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Method for recovering pyrazinamide from pyrazinamide-containing mother solution

A technology for recovering pyrazinamide and mother liquor, which is applied in the direction of organic chemistry, can solve problems such as consumption, increased production costs, and high energy consumption, and achieve the effects of reducing production costs, saving energy, and the method is simple and easy

Inactive Publication Date: 2018-08-24
JIANGSU SIHUAN BIOENGINEERING PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Pyrazinamide continues to be hydrolyzed at this temperature, the recovery rate can only reach 60%, and consumes a large amount of energy, which greatly increases the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Put 80 kg of diatomaceous earth and 800 kg of mother liquor into a 1000-liter enamel reaction kettle, adjust the pH of the system to 5.5, cool the temperature to 5°C-6°C, stir for 3 hours, so that pyrazinamide is fully adsorbed on the diatomite, and discharge Spin dry, put the dry mixture into an enamel reaction kettle, stir and mix according to the ratio of dry matter and purified water 1:3, and adjust the pH to 7.2 to elute pyrazinamide from diatomaceous earth. Pyrazinamide and diatomaceous earth are automatically separated, stirred at room temperature for 2 hours, discharged and dried, diatomaceous earth can be used repeatedly, the mother liquor is filtered, cooled and crystallized, dried, and vacuum-dried to obtain 7.2 kg of finished pyrazinamide. Diatomite is light, fine, loose, porous, strong in adsorption and permeability, and stable in chemical structure, so it is an ideal adsorption medium. Therefore, in the first embodiment, the porous adsorption medium is pref...

Embodiment 2

[0021] Put 100 kg of zeolite molecular sieve and 800 kg of mother liquor into a 1000-liter enamel reaction kettle, adjust the pH of the system to 6, cool the temperature to 5°C-6°C, stir for 3 hours, so that pyrazinamide is fully adsorbed on the zeolite molecular sieve, discharge and dry , put the spin-dried mixture into an enamel reaction kettle, stir and mix according to the mass ratio of dry matter and purified water 1:3, adjust the pH to 7.5, so as to elute pyrazinamide from the zeolite molecular sieve, and make pyrazinamide The pyrazinamide is automatically separated from the zeolite molecular sieve, stirred at room temperature for 2 hours, discharged and dried, the zeolite molecular sieve can be used repeatedly, the mother liquor is filtered, cooled and crystallized, dried, and vacuum-dried to obtain 7.5 kg of pyrazinamide finished product.

Embodiment 3

[0023] Put 80 kg of activated carbon and 800 kg of mother liquor into a 1000-liter enamel reaction kettle, adjust the pH of the system to 5.7, cool the temperature to 5°C-6°C, and stir for 2 hours to make pyrazinamide fully adsorbed on the activated carbon. Put the dry mixture into the enamel reaction kettle, stir and mix according to the mass ratio of dry matter and purified water 1:4, adjust the pH to 7.4, so as to elute pyrazinamide from the activated carbon, and make pyrazinamide and activated carbon Automatic separation, stirring at room temperature for 2 hours, discharging and drying, activated carbon can be used repeatedly, cooling and crystallization of the mother liquor after filtration, drying, and vacuum drying to obtain 6.5 kg of finished pyrazinamide.

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Abstract

The invention provides a method for recovering pyrazinamide from a pyrazinamide-containing mother solution. The method comprises the following steps: S1, adding a porous adsorbent medium and a pyrazinamide-containing mother solution into an enamel reactor, regulating the pH value of the system to be 5.5-6, cooling to 5-6 DEG C, continuously stirring, discharging and spin-drying to obtain a spin-dried mixture; S2, adding the mixture and purified water into the enamel reactor, regulating the pH value of the system to 7.2-7.5, stirring at a normal temperature for 2-3 hours, eluting the pyrazinamide from the porous adsorbent medium, discharging and spin-drying to obtain a mother solution; S3, filtering the mother solution, performing cooling crystallization, spin-drying, and performing vacuumdrying, thereby obtaining the finished pyrazinamide. The method disclosed by the invention is simple and feasible, the yield of the pyrazinamide can be up to 90%, and compared with the conventional process, the method in the invention has the advantage that the yield can be improved by 30%; meanwhile, lots of energy can be saved, and the production cost of the pyrazinamide is reduced.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a method for recovering pyrazinamide from a mother liquor containing pyrazinamide. Background technique [0002] Pyrazinamide is white or off-white crystalline powder; odorless or almost odorless, slightly bitter taste. This product is slightly soluble in water and very slightly soluble in ethanol. The melting point of this product is 188~192℃. Pyrazinamide has good antibacterial effect on Mycobacterium tuberculosis, and it has the strongest bactericidal effect at pH 5-5.5, especially for Mycobacterium tuberculosis in phagocytic cells that grow slowly in an acidic environment. It is currently the best bactericidal drug. The antibacterial concentration of this product in the body is 12.5μg / ml, up to 50μg / ml can kill Mycobacterium tuberculosis. The concentration of this product to inhibit Mycobacterium tuberculosis inside the cell is 10 times lower than that outside the cell, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/24
CPCC07D241/24
Inventor 徐益明沈振宇丁月萍江永红刘红宋紫薇
Owner JIANGSU SIHUAN BIOENGINEERING PHARM CO LTD