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Method for supercritical fluid extraction of juglone in walnut seed green skin waste residue

A supercritical and juglone technology, applied in quinone separation/purification, bulk chemical production, organic chemistry, etc., to avoid thermal decomposition, ensure effectiveness, and widely apply

Inactive Publication Date: 2012-09-19
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the use of supercritical fluids to extract and purify natural products such as medicines and foods is receiving widespread attention. However, after searching, the method of using supercritical fluids to extract juglone, especially the use of SC-CO 2 (supercritical carbon dioxide fluid) the method for extracting juglone has not yet been reported

Method used

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  • Method for supercritical fluid extraction of juglone in walnut seed green skin waste residue
  • Method for supercritical fluid extraction of juglone in walnut seed green skin waste residue
  • Method for supercritical fluid extraction of juglone in walnut seed green skin waste residue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 10 kg green bark is crushed with a crusher and filtered. Take the crushed powder and put it into the extraction column, and follow the supercritical extraction operation steps. adjust CO 2 The flow rate is 1.5L / min, the extraction pressure is 15MPa, the extraction temperature is 50°C, and the extraction time is 15min. Fully contact with the raw material, after ensuring about 30min contact time, start to receive the product. Extraction with CO 2 Throttling expansion by micro-adjustment valve, extract and CO 2 After the gas is separated in the receiving bottle, it is received by the receiving bottle, CO 2 The volume is measured by a flow meter and then discharged. recycle.

[0029] After the extract was shaken with a solvent, it was concentrated by rotary evaporation under reduced pressure to obtain the product juglone, which was then tested for various indicators. Wherein, by AVATAR360 type Fourier transform infrared spectrometer and GCMS-QP2011S type gas chromato...

Embodiment 2

[0037] 10 kg green bark is crushed with a crusher and filtered. Take the crushed powder and put it into the extraction column, and follow the supercritical extraction operation steps. adjust CO 2 The flow rate is 1.0L / min, the extraction pressure is 18MPa, the extraction temperature is 65°C, and the extraction time is 10min. . Fully contact with the raw material, after ensuring about 30min contact time, start to receive the product. Extraction with CO 2 Throttling expansion by micro-adjustment valve, extract and CO 2 After the gas is separated in the receiving bottle, it is received by the receiving bottle, CO 2 The volume is measured by a flow meter and then discharged.

[0038] After the extract was shaken with a solvent, it was concentrated by rotary evaporation under reduced pressure to obtain the product juglone, which was then tested for various indicators. The extraction rate of juglone was 85%, the purity was 92%, and the yield was 0.20%.

Embodiment 3

[0040] 10 kg green bark is crushed with a crusher and filtered. Take the crushed powder and put it into the extraction column, and follow the supercritical extraction operation steps. adjust CO 2 The flow rate is 3.0L / min, the extraction pressure is 10MPa, the extraction temperature is 30°C, and the extraction time is 20min. Fully contact with the raw material, after ensuring about 30min contact time, start to receive the product. Extraction with CO 2 Throttling expansion by micro-adjustment valve, extract and CO 2 After the gas is separated in the receiving bottle, it is received by the receiving bottle, CO 2 The volume is measured by a flow meter and then discharged.

[0041] After the extract was shaken with a solvent, it was concentrated by rotary evaporation under reduced pressure to obtain the product juglone, which was then tested for various indicators. The extraction rate of juglone was 80%, the purity was 89%, and the yield was 0.19%.

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Abstract

The invention discloses a method for supercritical fluid extraction of juglone in walnut seed green skin waste residue. In the invention, supercritical CO2 fluid in the supercritical fluid extraction method is adopted for extracting, walnut seed external skin (green skin) waste residue which is high in juglone content and easily available is preferably selected as the raw material for extraction. The best conditions are as follows: flow rate of the supercritical CO2 fluid is 1-3L / min, the extraction pressure is 10-18MPa, the extraction temperature is below 65 DEG C and the extraction time is within 20min. In the invention, one-time extraction yield of the juglone reaches 87%, the product purity is 92%, the productive rate is 0.21%. The method of the invention features not only high extraction yield but also innocuity, no taste, incombustibility, no erosion, low price and easy recovering of the extraction liquid, thus meeting the requirements of environmental protection and industrialization. The extracted juglone is wide in application, the active ingredients play a role in resisting bacterium and cancer and calming nervus centralis, thus enjoying very wide application prospect inmedicine, agricultural chemical, dye and pH indicator and other fields.

Description

technical field [0001] The invention relates to a method for extracting juglone, more particularly, to a supercritical extraction method for natural active ingredient juglone. Background technique [0002] Juglone is an active ingredient extracted from the immature exocarp (green skin) of the Juglandaceae plant - Juglans and its congener black walnut. It has antibacterial, anticancer and central nervous system sedative effects. The juglone precipitated from the mixture of benzene and petroleum ether is orange-yellow needle crystal, and the juglone precipitated from chloroform is red-yellow prismatic crystal, which has a special odor and has a melting point of 155°C and can be sublimated; and With water vapor can be volatile. Juglone is insoluble in cold water, slightly soluble in hot water, soluble in ethanol and ether, and miscible with chloroform and benzene. When it is dissolved in alkali solution, it is purple red, and when it is dissolved in concentrated sulfuric acid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C50/32C07C46/10
CPCY02P20/54
Inventor 刘淑萍闫路省
Owner NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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