Preparation method of hydrochloric acid aureomycin

A technique of chlortetracycline hydrochloride and chlortetracycline, which is applied in the field of preparation of chlortetracycline hydrochloride, can solve problems such as soil pollution, poor working environment, and increased production costs, so as to improve extraction yield, enhance competitiveness, and reduce production costs. low effect

Active Publication Date: 2015-07-15
宁夏泰瑞制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004]1 In the patent "Preparation Method of Chlortetracycline Hydrochloride", plate and frame are used as filter equipment in the fermentation broth filtration process. In order to ensure the filtration yield, a large amount of clear water is required Wash the filter cake in the plate frame repeatedly to reduce the aureomycin remaining in the filter cake as much as possible, so the wastewater discharge is basically more than twice the volume of the fermentation broth, resulting in high wastewater treatment costs for enterprises and increased product production costs; At the same time, due to the use of plate and frame filter press, it occupies a large area, requires a lot of labor for cleaning, and the working environment is poor.
In the [0005]2 patent "Preparation Method of Chlortetracycline Hydrochloride", a large amount of ZnSO4 and Oxalic acid, and in the patent "A New Process for Preparing Chlortetracycline Hydrochloride", a large amount of divalent metal salts and monohydric alcohols are used in the chlortetracycline filtrate. The use of the above substances has led to a continuous increase in the production cost of chlortetracycline
[0006]3 The above two patented technologies use a large amount of divalent metal salts in the extraction process of chlortetracycline. Due to metal pollution, the filter cake and filtrate cannot be recovered. use, causing serious pollution to the local soil
[0007]4 In the above two patented technologies, during the alkalization process of aureomycin filtrate, it is difficult to avoid the phenomenon that the local concentration is too high, leading to its degradation
[0008]5 The patented technology "A New Process for Preparation of Chlortetracycline Hydrochloride" has the problem of unqualified finished product quality, mainly because the impurity content of the finished product exceeds the standard
[0009]6 Among the above two patented technologies, the extraction yield of chlortetracycline is generally 75-80%, which is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] preprocessing

[0036] Chlortetracycline fermentation broth 50m 3 , The initial titer was 26307u / ml.

[0037] First, acidify the aureomycin fermented liquid, adjust the pH to 0.5 with 15% hydrochloric acid solution, and then adjust the pH to 2 and 4 respectively with 15% sodium hydroxide solution; let it stand for 20 minutes, and finally add drinking water to the fermented liquid The viscosity will be 3847cps.

[0038] membrane filtration

[0039] After the pretreatment of the fermentation broth is completed, the filtrate is heated to 61°C and enters the membrane filtration equipment, using an inorganic metal microporous microfiltration membrane made of zirconium dioxide, and the supporting material of the membrane filtration system is 316SS stainless steel. The filtration method adopts a high-speed cross-flow method, and the membrane pore size is 0.1um. During the filtration process, the pressure is controlled at 2.5-3.5bar, and the flow rate is controlled at 0.3-0...

Embodiment 2

[0053] preprocessing

[0054] Aureomycin fermentation 50m 3 , the initial titer was 25861u / ml.

[0055] At first aureomycin fermented liquid is carried out acidification, and 16% sulfuric acid solution adjusts pH to 0.7, secondly, adopts 16% ammoniacal solution to be adjusted to pH to 2.2 and 4.1 respectively; Leave standstill 23min, add drinking water at last, fermented liquid viscosity will to 3643 cps.

[0056] membrane filtration

[0057]After the pretreatment of the fermentation broth is completed, the filtrate is heated to 63°C and enters the membrane filtration equipment, using an inorganic metal microporous microfiltration membrane made of zirconium dioxide, and the supporting material of the membrane filtration system is 316SS stainless steel. The filtration method adopts a high-speed cross-flow method, and the membrane pore size is 0.2um. During the filtration process, the pressure is controlled at 2.5-3.5bar, and the flow rate is controlled at 0.3-0.5m 3 / m 2 ...

Embodiment 3

[0071] preprocessing

[0072] Aureomycin fermentation 50m 3 , initial titer 26024u / ml.

[0073] First, acidify the aureomycin fermentation liquid, adjust the pH to 1.1 with 17% phosphoric acid solution, and then adjust the pH to 2.3 and 4.3 respectively with 18% sodium hydroxide solution; let it stand for 25 minutes, and finally add drinking water to the fermentation liquid The viscosity will be 3587cps.

[0074] membrane filtration

[0075] After the pretreatment of the fermentation broth is completed, the filtrate is heated to 65°C and enters the membrane filtration equipment, using an inorganic metal microporous microfiltration membrane made of zirconium dioxide, and the supporting material of the membrane filtration system is 316SS stainless steel. The filtration method adopts a high-speed cross-flow method, and the membrane pore size is 0.3um. During the filtration process, the pressure is controlled at 2.5-3.5bar, and the flow rate is controlled at 0.3-0.5m 3 / m 2 ...

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PUM

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Abstract

The invention relates to a preparation method of hydrochloric acid aureomycin; the technical steps are listed below: firstly acidifying aureomycin broth; adjusting pH to 2-2.5; standing; continuously adjusting pH to 4-4.5; standing; adding water to reduce viscosity to 3000-4000cps pretreatment; carrying out membrane filtration, nanofiltration, crystallization, washing, salt forming, leaching and drying to obtain hydrochloric acid aureomycin powders. The method can improve extraction yield of the hydrochloric acid aureomycin, reduces production cycle and cost, and improves hydrochloric acid aureomycin output.

Description

technical field [0001] The invention belongs to the technical field of antibiotic extraction and synthesis, in particular to a preparation method of aureomycin hydrochloride. Background technique [0002] Chlortetracycline hydrochloride is a tetracyclic antibiotic with broad-spectrum antibacterial activity. Its antibacterial spectrum is similar to tetracycline, and it has antibacterial activity against most Gram-positive bacteria and Gram-negative bacteria. In addition, they inhibit Rickettsiae and trachoma and lymphogranuloma viruses. [0003] At present, domestically disclosed methods for producing aureomycin hydrochloride mainly include: "Preparation Method of Aureomycin Hydrochloride" with application number 201210426529.0 and "A New Process for Preparation of Aureomycin Hydrochloride" with application number 201010218988.0. There are following problems in above-mentioned patent: [0004] 1 In the patent "Preparation Method of Chlortetracycline Hydrochloride", the plat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C237/26C07C231/24
Inventor 任勇王义
Owner 宁夏泰瑞制药股份有限公司
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