CN102399257A - Method for extracting glycyrrhizic acid and liquorice flavonoid by using continuous countercurrent ultrasonic extraction machine - Google Patents
Method for extracting glycyrrhizic acid and liquorice flavonoid by using continuous countercurrent ultrasonic extraction machine Download PDFInfo
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- CN102399257A CN102399257A CN2011104336465A CN201110433646A CN102399257A CN 102399257 A CN102399257 A CN 102399257A CN 2011104336465 A CN2011104336465 A CN 2011104336465A CN 201110433646 A CN201110433646 A CN 201110433646A CN 102399257 A CN102399257 A CN 102399257A
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Abstract
The invention provides a method for extracting glycyrrhizic acid and liquorice flavonoid by using a continuous countercurrent ultrasonic extraction machine. The scheme process comprises the following steps of: 1, conveying liquorice subjected to treatment into an extraction pipe of the continuous countercurrent ultrasonic extraction machine through a quantitative feeder and inputting an extracting solvent into the extraction pipe from a dreg-discharging end of the ultrasonic extraction machine; 2, performing countercurrent ultrasonic extraction on the liquorice and the extracting solvent in the extraction pipe at the temperature of between 30 and 60 DEG C and under normal pressure; 3, after countercurrent ultrasonic extraction, discharging the liquorice dreg from a dreg-discharging port of the ultrasonic extraction machine, treating the liquorice dreg, recovering the solvent, and discharging the extracting solution from a liquid-discharging port of the ultrasonic extraction machine; 4, performing dreg liquid separation on the extracting solution and concentrating by using a concentrating tank to obtain a concentrated solution; and 5, performing solid liquid separation on the concentrated solution, drying the obtained solid to obtain a liquorice flavonoid product, adjusting pH value of the separated liquid by using inorganic acid, performing solid liquid separation, drying the separated solid to obtain a glycyrrhizic acid finished product, and concentrating and drying the separated liquid to obtain a mixture of angelica polysaccharide, liquorice flavonoid and glycyrrhizic acid.
Description
Technical field:
What the present invention relates to is a kind of process for extracting, especially utilizes the continuous countercurrent ultrasonic extractor to extract the method for Potenlini and licoflavone.
Background technology:
The production of Potenlini and licoflavone in the prior art uses relatively primary multi-function extractor thermal backflow to extract mostly, extracts in this way; The extraction temperature that requires is high, and extraction yield is low, and; Also to produce a large amount of waste gas and waste water in process of production, environment is polluted.
Summary of the invention:
Technical problem to be solved by this invention; Be exactly not enough to existing in prior technology, and a kind of method and technology scheme of utilizing the continuous countercurrent ultrasonic extractor to extract Potenlini and licoflavone is provided, this scheme is to be employed on the continuous countercurrent ultrasonic extractor; With compound extraction solvent countercurrent extraction Potenlini and licoflavone; Extraction efficiency is improved, and the consumption of solvent reduces, and has realized the serialization and the automatic operating of extraction separation; And under the condition of normal pressure and sealing, accomplish leaching process, guaranteed the extraction and the disintegrate-quality of Potenlini and licoflavone.
This programme is realized through following technical measures: utilize the continuous countercurrent ultrasonic extractor to extract the method for Potenlini and licoflavone, be characterized in being undertaken by following process step:
Step 1: will be through screening, removal of impurities, the Radix Glycyrrhizae after being crushed to the 10-30 order is through quantitative feeder; Be transported in the feeding unit of continuous countercurrent ultrasonic extractor; And be input in the extraction tube by opening for feed; To extract solvent simultaneously is that 1 extraction solvent than 4-10 through interchanger be heated to 30-60 ℃ with extracting the weight of solvent kilogram with the ratio that volume rises in Radix Glycyrrhizae, is input in the extraction tube by the deslagging end of continuous countercurrent ultrasonic extractor;
Step 2: Radix Glycyrrhizae with extract solvent in the extraction tube of continuous countercurrent ultrasonic extractor, under temperature 30-60 ℃, normal pressure, carried out the adverse current supersound extraction 30-40 minute;
Step 3: after the adverse current supersound extraction of completing steps two, discharge glycyrrhiza residue, again glycyrrhiza residue is handled the recovery solvent by the slag-drip opening of continuous countercurrent ultrasonic extractor; Leakage fluid dram by the continuous countercurrent ultrasonic extractor is discharged extracting solution;
Step 4: the extracting solution of completing steps three, the extracting solution after the slag liquid/gas separator separates is input to concentration tank and is concentrated into 40% of extracting solution, gets liquid concentrator;
Step 5: the liquid concentrator of completing steps four, after solid-liquid separation, separate the solid that obtains and be input to dryer, get the licoflavone product after the oven dry; The liquid that obtains after the separation is input to the acid adjustment stirred pot, with mineral acid PH is transferred to 2-3, again through solid-liquid separation, gets the glycyrrhizic acid inclusion compound finished product after the isolated solid oven dry; Isolated liquid is through the mixture that concentrates, oven dry obtains licorice polysaccharide, licoflavone, Potenlini.
The concrete characteristics of this programme also have, and the ethanol that the described extraction solvent of step 1 is 30-70% is 1 mixed solution than 0.001-0.1 with 18-28% ammoniacal liquor by weight proportion.It is that glycyrrhiza residue is input in the desolventizing machine that the glycyrrhiza residue of the said solvent recuperation of step 3 is handled; Earlier glycyrrhiza residue is preheating to 50-80 ℃; Input pressure makes the solvent vaporization at the saturation steam of 0.01-0.05Mpa then, and the condensing surface of the solvent gas after the vaporization through 10-30 ℃ is cooled to liquid and is input in the storage tank subsequent use.The said slag liquid/gas separator of step 4 is to adopt 40-100 order cylinder-rotating strainer, filters the coarse filtration liquid that obtains, and separates the slag liquid/gas separator that obtains containing the smart filtrating of the following particle of 3-10um through disk centrifugal separator again.It is the thickener that adopts outer circulation, up-down film that the said concentration tank of step 4 concentrates, and the control vaporization temperature makes the extraction solvent evaporation between 40-70 ℃, will extract solvent through condensing surface again and be condensed into liquid state by gaseous state, and it is subsequent use to be input to solvent tank.The said mineral acid of step 5 is sulfuric acid or hydrochloric acid.
The beneficial effect of this programme can be learnt according to the narration to such scheme; Because this scheme is to utilize the continuous countercurrent ultrasonic extractor to accomplish by extracting Potenlini and licoflavone in the Radix Glycyrrhizae through five steps; Leaching process has adopted the double solvents of ethanol and ammoniacal liquor, is easy to the disposable dissolving of the Potenlini in the Radix Glycyrrhizae, licoflavone and licorice polysaccharide is extracted.Opening for feed input Radix Glycyrrhizae at the continuous countercurrent ultrasonic extractor gets into extraction tube, and the slag-drip opening to the continuous countercurrent ultrasonic extractor moves in extraction tube.Extract solvent in the deslagging end input of continuous countercurrent ultrasonic extractor and get into extraction tube, and reverse mobile to the leakage fluid dram of continuous countercurrent ultrasonic extractor in extraction tube.Radix Glycyrrhizae is opposite with the flow direction that extracts solvent in extraction tube, and the Potenlini in the Radix Glycyrrhizae and licoflavone are dissolved in fast and extract in the solvent under the ultrasonic of extraction tube and the effect of stirring, and accomplish leaching process.Extracting solution is after slag liquid separates, concentrates; In the process solid-liquid separation; Isolated solid obtains the licoflavone product through oven dry; The pH value of isolated liquid process adjustment solution gets mixture of ingredients such as glycyrrhizic acid inclusion compound finished product and licorice polysaccharide, licoflavone, Potenlini, the product of Licorice by name again through solid-liquid separation.Because whole extraction, filtration, separation, concentrate, the precipitation process is under the condition of normal pressure and sealing, to accomplish, therefore, the good quality of product that obtains is once extracted and can be obtained three kinds of products.The glycyrrhizic acid content that obtains is higher, can be greater than 25%; The content of licoflavone can be greater than 10%.Because effect ultrasonic and stirring is arranged in leaching process, so extraction rate is fast, general extraction rate was less than 40 minutes, and the efficient of extraction is high, and the yield of extraction is also high, and general extract yield is more than 90%.In addition, the consumption that is exactly solvent is few, and in whole process of production, the waste less than 1% of solvent so reduced production cost, has also reduced the pollution to environment.This shows that the present invention compared with prior art has outstanding substantive distinguishing features and obvious improvement, the beneficial effect of its enforcement also is conspicuous.
Embodiment:
For clearly demonstrating the technical characterstic of this programme, through an embodiment, this programme is set forth below.
This programme utilizes the continuous countercurrent ultrasonic extractor to extract the method for Potenlini and licoflavone, and its process step is following:
Step 1: will be through screening, removal of impurities, the licorice powder 100kg after being crushed to 20 orders is through quantitative feeder; Be transported in the feeding unit of continuous countercurrent ultrasonic extractor; And be input in the extraction tube by opening for feed; To extract solvent simultaneously is 1 extraction solvent than 4-10 with extracting the weight of solvent kilogram with the ratio that volume rises in Radix Glycyrrhizae; This embodiment adopts Radix Glycyrrhizae and extracts the weight of solvent kilogram and ratio that volume rises is 1 to 6 extraction solvent 600L, and this this embodiment of extractions solvent is to be 1 to 0.01 mixed one-tenth extraction solvent by weight proportion by 50% ethanol and 0.5% ammoniacal liquor, is heated to 30-60 ℃ through interchanger; This embodiment is after being heated to 40 ℃, is input in the extraction tube by the deslagging end of continuous countercurrent ultrasonic extractor.
Step 2: Radix Glycyrrhizae with extract solvent in the extraction tube of continuous countercurrent ultrasonic extractor, under temperature 30-60 ℃, normal pressure, carried out the adverse current supersound extraction 30-40 minute, this embodiment is 30 minutes;
Step 3: after the adverse current supersound extraction of completing steps two; Slag-drip opening by the continuous countercurrent ultrasonic extractor is discharged glycyrrhiza residue, again glycyrrhiza residue is handled the recovery solvent, and it is that glycyrrhiza residue is input in the desolventizing machine that the glycyrrhiza residue of said solvent recuperation is handled; Earlier glycyrrhiza residue is preheating to 50-80 ℃; Control input pressure then and make water molecules substitute the solvent molecule in the slag, the solvent gas after the vaporization is become liquid and enters into separating tank through 10-30 ℃ of water coolant heat exchange postcooling in condensing surface, in separating tank, two kinds of solvents are carried out Separation and Recovery at the saturation steam of 0.01-0.05Mpa; Be input in the storage tank separately subsequent usely, solvent recovering yield is more than 98%.Leakage fluid dram by the continuous countercurrent ultrasonic extractor is discharged extracting solution;
Step 4: the extracting solution of completing steps three, the extracting solution after the slag liquid/gas separator separates is input to concentration tank and is concentrated into 40% of extracting solution, gets liquid concentrator.Said slag liquid/gas separator is to adopt 40-100 order cylinder-rotating strainer, filters the coarse filtration liquid that obtains, and separates the slag liquid/gas separator that obtains containing the smart filtrating of the following particle of 3-10um through disk centrifugal separator again.It is the thickener that adopts outer circulation, up-down film that said concentration tank concentrates, and the control vaporization temperature makes the extraction solvent evaporation between 40-70 ℃, will extract solvent through condensing surface again and be condensed into liquid state by gaseous state, and it is subsequent use to be input to solvent tank;
Step 5: the liquid concentrator of completing steps four, after solid-liquid separation, separate the solid that obtains and be input to dryer, get licoflavone product 8kg after the oven dry.The liquid that obtains after the separation is input to the acid adjustment stirred pot, with mineral acids such as sulfuric acid or hydrochloric acid PH is transferred to 2-3, again through solid-liquid separation, gets glycyrrhizic acid inclusion compound finished product 12kg after the isolated solid oven dry.Isolated liquid is through the mixture 25kg that concentrates, oven dry obtains licorice polysaccharide, licoflavone, Potenlini.
Claims (6)
1. method of utilizing the continuous countercurrent ultrasonic extractor to extract Potenlini and licoflavone is characterized in that process step is following:
Step 1: will be through screening, removal of impurities, the Radix Glycyrrhizae after being crushed to the 10-30 order is through quantitative feeder; Be transported in the feeding unit of continuous countercurrent ultrasonic extractor; And be input in the extraction tube by opening for feed; To extract solvent simultaneously is that 1 extraction solvent than 4-10 through interchanger be heated to 30-60 ℃ with extracting the weight of solvent kilogram with the ratio that volume rises in Radix Glycyrrhizae, is input in the extraction tube by the deslagging end of continuous countercurrent ultrasonic extractor;
Step 2: Radix Glycyrrhizae with extract solvent in the extraction tube of continuous countercurrent ultrasonic extractor, under temperature 30-60 ℃, normal pressure, carried out the adverse current supersound extraction 20-40 minute;
Step 3: after the adverse current supersound extraction of completing steps two, discharge glycyrrhiza residue, again glycyrrhiza residue is handled the recovery solvent by the slag-drip opening of continuous countercurrent ultrasonic extractor; Leakage fluid dram by the continuous countercurrent ultrasonic extractor is discharged extracting solution;
Step 4: the extracting solution of completing steps three, the extracting solution after the slag liquid/gas separator separates is input to the 20-40% that concentration tank is concentrated into extracting solution, gets liquid concentrator;
Step 5: the liquid concentrator of completing steps four, after solid-liquid separation, separate the solid that obtains and be input to dryer, get the licoflavone product after the oven dry; The liquid that obtains after the separation is input to the acid adjustment stirred pot, with mineral acid PH is transferred to 2-3, again through solid-liquid separation, gets the glycyrrhizic acid inclusion compound finished product after the isolated solid oven dry; Isolated liquid is through the mixture that concentrates, oven dry obtains licorice polysaccharide, licoflavone, Potenlini.
2. method according to claim 1 is characterized in that: the ethanol that the described extraction solvent of step 1 is 30-70% is 1 mixed solution than 0.001-0.1 with 18-28% ammoniacal liquor by weight proportion.
3. method according to claim 1; It is characterized in that: it is that glycyrrhiza residue is input in the desolventizing machine that the glycyrrhiza residue of the said solvent recuperation of step 3 is handled; Earlier glycyrrhiza residue is preheating to 50-80 ℃; Input pressure makes the solvent vaporization at the saturation steam of 0.01-0.05Mpa then, and the water coolant of the solvent gas after the vaporization through 10-30 ℃ is cooled to liquid and is input in the storage tank subsequent use in condensing surface.
4. method according to claim 1 is characterized in that: the said slag liquid/gas separator of step 4 is to adopt 40-100 order cylinder-rotating strainer, filters the coarse filtration liquid that obtains, and separates obtaining containing the smart filtrating of the following particulate of 3-10um again through disk centrifugal separator.
5. method according to claim 1; It is characterized in that: it is to adopt thickeners such as outer circulation, up-down film that the said concentration tank of step 4 concentrates; The control vaporization temperature is between 40-70 ℃; Make the extraction solvent evaporation, will extract solvent through condensing surface again and be condensed into liquid state by gaseous state, it is subsequent use to be input to solvent tank.
6. method according to claim 1 is characterized in that: the said mineral acid of step 5 is sulfuric acid or hydrochloric acid.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103588831A (en) * | 2012-08-14 | 2014-02-19 | 江苏汉邦科技有限公司 | Preparation method of glycyrrhizic acid |
| CN103788167A (en) * | 2012-10-31 | 2014-05-14 | 江苏汉邦科技有限公司 | Preparation method for glycyrrhetinic acid monoglucuronide (GAMG) |
| CN104069160A (en) * | 2014-07-17 | 2014-10-01 | 新疆鹏弘生物科技有限公司 | Ultrasonic countercurrent extraction process for glycyrrhiza |
| CN104876998A (en) * | 2015-05-28 | 2015-09-02 | 天津大学 | Method for adopting pH gradient elution method to synchronously separate triterpenoid saponins and licorice flavonoid |
| CN112679314A (en) * | 2020-12-29 | 2021-04-20 | 西安天美生物科技股份有限公司 | Preparation process of sclareol |
| CN113425760A (en) * | 2021-07-23 | 2021-09-24 | 江苏大学 | Method for extracting and separating effective components from liquorice |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588831A (en) * | 2012-08-14 | 2014-02-19 | 江苏汉邦科技有限公司 | Preparation method of glycyrrhizic acid |
| CN103788167A (en) * | 2012-10-31 | 2014-05-14 | 江苏汉邦科技有限公司 | Preparation method for glycyrrhetinic acid monoglucuronide (GAMG) |
| CN103788167B (en) * | 2012-10-31 | 2015-06-03 | 江苏汉邦科技有限公司 | Preparation method for glycyrrhetinic acid monoglucuronide (GAMG) |
| CN104069160A (en) * | 2014-07-17 | 2014-10-01 | 新疆鹏弘生物科技有限公司 | Ultrasonic countercurrent extraction process for glycyrrhiza |
| CN104876998A (en) * | 2015-05-28 | 2015-09-02 | 天津大学 | Method for adopting pH gradient elution method to synchronously separate triterpenoid saponins and licorice flavonoid |
| CN112679314A (en) * | 2020-12-29 | 2021-04-20 | 西安天美生物科技股份有限公司 | Preparation process of sclareol |
| CN113425760A (en) * | 2021-07-23 | 2021-09-24 | 江苏大学 | Method for extracting and separating effective components from liquorice |
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Application publication date: 20120404 |