Electrochemical synthesis method for tetra-n-butylammonium tribromide

A technology of tetra-n-butylammonium tribromide and a synthesis method, which is applied in directions such as electrolysis process, electrolysis components, electrolysis organic production, etc., can solve problems such as suboptimal, difficult transportation and storage, complicated process, etc., and achieve a favorable environment The effect of protection, convenient source and lower price

Inactive Publication Date: 2007-10-17
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This kind of synthetic method does not use elemental bromine or hydrogen bromide, which is more friendly to the environment, but uses hydrogen peroxid...

Method used

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Embodiment 1

[0018] The processing steps of the present embodiment are as follows:

[0019] Dissolve 9.5g of ammonium bromide in 20ml of distilled water to make an aqueous solution, then add 0.5g of tetra-n-butylammonium bromide, stir with a magnetic stirrer, after completely dissolving, add 30ml of dichloromethane, and stir vigorously; then Put the solution in a non-melted film electrolytic cell, use platinum mesh (3×3cm) as the cathode and anode of the electrolytic cell, input a constant current for electrolysis, and the constant current is 0.3A DC current; electrolyze at room temperature and under magnetic stirring 3 hours; now it can be seen that the oil phase is under the water phase, and the separated reddish-brown oil phase is tetra-n-butylammonium tribromide. Wash the reddish-brown oil phase with distilled water, evaporate the organic solvent, leave it in the open for a period of time, wait for the product to solidify, wash with water, recrystallize with methanol, wash with water, ...

Embodiment 2

[0021] The processing steps of the present embodiment are as follows:

[0022] Dissolve 9.5g of ammonium bromide in 20ml of distilled water to make an aqueous solution, then add 0.5g of tetra-n-butylammonium bromide, stir with a magnetic stirrer, after completely dissolving, add 30ml of acetonitrile, and stir vigorously; then the solution Put it in a non-melting film electrolytic cell, use platinum mesh (3×3cm) as the cathode and anode of the electrolytic cell, input a constant current for electrolysis, the constant current is 0.3A DC current; electrolyze for 3 hours at room temperature and under magnetic stirring Now it can be seen that the oil phase is above the water phase, and the separated yellow-brown oil phase is tetra-n-butylammonium tribromide. After washing the yellow-brown oil phase with distilled water, evaporate the organic solvent, leave it in the open for a period of time, wait for the product to solidify, wash with water, recrystallize with methanol, wash with ...

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Abstract

The present invention relates to an electrochemistry synthetic method of tetributyl tribromide of ammonium and belongs to the field of chemical formulation preparing technology. Sadi synthetic method in accordance with the present invention is as follow: dissolving tetrabutyl ammonium bromide in a aqueous solution of bromium salts such as ammonium bromide, potassium bromide or sodium bromide, magnetic-stirring it until reaching a entire solubilization, and then restirring it after adding organic solvent such as methylene dichloride or acetonitrile therein; putting the solution into an electrolytic tank of non-diaphragm type, selecting platinum meshwork as cathode and anode, inputting a constant electrical current for electroanalysis; electrolyzing for 3 hours under normal temperature and magnetic stirring to obtain tetributyl tribromide of ammonium in oil phase finally; washing the oil phase with distilled water, evaporating the organic solvent off and exposing it to air for a period of time, after the product solidifies, washing it with water, performing a recrystallization with methanol to obtain high-purity tetributyl tribromide of ammonium solid.

Description

technical field [0001] The invention relates to an electrochemical synthesis method of tetra-n-butylammonium tribromide, belonging to the technical field of chemical preparation. Background technique [0002] The tribromide of organic ammonium can replace elemental bromine for bromination reaction, and it is usually crystalline, easy to handle, easy to maintain stoichiometric in the reaction mixture, and is called "solid bromine". Among them, tetra-n-butylammonium tribromide, as a brominating agent or oxidizing agent with special properties, and other uses, has been paid attention to by organic synthesis researchers in recent years. [0003] In the traditional synthetic method of the tribromide of organic ammonium, there is elemental bromine Br 2 Or the participation of hydrogen bromide HBr; For example: (1) the synthesis of tetramethylammonium tribromide, it is in ethanol, by the reaction of tetramethylammonium bromide and elemental bromine; (2) tetraethyl tribromide The ...

Claims

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Application Information

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IPC IPC(8): C25B3/00
Inventor 成旦红陈欢曹铁华胡佩瑜洪亮铭
Owner SHANGHAI UNIV
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