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Device and method for recycling ethyl alcohol in refined mother solution of doxycycline hyclate

A technology of doxycycline hydrochloride and a recovery method, applied in the pharmaceutical field, can solve problems such as inability to treat solid waste, and achieve the effects of high recovery rate, stable process and reduced production cost

Pending Publication Date: 2019-10-01
CHANGZHOU PHARMA FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that: the final component of distillation is black carbon that cannot be separated, and the solid waste cannot be treated; and the recovered ethanol content is only 92-93%.

Method used

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  • Device and method for recycling ethyl alcohol in refined mother solution of doxycycline hyclate
  • Device and method for recycling ethyl alcohol in refined mother solution of doxycycline hyclate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Put 1500L doxycycline hydrochloride mother liquor (1706ppm ethyl chloride content) into a 3000L distillation still, open the vacuum valve, keep the vacuum at about -0.1Mpa, raise the temperature to 30°C, and cool the distillate vapor through a 0-10°C condenser Liquefied into the neutralization kettle. The vacuum distillation can be stopped when more than 1350L fraction is collected in the neutralization tank. Add 32% liquid caustic soda to the neutralization kettle under ice-brine cooling, control the temperature below 40°C, and adjust the pH to 9-10. The mixture of ethanol and sodium chloride in the kettle is separated by filtration, and the ethanol solution is vaporized at high temperature and filtered through a vaporization membrane. , to obtain 1278L of absolute ethanol finished product, the yield is about 85.2%, the content is 99.8%, the moisture is 0.1%, and the ethyl chloride content is 138ppm. Specifically, in this embodiment, the vaporization membrane is selec...

Embodiment 2

[0032] Put 1500L doxycycline hydrochloride mother liquor (2201ppm ethyl chloride content) into a 3000L distillation still, open the vacuum valve, keep the vacuum at about -0.08Mpa, raise the temperature to 40°C, and cool the distillate vapor through a 0-10°C condenser Liquefied into the neutralization kettle. The vacuum distillation can be stopped when more than 1350L fraction is collected in the neutralization tank. Add 32% liquid caustic soda to the neutralization kettle under ice-brine cooling, control the temperature below 40°C, adjust the pH to 9-10, filter and separate the mixture of ethanol and sodium chloride, vaporize the ethanol solution at high temperature and filter it through a vaporization membrane to obtain anhydrous The finished product of ethanol is 1312L, the yield is about 87.5%, the content is 99.75%, the moisture is 0.15%, and the ethyl chloride content is 121ppm. Specifically, in this embodiment, the vaporization membrane is selected from the NaA type in...

Embodiment 3

[0034] Put 1500L doxycycline hydrochloride mother liquor (2250ppm ethyl chloride content) into a 3000L distillation still, open the vacuum valve, keep the vacuum at about -0.09Mpa, raise the temperature to 35°C, and cool the distillate steam through a 0-10°C condenser Liquefied into the neutralization kettle. The vacuum distillation can be stopped when more than 1350L fraction is collected in the neutralization tank. Add 32% liquid caustic soda to the neutralization kettle under ice-brine cooling, control the temperature below 40°C, and adjust the pH to 9-10. The mixture of ethanol and sodium chloride in the kettle is separated by filtration, and the ethanol solution is vaporized at high temperature and filtered through a vaporization membrane. Obtain 1304L of absolute ethanol finished product, the yield is about 86.9%, the content is about 99.8%, the moisture content is 0.1%, and the ethyl chloride content is 104ppm. Specifically, in this embodiment, the vaporization membran...

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Abstract

The invention discloses a device and method for recycling ethyl alcohol in a refined mother solution of doxycycline hyclate. The specific device for recycling ethyl alcohol comprises a pressure reduction distillation kettle, a neutralization kettle, a press filter, a to-be-recycled ethyl alcohol intermediate tank, a distillation tower, a vaporization membrane separation device and a finished product tank which are connected in sequence; the distillation tower is connected with a side material solution inlet of the vaporization membrane separation device, and a side material solution outlet ofthe vaporization membrane separation device is connected with the finished product tank. According to the device and method for recycling the ethyl alcohol in the refined mother solution of the doxycycline hyclate, the rate of recycling absolute ethyl alcohol reaches 85% or above, the content of the recycled ethyl alcohol reaches 99.5% or above, the moisture content is smaller than 0.5%, the content of chloroethane is lower than 200 ppm, and the recycle device and method accord with the standard of recycle application. The technology is stable, the recycle rate is high, the production cost isgreatly lowered, low-temperature pressure reduction distillation is adopted, the energy is saved, the emission amount of the ethyl alcohol is lowered, and the environmental pollution is reduced.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and in particular relates to a recovery device and a recovery method for ethanol in doxycycline hydrochloride refined mother liquor. Background technique [0002] Doxycycline hydrochloride, also known as doxycycline, is a tetracycline antibiotic with a broad antibacterial spectrum and stronger antibacterial effect than other tetracyclines. It is mainly used for upper respiratory tract infections and tonsils caused by sensitive gram-positive cocci and gram-negative bacilli. Inflammation, biliary tract infection, lymphadenitis, cellulitis, senile chronic bronchitis, etc. It is also used for typhus, scrub typhus, mycoplasma pneumonia, etc. It can also be used to treat cholera, prevent falciparum malaria and leptospirosis infection. In the existing doxycycline hydrochloride refining process, the crystallization mother liquor is mainly ethanol hydrochloride, doxycycline, water and other impurities. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/74C07C31/08
CPCC07C29/74C07C31/08Y02P20/10Y02P20/50
Inventor 朱怡君宦玉亮孙忠华胡小丽芮俊蒋赟伍成祥
Owner CHANGZHOU PHARMA FACTORY
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