Method for preparing non-coalescence nicotinic acid crystal with large granularity and high bulk density
A technology of large particle size and nicotinic acid, applied in the direction of organic chemistry, can solve the problems of easy fracture, broken, low bulk density, small particle size, etc., and achieve the effect of low equipment requirements, high bulk density and large particle size
Pending Publication Date: 2021-11-30
HEBEI UNIV OF TECH
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Problems solved by technology
However, because niacin crystals are white needle-like crystals, they are easy to break and break during transportation, and they are also easy to agglomerate during storage.
However, the existing nicotinic acid crystallization methods have not been devoted to improving the related problems of the above-mentioned nicotinic acid crystals, namely small particle size, low bulk density and easy agglomeration
Method used
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preparation example 1
[0034] Take a certain amount of niacin crude product, put it into a mixing mill, grind it for 10 minutes, take out the ground product and pass it through a 400-mesh crystal sieve to obtain the target niacin seed crystal.
preparation example 2
[0036] Take a certain amount of crude nicotinic acid product, put it into a saturated solution of nicotinic acid whose solvent is water, soak for 30 minutes, ultrasonically treat it at room temperature for 5-10 minutes, and finally filter and dry to obtain the target nicotinic acid seed crystal.
preparation example 3
[0038] Take a certain amount of crude nicotinic acid product, put it into a saturated solution of nicotinic acid whose solvent is ethanol, soak for 30 minutes, ultrasonically treat it at room temperature for 5-10 minutes, and finally filter and dry to obtain the target nicotinic acid seed crystal. Seed crystal micrographs as figure 1 .
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Abstract
The invention relates to a method for preparing non-coalescence nicotinic acid crystals with large granularity and high bulk density. The method comprises the following steps: cooling a nicotinic acid solution with the temperature of 80-90 DEG C and the mass concentration of 5-15% for the first time under stirring at the cooling rate of 2-10 DEG C / h, and cooling the solution to 45-65 DEG C; cooling for the second time at the cooling rate of 10-30 DEG C / h, and cooling the solution to 10-30 DEG C; and filtering the solution, and drying a filter cake to obtain the nicotinic acid crystal which is large in particle size, high in bulk density and free of coalescence. The method is based on a single solvent and segmented cooling crystallization technology, the operation process is simple, the equipment requirement is low, industrial production is easy to achieve, and the obtained nicotinic acid crystal is large in particle size, high in bulk density, free of coalescence and good in application prospect.
Description
technical field [0001] The invention relates to the technical field of chemical and pharmaceutical crystallization, in particular to a method for preparing nicotinic acid crystals with large particle size, high bulk density and non-agglomeration. Background technique [0002] Niacin is a B vitamin 3 , also known as nicotinic acid, anti-pyeremia factor, molecular formula: C 6 h 5 NO 2 , the chemical name is 3-pyridinecarboxylic acid. The chemical structural formula is: [0003] [0004] Niacin is an important drug of the vitamin B family. It can combine with protein in the form of nicotinamide to form a coenzyme in the body. It is a component of coenzyme I (NAD) and coenzyme II (NADP). It is one of the important and necessary nutrients for the animal body to promote metabolism. Niacin can be directly used as an effective drug for the prevention and treatment of pellagra and other skin diseases and similar vitamin deficiencies. Intermediates, which can be used to syn...
Claims
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Login to View More IPC IPC(8): C07D213/803C07D213/80
CPCC07D213/803C07D213/80
Inventor 苏敏赵玉茹王磊
Owner HEBEI UNIV OF TECH