CN102659910A - High-efficiency extraction and cleaning production process for diosgenin - Google Patents
High-efficiency extraction and cleaning production process for diosgenin Download PDFInfo
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- CN102659910A CN102659910A CN201210138898XA CN201210138898A CN102659910A CN 102659910 A CN102659910 A CN 102659910A CN 201210138898X A CN201210138898X A CN 201210138898XA CN 201210138898 A CN201210138898 A CN 201210138898A CN 102659910 A CN102659910 A CN 102659910A
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Abstract
The invention relates to a high-efficiency extraction and cleaning production process for diosgenin, relates to the technical field of chemical industry and aims to solve the technical problems of low extraction efficiency, high production cost, difficulty in dehydration and concentration, serious pollution to environment and the like in the convention method for producing the diosgenin. The process comprises the following steps of: a) pretreating raw materials, namely crushing dioscorea zingiberensis; b) extracting dioscin, namely performing ultrasonic continuous countercurrent extraction on the crushed raw materials by using an alcohol water solvent, filtering to obtain filter residues and filtrate, and concentrating the filtrate to obtain a dioscin extract; c) performing enzymolysis or acid hydrolysis on the dioscin, namely performing the enzymolysis or the acid hydrolysis on the obtained dioscin extract; and d) extracting by using an organic solvent, namely performing countercurrent extraction on the obtained zymolyte or acid hydrolysate by using No.120 gasoline or No.6 gasoline, concentrating extract liquor, cooling for crystallizing, performing suction filtration and drying to obtain pure diosgenin.
Description
Technical field
The present invention relates to chemical technology field, particularly a kind of diosgenin high efficiency extraction and clean production technique.
Background technology
Diosgenin (also claiming diosgenin), its traditional technology adopts: saponin is extracted in spontaneous fermentation---acidolysis---.Saponin producing process is to be raw material with the Chinese yam, and filtering, leach thing through immersion, pulverizing, spontaneous fermentation, mineral acid hydrolysis, rinsing is that the extraction agent extraction leaches the saponin in the thing with 120# gasoline through drying after, the evaporation concentration extracting solution, and the saponin crystallization is separated out.
There are problems in this type of traditional processing technology:
1. Chinese yam is except that containing diosgenin; Also contain 40% starch and 50% compositions such as Mierocrystalline cellulose, in the diosellinic acid hydrolytic process, because starch and cellulosic interference; Saponin can not be discharged by abundant hydrolysis, causes the saponin extraction yield to reduce;
2. when carrying out solvent extraction, have more oil-soluble impurities and get in the product, cause saponin product fusing point low and deposit flavescence easily in the process, but also can produce the more reluctant colloidal substance mother liquor that contains saponin;
3. even more serious is; Owing to being hydrolyzed into sugar, starch a large amount of in the production process and Mierocrystalline cellulose residue in the waste water; Make wastewater through organic matter content high, color and luster is dark, and it is smelly to get rid of the back blackout; On the one hand environment is polluted, the difficulty of governance of saponin waste water is increased.
Summary of the invention
The present invention is intended to solve and has in traditional diosgenin working method that extraction efficiency is low, production cost is high, is difficult to that dehydration concentrates and technical problem such as environmental pollution is serious, has the extraction efficiency height to provide, production cost is low and the diosgenin high efficiency extraction of advantage such as non-environmental-pollution and clean production technique.
The objective of the invention is to realize through following technical scheme.
Diosgenin high efficiency extraction of the present invention and clean production technique comprises the steps:
A) raw materials pretreatment: pulverize Rhizome of Peltate Yam;
B) extract dioscin: carry out the ultrasonic continuous countercurrent extraction through the raw material of pulverizing with pure water solvent with above-mentioned, through filtering filter residue and filtrating, get dioscin medicinal extract behind the concentrated filtrate after the extraction;
C) dioscin enzymolysis or acid hydrolysis: the above-mentioned dioscin medicinal extract that obtains is carried out enzymolysis or acid hydrolysis;
D) organic solvent extraction: the above-mentioned zymolyte that obtains or acid hydrolysis liquid are carried out counter-current extraction with 120# gasoline or 6# gasoline or sherwood oil, extraction liquid through concentrate, after cooling crystallization, suction filtration and the oven dry the pure article of diosgenin.
Diosgenin high efficiency extraction of the present invention and clean production technique, the Rhizome of Peltate Yam among the wherein said step a is fresh material or dried feed, the feed particles after the powder essence is 30～40 orders.
Diosgenin high efficiency extraction of the present invention and clean production technique; Pure water solvent among the wherein said step b is the industrial methanol or the alcoholic acid aqueous solution; The volumetric concentration of alcohol is 30%～95%, and it is the ultrasonic generator of 20～200kw that said ultrasonic continuous countercurrent extraction is used power.
Diosgenin high efficiency extraction of the present invention and clean production technique, the power of wherein said ultrasonic generator is 50～120kw.
Diosgenin high efficiency extraction of the present invention and clean production technique, the enzymolysis among the wherein said step c uses the high temperature zymin.
Diosgenin high efficiency extraction of the present invention and clean production technique; Acid hydrolysis among the wherein said step c is pressurization acid hydrolysis or normal pressure acid hydrolysis; Hydrolysis temperature is 90 ℃～150 ℃; The acid hydrolysis working concentration that wherein pressurizes is the Hydrogen chloride of 1.5～2.5mol/L or the dilute sulphuric acid of concentration 0.75～1.5mol/L, and pressurized hydrolysis pressure is 0.2MPa～2Mpa, and the pressurized hydrolysis time is 4～6 hours; Wherein ordinary-pressure hydrolysis acid working concentration is the Hydrogen chloride of 3～5mol/L or the dilute sulphuric acid of concentration 1.5～3mol/L, and hydrolysis time is 7～9 hours.
Diosgenin high efficiency extraction of the present invention and clean production technique, employed 120# gasoline of counter-current extraction or 6# gasoline or sherwood oil are zymolyte or acid hydrolysis liquid volume 5～10 times in the wherein said steps d.
Diosgenin high efficiency extraction of the present invention and clean the beneficial effect of production technique:
1. the present invention utilizes the characteristic that dioscin polarity is big, be soluble in alcohols material, adopts pure water solvent to carry out the technological process of ultrasonic continuous countercurrent extraction-dioscin enzymolysis or acid hydrolysis-organic solvent extraction counter-current extraction, and extraction efficiency is high;
2. lifeless matter fermentation, no soda acid use, and do not produce discharge of wastewater;
A small amount of mother liquor (2 tons of mother liquor/1 ton saponin) of producing of extraction mix with the residue of extraction, extruding, granulation, drying, can be made into organic flower fertilizer;
4. in process of production, employed solvent is an organic solvent, in production technique, under the hermetic condition, recycle, thereby make do not have waste water in the whole process of production, waste gas, useless soluble solids produces, and reaches the purpose that cleans production.
Description of drawings
Fig. 1 process flow diagram of the present invention
Fig. 2 conventional process flow synoptic diagram
Embodiment
The present invention is that a kind of diosgenin high efficiency extraction and the concrete technical process that cleans production technique are: a) raw materials pretreatment: pulverize Rhizome of Peltate Yam; B) extract dioscin: carry out the ultrasonic continuous countercurrent extraction through the raw material of pulverizing with pure water solvent with above-mentioned, through filtering filter residue and filtrating, get dioscin medicinal extract behind the concentrated filtrate after the extraction; C) dioscin enzymolysis or acid hydrolysis: the above-mentioned dioscin medicinal extract that obtains is carried out enzymolysis or acid hydrolysis; D) organic solvent extraction: the above-mentioned zymolyte that obtains or acid hydrolysis liquid are carried out counter-current extraction with 120# gasoline or 6# gasoline or sherwood oil, extraction liquid through concentrate, after cooling crystallization, suction filtration and the oven dry the pure article of diosgenin.
Application principle of the present invention: in starch, saponin existence and the parenchyma cell, and by fiber, xylogen embedding, after Chinese yam was crushed to certain particle size, under action of ultrasonic waves, xylogen, Mierocrystalline cellulose, starch, saponin extracted.
Referring to accompanying drawing 2, conventional process flow is: spontaneous fermentation---acidolysis---extracts saponin.Saponin producing process is to be raw material with the Chinese yam, and filtering, leach thing through immersion, pulverizing, spontaneous fermentation, mineral acid hydrolysis, rinsing is that the extraction agent extraction leaches the saponin in the thing with 120# gasoline through drying after, the evaporation concentration extracting solution, and the saponin crystallization is separated out.
Through experimental verification, traditional technology and technology of the present invention are all to produce 1 ton of (T) saponin, both contrasts such as following table:
| Sequence number | Project | Traditional technology | Technology of the present invention |
| 1 | Product yield | 92% | 97% |
| 2 | The HCl quantity discharged | 16T | - |
| 3 | Saponin starch and saccharification pollutant discharge amount | 40-50T | - |
| 4 | Fermentation and wash sour quantity of wastewater effluent | 650-750T | - |
| 5 | Energy consumption | 13600 yuan | 7600 yuan |
| 6 | Use man-hour | 126 days/people | 82 days/people |
| 7 | Production cycle | 10-15 days | 1 day (24h) |
Below through specific embodiment the present invention is further specified.
Embodiment one
Get the dried raw material 100kg of Chinese yam (containing 2% diosgenin approximately), pulverize, cross 10 mesh sieves, with methanol solvate ultrasonic continuous countercurrent extraction, frequency is 25 Hz, and filter residue is used for doing bio-organic fertilizer, and filtrating concentrates.Liquid concentrator is dropped into the pressurized hydrolysis jar, add hydrochloric acid, making its concentration is 2mol/L, under 90 ℃, and enzymolysis 5 hours.Filter, oven dry, with the 120# gasoline continuous countercurrent extraction of 8 times of amount of liquid of zymolyte, extraction liquid concentrates the postcooling crystallization, suction filtration, oven dry gets the pure article 99.25% of diosgenin, and fusing point is more than 195.5 ℃.
Embodiment two
Get the dried raw material 200kg of Chinese yam (containing 2% diosgenin approximately), pulverize, cross 20 mesh sieves, with alcohol solvent ultrasonic continuous countercurrent extraction, frequency is 35Hz, and filter residue is used for doing bio-organic fertilizer, and filtrating concentrates.Liquid concentrator is dropped into the ordinary-pressure hydrolysis jar, add hydrochloric acid, making its concentration is 2mol/L, under 90 ℃, and hydrolysis 5 hours.Filter, hydrolyzed solution transfers pH value to neutral.To transfer to the neutral hydrolyzed solution with 5 times of amount of liquid 120# gasoline continuous countercurrent extractions, extraction liquid is concentrated into small volume, cooling crystallization, and suction filtration, oven dry gets the pure article 98.5% of diosgenin, and fusing point is more than 195 ℃.
Claims (7)
1. diosgenin high efficiency extraction and clean production technique is characterized in that this technology comprises the steps:
A) raw materials pretreatment: pulverize Rhizome of Peltate Yam;
B) extract dioscin: carry out the ultrasonic continuous countercurrent extraction through the raw material of pulverizing with pure water solvent with above-mentioned, through filtering filter residue and filtrating, get dioscin medicinal extract behind the concentrated filtrate after the extraction;
C) dioscin enzymolysis or acid hydrolysis: the above-mentioned dioscin medicinal extract that obtains is carried out enzymolysis or acid hydrolysis;
D) organic solvent extraction: the above-mentioned zymolyte that obtains or acid hydrolysis liquid are carried out counter-current extraction with 120# gasoline or 6# gasoline or sherwood oil, extraction liquid through concentrate, after cooling crystallization, suction filtration and the oven dry the pure article of diosgenin.
2. diosgenin high efficiency extraction according to claim 1 and clean production technique, it is characterized in that: the Rhizome of Peltate Yam among the said step a is fresh material or dried feed, the feed particles after the powder essence is 30～40 orders.
3. diosgenin high efficiency extraction according to claim 1 and clean production technique; It is characterized in that: the pure water solvent among the said step b is the industrial methanol or the alcoholic acid aqueous solution; The volumetric concentration of alcohol is 30%～95%, and it is the ultrasonic generator of 20～200kw that said ultrasonic continuous countercurrent extraction is used power.
4. diosgenin high efficiency extraction according to claim 3 and clean production technique, it is characterized in that: the power of said ultrasonic generator is 50～120kw.
5. diosgenin high efficiency extraction according to claim 1 and clean production technique is characterized in that: the enzymolysis among the said step c uses the high temperature zymin.
6. diosgenin high efficiency extraction according to claim 1 and clean production technique; It is characterized in that: the acid hydrolysis among the said step c is pressurization acid hydrolysis or normal pressure acid hydrolysis; Hydrolysis temperature is 90 ℃～150 ℃; The acid hydrolysis working concentration that wherein pressurizes is the Hydrogen chloride of 1.5～2.5mol/L or the dilute sulphuric acid of concentration 0.75～1.5mol/L, and pressurized hydrolysis pressure is 0.2MPa～2Mpa, and the pressurized hydrolysis time is 4～6 hours; Wherein ordinary-pressure hydrolysis acid working concentration is the Hydrogen chloride of 3～5mol/L or the dilute sulphuric acid of concentration 1.5～3mol/L, and hydrolysis time is 7～9 hours.
7. diosgenin high efficiency extraction according to claim 1 and clean production technique is characterized in that: employed 120# gasoline of counter-current extraction or 6# gasoline or sherwood oil are zymolyte or acid hydrolysis liquid volume 5～10 times in the said steps d.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964420A (en) * | 2012-11-25 | 2013-03-13 | 竹溪创艺皂素有限公司 | Technological method for producing yam diosgenin by utilizing ultrasound-assisted ethanol continuous countercurrent extraction |
| CN103319565A (en) * | 2013-06-28 | 2013-09-25 | 重庆启哲生物科技有限公司 | Clean and high-efficiency process for producing diosgenin |
| CN103755773A (en) * | 2014-02-28 | 2014-04-30 | 广东望天湖现代农业科技有限公司 | Preparing method of dioscorea composita saponin |
| CN104387441A (en) * | 2014-10-24 | 2015-03-04 | 广东工业大学 | Pollution-free new technique for extracting diosgenin from yellow ginger |
| CN104774240A (en) * | 2015-04-30 | 2015-07-15 | 陕西科技大学 | Method for extracting diosgenin through dioscin hydrolysis |
| CN105032282A (en) * | 2015-06-24 | 2015-11-11 | 陈琳仁 | Preparation method for high-purity gleditsia sinensis natural surfactant |
| CN112680496A (en) * | 2019-10-18 | 2021-04-20 | 河南度帮中药生物科技股份有限公司 | Production process for extracting diosgenin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450082A (en) * | 2003-04-25 | 2003-10-22 | 郭长合 | Process for extracting dioscin from yellow ginger and Rhizoma Dioscoreae Nipponicae and producing organic fertilizer using residue of same |
| CN101402669A (en) * | 2008-11-19 | 2009-04-08 | 湖南科源生物制品有限公司 | Environment friendly method for producing diosgenin |
| CN102432665A (en) * | 2011-09-27 | 2012-05-02 | 陕西科技大学 | Alcohol-free extraction method for dioscin |
-
2012
- 2012-05-08 CN CN201210138898XA patent/CN102659910A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450082A (en) * | 2003-04-25 | 2003-10-22 | 郭长合 | Process for extracting dioscin from yellow ginger and Rhizoma Dioscoreae Nipponicae and producing organic fertilizer using residue of same |
| CN101402669A (en) * | 2008-11-19 | 2009-04-08 | 湖南科源生物制品有限公司 | Environment friendly method for producing diosgenin |
| CN102432665A (en) * | 2011-09-27 | 2012-05-02 | 陕西科技大学 | Alcohol-free extraction method for dioscin |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964420A (en) * | 2012-11-25 | 2013-03-13 | 竹溪创艺皂素有限公司 | Technological method for producing yam diosgenin by utilizing ultrasound-assisted ethanol continuous countercurrent extraction |
| CN103319565A (en) * | 2013-06-28 | 2013-09-25 | 重庆启哲生物科技有限公司 | Clean and high-efficiency process for producing diosgenin |
| CN103319565B (en) * | 2013-06-28 | 2015-07-08 | 重庆启哲生物科技有限公司 | Clean and high-efficiency process for producing diosgenin |
| CN103755773A (en) * | 2014-02-28 | 2014-04-30 | 广东望天湖现代农业科技有限公司 | Preparing method of dioscorea composita saponin |
| CN104387441A (en) * | 2014-10-24 | 2015-03-04 | 广东工业大学 | Pollution-free new technique for extracting diosgenin from yellow ginger |
| CN104774240A (en) * | 2015-04-30 | 2015-07-15 | 陕西科技大学 | Method for extracting diosgenin through dioscin hydrolysis |
| CN105032282A (en) * | 2015-06-24 | 2015-11-11 | 陈琳仁 | Preparation method for high-purity gleditsia sinensis natural surfactant |
| CN112680496A (en) * | 2019-10-18 | 2021-04-20 | 河南度帮中药生物科技股份有限公司 | Production process for extracting diosgenin |
| CN112680496B (en) * | 2019-10-18 | 2022-03-08 | 河南度帮中药生物科技股份有限公司 | Production process for extracting diosgenin |
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Application publication date: 20120912 |