Method for separating high-purity cinnamyl aldehyde and cinnamyl acetate from cinnamon oil

A technology of cinnamyl acetate and cinnamon oil, which is applied in the separation/purification of carbonyl compounds, preparation of carboxylic acid esters, chemical instruments and methods, etc., can solve the problems of increasing environmental protection pressure, loss, and low purity, and achieve improved yield, Prevents oxidation at high temperature and increases separation efficiency

Inactive Publication Date: 2013-10-09
GUANGXI FORESTRY RES INST
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The cinnamon aldehyde is purified by the freeze-out method, although the stability of the heat-sensitive substance can be guaranteed, but the purity cannot meet the high requirements; the addition method adopts the addition of thiosulfite and aldehydes, and the addition Dissolve in water, separate and remove non-aldehyde substances, and then release aldehyde substances with acid substances to achieve the purpose of purifying aldehyde substances, but consume a large amount of thiosulfite, which increases the cost and increases environmental protection. pressure
Chinese patent CN101768510A discloses a method for increasing the content o

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  • Method for separating high-purity cinnamyl aldehyde and cinnamyl acetate from cinnamon oil

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Embodiment 1

[0014] The method for separating high-purity cinnamaldehyde, cinnamyl acetate from cinnamon oil of the present invention comprises the steps:

[0015] 1000.0 g of cinnamon oil with a cinnamaldehyde content of 83% and a acetic acid cinnamaldehyde content of 1.5% is divided into glass containers, and 250 g of NaCl is added for pretreatment. The temperature of the kettle is 145°C, the vacuum degree is 2mmHg, the total reflux is 30min, and then rectification is carried out with a reflux ratio of 10:1. When the purity of cinnamaldehyde reaches 99%, the reflux ratio is changed to 1:4, and the cinnamaldehyde product is received. After receiving the cinnamaldehyde product, the temperature of the kettle was raised to 150°C, the vacuum degree remained unchanged, and the total reflux was carried out for 30 minutes, and then rectification was carried out at a reflux ratio of 10:1. When the purity of cinnamyl acetate reached 95%, the reflux ratio became 1:4, receive cinnamyl acetate produc...

Embodiment 2

[0017] Another example of the method for separating high-purity cinnamaldehyde, cinnamyl acetate from cinnamon oil of the present invention, comprises the steps:

[0018] Pack 1000.0 g of cinnamon oil with cinnamaldehyde content of 83% and acetic acid cinnamaldehyde content of 1.5% into a glass container, add 125g of NaCl for pretreatment, put the treated cinnamon oil into the rectification tower kettle, and rectify tower kettle The temperature is 150°C, the vacuum degree is 8mmHg, the total reflux is 20min, and then rectification is carried out with a reflux ratio of 8:1. When the purity of cinnamaldehyde reaches 99%, the reflux ratio is changed to 1:4, and the cinnamaldehyde product is received. After receiving the cinnamaldehyde product, the temperature of the kettle was raised to 155°C, the vacuum degree remained unchanged, and the total reflux was carried out for 20 minutes, and then rectification was carried out at a reflux ratio of 8:1. When the purity of cinnamyl acetat...

Embodiment 3

[0020] Yet another example of the method for separating high-purity cinnamaldehyde, cinnamyl acetate from cinnamon oil of the present invention, comprises the steps:

[0021] Pack 1000.0 g of cinnamon oil with cinnamaldehyde content of 83% and acetic acid cinnamaldehyde content of 1.5% into a glass container, add 200g of NaCl for pretreatment, put the treated cinnamon oil into the rectification tower kettle, and rectify tower kettle The temperature is 148°C, the vacuum degree is 5mmHg, the total reflux is 40min, and then rectification is carried out with a reflux ratio of 7:1. When the purity of cinnamaldehyde reaches 99%, the reflux ratio is changed to 1:4, and the cinnamaldehyde product is received. After receiving the cinnamaldehyde product, the temperature of the kettle was raised to 153°C, the vacuum degree remained unchanged, and the total reflux was carried out for 40 minutes, and then rectification was carried out at a reflux ratio of 7:1. When the purity of cinnamyl ac...

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Abstract

The invention discloses a method for separating high-purity cinnamyl aldehyde and cinnamyl acetate from cinnamon oil. The method comprises the following steps of: (1) performing pre-treatment, specifically, taking the cinnamon oil obtained by extracting cinnamon branches and leaves via steam distillation as a raw material, and adding water-absorbed salt substances in the cinnamon oil to remove water; and (2) pouring the cinnamon oil after the pre-treatment is finished in the tower kettle of a rectification tower, controlling the temperature of the tower kettle, a reflux ratio and a vacuum degree, performing low-temperature and high-vacuum rapid rectification, and separating simultaneously to obtain two products, namely, high-purity cinnamyl aldehyde and cinnamyl acetate, wherein the purity of cinnamyl aldehyde is not less than 99%, and the yield thereof is not less than 80%; and the purity of cinnamyl acetate is not less than 95%, and the yield thereof is not less than 60%. With the adoption of the method disclosed by the invention, cinnamyl aldehyde can be prevented from being oxidized at a high temperature, thus increasing the yield and increasing the separation efficiency.

Description

technical field [0001] The invention relates to the field of purification and processing of spice monomers, in particular to a method for separating high-purity cinnamaldehyde and cinnamyl acetate from cinnamon oil. Background technique [0002] Cinnamon, also known as cinnamon, has a strong cinnamon aroma from its bark, branches, leaves, and fruit receptacle. It is extracted by steam distillation to obtain cinnamon oil. Its main chemical components are cinnamaldehyde, cinnamyl acetate, ethyl cinnamate, and benzyl benzoate. Esters, benzaldehyde, coumarin, trans-cinnamic acid, trans-methoxycinnamyl ester, etc. Cinnamaldehyde is mainly used to make daily flavors such as jasmine, lily of the valley, rose, etc. It is also used in food spices to make food have cinnamon flavor. Cinnamaldehyde is also an intermediate of medicine. Cinnamyl acetate is mainly used as a blending spice and fixative for hyacinth, clove, lily of the valley, jasmine, mast and other flavors, and a flavor c...

Claims

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Application Information

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IPC IPC(8): C07C47/232C07C45/82C07C69/157C07C67/54
Inventor 陆顺忠邱米黎贵卿关继华陈震华江燕陈平曾辉苏骊华
Owner GUANGXI FORESTRY RES INST
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