Preparation method for tetrapropyl ammonium bromide

A technology of tetrapropyl ammonium bromide and bromopropane, which is applied in the field of organic compound preparation, can solve the problem of low product yield and the like, and achieve 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 increas

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0016] Example one:

[0017] (1) Synthesis of tetrapropylammonium bromide

[0018] Into a 1000 ml reactor with heating device, electric stirring, thermometer and water circulation condenser, put 200 g of tri-n-propylamine, 100 g of bromopropane, 600 g of solvent methyl ethyl ketone, stir and heat to slow reflux, constant temperature reaction 22-24 hours;

[0019] (2) Obtain crude tetrapropylammonium bromide

[0020] The mixture obtained after the reaction was distilled at normal pressure to recover methyl ethyl ketone and excess bromopropane, heated to 100°C, and removed the remaining methyl ethyl ketone and bromopropane under reduced pressure. The resulting light yellow transparent liquid was crude tetrapropylammonium bromide ;

[0021] (3) Refined

[0022] Add 150 grams of ethyl acetate to the crude tetrapropylammonium bromide, heat to reflux and keep for 0.5 hours, then cool to crystallize, filter, and depressurize the product at 50°C, and keep the vacuum at a 30-35mmHg column to re...

Example Embodiment

[0023] Embodiment two:

[0024] (1) Synthesis reaction of tetrapropylammonium bromide

[0025] Into a 1000 ml reactor with heating device, electric stirring, thermometer and water circulation condenser, put 200 g of tri-n-propylamine, 100 g of bromopropane, 700 g of solvent methyl ethyl ketone, stir and heat to slow reflux, constant temperature reaction 22-24 hours;

[0026] (2) Obtain crude tetrapropylammonium bromide

[0027] The mixture obtained after the reaction is distilled under normal pressure to recover methyl ethyl ketone and excess bromopropane, heat to 100°C, and remove the remaining methyl ethyl ketone and bromopropane under reduced pressure. The obtained light yellow transparent liquid is crude tetrapropylammonium bromide ;

[0028] (3) Refined

[0029] Add 150 grams of ethyl acetate to the crude tetrapropylammonium bromide, heat to reflux and keep for 0.5 hours, then cool to crystallize, filter, and depressurize the product at 50°C, and keep the vacuum at 30-35mmHg colum...

Example Embodiment

[0030] Embodiment three:

[0031] (1) Synthesis of tetrapropylammonium bromide

[0032] Into a 1000 ml reactor with heating device, electric stirring, thermometer, and water circulation condenser, put 200 g of tri-n-propylamine, 100 g of bromopropane, 800 g of solvent methyl ethyl ketone, stir and heat to slow reflux, constant temperature reaction 22-24 hours;

[0033] (2) Obtain crude tetrapropylammonium bromide

[0034] The mixture obtained after the reaction was distilled at normal pressure to recover methyl ethyl ketone and excess bromopropane, heated to 100°C, and removed the remaining methyl ethyl ketone and bromopropane under reduced pressure. The resulting light yellow transparent liquid was crude tetrapropylammonium bromide ;

[0035] (3) Refined

[0036] Add 150 grams of ethyl acetate to the crude tetrapropylammonium bromide, heat to reflux and keep for 0.5 hours, then cool to crystallize, filter, and depressurize the product at 50°C, and keep the vacuum at 30-35mmHg column t...

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PUM

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Abstract

The present invention relates to a preparation method for tetrapropyl ammonium bromide, which is characterized by (1) the synthesis reaction of tetrapropyl ammonium bromide, (2) the preparation of the crude product of tetrapropyl ammonium bromide, and (3) purification. The present invention improves the product yield, meets the needs of the market, and increases the economic benefits and the social benefits of enterprises.

Description

technical field [0001] The invention relates to the field of preparation methods of organic compounds, in particular to a preparation method of tetrapropylammonium bromide. Background technique [0002] Tetrapropylammonium bromide is a common chemical product on the market. It is an ion-pairing reagent and is used in the preparation of catalysts in the petrochemical industry. It is also an effective cationic 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 tetrapropyl ammonium bromide is provided. [0004] In order to achieve the above object, the present invention adopts the following technical solutions: [0005] (1) synthetic reaction of tetrapropylammonium bromide [0006] Mix tri-n-...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/12
Inventor 徐博刚
Owner TIANJIN CHEM REAGENT RES INST
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