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A kind of synthesis process of benzalkonium chloride monomer

A technology of benzalkonium chloride and a synthesis process, which is applied in the field of benzalkonium chloride monomer synthesis technology, can solve the problems of increasing the cost of benzalkonium chloride pharmaceutical products, being difficult to apply to the medical field, and having complicated production methods and processes, and achieves alleviation The effect of shortage of raw material resources, enrichment of production methods, and avoidance of raw material loss

Active Publication Date: 2019-03-01
广东洛斯特制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis of benzalkonium chloride mostly uses dodecyl alcohol to synthesize dodecyl bromide, then reacts with dimethylamine to obtain dimethyl dodecylamine hydrogen bromide, and finally reacts with benzyl chloride to obtain benzalkonium chloride , most of the obtained benzalkonium chloride is industrial grade, which is difficult to apply in the field of medicine
Before the preparation of pharmaceutical-grade benzalkonium chloride, alkyldimethylamine and benzyl chloride must be refined. This production method is complicated and requires high equipment requirements. Many pharmaceutical benzalkonium chloride production companies cannot prepare benzalkonium chloride. Ammonium chloride, which increases the cost of benzalkonium chloride pharmaceutical products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of benzalkonium chloride monomer synthesis technique, comprises the steps:

[0025] (1) Measure dodecyldimethyl tertiary amine, benzyl chloride and ethyl acetate respectively according to the formula, and the molar mass ratio of said dodecyldimethyl tertiary amine and benzyl chloride is 1:1;

[0026] (2) Put ethyl acetate into a 300L glass-lined reaction kettle, pump dodecyldimethyl tertiary amine and benzyl chloride into the head tank respectively, turn on the stirring device of the reaction kettle, and Methyl tertiary amine and benzyl chloride are dropped into the reactor in the same proportion;

[0027] (3) Turn on the heating device, raise the temperature of the reactor to 85°C, and keep it warm for 10 hours;

[0028] (4) Turn on the circulating cooling water and cool the product to room temperature until the crystals are completely precipitated;

[0029] (5) Take out the precipitated crystals, filter under reduced pressure, wash the crystals with ethyl ace...

Embodiment 2

[0032] A kind of benzalkonium chloride monomer synthesis technique, comprises the steps:

[0033] (1) Measure tetradecyl dimethyl tertiary amine, benzyl chloride and ethyl acetate respectively according to the formula, and the molar mass ratio of the fatty alkyl dimethyl tertiary amine and benzyl chloride is 1:1.2;

[0034] (2) Put ethyl acetate into a 300L glass-lined reaction kettle, pump tetradecyl dimethyl tertiary amine and benzyl chloride into the head tank respectively, turn on the stirring device of the reaction kettle, and mix tetradecyl di Methyl tertiary amine and benzyl chloride are dropped into the reactor in the same proportion;

[0035] (3) Turn on the heating device, raise the temperature of the reactor to 95°C, and keep it warm for 10 hours;

[0036] (4) Turn on the circulating cooling water and cool the product to room temperature until the crystals are completely precipitated;

[0037] (5) Take out the precipitated crystals, filter under reduced pressure, ...

Embodiment 3

[0040] A kind of benzalkonium chloride monomer synthesis technique, comprises the steps:

[0041] (1) Measure cetyl dimethyl tertiary amine, benzyl chloride and ethyl acetate respectively according to the formula, and the molar mass ratio of cetyl dimethyl tertiary amine and benzyl chloride is 1:1.3;

[0042] (2) Put ethyl acetate into a 300L glass-lined reactor, pump cetyl dimethyl tertiary amine and benzyl chloride into the head tank respectively, turn on the stirring device of the reactor, Methyl tertiary amine and benzyl chloride are dropped into the reactor in the same proportion;

[0043] (3) Turn on the heating device, raise the temperature of the reactor to 95°C, and keep it warm for 9 hours;

[0044] (4) Turn on the circulating cooling water and cool the product to room temperature until the crystals are completely precipitated;

[0045] (5) Take out the precipitated crystals, filter under reduced pressure, wash the crystals with ethyl acetate 4 times during the suc...

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Abstract

The invention relates to the technical field of fine chemicals, and more specifically relates to a benzalkonium chloride monomer synthesis technology. The synthesis technology comprises the following steps: (1) according to a formula, weighing fatty alkyl dimethyl tertiary amines, benzyl chloride, and ethyl acetate; (2) adding ethyl acetate into a glass lined reactor, pumping fatty alkyl dimethyl tertiary amines and benzyl chloride into a head tank, starting the stirring device of the reactor, dropwise adding fatty alkyl dimethyl tertiary amines and benzyl chloride into the reactor at a room temperature according to a same ratio; (3) heating the reactor to a temperature of 70 to 100 DEG C, and maintaining the temperature to carry out reactions for 7 to 10 hours; (4) starting circulating cooling water to cool the products to the room temperature until crystals are precipitated completely; (5) taking out the crystals, subjecting the crystals to vacuum suction filtration, during the suction filtration process, washing the crystals by ethyl acetate for 2 to 5 times, and saving the filter cakes; and (6) adding ethyl acetate into the filter cakes, carrying out re-crystallization, and after the crystals are completely precipitated, drying the crystals. The production cost is low and the purity of prepared benzalkonium chloride is high.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, more specifically, the invention relates to a synthesis process of benzalkonium chloride monomer. Background technique [0002] Benzalkonium chloride is a cationic surfactant, also known as geeramine, which has broad-spectrum and high-efficiency bactericidal and algae killing capabilities, can effectively control the growth of bacteria and algae in water and the growth of slime, and has a good slime stripping effect It has a certain dispersion and penetration effect, and also has a certain degreasing, deodorizing ability and corrosion inhibition effect. It is often used as a fungicide in the medical field. [0003] At present, the synthesis of benzalkonium chloride mostly uses dodecyl alcohol to synthesize dodecyl bromide, then reacts with dimethylamine to obtain dimethyl dodecylamine hydrogen bromide, and finally reacts with benzyl chloride to obtain benzalkonium chloride , most of the o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/63C07C209/12C07C209/82
CPCC07C209/12C07C209/82C07C211/63
Inventor 吴琏
Owner 广东洛斯特制药有限公司
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