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Method for recovering 1,8-eucalyptol from eucalyptus oil by product

A technology of eucalyptol and eucalyptus oil, which is applied in the field of recycling, can solve the problems of many operation steps, unfavorable industrial production, waste acid liquid discharge and the like

Inactive Publication Date: 2013-01-02
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Since 1,8-cineole, limonene, and cymene have similar boiling points, it is difficult to recover high-purity 1,8-cineole from eucalyptus oil by-products by ordinary distillation methods
In the prior art, although Davis and Tan Xinzhi etc. have reported that the acidic solution composed of sulfuric acid and phosphoric acid is used as the extraction agent to reclaim eucalyptol from eucalyptus oil by-products (US3923837, CN8610884), the defect in this method is that the operation There are many steps and a large amount of waste acid is discharged, which is not conducive to industrial production and environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In the heating still equipped with rectification packing tower (30 plates), add 1210 parts of phenol, 2150 parts of eucalyptus oil by-products (1,8-cineole content 37wt%), maintain system pressure 2.4kPa , heating and stirring for 0.5h, after 40min of total reflux, adjust the reflux ratio to 2:2, remove pinene, limonene, p-cymene and other impurity components in the range of 52-70°C at the top of the kettle, and the removal time After 2h, the rectification was stopped and cooled to obtain 2432 parts of bottom liquid.

[0021] Use this rectification device to continue the experiment. Add 2,500 parts of tap water to the obtained bottom liquid, reflux for 1 hour, adjust the reflux ratio to 2:2, take the distillate whose top temperature is 96-98° C. for 3 hours, and stop rectification. The obtained fraction was placed in a separatory funnel, the water layer was separated, the oil layer was taken, and dried over anhydrous sodium sulfate to obtain 560 parts of 1,8-cineole wi...

Embodiment 2

[0023] In the heating still equipped with rectification packed tower (50 trays), add 1720 parts of phenol, 2150 parts of eucalyptus oil by-products (1,8-cineole content 45wt%), maintain system pressure 3.2kPa , heated and stirred for 0.5h, after 50min of total reflux, adjust the reflux ratio to 4:1, remove pinene, limonene, p-cymene and other impurity components within the temperature range of 55-68°C at the top of the kettle, and the removal time After 5h, the rectification was stopped and cooled to obtain 2840 parts of bottom liquid.

[0024] Use this rectification device to continue the experiment. Add 3000 parts of tap water to the obtained bottom liquid, reflux for 1 hour, adjust the reflux ratio to 2:2, take the distillate whose top temperature ranges from 95 to 100° C. for 2 hours, and stop rectification. The obtained fraction was poured into a slender beaker and allowed to stand, and the water layer was slowly poured off. The oil layer was taken and dried over anhydro...

Embodiment 3

[0026] In the heating still equipped with rectification packing tower (number of trays 70), add 1500 parts of phenol, 1500 parts of eucalyptus oil by-products (1,8-cineole content 50wt%), maintain system pressure 4.0kPa , heating and stirring for 40min, total reflux for 1h, adjust the reflux ratio to 2:2, remove pinene, limonene, p-cymene and other impurity components in the range of 50-75°C at the top temperature, and the removal time is 1.5h , stop the rectification, and cool down to obtain 2300 parts of bottom liquid.

[0027] The still bottom liquid was changed to another set of rectification device (tray number 20) to continue the experiment. Add 4000 parts of tap water to the obtained bottom liquid, reflux for 50 minutes, adjust the reflux ratio to 2:2, take the distillate at the top temperature of 92-100°C for 2.5 hours, and stop the rectification. The obtained fraction was poured into a separatory funnel, and the oil layer was taken and dried with anhydrous calcium ch...

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PUM

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Abstract

The invention discloses a method for recovering 1,8-eucalyptol from eucalyptus oil by products; the eucalyptus oil by products are subject to two-step rectification, wherein in the first step, phenol is added into the eucalyptus oil by products, and then reduced-pressure rectification is performed to obtain kettle bottom liquid; in the second step, water is added into the kettle bottom liquid, then normal pressure rectification is performed to obtain an azeotrope of 1,8-eucalyptol and water; a water layer of the azeotrope is removed by layering; the azeotrope is dried to obtain the 1,8-eucalyptol product. The method of the invention provides a 1,8-eucalyptol recovery rate of more than 70% and a purity of more than 98%, and has the advantages of simple operation, short rectification time, high recovery rate, green and environmental protection, and suitability for industrial application.

Description

technical field [0001] The invention relates to a method for recovering 1,8-cineole from eucalyptus oil by-products. The prepared 1,8-cineole can be used as spice essence in food or daily chemical industries, and can also be used as in the field of medicine. Background technique [0002] Eucalyptus oil is an aromatic essential oil secreted by eucalyptus leaf gland cells. It is one of the top ten essential oils in the world. It has a unique aroma and various biological activities. It is widely used in daily chemical, food, medicine and other fields. The main component of eucalyptus oil is 1,8-cineole. 1,8-Cineole has a camphor-like aroma, which can be used in the preparation of edible and daily flavors, and is also the main medicinal ingredient in medicine, which can play the role of antibacterial, anti-inflammatory, and insecticidal. Recent studies have shown that 1 , 8-cineole has a good effect on inhibiting the growth of white blood cells, which endows it with greater ap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/08
Inventor 谢建春王石孙宝国李友宏郑福平孙金沅黄明泉
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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