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Membrane separation method and device for recycling ceftazidime mother liquor

A ceftazidime and membrane separation technology, applied in organic chemistry, reverse osmosis, etc., can solve the problems of large equipment damage, environmental pollution, increase the solubility of ceftazidime, etc., and achieve the effects of strong anti-pollution ability, saving labor costs, and easy cleaning

Inactive Publication Date: 2018-02-23
南京志坤环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] No matter which synthesis route is adopted, the final crystallization and purification method is to dissolve and crystallize ceftazidime hydrochloride. Due to the salting-out effect, the solubility of ceftazidime in water is greatly increased. Therefore, the primary crystallization yield of ceftazidime is only 87%, and there is still 13% In the mother liquor, this not only increases the production cost of ceftazidime, but also causes no small pollution to the environment
The traditional process uses phosphoric acid to adjust the isoelectric point. Because it is a trivalent salt, the molecular weight is close to that of ceftazidime. It is difficult to remove inorganic salts by nanofiltration. Hydrochloric acid is used to adjust the isoelectric point. Because hydrochloric acid is highly corrosive to stainless steel, it is used for aseptic The production of raw materials will cause great damage to the equipment, and may bring metals into the drug

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0033] Embodiment 1: This embodiment illustrates the composition and connection relationship of the complete set of equipment from the desalination device of the ceftazidime mother liquor recovery method

[0034] A schematic diagram of the complete set of equipment is attached figure 1shown. Specifically, the equipment includes a modular pure water tank (1), a raw material tank device (2), a cleaning tank (3), a formic acid tank (4), a discharge pump (5), a feed pump (6), and a high-pressure pump (7), circulating pump (8), security filter (9), heat exchanger (10), nanofiltration membrane and membrane module (11), connecting pipeline and automatic control system.

[0035] Among them, the pure water tank (1), the raw material tank device (2), the discharge port of the cleaning tank (3) is connected with the discharge pump (5), the feed pump (6), and the feed pump (6) is connected with the security filter (9) Unicom; the formic acid tank (4) is connected with the security filte...

Embodiment 2

[0038] Embodiment 2: This embodiment illustrates the process of reclaiming ceftazime from ceftazime mother liquor after desalination

[0039] Cool the water in the reaction kettle to 0-5°C, add ceftazidime hydrochloride, and dissolve. Add sodium hydroxide dropwise, adjust the pH to 5.5-5.6, and filter to the crystallization tank. Maintain the temperature of the feed solution at 0-5°C, slowly adjust the pH to 4.3-4.4 with formic acid, crystallize, stop dropping, continue to add formic acid after growing the crystal for 2 hours, adjust the pH to 3.6-3.7, stop dropping, and grow the crystal again 4 hours. Solid-liquid separation, mother liquor collection into tank (2), the crystallization yield of ceftazidime at this moment is 87%. The crystallization mother liquor in the tank (2) is adjusted to pH 4.8-5.0 with sodium hydroxide solution earlier. The mother liquor is desalinated using membrane separation technology. In the desalination treatment, the pH of the mother liquor is ...

Embodiment 3

[0040] Embodiment 3: this embodiment illustrates the situation of implementing the process of the present invention in the equipment of embodiment

[0041] Take 50kg of ceftazidime hydrochloride and dissolve it in 800L stainless steel reaction kettle with 500L pure water, cool down to 0-5°C with refrigerant, stir at 80 rpm, and add dropwise 5N sodium hydroxide solution to adjust the pH of the solution to 5.5- 5.6, then filter, return the filtrate to the crystallization tank, maintain the temperature of the feed liquid at 0-5°C, slowly adjust the pH to 4.3-4.4 with formic acid, crystallize, stop dropping, continue to add formic acid after growing the crystal for 2 hours, adjust After the pH reaches 3.6-3.7, stop the dropwise addition, and grow the crystal for another 4 hours. Solid-liquid separation, the mother liquor is collected and poured into the raw material tank (2) of the desalination device, and the crystallization mother liquor in the tank (2) is first adjusted to pH 4...

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Abstract

The invention belongs to the technical field of pharmacy, and relates to a membrane separation method and device for recycling ceftazidime mother liquor. Ceftazidime belongs to a third generation antibiotics and has wider application than other third generation cephalosporin antibiotics. In a present production process of ceftazidime, due to the salting-out effect of the mother liquor in the crystallization process, the yield of ceftazidime is only 82%, 18% of ceftazidime is still in the mother liquor, and therefore not only is the production cost increased, but also certain pollution to the environment is caused. According to the membrane separation method and device for recycling the ceftazidime mother liquor, by utilizing the membrane separation technology and the adjustment of the process, the products in the mother liquor can be recycled, the production cost can be saved greatly, and pollution to environment can be reduced; besides, the device is simple to operate so that industrial amplification can be achieved easily.

Description

technical field [0001] The invention belongs to the field of biopharmaceuticals, and specifically relates to a new process and device for extracting ceftazidime from ceftazidime crystallization liquid by using the characteristics of the material itself and using the separation technology of a special membrane module integrated modular device. Background technique [0002] According to Wang Ronggeng's report in the Journal of Fine and Specialty Chemicals: Ceftazidime belongs to the third generation of cephalosporin antibiotics and was discovered in 1978. In 1983, Glaxo Company of the United Kingdom first developed and marketed it. In 1992, ceftazidime was listed for the first time in my country, and in 1993 it was officially included in the list of essential medicines in my country. After more than 10 years of clinical application verification, ceftazidime has the characteristics of broad antibacterial spectrum and enzyme resistance. It has strong antibacterial activity again...

Claims

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Application Information

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IPC IPC(8): C07D501/46C07D501/12B01D61/02
Inventor 张全华李干禄马喆坤
Owner 南京志坤环保科技有限公司
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