Method for producing ibuprofen through multistage continuous reaction crystallization

A technology of reaction crystallization and secondary reaction, which is applied in the field of medicine and chemical industry, can solve the problems of product purity specification and small crystal particle size, and achieve the effect of high main content of the product, uniform particle size and obvious effect

Inactive Publication Date: 2019-12-31
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is only applicable to the purification and removal of impurity 2-[4-(2-methyl-1-propenyl)phenyl]propionic acid, and the purity of the product is not fully explained, and the sodium salt of ibuprofen is in the process of acidification There will be explosive nucleation phenomenon caused by oil segregation, resulting in fine crystal particle size. The electron microscopic photos of ibuprofen crystal obtained by the applicant according to the conditions in the patent are as attached figure 1 As shown, the particle size of the product is about 100 μm

Method used

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  • Method for producing ibuprofen through multistage continuous reaction crystallization
  • Method for producing ibuprofen through multistage continuous reaction crystallization

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Experimental program
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Effect test

Embodiment 1

[0036] The sodium ibuprofen aqueous solution is used as the raw material, and hydrochloric acid is used for multi-stage reaction crystallization, and the formed ibuprofen crystal slurry is continuously discharged, and then enters the processes of separation, washing, drying, etc. to prepare the finished ibuprofen product. The concrete steps of the production method of its continuous crystallization are:

[0037] (1) Reaction into oil: continuously adding concentration to the oil tank is the ibuprofen sodium salt aqueous solution of 0.06g / ml, at the same time, the hydrochloric acid aqueous solution is added in the oil tank, the pH value of the oil tank is controlled at 6.9, and the feed liquid The temperature is controlled at 40°C, and the average residence time of the oil-forming tank based on the ibuprofen sodium salt aqueous solution feed is 0.5 hours;

[0038] (2) First-stage reaction crystallization: The oil-forming tank continuously transports materials to the first-stage...

Embodiment 2

[0043] The sodium ibuprofen aqueous solution is used as the raw material, and phosphoric acid is used for multi-stage reaction crystallization, and the formed ibuprofen crystal slurry is continuously discharged, and then enters the separation, washing, drying and other processes to prepare the finished ibuprofen product. The concrete steps of the production method of its continuous crystallization are:

[0044] (1) Reaction into oil: Continuously adding concentration to the oil tank is the ibuprofen sodium salt aqueous solution of 0.09g / ml, at the same time, adding phosphoric acid aqueous solution in the oil tank, the pH value of the oil tank is at 6.7, the feed liquid temperature Controlled at 35°C, the average residence time of the oil-forming tank based on the ibuprofen sodium salt aqueous solution feed is 0.5 hours;

[0045] (2) Primary reaction crystallization: Add the seed crystals with 0.05-0.1% ibuprofen sodium salt content in the raw material liquid flowing into the p...

Embodiment 3

[0051] The sodium ibuprofen aqueous solution is used as the raw material, and acetic acid is used for multi-stage reaction crystallization, and the formed ibuprofen crystal slurry is continuously discharged, and then enters the next steps of separation, washing, drying and other processes to prepare ibuprofen finished products. The concrete steps of the production method of its continuous crystallization are:

[0052] (1) Reaction into oil: Continuously adding concentration to the oil tank into the ibuprofen sodium salt solution of 0.07g / ml, the stock material flows into the oil tank from the top of the oil tank in the form of a distribution coil, and at the same time , add the acetic acid aqueous solution into the oil forming tank, and the acetic acid aqueous solution is also fed into the oil forming tank from the top of the oil forming tank in the form of a distribution coil. The pH value of the forming oil tank is 6.7, and the liquid temperature is 35°C. The average residen...

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Abstract

The invention discloses a continuous crystallization process for ibuprofen. The ibuprofen product is obtained in a multistage continuous crystallization manner; and multistage continuous reaction crystallization comprises the steps of oil forming through a reaction, 2-4-stage reaction crystallization and dehydrating washing, wherein a pH and a temperature of each step are regulated and controlled.According to the process, a burst nucleation phenomenon caused by oil separating during the reaction crystallization of the ibuprofen is effectively solved; the crystallization is stable in process conditions and simple in operation control; by taking water as a solvent, environmental pollution is reduced; and the obtained ibuprofen crystal is large and uniform in size, the product is high in purity and yield, the stability of running of the crystallization process and the quality of the product are improved, the production cost is reduced, and the stabilized industrial production of the ibuprofen is achieved.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and relates to a continuous crystallization method of ibuprofen. Background technique [0002] Ibuprofen, chemical name is 2-(4-isobutylphenyl)propionic acid, its molecular formula is C 13 h 18 o 2 ; Soluble in organic solvents such as ethanol, acetone, chloroform or ether, almost insoluble in water. Its anti-inflammatory, antipyretic and analgesic effects are exact, and its adverse reactions are small. It has become the three pillar drugs for antipyretic and analgesic alongside aspirin and acetaminophen. Ibuprofen is a safe and effective antipyretic drug in clinical application. Its antipyretic effect is more obvious than paracetamol in high fever, and the antipyretic time is longer; the analgesic effect is 16-32 times stronger than aspirin, and the antipyretic effect is similar to that of aspirin However, the effect is longer lasting, and the gastrointestinal adverse reactions ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/02C07C51/43C07C57/30
CPCC07C51/02C07C51/43C07C57/30Y02P20/10C07C53/134C07B2200/13
Inventor 杜德平张美景寇祖星周玲孙科夏丙堃郭发志张玲
Owner SHANDONG XINHUA PHARMA CO LTD
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