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Tylosin tartrate or tylosin phosphate extraction from reextraction liquid

A technology of tylosin tartrate and tylosin phosphate, which is applied in the preparation of sugar derivatives, sugar derivatives, sugar derivatives, etc., can solve dust pollution, reduce the production yield of tylosin, and cause large product losses And other issues

Active Publication Date: 2014-02-19
中农华威制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. High energy consumption: producing 1 ton of tylosin tartrate or tylosin phosphate requires about 3,000 kWh of electricity and about 3 tons of steam, equivalent to RMB 3,000-4,500 in total
[0005] 2. Large product loss: 4.5-9.6% of tylosin is lost during the spray drying process. Therefore, the production yield of tylosin is greatly reduced. A factory with an annual output of 1,000 tons of tylosin, In this production process alone, 45-96 tons of tylosin are lost every year, worth about 12-27 million yuan
[0006] 3. There is dust pollution in spray drying

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0022] Example 1, the preparation of stripping solution

[0023] 1. Fermentation broth pretreatment: After the fermentation is over, add water in an amount approximately equal to the volume of the fermentation broth, add aluminum chloride (AlCl 3 ) to flocculate the bacteria in the fermentation broth, AlCl 3 The added amount is 0.5-2% of the volume of the fermentation broth.

[0024] 2. Plate and frame filter press: under the condition of 15-25°C, put the fermentation hydraulic pressure into the high-pressure diaphragm plate frame, and press filter to obtain fermentation filtrate and mycelium filter cake (water content should be less than 50%). The mycelium filter cake goes to environmental protection treatment or extracts mycelial protein, etc.

[0025] 3. Extraction of tylosin: the fermentation filtrate is further fine-filtered with a 5 μm membrane and a 0.2 μm membrane filter to obtain a fine filtrate; the fine filtrate is further deproteinized and then extracted with but...

example 2

[0028] Example 2, extract tylosin tartrate from back extract with chloroform

[0029] Get 3000 liters of back extract containing 80.1 kg of tylosin tartrate component A (measured by HPLC method), add 200 liters of refined chloroform, add 690 kg of Na 2 SO 4, fully stirred for 10 to 30 minutes, left to stand or centrifuged to separate phases to obtain an aqueous phase and a chloroform phase, and the aqueous phase was used to recover Na 2 SO 4 And environmental protection treatment, the chloroform phase is distilled and concentrated in the distillation tank until the residual amount of chloroform is about 10% (about 20 liters) of the initial amount (200 liters), add 200 liters of petroleum ether, and fully stir at 1 to 5 ° C About 60 minutes, then press filter with nitrogen to obtain the filtrate (mother liquor) and tylosin tartrate, apply the mother liquor, and dry tylosin tartrate at 50°C and -0.05~-0.09mPa for 4~6 hours to obtain tartaric acid 95 kg of tylosin, analyzed by...

example 3

[0030] Example 3, extract tylosin tartrate with dichloromethane from back extract

[0031] Take 3000 liters of stripping solution containing 80.1 kg of tylosin tartrate component A (determined by HPLC method), add 200 liters of refined dichloromethane, add NaCl to saturation at 5-15°C, and stir thoroughly for 5 ~ 10 minutes, stand still and separate the phases to obtain the water phase and the dichloromethane phase, the water phase is removed to reclaim NaCl and environmental protection treatment, and the dichloromethane phase is distilled and concentrated in the retort until the dichloromethane residue is the initial amount (200 liters). About 10% (about 20 liters), add 200 liters of ethyl acetate, continue to distill to remove dichloromethane, fully stir at 1-5°C for about 60 minutes, and then filter with nitrogen to obtain mother liquor (filtrate) and Tylenol tartrate Tylosin tartrate was applied mechanically as a mother liquor, and tylosin tartrate was dried for 4 to 6 hou...

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PUM

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Abstract

The invention improves a spray drying step in the tylosin production process in the prior art. The improvements are as follows: extracting tylosin tartrate or tylosin phosphate into an organic phase from a reextraction liquid (a water phase) by using trichloromethane or dichloromethane (an organic phase); then removing a solvent to obtain tylosin tartrate or tylosin phosphate; or after removal of most solvent, adding petroleum ether or ethyl acetate or butyl acetate into a concentrate, so as to precipitate the tylosin tartrate or tylosin phosphate. The method for the preparation of tylosin tartrate and phosphate tylosin has lower energy consumption and higher product yield than a spray drying dehydration method, and can increase the output value by more than 10 thousand yuan calculated by production of per ton of products.

Description

technical field [0001] The present invention relates to the refining technology of antibiotics, in particular to the refining technology of tylosin, which is a method for extracting tylosin tartrate or tylosin phosphate from stripping solution (aqueous solution). Background technique [0002] Tylosin is a special antibiotic for livestock and poultry, which is a fermentation product of Streptomyces freundii. At present, liquid submerged fermentation is used in China. After the fermentation liquid is treated with a flocculant (such as aluminum sulfate or aluminum chloride), the fermentation filtrate is obtained through solid-liquid separation; the fermentation filtrate is subjected to liquid-liquid extraction with butyl acetate to obtain an ester phase liquid; The ester phase liquid is back-extracted with acid water, that is, tylosin and tartaric acid or phosphoric acid are salted into tylosin tartrate or tylosin phosphate, and transferred to the water phase to obtain tylosin ...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/08
Inventor 王玉万
Owner 中农华威制药股份有限公司
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