CN100460419C - New cleanproduction process for extracting saponin from dioscorea zingiberensis - Google Patents
New cleanproduction process for extracting saponin from dioscorea zingiberensis Download PDFInfo
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- CN100460419C CN100460419C CNB2005101245098A CN200510124509A CN100460419C CN 100460419 C CN100460419 C CN 100460419C CN B2005101245098 A CNB2005101245098 A CN B2005101245098A CN 200510124509 A CN200510124509 A CN 200510124509A CN 100460419 C CN100460419 C CN 100460419C
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Abstract
This invention provides a new technology of cleaning production that extract sapogenin from dioscorea zingiberensis wright. It uses rhizome of fresh dioscorea zingiberensis or fresh dioscorea nipponica that are 2 -3 perennials as raw material. Its technology is that: raw material-microwave processing-ultramicro-pulverization-dynamic state continuous extracting-rectification-hydrolization-crude sapogenin-dissolving adsorption for purification-rectification-crystallization-drying-depurating sapogenin. This invention provides a new technology that produces diosgenin. Its technology is advanced, investment is little, material expenditure is low, production yield is high, quality is satisfactory, production period is so short that extracting technology can complete in 20 hours. It has no pollution. Content of COD in the water is less than 300mg/l.
Description
One technical field
The present invention is new cleanproduction process for extracting saponin from Rhizome of Peltate Yam, particularly adopts a series of vanguard technologies and technology to reach cleaner production, shortened extraction time, has increased extraction efficiency; Contaminated solution discharging simultaneously.
Two background technologies:
Extracting sapogenin from yellow ginger or Ningpo Yam Rhizome is saponin (dioscin), is the precursor of steroid hormone class medicine, accounts for 70% in the raw material of synthesizing steroid medicine.The steroid hormone medicine is the second largest class medicine that is only second to antibiotic in world's medicine.The steroid hormone types of drugs of producing in the world reaches 292 kinds more than at present.The steroid hormone medicine has very strong anti-infective, antianaphylaxis, antiviral and antishock pharmacological action, clinically at home and abroad pharmaceutically widely uses.So far diosgenin is still the synthetic optimal raw material of this class medicine.But the technology of domestic production saponin processing is to use the fermentation-hydrochloric acid hydrolysis-gasoline extraction method that has continued 50 years always at present; Raw material consumption is big, and the cycle is long seriously polluted, and COD is up to 25000mg/L (BOD8000mg/L), pH value 1.0-2.5 in the waste water.Make the peripheral deterioration of the ecological environment, and produce biologic chain destruction.
The traditional processing technology of diosgenin is:
1, the fermentation extraction sapogenin that combines with acid hydrolysis
Fresh ginger cleaning → pulverizing → fermentation → acidolysis → washing neutrality → drying → gasoline extraction → sapogenin
2, the fermentation method extraction sapogenin that combines with enzymolysis
Fresh ginger cleaning → pulverizing → fermentation → enzymolysis → drying → gasoline extraction → sapogenin
Domestic main employing at present be that fermentation is extracted sapogenin with acid-hydrolysis method.
Extraction process is the acidolysis zymotechnique that prolongs with 50 years always in existing actual production, extraction time is long, wastage of material is big, environmental pollution is big, quality product is lower, the problem that the high no added value of production cost, production exist is the technical big breakthrough that do not have, and saponin produces and prolongs the production technique of extracting with spontaneous fermentation, hydrochloric acid hydrolysis, industrial naptha always, and gained saponin quality is lower.Traditional technology is keeping effective constituent, removes the invalid components aspect, exists that energy consumption is big, material consumption is big, loss of effective components is big, impurity is many, efficient is low, the cycle is long, operation is many, the not high shortcoming of extraction yield.Concrete manifestation is as follows:
1, fermentation period is long, easily goes mouldy, and it is not thorough to ferment.
When 2, being washed to neutrality, the big pollution of water loss is big, and the more part sapogenin that causes of wash number runs off.
3, finished product acid consumption per ton is 15-20 tons.
4, finished product loss gasoline per ton is 5-6 tons.
5, finished product per ton consumes raw material 130-160 ton.
6, finished product per ton causes about 500 tons of the pollution water yield that exceeds standard.
Along with country puts more effort to the supervision of ecotope, manufacturer stops production one after another, rectification.
Three, summary of the invention
Investigate by research practice, summary, researched and developed and can solve environmental pollution, one cover that can improve the output value and economic benefit again has the novel process of independent intellectual property right, all can reach the GMP standard on production environment and complete processing, discharging reaches the requirement that the discharging safe level 300mg/L of pollutent COD is determined in " saponin emission of industrial pollutants standard and measuring method " research topic first trial that State Environmental Protection Administration assigns.Changing the traditional technology extraction was the new technological flow of finishing whole extractions in 20 hours in 7-10 days.
Purpose of the present invention is for overcoming disadvantages of background technology, and providing a kind of is the novel extractive technique that raw material extracts saponin with Chinese yam class plant.This technology has shortened the production cycle improving product quality simultaneously, and is free from environmental pollution, and the fiber of (dry weight) 50% in the raw material, and 40% starch is able to machinery and reclaims; Increased the byproduct income.Production Flow Chart is reclaimed acid solution after acidolysis because of low with the acid amount, reduces production costs and has reduced pollution simultaneously.
The purpose of this invention is to provide a kind of technology advanced person, less investment, raw material consumption is low, quality product is high, with short production cycle, free of contamination from Rhizome of Peltate Yam new cleanproduction process for extracting saponin.
The object of the present invention is achieved like this:
1. choose 2-3 living Chinese yam cadmium yellow ginger or bright Ningpo Yam Rhizome and clean other impurity of removing earth, sandstone and carrying secretly, behind the moisture on the raw material surface of volatilizing again; Carry out slicing treatment;
2. adopt frequency at the microwave equipment of 300MHz～40GHz raw material to be carried out radiation and make the water molecules of cell interior do reversal of pole campaign, a large amount of heat energy of generation rapidly impels the water vapor of intracellular fluid attitude simultaneously; The pressure that generates breaks through cell walls and cytolemma, causes cell rupture and discharges effective constituent in the cell, finishes drying treatment simultaneously;
3. cooperate the emulsification pretreatment technology, the ethanol that adds 35%-95% content to material carry out the emulsification fragmentation, granularity reaches 2-10um, the volume that purpose reduces raw material increases surface volume;
4. adopt dynamic continuous backflow to extract equipment to material circulation extraction, solvent continuous backflow Jin proposes aqueous saponin; Vacuum concentration extracting solution and distillating recovering solvent ethanol carry out drying treatment, the abundant residual ethanol that volatilizees with spissated saponin solution, and saponin is existed with solid form;
5. heating is dissolved in 10%-37% hydrochloric acid soln heating acidolysis 4-6 hour with saponin, obtains solid sediment and hydrochloric acid soln as solid-liquid separation; Hydrochloric acid liquid distillation recycling use;
6. solid sediment washes that cryodrying makes its water ratio be lower than 7% to the neutrality with water.Get the crude product sapogenin;
7. crude product sapogenin heating for dissolving adds activated carbon powder adsorpting pigment and impurity in dehydrated alcohol.Filtering separation activated carbon powder, pure liquid improve the solution purity through the micro-pore-film filtration tiny solid particle that dams;
8. direct evaporated under reduced pressure or obtain needle crystal through distillating recovering solvent is lower than 80 ℃ and dryly must makes with extra care sapogenin.
The correlation technique that the present invention uses:
(1) emulsification pretreatment technology; (2) screw settling centrifugal separation technique; (3) microwave leaching technology that dynamically refluxes; (4) vacuum concentration distillation recovery technology; (5) membrane filtration technology; (6) microwave technology.
1. emulsification pretreatment technology: material in entering the working chamber of high-shear emulsion machine after, moment bears hundreds of thousands of and shears, produced simultaneously turbulent flow makes material be subjected to more powerful fluid power and shears.Because the comprehensive action of some kinds of Cracking Mechanisms such as shearing, bump, extruding, grinding makes material just fully reach the purpose of dispersion, mixing, emulsification, homogeneous, fragmentation in the extremely short time, makes the target product complete processing more superior, quality product is more stable.Powder particle diameter is brought up to 2um-10um, and plant powder can reach 95% broken wall level.Ultra-micro powder can make that effective constituent is able to abundant reservation in the crude drug, and the stripping of effective constituent is rapider, it is faster, more abundant to discharge, and process is more direct, quick, and utilization ratio of drug improves.
2. screw settling centrifugal separation technique: its principle of work: suspension to be separated by the centre charging pipe add screw feeder the time feed bin in, quicken the back and enter in the rotary drum by the feed port on the spiral.Under action of centrifugal force, the suspension that enters in the rotary drum is divided into two-layer very soon: heavier solid precipitation forms the sediment layer on drum inner wall; Ring separated liquid layer in lighter liquid phase then formed.Sediment is pushed to the rotary drum small end by screw feeder has the slag notch of rotary drum small end to throw away rotary drum in the further dehydration of awl section.
3. microwave leaching technology dynamically refluxes: select suitable solvent, be added in the suitable herbal raw material of pulverizing, solvent dissolves soluble substance owing to diffusion, osmosis can penetrate in the cell by cell walls gradually, and causes the concentration difference inside and outside the cell, so intracellular strong solution is constantly to external diffusion, extracellular solvent then constantly enters in the medicinal material histocyte, so comes and goes repeatedly, when strength of solution reaches running balance inside and outside cell, this saturated solution is leached, concentrate; Continue to add novel solvent in the dregs of a decoction after filter, repeat above process, repeated multiple times just can be bordering on needed composition complete stripping or stripping substantially.
4. vacuum concentration distills recovery technology: the saturated solvent that Jin is carried adopts conventional distillation technique to reclaim solvent, and the time, long equipment volume was big, volatilization loss amount height; At above problem, use the vacuum distilling of spray curtain formula to reclaim in this technology concentrated distillation is finished simultaneously.
5. membrane filtration technology: the separating mechanism of microporous membrane mainly is sieving action; The separating mechanism of dense film generally is a dissolving-diffusion.The former is mainly used in ultrafiltration, micro-filtration, dialysis etc.; The latter is mainly used in reverse osmosis, gas delivery, infiltration gasification etc.The liquid film separating mechanism is that dissolving-diffusion is transmitted with promotion.Improve the purity of purifies and separates, utilize microporous membrane to purify extracting solution in this technology and sneak into impurity.
6. microwave technology: microwave is a kind of wavelength at 1～0.001m, the frequency hertzian wave at 300MHz～300GHz.Because it has unique character---like light characteristic, through characteristic, thermal property, biological effect.
Microwave technology is extracted the herbal medicine effective ingredient: Chinese herbal medicine effective ingredients often is embedded in the cell, has only cell walls and cytolemma fragmentation or dissolving, extracts active ingredients could be come out.The microwave extraction technology mainly is based on the thermal property of microwave, its heating principle is to utilize the time and the identical characteristics of microwave frequency of dipole pilot polarization with the interfacial polarization of microwave field medium, impel the transition of medium rotational level, the aggravation thermal motion is converted into heat energy with electric energy.
The microwave radiation process is that frequency electromagnetic waves penetrates medium, arrives the inside vascular bundle and the glandular cell system of material.Because absorb micro-wave energy, the cell interior temperature rises rapidly, make its cell interior pressure surpass cell walls expansion ability to bear with cell rupture.Effective constituent freely flows out in the cell, and micro-wave energy is a kind of form of energy, and it can be to many material generation effects of being made up of polar molecule in transmission course, and microwave electromagnetic field makes the molecule of material produce instantaneous polarization.
The present invention compared with prior art has following advantage:
1. extraction efficiency height: existing extractive technique is expected that saponin produces and is needed 7-10 days from former.And new technology is extracted in 20 hours and finishes.
2. extract the yield height: on extraction yield, be higher than traditional technology 10%.Save material, separating starch and fiber before acidolysis have increased the byproduct income simultaneously.
3. environmental nonpollution: 1 ton of finished product of the every production of traditional technology consumes sour 15-20 ton, can't reclaim to be mixed in (about 500 tons) in the blowdown water.This technology is 1/20 of traditional technology with acid amount, and the rate of recovery is up to more than 90%, 200 kilograms of blowdown acid content less thaies.Can save required equipment of wastewater treatment and fund.Blowdown liquid is the clear shape; COD content is below 300mg/L in the waste water.
Four: description of drawings
Accompanying drawing 1 extracts sapogenin new cleanproduction process schema for the present invention from Rhizome of Peltate Yam.
Five: embodiment:
Embodiment:
Take by weighing fresh yellow ginger 1000Kg, clean the back section,, add alcohol solvent and shear 30min with behind the microwave equipment broken wall material being dropped in the high-shear emulsifying jar.Emulsification to 400 order.Adopt dynamically continuous extraction equipment to material circulation extraction, Jin proposes aqueous saponin; Saponin solution is carried out vacuum concentration and drying treatment, get the total saponin of residue.Add the water suspendible, add 20% hydrochloric acid reacting by heating 6 hours.The filtering acid solution is washed to neutral back, the dry crude product sapogenin that gets with the acidolysis throw out.Add anhydrous alcohol solution crude product glucoside unit, and add the activated carbon powder absorption impurity of equal weight.The filtering separation activated carbon powder, and with filter solvents after the micro-pore-film filtration removal of impurity, solvent evaporated under reduced pressure is separated out needle crystal fully, 80 ℃ of evaporates to dryness get 8.2 kilograms of elaboration sapogenins behind the suction filtration.
Claims (1)
1. from Rhizome of Peltate Yam, extract the saponin process for cleanly preparing, it is characterized in that:
(1), chooses fresh yellow ginger of 2-3 or Ningpo Yam Rhizome rhizome; Clean foreign material impurity such as removing the earth carry secretly, sandstone, carry out slicing treatment;
(2), adopt frequency raw material to be carried out radiation to make the water molecules of cell interior do reversal of pole campaign at the microwave equipment of 300MHz～40GHz, a large amount of heat energy of generation rapidly impels the water vapor of intracellular fluid attitude simultaneously; The pressure that generates breaks through cell walls and cytolemma, causes cell rupture and discharges effective constituent in the cell, finishes drying treatment simultaneously;
(3), add the 35%-95% alcohol solvent and cooperate the emulsification pretreatment technology to carry out the emulsification particle size after cracking in the material to reach 2-10um, adopt thereafter the dynamic extraction facility to material circulation extract, solvent continuous backflow Jin proposes aqueous saponin;
(4), adopt the vacuum concentration distillation to reclaim alcohol solvent and concentrate drying aqueous saponin;
(5), with the saponin heating for dissolving in the hydrochloric acid soln of 10%-37%, to saponin pressurization acidolysis 4-6 hour, hydrochloric acid solution and solid particles shape throw out, filter out acid solution;
(6), the solids precipitation water of solid shape cleans to presenting neutrality, cryodrying gets water content and is less than 7% crude product sapogenin;
(7), adding alcohol solvent in the crude product sapogenin is heated to after crude product sapogenin solid substance dissolves fully, add activated carbon pulvis absorption impurity and pigment, filtering separation activated carbon pulvis, alcoholic solution are through the micro-pore-film filtration tiny solid particle that dams, to improve the solution purity;
(8), direct evaporated under reduced pressure or obtain needle crystal through distillating recovering solvent, be lower than 80 ℃ and dryly must make with extra care sapogenin.
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| CNB2005101245098A CN100460419C (en) | 2005-12-08 | 2005-12-08 | New cleanproduction process for extracting saponin from dioscorea zingiberensis |
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| CN100460419C true CN100460419C (en) | 2009-02-11 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102061280A (en) * | 2010-11-29 | 2011-05-18 | 西南大学 | Bacillus subtilis SWB8 for producing diosgenin |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967178B (en) * | 2010-08-23 | 2012-09-05 | 王元华 | Method for extracting high-content diosgenine hydrolysate |
| CN102100875B (en) * | 2011-01-28 | 2012-02-01 | 张海 | Process method for microwave assistant supercritical extraction of active ingredients of curcuma |
| CN102161691B (en) * | 2011-04-11 | 2012-03-21 | 湖北芳通药业股份有限公司 | Process method for producing diosgenin by combining microwave irradiation, alcohol extraction and oil extraction technologies |
| CN108148107A (en) * | 2017-12-25 | 2018-06-12 | 华远医药研究院有限公司 | The method for extraction and purification of Dioscin |
| CN116789715A (en) * | 2019-05-15 | 2023-09-22 | 山东洲星生物技术有限公司 | Extraction process of water-soluble saponin |
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| CN1414013A (en) * | 2001-10-26 | 2003-04-30 | 周航 | New method and equipment system for separating, drying dioscorea extract |
| CN1418888A (en) * | 2002-12-09 | 2003-05-21 | 吉林天药科技股份有限公司 | Novel process for preparing diosgenin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102061280A (en) * | 2010-11-29 | 2011-05-18 | 西南大学 | Bacillus subtilis SWB8 for producing diosgenin |
| CN102061280B (en) * | 2010-11-29 | 2012-07-25 | 西南大学 | Bacillus subtilis SWB8 for producing diosgenin |
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Effective date of registration: 20170524 Address after: 712000 Xianyang City, Shaanxi Province town of Sanyuan County Da Cheng Qiao Cun Jin Meng Bridge Company Patentee after: Hou Hao Address before: 712000 Xianyang province Shaanxi City Weicheng district emerging North Bureau 14 iron room No. 101 Patentee before: Wang Xijun |
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