Preparation method of fine aspirin crystals

A technology of aspirin and crystallization, which is applied in the preparation of organic compounds, carboxylic acid esters, chemical instruments and methods, etc., can solve problems such as gastrointestinal irritation, gastric bleeding or cerebral hemorrhage, and destroy crystal forms, so as to improve product yield, The effect of reducing production costs

Active Publication Date: 2014-03-05
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the main problem in the clinical use of aspirin preparations is gastrointestinal irritation, and even the risk of gastric hemorrhage or cerebral hemorrhage. In order to effectively control the release rate of the drug and reduce the side effects on the stomach and intestinal mucosa, various preparation units have researched Aspirin sustained-release technology, most manufacturers rely on crushing to obtain fine crystals, but the crushing destroys the crystal form and the crushing process has an adverse effect on product quality. Therefore, strict and almost harsh regulations are put forward for preparation manufacturers on aspirin crystals, especially fine crystals. Require

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Put 2000kg of salicylic acid and 2000kg of acetic anhydride into the above-mentioned dissolving tank, add 1000kg of aspirin fine crystal mother liquor, open the dissolving tank and stir, heat up to 80°C to dissolve and keep warm for 2 hours to obtain a hot solution;

[0018] (2) Add 300kg of aspirin crystallization mother liquor into the crystallization tank and stir to obtain a cold solution;

[0019] (3) Filter the hot solution after heat preservation into the crystallization tank, and control the temperature of the crystallization tank to rise gradually during the filtration process. When the filtration is over, the temperature in the tank rises to 40°C. After the filtration is over, keep the temperature at 40°C for 30 minutes, and then cool down Centrifuge at 20°C, the solid state after separation is aspirin fine crystals, and the mother liquor of aspirin fine crystals is separated and reused in steps (1) and (2).

[0020] Analysis result: The yield rate is 75%....

Embodiment 2

[0022] (1) Put 2000kg of salicylic acid and 2000kg of acetic anhydride into the above-mentioned dissolving tank, add 1200kg of aspirin fine crystal mother liquor, open the dissolving tank and stir, heat up to 85°C to dissolve and keep warm for 1.5 hours to obtain a hot solution;

[0023] (2) Add 300kg of acetic anhydride into the crystallization tank and stir to obtain a cold solution;

[0024] (3) Filter the hot solution after heat preservation into the crystallization tank, and control the temperature of the crystallization tank to rise gradually during the filtration process. At the end of the filtration, the temperature in the tank rises to 80°C. After the filtration is completed, keep the temperature at 80°C for 35 minutes, and then cool down Centrifuge at 15°C, the solid state after separation is fine crystals of aspirin, and the mother liquor of fine crystals of aspirin is separated and reused in step (1).

[0025] Analysis result: The yield rate is 85%.

Embodiment 3

[0027] (1) Put 2000kg of salicylic acid and 2000kg of acetic anhydride into the above-mentioned dissolving tank, add 1100kg of aspirin fine crystal mother liquor, open the dissolving tank and stir, heat up to 90°C to dissolve and keep warm for 1 hour to obtain a hot solution;

[0028] (2) Add 200kg of aspirin fine crystallization mother liquor and 100kg of acetic anhydride into the crystallization tank and stir to obtain a cold solution;

[0029] (3) Filter the hot solution after heat preservation into the crystallization tank, and control the temperature of the crystallization tank to rise gradually during the filtration process. When the filtration is over, the temperature in the tank rises to 65°C. Centrifugal separation at 10°C. After separation, the solid state is aspirin fine crystals, and the separated aspirin fine crystal mother liquor is reused in steps (1) and (2).

[0030] Analysis result: the yield rate is 79%.

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PUM

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Abstract

The invention relates to a preparation method of fine aspirin crystals, belonging to the field of medical and chemical engineering. The preparation method comprises the following steps: (1) putting salicylic acid, acetic anhydride and fine aspirin crystal mother liquor into a dissolving tank to be stirred, and after rising the antipyretic temperature to 80-90 DEG C to dissolve, preserving the temperature for 1-2 hours to obtain hot liquor; (2) adding acetic anhydride, fine aspirin crystal mother liquor or the mixture of acetic anhydride and fine aspirin crystal mother liquor into a crystallizing tank to stir to obtain cold liquor; (3) filtering the hot liquor after preserving temperature to the crystallizing tank, controlling the temperature of the crystallizing tank in the filtering process to gradually rise, after preserving temperature after filtering, and then cooling and carrying out centrifugal separation to obtain solid state fine aspirin crystals. The obtained fine aspirin crystals mother liquor is recycled to the steps (1) and (2). According to the method provided by the invention, the crystal form, the uniformity and the granularity which are fine aspirin crystals are effectively controlled, so that the preparation method is environment-friendly, and the product yield is improved and the production cost is lowered.

Description

technical field [0001] The invention relates to a method for preparing aspirin fine crystals, belonging to the field of medicine and chemical industry. technical background [0002] Since the advent of aspirin, it has been widely used as an antipyretic and analgesic drug for the treatment of fever, headache, neuralgia, muscle pain, toothache, acute rheumatoid arthritis, rheumatoid arthritis, etc., with remarkable curative effect. In recent years, it has been commonly used clinically to prevent and treat acute ischemic stroke and cardiovascular and cerebrovascular diseases, and has attracted public attention and recognition. However, the main problem in the clinical use of aspirin preparations is gastrointestinal irritation, and even the risk of gastric hemorrhage or cerebral hemorrhage. In order to effectively control the release rate of the drug and reduce the side effects on the stomach and intestinal mucosa, various preparation units have researched Aspirin sustained-rel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/157C07C67/52
CPCC07C67/52C07C69/157
Inventor 吴孝好韩新利陈洪全马新宁杨斌
Owner SHANDONG XINHUA PHARMA CO LTD
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