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A kind of production process of extracting usnic acid from long usnea

A production process and technology of usnic acid, applied in organic chemistry and other directions, can solve the problems that the application effect is not as good as countercurrent extraction, silica gel column chromatography purification, high process cost, etc., and achieve the effect of reducing content, complete extraction and high extraction efficiency.

Inactive Publication Date: 2016-03-30
DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The usnic acid extraction process in the above-mentioned patent documents is mainly purified through the steps of alkali alcohol reflux extraction, cationic resin and macroporous resin separation. Although the final usnic acid has a high purity, the process itself is expensive and practical The effect is far inferior to that of countercurrent extraction combined with solvent extraction and silica gel column chromatography purification

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 500kg of Usnea longissima body, crush it into coarse powder and pass through a 40-mesh sieve, add it at a constant speed of 50kg / h from the feeding port of the elevator, and use a pipeline pump to feed 75% acetone aqueous solution through the liquid inlet pipe at a flow rate of 200kg / h. Join, the frequency of the elevator is set to 20Hz, the frequency of the host 1 is set to 16Hz, the frequency of the juicer 1 is set to 50Hz, the frequency of the host 2 is set to 22Hz, the frequency of the juicer 2 is set to 45Hz, and the usnic acid is obtained Crude extract 2T; The crude extract of usnic acid flows to the temporary storage tank by itself and is continuously pumped to the concentration tank by the outlet pump to concentrate to obtain 200L of the crude concentrate of usnic acid; adjust the valve of the material pump to make the crude concentrate of usnic acid to 1L / min enters the extraction tower, and adjusts the solvent pump valve so that ethyl acetate enters the e...

Embodiment 2

[0027] Weigh 1.4T of Usnea licheniformis, crush it into coarse powder and pass through an 80-mesh sieve, add it at a constant speed of 200kg / h from the feeding port of the elevator, and use a pipeline pump to feed 75% acetone aqueous solution at a flow rate of 600kg / h. The tube is added, the frequency of the elevator is set to 25Hz, the frequency of the host 1 is set to 18Hz, the frequency of the juicer 1 is set to 45Hz, the frequency of the host 2 is set to 20Hz, the frequency of the juicer 2 is set to 40Hz, and the Usnea Crude acid extract 4.2T: The crude extract of usnic acid flows to the temporary storage tank by itself and is continuously pumped to the concentration tank by the outlet pump to concentrate to obtain 400L crude concentrate of usnic acid; adjust the valve of the material pump to make the crude concentrate of usnic acid Liquid enters extraction tower with 0.5L / min, adjusts solvent pump valve, makes ethyl acetate enter extraction tower with 2L / min, obtains usnic...

Embodiment 3

[0029] Weigh 800kg of Usnea longissima body, crush it into a coarse powder and pass through a 60-mesh sieve, add it at a constant speed of 80kg / h from the feeding port of the elevator, and use a pipeline pump to feed 80% acetone aqueous solution through the liquid inlet pipe at a flow rate of 250kg / h. Join, the frequency of the elevator is set to 22Hz, the frequency of the host 1 is set to 18Hz, the frequency of the juicer 1 is set to 50Hz, the frequency of the host 2 is set to 22Hz, the frequency of the juicer 2 is set to 45Hz, and the usnic acid is obtained The crude extract of usnic acid is 2.5T; the crude extract of usnic acid flows automatically to the temporary storage tank and is continuously pumped to the concentration tank through the liquid pump to concentrate to obtain 250L of crude concentrate of usnic acid; adjust the valve of the material pump to make the crude concentrate of usnic acid Enter the extraction tower with 0.8L / min, adjust the solvent pump valve, make ...

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PUM

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Abstract

The invention discloses a production technology for extracting usnic acid from usnea longissima. The technology comprises the steps that a raw material is subjected to coarse grinding, and fed in from a feeding hopper; an extraction tank unit host rotates to slowly push the material from the front end of a unit backwards; an extraction solvent enters an extraction tank from a liquid inlet tube at the tail end of the unit, passes through the moving material from the back end of the tank, and flows towards the front end; and solid and liquid substances are contacted fully in an inverse motion, so that effective components in the medicinal material are extracted. Dregs are forcibly pushed to a dreg discharge port by a discharge transport and then discharged; a special juice squeezer squeezes the dregs; residual medicine liquor in the dregs is squeezed out of a medicinal material tissue; and the content of the residual medicine liquor in the dregs is reduced. The extraction efficiency is higher, and the extraction is more complete. The method adopts a continuous extraction tank unit for extraction, and is combined with a silica gel column chromatography for purification, so that a separating effect is better. Finished usnic acid with a maximum yield of 1% and the content above 95% can be obtained.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry and relates to a production process of usnic acid, in particular to a production process of utilizing countercurrent extraction combined with solvent extraction and silica gel column chromatography to purify usnic acid. Background technique: [0002] Usnea long, alias female dill, parasitic on pine, pine off, tree hanging, ceiling grass, snow wind rattan, mountain vermicelli, asparagus, canopy grass, tree beard is Usnea longus Usnea U. longissimaAch., used as medicine with lichen body. The lichen filaments of Usnea longus contain barbatic acid, usnicacid, diffractaicacid, ramalic acid, lichenin, long pine Radish polysaccharide, ethyleverninate, has the effects of eliminating phlegm and relieving cough; clearing heat and detoxification; dehumidifying and dredging collaterals; [0003] Usnic acid is a broad-spectrum antibiotic that has a strong inhibitory effect on most Gram-positive bact...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/91
Inventor 姚德坤姚德利张亚红姚航黄运生吴海龙
Owner DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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