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Method for preparing superfine salicylic acid by adding polyhydroxy alcohol organic compounds

A technology for organic compounds and polyhydric alcohols, applied in the field of preparing ultrafine salicylic acid, can solve the problem of high production cost of supercritical technology, and achieve the effects of uniform precipitate size distribution, fine particles and high yield

Inactive Publication Date: 2005-07-06
JIANGSU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is reported in the literature that Concepcion Domingo and others used supercritical technology to synthesize rod-shaped ultrafine salicylic acid with a particle size of 1-5 microns using the characteristics of supercritical fluid, but the production cost of supercritical technology is relatively high

Method used

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  • Method for preparing superfine salicylic acid by adding polyhydroxy alcohol organic compounds
  • Method for preparing superfine salicylic acid by adding polyhydroxy alcohol organic compounds
  • Method for preparing superfine salicylic acid by adding polyhydroxy alcohol organic compounds

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Effect test

Embodiment 1

[0016] Such as figure 1 , Weigh 1.6g of technical grade salicylic acid, add 0.1mol / L sodium hydroxide solution, make the pH value of the solution equal to 7.2, add 5.4g of 5% polyethylene glycol (molecular weight is 600), slowly add 0.2 mol / L hydrochloric acid solution, adjust the pH value to 2.2, and a white precipitate appears in the solution. Suction filter with a Buchner funnel with 3 layers of filter paper, wash with distilled water until there is no chloride ion, drain, and dry at 30°C for 12 hours to obtain the finished product of salicylic acid microcrystals. The obtained ultrafine salicylic acid microcrystals were dried at 30°C to constant weight, and weighed accurately. The product was analyzed by a scanning electron microscope as acicular bodies with a width of 3 microns and a length of 100 microns.

Embodiment 2

[0018] Such as figure 2 , Weigh 1.6g of technical grade salicylic acid, add 0.2mol / L sodium hydroxide solution, make the pH value of the solution equal to 10.2, add about 15% polyethylene glycol (molecular weight is 600) 16.2g, slowly add 0.3mol / L hydrochloric acid solution, adjust the pH value to 2.0, white precipitate appears in the solution. Suction filter with a Buchner funnel with 3 layers of filter paper, wash with distilled water until there is no chloride ion, drain, and dry at 50°C for 10 hours to obtain the finished product of salicylic acid microcrystals. The obtained ultrafine salicylic acid microcrystals were dried at 50°C to constant weight, and weighed accurately. The product was analyzed by a scanning electron microscope as acicular bodies with a width of 5 microns and a length of 100 microns.

Embodiment 3

[0020] Such as image 3 , Weigh 1.6g of technical grade salicylic acid, add 0.3mol / L sodium hydroxide solution, make the pH value of the solution equal to 9, add about 30% polyethylene glycol (molecular weight is 2000) 45g, slowly add 0.5 mol / L hydrochloric acid solution, adjust the pH value to 3.2, and a white precipitate appears in the solution. Suction filter with a Buchner funnel with 3 layers of filter paper, wash with distilled water until there is no chloride ion, drain, and dry at 60°C for 6 hours to obtain the finished product of salicylic acid microcrystals. The obtained ultrafine salicylic acid microcrystals were dried at 60°C to constant weight, and weighed accurately. The product is analyzed by a scanning electron microscope to be acicular bodies with a width of 20 nanometers to 1 micron.

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Abstract

The invention relates to a method for preparing superfine salicylic acid, especially for preparing superfine salicylic acid by adding polyhydroxy alcohol organic compounds, characterized by weighing some industrial salicylic acid, adding sodium hydroxide solution with the mol concentration of between 0.05mol / l to 0.5mol / l to pH between 6 and11, weighing polyhydroxy alcohols organic compound of 5% to 30% by weight according to the proportion of polyhydroxy alcohols organic compound to salicylic acid between 3:1 and 30:1 by weight, and adding the organic compound into the solution to solve, adding hydrochloric acid solution with the mol concentration of between 0.1mol / L to 0.5mol / L to pH between 2 and 4, and producing white precipitate in solution, filtering and washing the white precipitate, drying for 5 to 12 hours at a temperature of between 30C. and 100C. to produce superfine salicylic acid microcrystalline product. The superfine salicylic acid particle made by the method has good dispersibility and even precipitate-size distribution.

Description

technical field [0001] The invention relates to a method for preparing superfine salicylic acid, in particular to a method for preparing superfine salicylic acid by adding polyhydric alcohol organic compounds. Background technique [0002] Superfine salicylic acid is an important fine chemical new product and new material. Salicylic acid is an antifungal drug and cuticle softening drug commonly used in clinical practice. Plastics, metallurgy and electronics and other industries. [0003] Because salicylic acid is insoluble in water, it is greatly restricted in dosage form preparation. Uneven dispersion in powders, ointments and other dosage forms is likely to cause irritation and affect the curative effect. Therefore, it is of great significance to make it into ultrafine microcrystals for the clinical use of the drug. Literature reports that Concepcion Domingo et al have synthesized rod-shaped ultrafine salicylic acid with a particle size of 1-5 microns using supercritica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C65/10
Inventor 殷恒波姜廷顺姜本鹏徐艺青胡童杰祝九庚
Owner JIANGSU UNIV
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