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Method for extracting sodium p-toluenesulfonate from tiamulin synthesis wastewater

A technology of sodium p-toluenesulfonate and tiamulin, which is applied in the field of medicine and chemical industry, can solve the problems of high COD of wastewater, increase the difficulty of treatment, and high cost of wastewater treatment, so as to reduce the COD of wastewater, reduce the pressure of wastewater treatment, The effect of reducing the cost of wastewater treatment

Active Publication Date: 2015-01-07
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

The general wastewater treatment method is to directly treat tiamulin wastewater. Due to the high COD of wastewater, the cost of wastewater treatment remains high, and it also increases the difficulty of treatment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 500mL of tiamulin ammoniation production wastewater from the workshop, adjust the pH to 8 with 36% concentrated hydrochloric acid, and concentrate at a vacuum of 0.085MPa and a temperature of 65°C. After concentration, the volume is 375mL; the concentrated wastewater is cooled to 2°C, and then filtered after insulated and stirred for 1 hour; the wet weight of the filter cake is 186.75g; the filter cake is mixed with 186mL of water, 1.9g of activated carbon is added, and the temperature is raised to 80°C for decolorization After stirring for 30 minutes, perform hot filtration, cool down the temperature of the obtained mother liquor to 3°C, filter, and dry the filter cake, and the mother liquor can be recycled for next crystallization. After drying, the sodium p-toluenesulfonate is 155.4g, the active matter is 79%, the pH is 7.6, and the COD of the treated wastewater is 451mg / L.

Embodiment 2

[0019] 20% sulfuric acid was used when adjusting the pH, and the other process steps were the same as in Example 1. Finally, 152.2 g of sodium p-toluenesulfonate was obtained, the active matter was 77%, the pH was 7.2, and the COD of the treated wastewater was 494 mg / L.

Embodiment 3

[0021] Take 500mL of tiamulin ammoniation production wastewater from the workshop, adjust the pH to 7 with 15% phosphoric acid, and concentrate at a vacuum of 0.085MPa and a temperature of 65°C. The volume after concentration is 400mL; the concentrated wastewater is cooled to 0°C, and then filtered after being kept warm and stirred for 1.5 hours; the wet weight of the filter cake is 175.6g; the filter cake is mixed with 140mL of water, 3.5g of activated carbon is added, and the temperature is raised to 80°C for decolorization After stirring for 30 minutes, perform hot filtration, cool down the temperature of the obtained mother liquor to 3°C, filter, and dry the filter cake, and the mother liquor can be recycled for next crystallization. After drying, the sodium p-toluenesulfonate is 152.8g, the active matter is 79%, the pH is 7.4, and the COD of the treated wastewater is 504mg / L.

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PUM

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Abstract

The invention relates to a method for extracting sodium p-toluenesulfonate from tiamulin synthesis wastewater, which comprises the following steps: regulating the pH value of tiamulin ammonification production wastewater to 7-8, and concentrating to 75-80% of the original volume under reduced pressure; cooling to 0-4 DEG C, stirring for 1-2 hours while keeping the temperature, and filtering; mixing the filter cake with purified water, adding activated carbon, heating to 80 DEG C, stirring for 30-60 minutes while keeping the temperature, and carrying out hot filtration; and cooling the mother solution to 2-4 DEG C to recrystallize, and filtering to obtain the sodium p-toluenesulfonate. A simple method is utilized to extract and recover the sodium p-toluenesulfonate, thereby changing wastes into valuable substances, increasing the available resources, lowering the wastewater COD (chemical oxygen demand), reducing the wastewater treatment pressure and lowering the wastewater treatment cost; and the method is green and environment-friendly, and has sustainable development meanings for production. The COD of the ammonification wastewater treated by the method is lowered by 50-60%, and the concentration of the sodium p-toluenesulfonate is 310 kg / m<3>.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a method for extracting sodium p-toluenesulfonate from tiamulin synthesis wastewater. Background technique [0002] Tiamulin (Tiamulin) is obtained by fermenting the higher fungus Basidiomycetes Pleuroyus mutilus to obtain pleuromutilin, and then chemically synthesized to obtain Tiamulin fumarate, which is a special diterpene antibiotic for livestock and poultry. The synthesis process of tiamulin is to generate an intermediate through sulfonation reaction and reaction of pleuromutilin and p-toluenesulfonyl chloride, and the intermediate is then reacted with 2-ethylaminoethanethiol, that is, ammoniation reaction to generate tiamulin product. During the ammonification reaction, due to the substitution reaction, the p-toluenesulfonyl group interacts with sodium hydroxide to generate a large amount of by-product—sodium p-toluenesulfonate, resulting ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/44C07C309/30
Inventor 王义王忠中任勇李晓楠王彬奇乃李小萍董媛
Owner 宁夏泰瑞制药股份有限公司
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