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Preparation method of alkyl trimethylammonium calcium oxytetracycline

A technology of alkyl trimethyl ammonium and calcitetracycline is applied in the preparation of amino compounds, the preparation of organic compounds, the preparation of carboxylic acid amides, etc., to achieve the effects of good fluidity, mild conditions and uniform particles

Active Publication Date: 2015-04-08
HEBEI SHENGXUE DACHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Oxytetracycline quaternary ammonium salt mainly exists in the form of alkyltrimethylammonium calcotetracycline, and its production and preparation methods have not been reported yet

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 60 g of oxytetracycline and disperse it in 500 mL of deionized water, then add concentrated sulfuric acid with a mass ratio concentration of 98% while stirring, slowly adjust the pH of the oxytetracycline solution to 1.2, and react at a temperature of 25 °C for 1 h Finally, stir until the oxytetracycline is completely dissolved, then add 18 g of calcium carbonate powder to the oxytetracycline solution, stir, and react at a temperature of 25°C for 3 h to obtain the reaction solution I, and then add twelve Alkyltrimethylammonium chloride 18 g, stirred, and reacted at a temperature of 25°C for 3 h to obtain reaction solution II, and then added a sodium hydroxide solution with a mass ratio concentration of 30% to the reaction solution II, and slowly adjusted The pH of the reaction solution II is 7.8, react at a temperature of 25°C for 2 hours to obtain the reaction solution III, and spray the reaction solution III with a spray drying tower, the inlet air temperature of...

Embodiment 2

[0025] Weigh 100 g of oxytetracycline, disperse it in 500 mL of deionized water, then add concentrated sulfuric acid with a mass ratio concentration of 98% while stirring, slowly adjust the pH of the oxytetracycline solution to 2.0, and react at a temperature of 28 °C for 1 After h, stir until the oxytetracycline is completely dissolved, then add 60 g of calcium carbonate powder to the oxytetracycline solution, stir, and maintain the reaction at a temperature of 28°C for 10 h to obtain the reaction solution I, and then add 60 g of octadecyltrimethylammonium chloride, stirring, and maintaining the reaction at a temperature of 28 °C for 20 h to obtain reaction solution II, and then adding a sodium hydroxide solution with a mass ratio concentration of 30% to the reaction solution II , slowly adjust the pH of the reaction solution II to 10.5, and react at a temperature of 20°C for 2 hours to obtain the reaction solution III, and spray the reaction solution III with a spray drying t...

Embodiment 3

[0027] Weigh 25 g of oxytetracycline, disperse it in 500 mL of deionized water, then add concentrated sulfuric acid with a mass ratio concentration of 98% while stirring, slowly adjust the pH of the oxytetracycline solution to 0.5, and react at a temperature of 20 °C for 1 After h, stir until the oxytetracycline is completely dissolved, then add 2.5 g of calcium carbonate powder to the oxytetracycline solution, stir, and maintain the reaction at a temperature of 20°C for 30 min to obtain the reaction solution I, and then add to the reaction solution I 2.5 g of octadecyltrimethylammonium chloride, stirred, and maintained at a temperature of 20°C for 30 minutes to obtain reaction solution II, and then added a sodium hydroxide solution with a mass ratio concentration of 30% to the reaction solution II , slowly adjust the pH of the reaction solution II to 7.0, and react at a temperature of 20°C for 1 h to obtain the reaction solution III, and spray the reaction solution III with a ...

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Abstract

The invention discloses a preparation method of alkyl trimethylammonium calcium oxytetracycline. The preparation method of the alkyl trimethylammonium calcium oxytetracycline comprises the following steps: (a), with water as a solvent, preparing an oxytetracycline solution, and regulating the pH value of the oxytetracycline solution with sulfuric acid; (b), adding calcium carbonate into the oxytetracycline solution, stirring, and reacting for 0.5-10h to obtain a reaction solution I; (c), adding a quaternary ammonium salt-type cationic surfactant into the reaction solution I, stirring, and reacting 0.5-20h to obtain a reaction solution II; (d), adding a sodium hydroxide solution into the reaction solution II to regulate the pH value, and standing to obtain a reaction solution III; and (e), performing spray drying on the reaction solution III to obtain an alkyl trimethylammonium calcium oxytetracycline granular preparation. The preparation method is simple in process and easy to operate; the prepared granular product is high in content, convenient to use and stable in quality and can be widely added into feed for young pigs, chickens and cattle, adult chickens and the like as an antibiotic feed additive so as to promote the growth and prevent and treat diseases.

Description

technical field [0001] The invention relates to a preparation method of a feed additive of oxytetracycline quaternary ammonium salt, in particular to a preparation method of alkyltrimethylammonium calcoxytetracycline. Background technique [0002] Oxytetracycline (Oxytetracycline) is a kind of tetracycline antibiotics. It has antibacterial effect on most Gram-positive bacteria, negative bacteria, cocci and bacilli, and also has inhibitory effect on Rickettsia and amoeba pathogens. It is widely added to young children. Antibiotic feed additives in the feed of older pigs, chickens, cattle and adult chickens to promote growth and prevent diseases. There are two main formulations of oxytetracycline as a feed additive, namely oxytetracycline hydrochloride and oxytetracycline quaternary ammonium salt. Among them, oxytetracycline quaternary ammonium salt has more advantages than oxytetracycline hydrochloride in terms of use method and drug resistance. Therefore, it has higher and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C237/26C07C231/12C07C211/63C07C209/00
Inventor 谷新华孟繁珠宋志倩常国栋刘磊
Owner HEBEI SHENGXUE DACHENG PHARMA