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Novel technique for synthesizing quaternary ammonium salt

A synthesis process and quaternary ammonium salt technology, which is applied in the field of direct reaction of carbonic acid diester and amine salt to prepare quaternary ammonium salt under the condition of no catalyst, can solve the problems that the catalyst cannot be reused and the product is impure, and achieve high product purity , The effect of low process cost

Inactive Publication Date: 2008-08-20
安徽奔马先端科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is aimed at the deficiencies that the carbonic acid ester (fat) and amine salt announced by the document (patent No. 200510061094.4) must be reacted under the action of a catalyst to synthesize the quaternary ammonium salt. The reaction is carried out, and the yield of products such as halide quaternary ammonium salt and sulfate quaternary ammonium salt reaches more than 99%, which eliminates the problems of product impurity and catalyst that cannot be reused due to the difficulty in separating the catalyst from the product in the original process

Method used

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  • Novel technique for synthesizing quaternary ammonium salt
  • Novel technique for synthesizing quaternary ammonium salt
  • Novel technique for synthesizing quaternary ammonium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Weigh 927g of dodecylamine and place it in a beaker, add concentrated hydrochloric acid dropwise (the total amount of HCl added is about 180g), stir magnetically, remove about 80% of the water by evaporation in a constant temperature water bath after the neutralization reaction is completed, and then vacuum dry to obtain Product lauryl ammonium chloride; Take by weighing 1109g lauryl ammonium chloride and 455g dimethyl carbonate respectively, join in the 10L autoclave successively, after blowing away the air in the still with nitrogen, airtight reaction, The reaction temperature was 170°C, and stirring was started after the reaction temperature reached 170°C, and the reaction time was 8 hours; after the reaction, about 1308g of dodecyltrimethylammonium chloride was obtained.

Embodiment 2

[0018] Take by weighing 927g dodecylamine and place it in a beaker, add aqueous hydrogen bromide solution (about 405g of HBr adding total amount) drop by drop, magnetically stir, remove about 80% water with constant temperature water bath evaporation after neutralization reaction finishes, then vacuum Dry to obtain the product dodecyl ammonium bromide; weigh 1331g of dodecyl ammonium bromide and 455g of dimethyl carbonate respectively, add them to a 10L autoclave in turn, blow away the air in the autoclave with nitrogen, and seal the Reaction, the reaction temperature is 170°C, stirring is started after the reaction temperature reaches 150°C, and the reaction time is 4 hours; after the reaction is completed, about 1540g of dodecyltrimethylammonium bromide can be obtained.

Embodiment 3

[0020] Take by weighing 1000g dodecyl dimethylamine and place it in a beaker, add concentrated hydrochloric acid (HCl adds about 171g total amount) dropwise, magnetically stir, remove about 80% water with constant temperature water bath evaporation after neutralization reaction finishes, then Vacuum-dried to obtain the product dodecyldimethylammonium chloride; Weigh 1000g of dodecyldimethylammonium chloride and 365g of dimethyl carbonate respectively, add them to a 10L reaction kettle in turn, and blow them away with nitrogen After the air in the still, airtight reaction, reaction temperature 170 ℃, start to stir after reaction temperature reaches 160 ℃, reaction time 8 hours; after reaction finishes, make about 1050g of dodecyltrimethylammonium chloride.

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Abstract

The invention relates to a technique method for preparing quaternary ammonium salt through a reaction of carbonate and ammonium salt without any catalyst; aiming at the shortcoming showed in the former documents (the application number is 200510061094.4) that catalyst is used in the synthesis reaction of the carbonate and the ammonium salt, through improving the technique, the method makes the reaction possible in the condition of no catalyst, which also leads the yield of products of halide quaternary ammonium and sulfuric quaternary ammonium salt to be equal or more than 99 percent so as to avoid the problems such as the impurity of products caused by the difficult separation of catalyst and products and the catalyst which can not be used repeatedly; the technique process of the method is as following, amine is in a neutralization reaction with acid or the solution of acid, when an end point is reached, absolute ammonium salt is obtained after water elimination and drying, then certain amount of carbonate and ammonium salt are separately weighted and put in to a reaction kettle which is then sealed, the carbonate and ammonium salt are in reaction with agitation, the reaction temperature is between 50 to 300 DEG C and the reaction time is between 0.5 to 20 hours.

Description

technical field [0001] The invention relates to a new process for synthesizing quaternary ammonium salts, in particular to a process for preparing quaternary ammonium salts through the direct reaction of carbonic acid diester (fat) and amine salts under the condition of no catalyst. Background technique [0002] Quaternary ammonium salts are a class of cationic surfactants, in which quaternary ammonium halides (R 1 R 2 R 3 R 4 N + x - ) series of compounds are widely used in various fields such as daily chemical industry, textile, printing and dyeing, mining, asphalt, construction, plastic processing, oil exploration, petrochemical industry, etc., and have played an important role. [0003] People have carried out a large amount of research and development to the production technology of quaternary ammonium salt, and the number of quaternary ammonium salt preparation technology disclosed by the Chinese patent literature is numerous, and wherein the patent No. is 2005100...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/00C07C209/68C07D233/10
Inventor 郑卓群周小平
Owner 安徽奔马先端科技有限公司
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