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Ultrasonic reinforced subcritical water extraction method of natural product effective ingredient and device

A technology of ultrasonic strengthening and active ingredients, applied in separation methods, chemical instruments and methods, solvent extraction, etc., can solve the problems of long extraction time, low extraction efficiency, high energy consumption, shorten extraction time, easy to popularize and apply, The effect of the simple structure of the device

Inactive Publication Date: 2008-10-01
SOUTH CHINA UNIV OF TECH
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  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Heat reflux extraction and organic solvent extraction are traditional extraction methods of active ingredients in natural products, which are simple in process and easy to operate, but there are problems such as long extraction time, low extraction efficiency, and high energy consumption.
In order to solve these problems, in recent years, supercritical CO 2 Extraction technology has been applied to the extraction of active ingredients of natural products. This technology has been praised for its advantages of environmental protection, high product quality, and easy control of the production process. However, due to the commonly used fluid CO 2 Due to the characteristics of non-polarity and low relative molecular weight, this technology can only be used for the extraction of non-polar compounds. It lacks sufficient solubility for many substances with polarity and large relative molecular weight, so the extraction efficiency is not high, and it is difficult to achieve the ideal extraction efficiency. extraction effect
Therefore, in actual operation, an organic entrainer must be added to the extraction system to increase the solute in CO 2 Solubility and selectivity in the fluid, which not only increases the complexity of the operation, but also has the problem of residual organic solvents
In addition, since water is insoluble in CO 2 , so supercritical CO 2 The extraction process often needs to pre-dry the raw materials, which increases the cost

Method used

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  • Ultrasonic reinforced subcritical water extraction method of natural product effective ingredient and device
  • Ultrasonic reinforced subcritical water extraction method of natural product effective ingredient and device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0033] Example 1: Extraction of volatile oil from cloves

[0034] Slowly open the regulating valve of the nitrogen tank, pass the nitrogen gas into the deionized water of the reservoir, and process for about 30 minutes; weigh 0.5 kg of clove powder that has been crushed to 60 meshes, put it into a 2L extraction kettle, and set the Temperature, pressure, ultrasonic and other parameters, turn on the pre-heater and pressure pump, add about 1.5 kg of pre-heated water at a flow rate of 10ml / min, under the conditions of temperature 150°C, pressure 2MPa, ultrasonic power 100W, ultrasonic frequency 20KHz, the effect After 60min, the extract was discharged from the bottom of the extraction kettle, cooled and collected by a cooler; then 50g of sodium chloride was added to the collected extract to break the water-oil equilibrium state of the extract, and 400ml of hexane was separated hexane layer, and remove the hexane with a vacuum rotary evaporator to obtain the volatile oil of cloves;...

Embodiment example 2

[0035] Implementation Case 2: Extraction of Anthraquinones from Morinda Citrifolia Root

[0036] Slowly open the regulating valve of the nitrogen tank, pass nitrogen gas into the deionized water of the reservoir, and process for about 60 minutes; weigh 0.6 kg of Morinda officinalis powder that has been crushed to 100 meshes, put it into a 2L extraction kettle, and set up the control panel Turn on the pre-heater and pressure pump, add about 1.6 kg of pre-heated water at a flow rate of 30ml / min, under the conditions of temperature 120°C, pressure 5MPa, ultrasonic power 150W, and ultrasonic frequency 40KHz After 120 minutes of action, the extract was released from the bottom of the extraction kettle, cooled and collected by a cooler. At the same time, a comparative experiment between ultrasonically enhanced subcritical water extraction and traditional solvent method and ultrasonic-assisted extraction method was carried out. The experimental results showed that when the extraction...

Embodiment example 3

[0037] Example 3: Extraction of fennel oil from fennel leaves

[0038] Slowly open the regulating valve of the nitrogen tank, pass the nitrogen gas into the deionized water of the reservoir, and process for about 20 minutes; weigh 0.2 kg of fennel coarse powder crushed to 40 meshes, put it into a 2L extraction kettle, and set the Temperature, pressure, ultrasonic and other parameters, turn on the preheater and pressure pump, add about 1 kg of preheated water at a flow rate of 70ml / min, under the conditions of temperature 110°C, pressure 7MPa, ultrasonic power 200W, ultrasonic frequency 80KHz, the effect After 30 minutes, the extract was discharged from the bottom of the extraction kettle, cooled and collected by a cooler; then 30 g of sodium chloride and 100 ml of hexane were added to the collected extract, the hexane layer was separated, and the hexane was removed by a vacuum rotary evaporator. Alkanes can be used to obtain volatile oil; then the resulting volatile oil is ana...

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Abstract

The invention provides an extraction method and a device used for extracting ultrasonic reinforced sub-critical water of effective component of a natural outcome. The method is mainly characterized in that a pre-disposed raw material is arranged in an extraction kettle; the sub-critical water is taken as an extraction solvent to carry out the exaction under the conditions of 1 to 20MPa of extraction pressure, 50 to 500W of ultrasonic power and 20 to 80KHz of ultrasonic frequency. The method has high extraction efficiency and short extraction time. The device is mainly characterized in that the extraction kettle is provided with an ultrasonic reinforced part which comprises an ultrasonic generator and an energy changing head; the ultrasonic generator is arranged on the external surface of the extraction kettle and at the upper part of the extraction kettle; the energy changing head and the extraction kettle cover are processed into a whole; the piezoelectric ceramic wafer of the energy changing head is arranged at the upper end of the extraction kettle cover; the variable-spoke rod of the energy changing head is directly arranged in the extraction kettle by the extraction kettle cover. The device can carry out selectable exaction of the articles to be extracted by changing the extraction parameters (temperature, pressure, time, etc.), thus realizing static extraction or dynamic circulation extraction.

Description

technical field [0001] The invention relates to a device and a method for extracting active ingredients in natural products, in particular to a device and a method for extracting active ingredients in natural products by ultrasonic enhanced subcritical water extraction technology. Background technique [0002] Heat reflux extraction and organic solvent extraction are traditional extraction methods of active ingredients in natural products, which are simple in process and easy to operate, but there are problems such as long extraction time, low extraction efficiency, and high energy consumption. In order to solve these problems, in recent years, supercritical CO 2 Extraction technology has been applied to the extraction of active ingredients of natural products. This technology has been praised for its advantages of environmental protection, high product quality, and easy control of the production process. However, due to the commonly used fluid CO 2 Due to the characteristi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/02B01J19/10
CPCB01D11/0203B01D11/0265
Inventor 丘泰球郭娟杨日福范晓丹邢晓阳孔令会吴进卫邢光辉
Owner SOUTH CHINA UNIV OF TECH
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