then added to the solvent ethyl acetate for natural crystallization. The method has a high crystallization stock solution concentration, a solid-liquid ratio as high as (0.8-1):1, a primary crystallization rate as high as 90-95%, and a simple process. However, this method takes too long, ...

Claims

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Application Information

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IPC IPC(8): C07C209/84C07C211/63
CPCC07C209/84C07C211/63
Inventor 魏晓廷朱仁发张勇殷继平朱金玉
Owner 安徽赛迪生物科技股份有限公司
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