Method for purifying trans-anethole

A kind of technology of trans-anethole and purification method, applied in the purification field of trans-anethole, can solve the problems of oxidation or polymerization reaction of anethole, large solvent consumption, large consumption of organic solvent and energy consumption, etc. Biological activity, avoiding the use of organic solvents, the effect of solving product quality problems

Active Publication Date: 2010-12-01
SUN YAT SEN UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0005] 1. Solvent freezing and crystallization method (Wang Haiying et al., Natural Product Research and Development, 2000, 12(4): 105-108), this method is to utilize each component in fennel oil in an organic solvent (such as methanol, ethanol) at low temperature and acetone, etc.) for separation, but repeated freezing and crystallization treatment is required to consume a large amount of organic solvents and energy consumption, and the product has problems such as solvent residues that affect its quality
[0006] 2. Molecular distillation (Wang Qin et al., Forest Products Chemistry and Industry, 2007, 27 (3): 77-80), the operating conditions of this method are relatively mild, and can protect the unique biological activity of anethole to the greatest extent, but due to There are many components with the s

Method used

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Examples

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Embodiment 1

[0021] Place the beaker containing 100g of fennel oil in a low-temperature environment of -25°C and freeze for 8 hours, quickly crush the frozen body to 10 mesh, and separate it by suction filtration to obtain crystals and a filtrate containing more light components. After the crystals were slowly melted, through molecular distillation, the conditions of molecular distillation were as follows: the evaporation temperature was 25°C, the evaporation pressure was 100Pa, and the feed rate was 4.0mL / min to obtain 44.2g of anethole. The purity of anethole was 97.1%. The rate is 44.2%.

Embodiment 2

[0023] Place the beaker containing 100g of fennel oil in a low-temperature environment of -10°C and freeze for 2 hours, quickly crush the frozen body to 20 mesh, and separate it by suction filtration to obtain crystals and a filtrate containing more light components. After the crystals were slowly melted, molecular distillation was carried out. The conditions of molecular distillation were as follows: the evaporation temperature was 30° C., the evaporation pressure was 2 Pa, and the feed rate was 1.6 mL / min. 59.5 g of anethole was obtained, and the purity of anethole was 99.5%. The yield was 59.5%.

Embodiment 3

[0025] Place the beaker containing 100g of fennel oil in a low-temperature environment of 0°C for 5 hours, and quickly crush the frozen body to 30 mesh, and separate it by suction filtration to obtain crystals and a filtrate containing more light components. After the crystals were slowly melted, molecular distillation was carried out. The conditions of molecular distillation were as follows: the evaporation temperature was 50° C., the evaporation pressure was 10 Pa, and the feed rate was 1.0 mL / min to obtain 60.9 g of anethole. The purity of anethole was 99.1%. The yield was 60.9%.

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Abstract

The invention discloses a method for purifying trans-anethole. In the method, star anise oil is purified mainly by two steps of coupling freezing crystallization and molecular distillation so as to obtain the trans-anethole. The method comprises the following steps of: freezing the star anise oil at a low temperature, crushing the frozen product, performing separation of a crystal and residue liquid on the crushed frozen product by filtration, high-speed centrifugation or pressure filtration, melting the crystal, and performing molecular distillation on the liquid obtained by melting to obtain high-purity anethole. The method has the advantages of no need of solvent, mild operating conditions, low cost, low energy consumption, high purity, simple process and the like.

Description

technical field [0001] The invention relates to a method for purifying trans-anethole. Background technique [0002] Fennel oil, namely star anise oil, is an advantageous characteristic resource in southern my country, accounting for more than 90% of world trade. Its main component is trans-anethole, with a content of 83%-90%. Anethole is widely used in food, medicine, daily necessities, veterinary drugs, feed, pesticides and other fields; it can also be used to produce anisaldehyde, anisonitrile, anisyl alcohol, raspberry ketone, ethestrol and other products. [0003] With the development of refined products of fennel oil, especially in the fields of high-end spices, daily necessities, and pharmaceuticals, the demand for high-purity natural anethole is also increasing, and the market prospect is very broad. However, the composition of fennel oil extracted from natural plants is complex. In addition to containing a large amount of trans-anethole, other components with highe...

Claims

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Application Information

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IPC IPC(8): C07C43/215C07C41/40
Inventor 纪红兵陈英姚煜东周贤太曾晖柴坤刚
Owner SUN YAT SEN UNIV
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