Preparation method of high-bulk-density ibuprofen spherical crystal and product of high-bulk-density ibuprofen spherical crystal
A spherical crystal, bulk density technology, applied in organic chemistry methods, separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of complex process control, high cost, unfavorable for industrial production, etc. Good tableting properties and high bulk density
Active Publication Date: 2021-08-03
ZHEJIANG NHU CO LTD
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Problems solved by technology
This method uses a variety of solvents, the process control is complicated, the cost is high, and it is not conducive to industrial production
Method used
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Embodiment 1
[0049] (1) First, 5kg of ibuprofen is put into a melting tank, heated to 77-85°C for melting;
[0050] (2) Add 10kg of purified water into the crystallizer, open the jacket of the crystallizer to cool with frozen brine, and cool the purified water to 5-10°C;
[0051] (3) Open the double-layer paddle stirrer in the crystallizer, and control the rotating speed to be 300-350rpm;
[0052] (4) Pressurize the melting tank of step (1) to 0.15-0.20MPa with nitrogen, then drop the ibuprofen molten liquid from the melting tank into the crystallizer through the rotating ball liquid distributor, and the rotating ball liquid distribution The diameter of the liquid hole of the device is 0.6mm, and the droplets evenly fall to the water surface after being sprayed by rotation, and the flow control valve is adjusted so that the whole batch of feed liquid is added in 1.5 to 2 hours;
[0053] (5) During the dropping process, the temperature in the crystallizer is controlled at 5-10°C, and cryst...
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Abstract
The invention discloses a preparation method of a high-bulk-density ibuprofen spherical crystal and a product thereof. The preparation method comprises the following steps: (1) heating ibuprofen to a molten liquid state; and (2) pressurizing the ibuprofen in the molten liquid state, dropwise adding the ibuprofen in the molten liquid state into a crystallizer containing water through a liquid distributor, carrying out crystallization while dropwise adding under a stirring condition until the ibuprofen in the molten liquid state is completely dropwise added, reducing the rotating speed of stirring, carrying out crystal growing, and finally carrying out post-treatment on crystal slurry to obtain the ibuprofen spherical crystal with the bulk density of 0.50-0.70 g / mL, the median particle size of 300-1000 [mu]m and the repose angle of 22-29 degrees. The preparation method is simple in process, free of additives and suitable for industrial production, the prepared ibuprofen spherical crystal is regular in crystal habit, smooth in crystal face, good in fluidity, high in bulk density and high in product purity, and the product quality meets the requirements of pharmacopoeia such as CP2020, EP9.8 and USP41.
Description
technical field [0001] The invention relates to the technical field of drug synthesis, in particular to a method for preparing spherical ibuprofen crystals with high bulk density and a product thereof. 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 206.29, usually white crystalline powder, melting point is 75-77°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. Since the 1980s, the drug has been included in the pharmacopoeias of the United States, the United Kingdom, the European Union, and...
Claims
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IPC IPC(8): C07C51/43C07C57/30
CPCC07C51/43C07B2200/13C07C57/30
Inventor 刘金龙吕叔敏胡瑞君何雪忠杜梦良王晓春汪紫玉梁兰英
Owner ZHEJIANG NHU CO LTD