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Synthesis method of tetrabutylammonium bromide

A technology of tetrabutylammonium bromide and synthesis method, applied in the field of tetrabutylammonium bromide synthesis, can solve problems such as increasing energy consumption, increasing equipment cost, large amount of solvent added, avoiding evaporation loss, improving color degree, the effect of saving raw materials

Pending Publication Date: 2021-08-13
SHANDONG TONGCHENG MEDICINE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. The amount of solvent added is large, and the solvent needs to be desolvated, which leads to a long process cycle, increases equipment costs, and increases energy consumption
[0005] 2. Ethyl acetate obtained during vacuum distillation contains acetonitrile, which makes separation difficult due to their similar boiling points. Forcible separation requires higher-precision distillation equipment as a support, which increases equipment investment and energy consumption caused by distillation
[0006] 3. In the micro-test stage, the product production cycle and yield are acceptable, but there are problems of long process cycle and low product yield in large-scale production

Method used

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  • Synthesis method of tetrabutylammonium bromide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of synthetic method of tetrabutylammonium bromide is characterized in that comprising the following steps:

[0026] (1) Prepare 640kg of dichloroethane solvent, 960kg of bromobutane and 1200kg of tri-n-butylamine to the corresponding batching tanks respectively, and add them to the reaction kettle in turn, and reflux at 95°C for 40 hours to obtain tetrabutyl Crude ammonium bromide;

[0027] (2) material in the reaction kettle is cooled to 60 ℃, and the tetrabutylammonium bromide crude product obtained in the step (1) is transferred in the crystallization kettle;

[0028] (3) Continue to lower the temperature of the crystallization kettle to 20°C for crystallization, and after the crystallization is completed, transfer the material to a centrifuge for centrifugation to obtain the centrifuged mother liquor in the previous stage;

[0029] (4) When the centrifuge no longer has mother liquor to flow out, rinse the centrifuge with 40kg ethyl acetate, centrifuge again ...

Embodiment 2

[0031] A kind of synthetic method of tetrabutylammonium bromide is characterized in that comprising the following steps:

[0032] (5) Detect the front-stage centrifugal mother liquor obtained in step (3) in Example 1, the mass fraction of amine salt is 2.3%, prepare the front-stage centrifugal mother liquor in the step (3) of Example 1 to the batching tank, and replenish inwardly Dichloroethane to 640kg, in addition, 960kg of bromobutane and 1200kg of tri-n-butylamine were respectively prepared into corresponding batching tanks, and added to the reaction kettle in turn, and refluxed at 95°C for 40h to obtain tetrabutyl bromide Crude ammonium;

[0033] (6) material in the reaction kettle is cooled to 60 ℃, and the tetrabutylammonium bromide crude product obtained in the step (5) is transferred in the crystallization kettle;

[0034] (7) Continue cooling the crystallization kettle to 20°C for crystallization, transfer to a centrifuge for centrifugation after the crystallization...

Embodiment 3

[0037] A kind of synthetic method of tetrabutylammonium bromide is characterized in that comprising the following steps:

[0038] (9) Detect the front-stage centrifugal mother liquor obtained in step (7) in Example 2, the mass fraction of amine salt is 4.1%, prepare the front-stage centrifugal mother liquor in the step (7) of Example 2 to the batching tank, and supplement inwardly Dichloroethane to 640kg, in addition, 960kg of bromobutane and 1200kg of tri-n-butylamine were respectively prepared into corresponding batching tanks, and added to the reaction kettle in turn, and refluxed at 95°C for 40h to obtain tetrabutyl bromide Crude ammonium;

[0039] (10) material in the reaction kettle is cooled to 60 ℃, and the tetrabutylammonium bromide crude product obtained in the step (9) is transferred in the crystallization kettle;

[0040] (11) Continue cooling the crystallization kettle to 20°C for crystallization, transfer to a centrifuge for centrifugation after the crystallizat...

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Abstract

The invention discloses a synthesis method of tetrabutylammonium bromide, which comprises the steps of reflux reaction, crystallization, centrifugation, mother liquor application, centrifugal machine washing and the like, the desolvation operation of dichloroethane is omitted, the evaporation loss of dichloroethane in the desolvation process is avoided, the raw materials are saved, and after the front-section centrifugal mother liquor is supplemented to the formula amount, infinite times of return use can be basically realized, bromobutane and a small amount of tetrabutylammonium bromide contained in the front-section centrifugal mother liquor can be completely put into the production of the next batch, the yield of the product is improved, impurities in the product can be washed away by washing a centrifugal machine with ethyl acetate, the chromaticity of the product is improved, and meanwhile, the post-stage centrifugal mother liquor obtained after centrifugation can be repeatedly used under the condition that the post-stage centrifugal mother liquor is inspected to be qualified, so that raw materials are saved.

Description

technical field [0001] The invention relates to the technical field of tetrabutylammonium bromide synthesis, in particular to a synthesis method of tetrabutylammonium bromide. Background technique [0002] Tetrabutylammonium bromide is an organic salt with the molecular formula C16H36BrN. The pure product is white crystal or powder with deliquescence and special odor. It is stable at normal temperature and pressure. Soluble in water, alcohol and acetone, slightly soluble in benzene. Toxic, often used as organic synthesis intermediates, phase transfer catalysts, ion-pair reagents. [0003] Application number CN200910070539.3 discloses a kind of preparation method of tetrabutylammonium bromide, uses bromobutane and tri-n-butylamine as raw material, and acetonitrile is made solvent, and specific process is that bromobutane and tri-n-butylamine are carried out in acetonitrile Synthesis, and then carry out desolvation in the desolventizer to remove acetonitrile, and then add et...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/12C07C209/84
CPCC07C209/12C07C209/84C07C211/63
Inventor 李慧鹏刘国先
Owner SHANDONG TONGCHENG MEDICINE TECH CO LTD
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