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Isolation method for high purity anethole

A high-purity, anethole technology, applied in ether separation/purification, ether preparation, organic chemistry, etc., can solve the problems of low product yield and purity, and achieve the effects of reducing production costs and avoiding solvent residues

Inactive Publication Date: 2012-06-13
GUANGXI FORESTRY RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN101898941A "A Method for Purifying Trans-Anethole" discloses a method for purifying trans-anethole from anise oil through a two-step process coupled with freezing crystallization and molecular distillation. Although no solvent is used, the product is obtained Both the rate and the purity are not high

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  • Isolation method for high purity anethole

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Effect test

Embodiment 1

[0016] A kind of high-purity anethole isolation method of the present invention comprises the following steps:

[0017] Pack 7000kg of fennel oil with anethole content of 88.5% into stainless steel trays, freeze at 4°C for 20 hours, crush the frozen blocky fennel crystals with a crusher, the particle size is 20 mesh, and then crush the fennel oil Put the crystals into a centrifuge with a cloth bag, centrifuge for 20 minutes at 1600r / min, thaw the centrifuged anethole crystals, and then put them into the rectification column. The reflux ratio at the beginning of the rectification is 10:3. The kettle temperature is 125°C, the vacuum degree is 5mmHg, and when the purity of anethole reaches 99.6%, the reflux ratio becomes 1:7. After rectification, a total of 5952 kg of anethole products with a content greater than 99.6% were obtained.

Embodiment 2

[0019] A kind of high-purity anethole isolation method of the present invention comprises the following steps:

[0020] Pack 6000kg of fennel oil with anethole content of 88.5% into stainless steel trays, freeze at 2°C for 15 hours, crush the frozen blocky fennel crystals with a crusher, the particle size is 40 mesh, and then crush the fennel oil Put the crystals into a centrifuge with a cloth bag, centrifuge for 15 minutes under the condition of 1800r / min, thaw the centrifuged anethole crystals, and then put them into the rectification column. The reflux ratio at the beginning of the rectification is 10:4, The temperature of the tower kettle is 129° C., the vacuum degree is 7 mmHg, and when the purity of anethole reaches 99.6%, the reflux ratio becomes 1:6. After rectification, a total of 5039 kg of anethole products with a content greater than 99.6% were obtained.

Embodiment 3

[0022] A kind of high-purity anethole isolation method of the present invention comprises the following steps:

[0023] Pack 6500kg of fennel oil with anethole content of 88.5% into stainless steel trays and freeze at 0°C for 18 hours, crush the frozen blocky fennel crystals with a crusher to a particle size of 30 mesh, and then crush the crushed fennel oil Put the crystals into a centrifuge with a cloth bag, centrifuge for 18 minutes under the condition of 2000r / min, thaw the centrifuged anethole crystals, and then put them into the rectification column. The reflux ratio at the beginning of the rectification is 10:3, The temperature of the tower kettle is 135° C., the vacuum degree is 10 mmHg, and when the purity of anethole reaches 99.6%, the reflux ratio becomes 1:5. After rectification, a total of 5520 kg of anethole products with a content greater than 99.6% were obtained.

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Abstract

The invention provides an isolation method for high purity anethole. Anise oil is used as a raw material, and a product of high purity anethole is produced after the steps of refrigeration, fragmentation, centrifugation and rectification are carried out. According to the invention, crystallization separating and rectification separating are combined, anethole with a high purity of no less than 99.6% is produced, and no solvent is needed for rinsing of crystals, which enables residual of solvents to be avoided, production procedures to be reduced and production cost to be lowered down.

Description

technical field [0001] The invention relates to the field of spice processing, in particular to a method for isolating high-purity anethole, which is suitable for producing high-purity anethole from anet oil. Background technique [0002] my country is a big country in the production and export of natural spices, and many varieties can influence the international market, among which fennel oil accounts for more than 90% of the world trade. [0003] Anise oil, or star anise oil, is composed mainly of α-pinene, limonene, linalool, fennel, cis-anethol, anisaldehyde, trans-anethole, styroene, and cumin Ling et al., wherein the content of trans-anethole is 83-91%, and that of artemisinin is 3-8%. Anethole is widely used in food, medicine, daily necessities, veterinary medicine, feed, pesticide and other fields. Anethole can also be used to produce products such as anisaldehyde, anisonitrile, anisitol, raspberry ketone, and ethestrol. [0004] The high-purity isolated product o...

Claims

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Application Information

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IPC IPC(8): C07C43/215C07C41/40
Inventor 陆顺忠曾辉黎贵卿关继华邱米苏骊华
Owner GUANGXI FORESTRY RES INST
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