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Method for extracting cedrene and cedrol from cedar oil

A technology of cedar alcohol and fir oil, which is applied in chemical instruments and methods, purification/separation of hydrocarbons, preparation of organic compounds, etc., can solve the problems of solvent loss, high energy consumption, solvent residue, etc., to avoid solvent loss and energy The effect of consumption

Active Publication Date: 2014-12-24
广西庚源香料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing technology of extracting cedarwood alcohol from Chinese fir oil, through the method of cryogenic freezing and crystallization, requires refrigeration, consumes a lot of energy, and also uses a large amount of solvent ethanol (solid-liquid ratio60%), There is solvent loss and solvent carryover

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 5t of Chinese fir oil obtained by extracting Chinese fir roots by water vapor method, properties: colorless liquid, with characteristic aroma of Chinese fir, relative density 0.9885, refractive index 1.4608, optical rotation +0.5°, main components: α-pinene 3.7%, α-pine Oleyl alcohol 3.5%, Terpine acetate 1.6%, Longifolene 1.3%, β-Elemene 2.3%, α-Cedrene 21.8%, β-Cedrene 9.5%, Thumbene 2.0%, Geranium 3.3% %, 2.2% of α-cyperene, 1.7% of cedrene, 28.9% of cederyl alcohol, and 1.1% of cederyl acetate.

[0026] Add fir oil to the still of the distillation column. Control the temperature of the tower bottom at 130-150°C, the temperature of the top of the tower at 80-110°C, the degree of vacuum <-0.09MPa, the fractionation time of 1-2h, fractionate α-pinene, cedrene and other light components from the top of the tower, The cedaryl alcohol content of the heavy component is more than or equal to 60%. The tower kettle is cooled to 70-90°C, and the heavy components in the tower...

Embodiment 2

[0029] 5t of Chinese fir oil obtained by extracting Chinese fir root by water vapor method, properties: yellow liquid, characteristic aroma of Chinese fir, relative density 0.9875, refractive index 1.4610, optical rotation +0.5°, main components: α-pinene 2.8%, α-pine oil Alcohol 3.7%, α-cedrene 20.9%, β-cedrene 10.0%, geranol 3.2%, cedrene alcohol 30.5%.

[0030]Adding 0.5% of activated carbon by mass to Chinese fir oil, stirring at 60-75° C. for 0.5-1 hour, and filtering to remove the activated carbon to obtain a pretreated colorless Chinese fir oil. It is then added to the distillation column pot. Refer to Example 1 for other operating procedures. At this time, 1.2t of cedaryl alcohol was obtained, with a yield of 75%, and a cedaryl alcohol content of 92%. The obtained cedrene was 1.55t, the yield was 90%, and the cedrene content was 90%.

Embodiment 3

[0032] 5t of Chinese fir oil obtained by extracting Chinese fir root by water vapor method, properties: colorless liquid, with characteristic aroma of Chinese fir, relative density 0.9884, refractive index 1.4607, optical rotation +0.5°, main components: α-pinene 3.9%, β-olium 2.5% myrcene, 23.8% α-cypressene, 9.8% β-cypressene, 2.3% pagodacene, 3.2% geranyl, 2.4% α-cypressene, and 25.9% cedrene.

[0033] Add 2% of its weight anhydrous sodium sulfate in fir oil, filter after stirring, remove residual moisture in fir oil, then add distillation tower still. Refer to Example 1 for other operating procedures. At this time, 0.9t of cedaryl alcohol was obtained, the yield was 75%, and the content of cedaryl alcohol was 97%. The obtained cedrene was 1.52t, the yield was 85%, and the cedrene content was 94%.

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Abstract

The invention discloses a method for extracting cedrene and cedrol from cedar oil. The method comprises the following steps: firstly, distilling out light components from cedar oil by using a distillation method, so that the content of cedrol in heavy constituent cedar oil in the kettle is greater than or equal to 60%; naturally cooling and crystallizing; crushing and carrying out high-speed centrifugal separation to obtain crude cedrol; fusing and recrystallizing the crude cedrol, removing impurities clad in the cedrol crystallization process, so as to obtain a cedrol product; mixing centrifugate obtained after centrifuging twice with the light component obtained through distillation; and adding to a packing tower, so as to obtain the product cedrene by adopting vacuum fractionation, wherein the cedrene content of the product is greater than or equal to 90%, and the cedrene content is greater than or equal to 85%.

Description

technical field [0001] The invention relates to the technical field of extracting natural flavors and fragrances, in particular to a method for extracting cedrene and cedrene from fir oil. Background technique [0002] Chinese fir oil is mainly obtained by steam distillation of fir roots, sawdust, branches and leaves, fruits, etc., and its main components are cedryl alcohol, α-cedryne, β-cedryne, α-terpineol, myrcene, elemi ene, cypressene, phoenixene, etc. The deep-processed products of Chinese fir oil, such as acetyl cedrene, methyl cedryl ether, cedryl acetate and cedryl ketone, etc., have a relatively long lasting time because of their sweet woody, sandalwood and ambergris aromas. High aroma value, widely used in various types of perfumes, including cologne and toilet water, also used in cosmetic essences (lipstick, cream, powder, etc.) and soap essences, as well as fragrances of various household products. Fragrance is the soul of spices. To use fir oil to synthesize ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C35/37C07C29/76C07C29/78C07C7/00C07C7/04C07C13/605
CPCC07C7/005C07C7/04C07C29/76C07C29/78C07C29/80C07C2603/66C07C35/37C07C13/605
Inventor 陆顺忠孟中磊李秋庭杨漓关继华黎贵卿邱米杨素华苏骊华党中广
Owner 广西庚源香料有限责任公司
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