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Preparation method of tetramethylammonium bromide

A technology of tetramethyl ammonium bromide and methyl bromide is applied in the field of organic compound preparation, can solve the problem of low product yield and the like, and achieves the effects of improving product yield and improving economic and social benefits

Inactive Publication Date: 2011-04-20
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the yield of the synthesized product is not high without increasing advanced equipment and increasing the technical requirements of operators

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) synthetic reaction of tetramethylammonium bromide

[0018] In a 1000 milliliter reactor with heating device, electric stirring, thermometer, water circulation condenser, drop into 200 grams of methyl bromide, 200 grams of solvent ethanol, stir and slowly pass into 400 grams of trimethylamine, to no precipitation, reaction termination;

[0019] (2) filter

[0020] The mixture obtained after the reaction was filtered under reduced pressure, and the obtained pale yellow solid was crude tetramethylammonium bromide;

[0021] (3) refined

[0022] Add 150 grams of ethyl acetate to the crude product of tetramethylammonium bromide, heat to reflux and keep warm for 0.5 hours, then cool and crystallize, filter, and decompress the product at 50°C, keep the vacuum at 30-35mmHg, remove the remaining ethyl acetate, the resulting white crystals are tetramethylammonium bromide finished product.

Embodiment 2

[0024] (1) synthetic reaction of tetramethylammonium bromide

[0025] In a 1000 ml reactor with heating device, electric stirring, thermometer and water circulation condenser, drop 200 grams of methyl bromide and 250 grams of ethanol as solvent, stir and slowly feed 400 grams of trimethylamine until no precipitation occurs , the reaction terminates;

[0026] (2) filter

[0027] The mixture obtained after the reaction was filtered under reduced pressure, and the obtained pale yellow solid was crude tetramethylammonium bromide;

[0028] (3) refined

[0029] Add 150 grams of ethyl acetate to the crude product of tetramethylammonium bromide, heat to reflux and keep warm for 0.5 hours, then cool and crystallize, filter, and decompress the product at 50°C, keep the vacuum at 30-35mmHg, remove the remaining ethyl acetate, the resulting white crystals are tetramethylammonium bromide finished product.

Embodiment 3

[0031] (1) synthetic reaction of tetramethylammonium bromide

[0032] In a 1000 ml reactor with heating device, electric stirring, thermometer and water circulation condenser, drop 200 grams of methyl bromide and 300 grams of ethanol as solvent, stir and slowly feed 400 grams of trimethylamine until no precipitation occurs , the reaction terminates;

[0033] (2) filter

[0034] The mixture obtained after the reaction was filtered under reduced pressure, and the obtained pale yellow solid was crude tetramethylammonium bromide;

[0035] (3) refined

[0036] Add 150 grams of ethyl acetate to the crude product of tetramethylammonium bromide, heat to reflux and keep warm for 0.5 hours, then cool and crystallize, filter, and decompress the product at 50°C, keep the vacuum at 30-35mmHg, remove the remaining ethyl acetate, the resulting white crystals are tetramethylammonium bromide finished product.

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PUM

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Abstract

The invention relates to a preparation method of tetramethylammonium bromide. The preparation method is characterized by comprising the following steps of: (1) performing a synthetic reaction on the tetramethylammonium bromide; (2) filtering; and (3) refining. The preparation method increases product yield, meets the market demand and enhances the economic and social benefits of an enterprise.

Description

technical field [0001] The invention relates to the field of preparation methods of organic compounds, in particular to a preparation method of tetramethylammonium bromide. Background technique [0002] Tetramethylammonium bromide is a common chemical product in the market. It is an ion pairing reagent, a polarographic analysis reagent, and an effective phase transfer catalyst. At present, the yield of the synthesized product is not high without increasing the advanced equipment and increasing the technical requirements of the operators. Contents of the invention [0003] The object of the invention is to overcome the deficiencies in the prior art, and a kind of preparation method of tetramethylammonium bromide is provided. [0004] In order to achieve the above object, the present invention adopts the following technical solutions: [0005] (1) synthetic reaction of tetramethylammonium bromide [0006] Add methyl bromide to the solvent ethanol, the ratio of methyl brom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/63C07C209/12
Inventor 徐博刚
Owner TIANJIN CHEM REAGENT RES INST
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