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Synthesis method of benzethonium chloride

A synthesis method and technology of benzethonium chloride, applied in the field of chemistry, can solve problems such as hidden dangers of large production safety, and achieve the effects of good purity and high yield

Pending Publication Date: 2022-02-11
扬州虹光生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ammonolysis reaction is required in this process route, which can only be carried out under high temperature and high pressure conditions, and there is a large production safety hazard

Method used

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  • Synthesis method of benzethonium chloride
  • Synthesis method of benzethonium chloride

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preparation example Construction

[0015] A kind of synthetic method of benzethonium chloride, this synthetic method comprises the steps:

[0016] (1) According to the mass ratio of 52% sodium hydroxide solution, dichloroethyl ether, phase transfer catalyst, and octylphenol, the mass ratio is 90:80:0.6~0.8:30, and the material is taken, and the mass fraction is 52 % sodium hydroxide solution, dichloroethyl ether, phase transfer catalyst, and octylphenol are put into the reactor, stirred, heated up, and kept warm to react to obtain Compound A; the phase transfer catalyst is benzyltriethylammonium chloride;

[0017] (2) According to the mass ratio of compound A, benzyldimethylamine and water of 45:20:30~35, take the material, stir compound A, benzyldimethylamine and water evenly, protect with nitrogen, heat up, and react , cooling, that is, benzethonium chloride.

Embodiment 1

[0019] A kind of synthetic method of benzethonium chloride, this synthetic method comprises the steps:

[0020] (1) Put 900kg of sodium hydroxide solution with a mass fraction of 52% into the reaction kettle, add 800kg of dichloroethyl ether, 6kg of phase transfer catalyst, 300kg of octylphenol, start stirring, slowly raise the temperature to reflux, and keep it warm for 3 hours , TLC tracking and detection of the reaction process, until the end of the reaction, add water to the reaction kettle, wash and separate the layers, separate the organic layer, wash with water once, and recover the solvent under reduced pressure in the organic phase. After the solvent recovery is completed, change to distillation under reduced pressure to obtain 513kg of Compound A, with a purity of 97.8%;

[0021] (2) Put 450kg of compound A, 200kg of benzyldimethylamine and 300kg of water into the reactor, start stirring, replace with nitrogen, protect with nitrogen, heat up to 115°C, continue to rea...

Embodiment 2

[0024] A kind of synthetic method of benzethonium chloride, this synthetic method comprises the steps:

[0025] (1) Put 900kg of sodium hydroxide solution with a mass fraction of 52% into the reactor, add 800kg of dichloroethyl ether, 7kg of phase transfer catalyst, 300kg of octylphenol, start stirring, slowly raise the temperature to reflux, and keep it warm for 3 hours , TLC tracking and detection of the reaction process, until the end of the reaction, add water to the reaction kettle, wash and separate the layers, separate the organic layer, wash with water once, and recover the solvent under reduced pressure in the organic phase. After the solvent recovery is completed, change to distillation under reduced pressure to obtain 546kg compound A, purity 98.8%;

[0026] (2) Put 450kg of compound A, 200kg of benzyldimethylamine and 330kg of water into the reactor, start stirring, replace with nitrogen, protect with nitrogen, heat up to 115°C, continue to react for 7h, cool down,...

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Abstract

The invention belongs to the technical field of chemistry, and particularly relates to a synthetic method of benzethonium chloride. According to the method, dichloroethyl ether, octyl phenol and the like are used as raw materials, synthesis is performed through two steps, meanwhile, in the synthesis process, compared with the prior art, lower temperature is kept, high pressure is not used in the synthesis process, the yield in the synthesis process is higher, and the product has better purity.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and in particular relates to a synthetic method of benzethonium chloride. Background technique [0002] Benzethonium chloride is a new type of cationic surfactant, which is easily soluble in water to form a foamy soapy water solution, and has been widely used as a daily chemical additive. Benzethonium chloride also has good bactericidal and antiseptic effects. As a new generation of detergents, bactericides, and preservatives, it has been widely used in the field of medicine. [0003] The current production of benzethonium chloride is mainly to synthesize benzethonium chloride from p-tertyl phenol, dichlorodiethyl ether, dimethylamine and benzyl chloride. Ammonolysis reaction needs to be carried out in this technological route, and this reaction can only be carried out under the condition of high temperature and high pressure, and there is a big hidden danger of production safety. Contents o...

Claims

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Application Information

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IPC IPC(8): C07C213/08C07C213/02C07C217/08
CPCC07C213/08C07C213/02C07C41/16C07C217/08C07C43/225
Inventor 陈健龙刘超戴红升
Owner 扬州虹光生物科技有限公司
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