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Method for separating coumarin from cinnamon oil heavy fraction

A technology for heavy fractions and cinnamon oil, applied in directions such as organic chemistry, can solve problems such as being unsuitable for industrial production, large consumption of organic solvents, high consumption of organic solvents, etc., to achieve environmental protection, reduce production costs, and avoid yields reduced effect

Pending Publication Date: 2020-08-18
GUANGXI FORESTRY RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although solvent extraction of coumarin is simple in operation and low in cost, it consumes a lot of organic solvents, takes a long time to extract, and the purity is difficult to guarantee; the separation and purification of coumarin by thin-layer chromatography has a low yield and a small amount of treatment, so it is not suitable for industrial production; The extraction and purification of coumarin by resin adsorption method is fast and the processing capacity is large, but the consumption of organic solvent is large and the cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A method for separating coumarin from cinnamon oil heavy fraction, it may further comprise the steps:

[0024] (1) Mix 100kg of heavy fraction of cinnamon oil with 600kg of water at 90°C to obtain an oil-water mixture, then stir the oil-water mixture for 2.5 hours at a stirring rate of 40r / min and then transport it to an oil-water separator for oil-water separation. Next, cool the water phase obtained from the oil-water separation to 15°C, then let it stand at constant temperature for 8 hours to precipitate the precipitate, and filter it with a 200-mesh filter membrane to obtain the enriched precipitate; the cooling rate is controlled at 7°C / min;

[0025] (2) The precipitate obtained in step (1) is pre-cooled at -80°C, and then freeze-dried. The freeze-drying time is 48h, and the cold trap temperature is -60°C, and then homogenized , can obtain coumarin, and the obtained coumarin yield is 83.1%;

[0026] (3) The liquid obtained by filtering in step (1) is subjected to ...

Embodiment 2

[0028] A method for separating coumarin from cinnamon oil heavy fraction, it may further comprise the steps:

[0029] (1) Mix 100kg of cinnamon oil heavy fraction with 600kg of water at 90°C to obtain an oil-water mixture, then stir the oil-water mixture for 0.5h at a stirring rate of 40r / min and then transport it to an oil-water separator for oil-water separation, then Cool the water phase obtained from the oil-water separation to 10°C, and then stand at constant temperature for 7 hours to precipitate the precipitate, and use a filter membrane with a size of 250 mesh to filter to obtain the enriched precipitate; the cooling rate is controlled at 6°C / min;

[0030] (2) The precipitate obtained in step (1) is pre-cooled at -80°C, and then freeze-dried. The freeze-drying time is 48h, and the cold trap temperature is -60°C, and then homogenized , can obtain coumarin, and the obtained coumarin yield is 82.7%;

[0031] (3) The liquid obtained by filtering in step (1) is subjected t...

Embodiment 3

[0033] A method for separating coumarin from cinnamon oil heavy fraction, it may further comprise the steps:

[0034] (1) Mix 100kg of cinnamon oil heavy fraction with 600kg of water at 90°C to obtain an oil-water mixture, then stir the oil-water mixture for 1.5h at a stirring rate of 40r / min and then transport it to an oil-water separator for oil-water separation, then Cool the water phase obtained from the oil-water separation to 13°C, and then stand at constant temperature for 6 hours to precipitate the precipitate, and use a filter membrane with a size of 300 mesh to filter to obtain the enriched precipitate; the cooling rate is controlled at 5°C / min;

[0035] (2) The precipitate obtained in step (1) is pre-cooled at -80°C, and then freeze-dried. The freeze-drying time is 48h, and the cold trap temperature is -60°C, and then homogenized , can obtain coumarin, and the obtained coumarin yield is 82.9%;

[0036] (3) The liquid obtained by filtering in step (1) is subjected t...

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Abstract

The invention discloses a method for separating coumarin from a cinnamon oil heavy fraction. The method comprises the following steps: (1) mixing a cinnamon oil heavy fraction and water according to amass ratio of 1:(6-15) to obtain an oil-water mixture, stirring the oil-water mixture for 0.5-2.5 hours, carrying out oil-water separation, cooling the water phase obtained in oil-water separation to10-15 DEG C, standing at a constant temperature to separate out precipitates, and filtering to obtain enriched precipitates; (2) carrying out freeze drying on the precipitates, and then carrying outa homogenization treatment to obtain coumarin; and (3) purifying the liquid obtained by filtering in the step (1), heating to 90 DEG C, and mixing with the cinnamon oil heavy fraction as the water inthe step (1). The method is simple to operate, low in cost, green, environment-friendly, high in coumarin yield and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of spice monomer processing, and in particular relates to a method for separating coumarin from heavy fractions of cinnamon oil. Background technique [0002] Cinnamon( Cinnamomum cassia Presl .) Also known as cinnamon, it belongs to the evergreen tree of Lauraceae, mainly distributed in Guangxi, Guangdong, Yunnan, Fujian and other places. It is the main economic tree species in subtropical regions of my country. Chinese cinnamon accounts for 70% of the world's cinnamon production, and Guangxi's production accounts for 50% of. Cinnamon oil is an aromatic oil obtained by distillation of cinnamon leaves, in which the content of cinnamaldehyde is about 75-85%, the content of cinnamyl acetate is about 6-9%, and the content of coumarin is about 1-4%. At present, the deep processing direction of cinnamon oil mainly includes the isolation of main components such as cinnamaldehyde, cinnamyl acetate, and o-methoxyci...

Claims

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Application Information

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IPC IPC(8): C07D311/10
CPCC07D311/10
Inventor 吴建文陆顺忠陆葆荣杨素华黎贵卿关继华邱米汤星月
Owner GUANGXI FORESTRY RES INST
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