A kind of refining method of thymol

Abstract

The present invention is applicable to the technical field of medicine and chemical industry, and provides a method for refining thymol, comprising: adding a refining solvent to the crude thymemol, heating and stirring sufficiently to obtain a first mixed solution; the amount of the refining solvent is 0.5~3 times of the mass-volume ratio of the thymemol crude product; add an adsorbent to the first mixed solution, carry out heat preservation and decolorization treatment, and obtain the second mixed solution; filter the second mixed solution, and obtain The filtrate is subjected to cooling crystallization, heat preservation crystallization, cooling crystallization, and rejection filtration to obtain the filtrate. The refining method of the present invention can refine the impurities such as citronellal and isopulegol in the crude product of thymol to almost no detection, effectively improve the product purity, and meet the requirements of medicine; at the same time, compared with the traditional rectification method, the present invention The refining method is simple, and the refining cost is greatly reduced.

Description

technical field

[0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a method for purifying thymol. Background technique

[0002] Thymol (1963 Chinese Pharmacopoeia), also known as thymol, thymol, thymol, chemical name is 2-isopropyl-5-methylphenol, thymol has stronger bactericidal effect than phenol, and is toxic Low, it has bactericidal and fungicidal effects on the oral and throat mucosa, and has antiseptic and local anesthetic effects on the caries cavity; it can promote the movement of tracheal cilia, which is conducive to the secretion of tracheal mucus, and it is easy to play an expectorant effect, and has a bactericidal effect, so it can be used It is used in the treatment of bronchitis, whooping cough, etc.; it has a strong acaricidal effect, the mortality rate of 1% solution is 100% in half an hour, and the 0.03% solution kills 100% in 24 hours; it can also be used as an anthelmintic agent, which is a w...

Examples

Embodiment 1

[0035] In a 1000ml three-necked flask, add 250g of technical grade thymol, add 200ml of n-hexane solvent, introduce nitrogen to replace the air in the reaction flask, under nitrogen protection, turn on stirring, heat up to 70±3°C, keep stirring for 0.5 hours to make thymol Fully dissolve and clear; add activated carbon 2.5g, keep heat for decolorization for about 1h; filter, cool the filtrate naturally, slowly stir until granular solids are precipitated on the wall of the reaction vessel, adjust the stirring speed, keep stirring for about 1h, and precipitate a large amount of crystalline solids ( about 40°C), cooled to 5°C, kept stirring for 4 hours for crystallization, filtered to obtain 233g of pure white product, and dried to obtain 214g of white transparent crystalline powder solid.

Embodiment 2

[0037]In a 1000ml three-necked flask, add 250g of technical grade thymol, add 250ml of n-heptane solvent, and replace the air in the reaction flask with nitrogen. The brain was fully dissolved and clear; 5.0 g of activated clay was added, and the decolorization was maintained for about 30 minutes; filtered, the filtrate was naturally cooled, and slowly stirred until granular solids were precipitated on the wall of the reaction vessel. The solid (about 40°C) was cooled to 3°C, kept stirring for 2 hours for crystallization, filtered to obtain 231g of pure white product, and dried to obtain 206g of white transparent crystalline powder solid.

Embodiment 3

[0039] In a 1000ml three-necked flask, add 250g of technical grade thymol, add 250ml of n-octane solvent, and replace the air in the reaction flask with nitrogen. The brain was fully dissolved and clear; 2.0 g of chromatographic silica gel powder was added, and the decolorization was maintained for about 1 h; filtered, the filtrate was cooled naturally, and slowly stirred until granular solids were precipitated on the wall of the reaction vessel, and the stirring speed was adjusted. Crystalline solid (about 40°C), cooled to 1°C, kept stirring for 6 hours, filtered to obtain 248g of pure white product, and dried to obtain 186g of white transparent crystalline powder solid.

[0040] The components of the white transparent crystalline powder solids obtained in Examples 1-3 of the present invention were analyzed, and the results are shown in Table 1.

[0041] Component analysis method:

[0042] Detection instrument: gas chromatograph, Shimadzu GC-2030

[0043] Detector: FID

[...

technical field

[0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a method for purifying thymol. Background technique

[0002] Thymol (1963 Chinese Pharmacopoeia), also known as thymol, thymol, thymol, chemical name is 2-isopropyl-5-methylphenol, thymol has stronger bactericidal effect than phenol, and is toxic Low, it has bactericidal and fungicidal effects on the oral and throat mucosa, and has antiseptic and local anesthetic effects on the caries cavity; it can promote the movement of tracheal cilia, which is conducive to the secretion of tracheal mucus, and it is easy to play an expectorant effect, and has a bactericidal effect, so it can be used It is used in the treatment of bronchitis, whooping cough, etc.; it has a strong acaricidal effect, the mortality rate of 1% solution is 100% in half an hour, and the 0.03% solution kills 100% in 24 hours; it can also be used as an anthelmintic agent, which is a w...

Examples

Embodiment 1

[0035] In a 1000ml three-necked flask, add 250g of technical grade thymol, add 200ml of n-hexane solvent, introduce nitrogen to replace the air in the reaction flask, under nitrogen protection, turn on stirring, heat up to 70±3°C, keep stirring for 0.5 hours to make thymol Fully dissolve and clear; add activated carbon 2.5g, keep heat for decolorization for about 1h; filter, cool the filtrate naturally, slowly stir until granular solids are precipitated on the wall of the reaction vessel, adjust the stirring speed, keep stirring for about 1h, and precipitate a large amount of crystalline solids ( about 40°C), cooled to 5°C, kept stirring for 4 hours for crystallization, filtered to obtain 233g of pure white product, and dried to obtain 214g of white transparent crystalline powder solid.

Embodiment 2

[0037]In a 1000ml three-necked flask, add 250g of technical grade thymol, add 250ml of n-heptane solvent, and replace the air in the reaction flask with nitrogen. The brain was fully dissolved and clear; 5.0 g of activated clay was added, and the decolorization was maintained for about 30 minutes; filtered, the filtrate was naturally cooled, and slowly stirred until granular solids were precipitated on the wall of the reaction vessel. The solid (about 40°C) was cooled to 3°C, kept stirring for 2 hours for crystallization, filtered to obtain 231g of pure white product, and dried to obtain 206g of white transparent crystalline powder solid.

Embodiment 3

[0039] In a 1000ml three-necked flask, add 250g of technical grade thymol, add 250ml of n-octane solvent, and replace the air in the reaction flask with nitrogen. The brain was fully dissolved and clear; 2.0 g of chromatographic silica gel powder was added, and the decolorization was maintained for about 1 h; filtered, the filtrate was cooled naturally, and slowly stirred until granular solids were precipitated on the wall of the reaction vessel, and the stirring speed was adjusted. Crystalline solid (about 40°C), cooled to 1°C, kept stirring for 6 hours, filtered to obtain 248g of pure white product, and dried to obtain 186g of white transparent crystalline powder solid.

[0040] The components of the white transparent crystalline powder solids obtained in Examples 1-3 of the present invention were analyzed, and the results are shown in Table 1.

[0041] Component analysis method:

[0042] Detection instrument: gas chromatograph, Shimadzu GC-2030

[0043] Detector: FID

[...

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