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Preparation method of ibuprofen spherical crystal

A technology of spherical crystals and spheres is applied in the field of preparation of spherical ibuprofen crystals to achieve the effects of reducing industrialization costs, preventing agglomeration and having good fluidity

Active Publication Date: 2019-07-02
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome the defect of existing ibuprofen product preparation method, the invention provides a kind of method that utilizes liquid-liquid phase separation to prepare ibuprofen spherulite, prepare spherical ibuprofen crystal product particle compact, product does not coalesce, Good fluidity, simple process, green and environmental protection

Method used

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  • Preparation method of ibuprofen spherical crystal
  • Preparation method of ibuprofen spherical crystal
  • Preparation method of ibuprofen spherical crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0028] (1) Prepare 150 mL of 0.01 g / mL ibuprofen-water mixed solution at 75°C, stir until liquid-liquid phase separation occurs and ibuprofen droplets are evenly distributed in the water;

[0029] (2) Cool the solution to 1° C. at a cooling rate of 50° C. / 10 min, maintain a stirring rate of 600 rpm until crystallization, and add 0.02% surfactant sodium stearate (based on the quality of the ibuprofen-water mixed solution). Stir continuously for 0.5h to make the crystals coalesce into compact spheres;

[0030] (3) After vacuum filtration, washing with water, and drying at normal pressure at 30° C. for 12 hours, spherical ibuprofen crystals were obtained.

[0031] The XRD pattern of the product is shown in figure 1 , it can be seen that the product is a stable crystal; the average particle size of spherical particles is 500 microns, the angle of repose is 29°, and the tap density is 0.47g / cm 3 .

Embodiment 2

[0033] (1) At 80°C, prepare 150 mL of a 0.10 g / mL ibuprofen-water mixed solution, stir until liquid-liquid phase separation occurs and the ibuprofen droplets are evenly distributed in the water;

[0034] (2) Cool the solution to 5°C at a cooling rate of 45°C / 10min, maintain a stirring rate of 450rpm until crystallization, and add 0.15% surfactant sodium hexametaphosphate (based on the quality of the ibuprofen-water mixed solution). Continue to stir for 2 hours to make the crystals coalesce into compact spheres;

[0035] (3) After vacuum filtration, washing with water, and drying at 40° C. under normal pressure for 24 hours, spherical ibuprofen crystals were obtained.

[0036] The XRD pattern of the product is shown in figure 1 , it can be seen that the product is a stable crystal; the average particle size of spherical particles is 700 microns, the angle of repose is 29°, and the tap density is 0.55g / cm 3 .

Embodiment 3

[0038] (1) At 85°C, prepare 150 mL of a 0.15 g / mL ibuprofen-water mixed solution, stir until the liquid-liquid phase separation occurs and the ibuprofen droplets are evenly distributed in the water;

[0039] (2) The solution is cooled to 20°C at a cooling rate of 40°C / 10min, and the stirring rate is maintained at 300rpm to crystallize, and 0.40% of the surfactant sodium dodecylbenzenesulfonate (based on ibuprofen-water mixed solution) is added. quality). Continue stirring for 3 hours to make the crystals coalesce into compact spheres;

[0040] (3) After vacuum filtration, washing with water, and drying at normal pressure at 50° C. for 36 hours, spherical ibuprofen crystals were obtained.

[0041] The XRD pattern of the product is shown in figure 1 , it can be seen that the product is a stable crystal; the average particle size of spherical particles is 800 microns, the angle of repose is 30°, and the tap density is 0.50g / cm 3 .

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Abstract

The invention discloses a preparation method of ibuprofen spherical crystal, comprising the following steps: preparing an ibuprofen-water mixed solution with the ibuprofen concentration of 0.01-0.25 g / mL at 75-85 DEG C; continuously stirring until the solution is subjected to liquid-liquid phase separation; abruptly cooling the solution to 1-30 DEG C, and continuously stirring until crystal appears; adding 0.02-0.53 wt% of a surfactant (based on the mass of the ibuprofen-water mixed solution), keeping stirring for 0.5-5 h until crystal is aggregated into spheres; filtering, washing, and dryingto obtain the ibuprofen spherical crystal. The raw material of the crystallization process is single, the solvent only involves water which is green and environmentally-friendly, and the process is simple. The particle diameter of the spherical crystal product can be effectively adjusted by stirring speed, and the average particle size of the product is about 500-1000 microns. The crystal particle is rounded and has high fluidity. The angle of repose is 29-31 degrees, and the tap density is 0.47-0.55 g / cm<3>.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering industrial crystallization, and in particular relates to a preparation method of spherical ibuprofen crystals. Background technique [0002] Ibuprofen (CAS: 15687-27-1), chemical name 2-methyl-4-(2-methylpropyl) phenylacetic acid, aliases, ibuprofen, ibuprofen. Ibuprofen is a non-steroidal anti-inflammatory drug widely used clinically, with a history of more than 50 years of use. English name is Ibuprofen, molecular formula C 13 h 18 o 2 , molecular weight 206.28, usually white crystalline powder, melting point is 75°C-77°C. Insoluble in water, easily soluble in ethanol, chloroform, ether, acetone and other solvents. It is mainly used for analgesic and anti-inflammatory effects such as sprains, strains, headaches, low back pain, and postoperative pain. The drug has been included in the pharmacopoeias of the United States, the United Kingdom, the European Union, Japan and other c...

Claims

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Application Information

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IPC IPC(8): C07C51/43C07C57/30
CPCC07C51/43C07C57/30
Inventor 龚俊波孙萌萌汤伟伟陈明洋侯宝红
Owner TIANJIN UNIV
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