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Prepn process and plant of high-purity eudesmin

A high-purity technology for eucalyptol, applied in the field of preparation of high-purity eucalyptol, can solve the problems of complex operation, low single-step yield, strict process requirements, etc., and achieve simple operation, high separation efficiency and high yield Effect

Inactive Publication Date: 2004-10-20
YUNNAN CHEM RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent (CN1064700A) introduces the traditional method of crystallization and purification, using eucalyptus oil with a purity of 80% as a raw material to freeze and crystallize at -8°C to -20°C for 48 hours, and to separate the raffinate with a high-speed centrifuge to obtain the purity The yield of 99% eucalyptol is 21%-42.5%. This method has simple process and small investment in equipment, but this method cannot produce products with higher purity, and the production cycle is long, so it is difficult to adjust the production through the process according to market conditions. different purity products
But to make a product with a purity greater than or equal to 99%, it is necessary to prepare a eucalyptus oil raw material with a purity greater than or equal to 90%. Another shortcoming of this process is that the single-step yield is low and the process requirements are strict. Operation under temperature curve conditions, the operation is more complicated

Method used

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  • Prepn process and plant of high-purity eudesmin

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Experimental program
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Effect test

Embodiment 1

[0028] Put 2000 grams of eucalyptus oil with a purity of 80% into the crystallizer, and feed -11°C circulating freezing liquid into the jacket. Under stirring, lower the temperature of the material to -9°C, put in a small amount of eucalyptol seed crystals, and confirm that the crystallization is triggered successfully, and keep it at -11°C in the jacketed circulating refrigerant for 1 hour; then average the bath temperature every 30 minutes Lower the temperature at a rate of 2-3°C, drop to -20°C after two hours, and keep at the bath temperature of -20°C for 2 hours. Stop stirring, discharge the raffinate in the crystallizer, and use vacuum filtration to extract the raffinate as much as possible. Stop suction filtration and pass hot water of about 30°C to 40°C into the top heat exchanger in the crystallizer to raise the temperature of the upper space in the crystallizer to about 10°C to 20°C, and the surface of the crystal layer is 0°C to -2°C , to sweat the crystals left in ...

Embodiment 2

[0030] Put 2500 grams of eucalyptus oil with a purity of 83% into the crystallizer, and feed -11° C. circulating freezing liquid into the jacket. Under stirring, lower the temperature of the material to -9°C, put in a small amount of eucalyptol seed crystals, and confirm that the crystallization is triggered successfully, and keep it at -11°C in the jacketed circulating refrigerant for 1 hour; then average the bath temperature every 30 minutes Decrease the bath temperature to -27°C at a rate of 2.5°C to 4°C, and keep the bath temperature at -27°C for two hours. Stop stirring, discharge the raffinate in the crystallizer, and use vacuum filtration to extract the raffinate as much as possible. Stop the suction filtration and pass hot water of about 30°C to 40°C into the top heat exchanger in the crystallizer to raise the temperature of the upper space in the crystallizer to about 10°C to 20°C, and carry out the crystallization process on the crystallization left in the crystalliz...

Embodiment 3～ Embodiment 7

[0032] Example name

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Abstract

The present invention is preparation process and plant of high-purity eudesmin. The purification process includes three steps of crystallization, sweating and fusion crystallization completed in one identical apparatus and needs no subsequent treatment before obtaining ultimate product. Compared with falling-film crystallization process and conventional fusion crystallization process, the process is simple, high in separation efficiency and yield. Through the said process and with eucalyptus oil with eudesmin content greater than 70% as material, eudesmin product of 99.5% higher purity may be produced in the eudesmin yield of 33-51%.

Description

technical field [0001] The invention relates to a method for separating and purifying fine chemical products, more specifically the invention relates to a method for preparing high-purity eucalyptol and a device for realizing the method. Background technique [0002] Eucalyptol is an important fine chemical product, widely used in industrial catalysis, medicine, food, daily necessities and other fields; it can be obtained from terpenoids such as pinene, and can also be refined from eucalyptus oil. After 60% crude eucalyptus oil is rectified, its purity can generally be increased to about 80% to 88%. Since the main components of crude eucalyptus oil are eucalyptol, limonene and p-cymene, their boiling points are 176.0°C, 177.7°C and 177.1°C respectively, and the difference is very small. element content. [0003] At present, the methods for refining eucalyptol from eucalyptus oil include: supercritical extraction, silica gel column chromatography, c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/08
Inventor 王志刚吴佳和国红范艳红
Owner YUNNAN CHEM RES INST