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Recovery method of demeclocy cline hydrochloride crystal mother liquor

A technology of chlortetracycline hydrochloride and crystallization mother liquor, applied in the separation/purification of carboxylic acid amides, organic chemistry, etc., can solve the problems of low extraction rate, fast decay of multi-stage extraction partition coefficient, and difficulty in realizing industrialization, etc. Achieve the effect of avoiding waste, saving production costs and reducing environmental pollution

Inactive Publication Date: 2005-11-09
NORTH CHINA PHARMA GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the low extraction rate of this method and the fast decay of the multi-stage extraction partition coefficient, it is difficult to realize industrialization; about 150M tetracycline is produced per ton of tetracycline 3 Crystallization mother liquor, the residual tetracycline potency is about 750u / ml, and its crystallization mother liquor is recovered by magnesium salt precipitation method
In actual production, these recovery methods cannot be used for the recovery of demeclocycline hydrochloride crystallization mother liquor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] When demeclotetracycline hydrochloride is produced, a demeclotetracycline hydrochloride crystallization mother liquor is obtained, and the potency unit of demeclotetracycline in the mother liquor is 4000-6000u / ml. Naturally settle the crystallization mother liquor below 20°C for 8 hours, separate the clear liquid, adjust the pH to 7.0-9.5 with ammonia water, add 5% perlite, stir evenly, filter, and dissolve the filter cake with 0.3% oxalic acid solution, continue Add excess oxalic acid to make the pH of the solution 1.0-3.0, add a scavenger (0.3% zinc sulfate), stir and stand still, filter, dilute the filtrate with purified water until the titer unit of demeclocycline is 1500u / ml, and use ammonia water Adjust the pH to 7.0-10.0, add 8-11% (v / v) butanol: butyl acetate mixed solution (butanol and butyl acetate in the mixed solution are formulated at a weight ratio of 5:95) and stir Homogenize, extract, and the titer unit of demeclocycline in the extract is 13000-18000u / ml...

Embodiment 2

[0025] When producing demeclotetracycline hydrochloride, obtain demeclotetracycline hydrochloride crystallization mother liquor, the total potency unit of crystallization mother liquor is 5184u / ml, the crystallization mother liquor is naturally settled at 18 ℃ for 5 hours, separates its supernatant liquid, 20% carbonic acid Adjust the pH of the sodium solution to 8.5, add 2% diatomaceous earth, stir evenly, filter, dissolve the filter cake with 3% (w / v) oxalic acid solution, continue to add excess oxalic acid to make the solution pH 2, add demethyl gold Mycelia wet mycelium into 30% (w / v) of 0.3% potassium ferricyanide and 0.3% zinc sulfate, stirred and left standstill, filtered, and the filtrate was diluted with purified water to make the titer unit of aureomycin to 1500u / ml, adjust the pH to 9.5 with 20% sodium carbonate solution, add 10% (v / v) butanol; the weight ratio of butyl acetate is (15:85) and mix well, add 10% chlorodeca Trialkyl trimethane aqueous solution until th...

Embodiment 3

[0027] When producing demeclotetracycline hydrochloride, obtain demeclotetracycline hydrochloride crystallization mother liquor, record the total potency unit of crystallization mother liquor to be 4636u / ml, the crystallization mother liquor is naturally settled at 18 ℃ for 3 hours, separate its supernatant liquid, use Ammonia solution to adjust the pH to 9.5, add 5% perlite, stir evenly, filter, dissolve the filter cake with 3% (w / v) oxalic acid solution, continue to add excess oxalic acid to make the solution pH 3, add 0.4% iron Potassium chloride, stir and leave standstill, filter, the titer unit of filtrate diluted to demeclotetracycline with purified water is 1300u / ml, ammonia solution is adjusted pH8.5, adds the butanol of 10% (v / v): acetic acid Mix butyl ester (15:85), add 10% cetylpyridinium chloride aqueous solution until the emulsified layer disappears, add 0.8% (w / v) sodium chloride, stir evenly, let it stand still, make it fully layered, Separation, the potency uni...

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PUM

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Abstract

The invention discloses a method for recovering a chlortetracycline hydrochloride crystal mother liquor. The method includes the following steps: a. natural sedimentation of the chlortetracycline hydrochloride crystallization mother liquor at low temperature, and filtering; b. adjusting the pH of the filtrate with an alkaline solution, adding a filter aid, and filtering; c. dissolving the filter cake with an oxalic acid solution , add a purifying agent and filter; d. perform solvent extraction with multi-carbon alcohol or a mixed solution of multi-carbon alcohol and acetate, and cool the extract; e. use urea double salt, wash, crystallize, and dry. The method for recovering the chlortetracycline hydrochloride crystal mother liquor provided by the invention can make the recovered chlortetracycline hydrochloride content reach more than 80%, the titer unit can reach more than 900u / ml, and the recovery yield can reach more than 50%. The method of the invention effectively avoids the waste caused by discarding the chlortetracycline crystal mother liquor in the production process of chlortetracycline hydrochloride, can save 5% of the production cost, and simultaneously reduces the environmental pollution in the production process.

Description

technical field [0001] The invention relates to a preparation method of pharmaceutical raw materials, in particular to a recovery method of demeclocycline hydrochloride crystallization mother liquor. Background technique [0002] Demeclocycline hydrochloride is a tetracyclic broad-spectrum antibiotic that has antibacterial effects on most Gram-positive and Gram-negative bacteria, and its antibacterial spectrum is similar to that of oxytetracycline and tetracycline. Demeclocycline hydrochloride is also an important starting material for the synthesis of minocycline. Demeclotetracycline hydrochloride can be produced through biological fermentation, acidification filtration, double salt formation, salt conversion, crystallization and drying. At present, in the process of producing demeclotetracycline hydrochloride, its crystallization mother liquor is generally not recycled and directly enters the sewage treatment process. Usually every ton of demeclotetracycline hydrochlorid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/24C07C237/26
Inventor 王正林孙秀英李保荣田彩霞金朝东
Owner NORTH CHINA PHARMA GROUP CORP
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