CN105734108A - Method for producing diosgenin in clean and environment-friendly manner - Google Patents
Method for producing diosgenin in clean and environment-friendly manner Download PDFInfo
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Abstract
The invention relates to the field of biotechnologies, and in particular relates to a method for producing diosgenin in a clean and environment-friendly manner by utilizing the biotechnology. According to the method, starch is completely converted into alcohol through a biological fermentation technology, compared with the traditional technology, the method has the advantages that the severe pollution caused by the fact that the residual starch can not be utilized is reduced, moreover, saponin is extracted by utilizing the self-produced ethanol, therefore, the energy consumption is reduced, the cost is greatly reduced, and the comprehensive utilization ratio of the raw material, namely, rhizoma dioscoreae zingiberensis is improved; crude fibers are prepared into a biomass fuel through a separation technology, meanwhile, the effective degradation separation enables the saponin matter with the final amount being 10% of the total amount of the dry matter to participate in acidolysis, therefore, the consumption of hydrochloric acid and solvent oil and other power consumption are greatly reduced, further, the added value of a product is increased, and the comprehensive utilization of resources is realized.
Description
Technical field
The present invention relates to biological technical field, especially relate to a kind of method utilizing biotechnology clean environment firendly to produce diosgenin.
Background technology
Diosgenin (diosgenin) is the aglucon of dioscin in yam, it has the multiple pharmacological effect such as antiinflammatory, antibacterial, anticancer and blood fat reducing, the primary raw material of synthesizing steroid hormone medicine especially, accounts for the 70% of required steroid total amount.Modern medicine proves that plant sapogenin glycoside can not chemosynthesis, in addition the dioscin content in Rhizoma Dioscoreae rhizome is significantly high, such as: Rhizoma Dioscoreae Zingiberensis Dioscorea camposita, Dioscorea nipponica Mak. Ningpo Yam Rhizome Mount Huang medicated powder back of the body Rhizoma Dioscoreae Rhizoma Dioscoreae Hypoglaucae etc., wherein Dioscorea zingiberensis (formal name used at school Rhizoma Dioscoreae Zingiberensis) is the perennial herbaceous stem prehensile liana of the distinctive Dioscoreaceae of China, also it is one of maximum containing diosgenin in the world species, generally containing diosgenin 1.1%-16.15% in its rhizome, there is the good reputation of " medicinal gold ".The Saponin extracted from Dioscorea zingiberensis can synthesize processing such as hormones series of products such as the intermediate feed medicine product such as diene, 16ALPHA,17ALPHA-epoxyprogesterone and Progesterone, prednisoni acetas, budesonide, prednisolone acetate, methyl testosterone, cyproterone, rice department ketone, androstene work ketone, betamethasone, dehydroepiandros-sterones based on it.These medicinal usages are extremely wide, are the world's second largest class medicines of being only second to antibiotics.Development Dioscorea zingiberensis (Rhizoma Dioscoreae) produces and processing, has a extensive future.
Since China's diosgenin extractive technique is born nearly 50 years, both at home and abroad around improving the Saponin response rate, improve comprehensive utilization of resources, reduce the aspects such as pollutant emission to improve, in Chinese patent (CN1232529C) and Chinese patent (CN101402669B), have introduction.
Current industrial processes produces Saponin and mainly adopts following several method:
(1) tradition pre fermentation-acid-hydrolysis method: cadmium yellow Rhizoma Zingiberis Recens-cleaning-pulverizing-natural fermentation-hydrolysis-filtration-washing-dry-extraction-finished product；
(2) separating starch-acid-hydrolysis method: cadmium yellow Rhizoma Zingiberis Recens-cleaning-pulverizing-separating starch-hydrolysis-filtration-washing-dry-extraction-finished product；
(3) cellulose, starch-acid-hydrolysis method are separated: cadmium yellow Rhizoma Zingiberis Recens-cleaning-pulverizing-separation cellulose-separating starch-hydrolysis-filtration-washing-dry-extraction-finished product.
The first traditional method Problems existing: 1. tradition pre fermentation raw material direct hydrolysis is not thorough, and Saponin yield is low；2. raw material is directly extremely neutral with water cyclic washing after hydrolysis, and water consumption is big, produces 1 ton of Saponin water consumption and reaches 4800 tons, produces waste water many, and particularly in washing process, semi-finished product run off seriously.
The problem that the second and the third traditional method are primarily present: 1. Saponin main form with dioscin in plant is combined with cellulose by starch parcel and is present in cell wall, owing to plant cell wall is tougher, separation cellulose, starch are inefficient, and in Dioscorea zingiberensis, substantial amounts of starch and cellulose are not comprehensively utilized；2. enter acid hydrolysis stage invalid components too much, produce 1 ton of Saponin on average by 140-150 ton Dioscorea zingiberensis, expend hydrochloric acid 10-20 ton, process acidolysis and at least produce high-concentration acid organic wastewater 400-500 ton, process waste water costly；3. invalid components too much also leads to finally extract stage petroleum ether consumption increases, and energy consumption is huge；4. seriously polluted, the processing enterprise of the current diosgenin total output more than 80% of China is positioned at the catchment basin of Danjiangkou Reservoir upstream, and the Saponin acid waste water of annual more than 1,000,000 tons finally all imports Danjiangkou Reservoir, and waste water COD is up to 30000mg/l, BOD8000mg/l, wastewater pH 1.0-2.5.
Summary of the invention
It is an object of the invention to provide a kind of method that clean environment firendly produces diosgenin, solve the with serious pollution problem producing high energy consumption in diosgenin process in prior art, making a low multiple use and produce.
This invention address that technical problem be the technical scheme is that a kind of method that clean environment firendly produces diosgenin, comprise the following steps that
A, liquefaction: by Dioscorea zingiberensis by using amylase to liquefy, heating enzymolysis obtains starch fluid；
B, saccharifying: starch fluid cooling liquefaction obtained, add saccharifying enzyme in described starch fluid and obtain converted mash；
C, fermentation: cooled down by converted mash, add yeast wine zymocyte in described converted mash and carry out biofermentation, obtain karusen and CO2；
D, separation: described karusen is carried out solid-liquid separation and obtains fermentation liquid and fermentation residue；
E, distillation: described fermentation liquid is carried out distillation and prepares an ethanol；
F, extraction: the fermentation residue obtained by step D is dried, add the ethanol-water formed by the ethanol prepared in water and step E, described fermentation residue extracted and separated, obtains Saponin extracting solution and crude fibre；
G, concentration: concentrated by described Saponin extracting solution, obtain concentrated solution and secondary ethanol；
H, acid hydrolysis: add acid in described concentrated solution and be hydrolyzed and obtain hydrolyzate, carry out filter pressing and obtain filter cake described hydrolyzate, and add alkali and be neutralized washing, obtains hydrolysis dried object after drying；
I, extraction: described hydrolysis dried object organic solvent extraction is obtained diosgenin.
Produce in the method for diosgenin at the clean environment firendly of the present invention, in step E, also remain vinasse after distillation ethanol, described vinasse is evaporated under 60 DEG C of-85 DEG C of conditions 6h-12h, after evaporation and concentration, obtains the residual underflow that water content is 40%-60%；In step I, after extraction, also remain extraction leftover；Clean environment firendly produces the method for diosgenin and also includes step J: is merged by the described crude fibre of residual after extraction in described residual underflow, extraction leftover and step F and makes biomass fuel.
Producing in the method for diosgenin at the clean environment firendly of the present invention, also included step KET broken: Dioscorea zingiberensis pulverized, added water and grind to form slurry before step A, described slurry is milled to granularity 2mm, and the solid content of described slurry is 15%-30%.
Produce in the method for diosgenin at the clean environment firendly of the present invention, in step, after heating, temperature during enzymatic liquefaction controls at 85 DEG C-110 DEG C, the time of enzymatic liquefaction is 60min-120min, described diastatic vigor is 20000u/ml-40000u/ml, and described diastatic consumption is according to 8u/g-12u/g starch.
Produce in the method for diosgenin at the clean environment firendly of the present invention, in stepb, the starch fluid that liquefaction obtains is cooled to 60 DEG C-65 DEG C, and saccharificatinn period is 20min-60min, the vigor of described saccharifying enzyme is 80000u/ml-120000u/ml, and the consumption of described saccharifying enzyme is according to 100u/g-200u/g starch.
Produce in the method for diosgenin at the clean environment firendly of the present invention, in step C, described yeast wine zymocyte is that the zymogenic interpolation mass ratio of described yeast wine is 10-15% by being deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center and Wine brewing yeast strain that preserving number is CGMCCNo.9518 is cultivated and obtained；Wherein the Classification And Nomenclature of Wine brewing yeast strain is saccharomyces cerevisiae (Saccharomycescerevisaie), this bacterial strain on August 15th, 2014 in China Committee for Culture Collection of Microorganisms's common micro-organisms center (address: Yard 1, BeiChen xi Road, Chaoyang District, Beijing City 3, Institute of Microorganism, Academia Sinica) preservation.
Producing in the method for diosgenin at the clean environment firendly of the present invention, in step C, described converted mash is cooled to 28 DEG C-36 DEG C and ferments, fermentation time is 40h-72h.
Produce in the method for diosgenin at the clean environment firendly of the present invention, in step F, moisture after the drying of described fermentation residue is 10%-15%, and described ethanol-water concentration by volume is 50%-80%, and described fermentation residue per ton uses the consumption of ethanol-water to be 5000L-12000L.
Produce in the method for diosgenin at the clean environment firendly of the present invention, in step G, temperature when being concentrated by described Saponin extracting solution controls at 60 DEG C-85 DEG C, wherein the secondary ethanol obtained in step H is reclaimed and be concentrated into 90-95% concentration, be cycled to used in step F and prepare ethanol-water.
Producing in the method for diosgenin at the clean environment firendly of the present invention, in steph, described acid is hydrochloric acid or the sulphuric acid of 0.3mol/L-0.6mol/L concentration, and in wherein said concentrated solution, every 20g-25g Saponin adds the acid of 100ml；Acid-hydrolyzed condition is: temperature is 126 DEG C-136 DEG C, and pressure is 0.2MPa-0.3MPa, and the time is 2h-3h.
Implement the method that the clean environment firendly of the present invention produces diosgenin, have the advantages that present invention process utilizes biofermentation technique (by being deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center and preserving number is the Wine brewing yeast strain of CGMCCNo.9518) that starch is completely converted into ethanol and CO2, and utilize the ethanol self produced to carry out extracting dioscin, reduce energy consumption, greatly reduce cost, improve the comprehensive utilization ratio of raw material Dioscorea zingiberensis；Solid-liquid separation technique is utilized to obtain the residue-less fermentation liquid for distilling ethanol and crude fibre, wherein residue-less fermentation liquid can effectively distill ethanol, reduce energy consumption, crude fibre can make biomass fuel, this effective degraded separates and makes the Saponin thing finally only having dry substance mixture 10% enter acidolysis, greatly reduce hydrochloric acid, solvent naphtha and other power consumption, add added value of product, it is achieved comprehensive utilization of resources.This technique is adopted to be advantageous in that:
(1) through biofermentation (by being deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center and preserving number is the Wine brewing yeast strain of CGMCCNo.9518), the starch in raw material is made to be completely converted into ethanol and CO2, wherein ethanol can be autonomous for extracting diosgenin process, improves comprehensive utilization ratio, saves cost, CO2Processing can be reclaimed for the field such as food and machine-building, increase added value, reduce greenhouse effect impact；
(2) adopt isolation technics, before distillation, fermentation liquid is separated with filtering residue, utilize without slag distillation technique, decrease the thermal energy consumption of ethanol distillation；
(3) biomass fuel is made in the crude fibre merging that the vinasse after distilling ethanol, the extraction leftover after extraction dioscin and extraction remain after separating, and makes raw material be fully used, improves comprehensive utilization ratio further；
(4) salt acid consumption is only the 10-15% of tradition prevailing technology, and the comprehensive wastewater for washing the water consumption and generation that neutralize washing is reduced to 1/30, and environmental protection treatment cost reduces and is easily achieved qualified discharge；
(5) finally enter the invalid components minimizing of gasoline extraction, finished product impurity reduces, and quality increases, fuel consumption, coal consumption, greatly reducing of extraction time, and enterprise operation cost reduces, and production efficiency significantly improves.
In sum, the present invention not only diosgenin prepares response rate height, and energy consumption is low, active substance can high efficiency separation, farthest by resource conversion utilize, from source remove starch produce severe contamination.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet that clean environment firendly of the present invention produces the method for diosgenin.
Detailed description of the invention
Below in conjunction with drawings and Examples, the method for the clean environment firendly production diosgenin of the present invention is described further:
The present invention is a kind of method utilizing biotechnology clean environment firendly to produce diosgenin, is mainly used in solving to produce high energy consumption in diosgenin process in prior art, makes a low multiple use and problem that waste water, waste residue cause environment pollution.
As it is shown in figure 1, the method that the clean environment firendly of the present invention produces diosgenin comprises the following steps that
S1, pretreatment: Dioscorea zingiberensis be carried out, carry out remove impurity simultaneously, and washings use through natural sedimentation Posterior circle, saves the energy, saves cost；
S2, pulverizing: being pulverized by the Dioscorea zingiberensis pulverizer after cleaning, remove impurity, add water and grind to form the slurry of granularity 2mm, wherein the solid content of slurry is 15%-30% by weight percentage；
S3, liquefaction: add slurry into amylase and carry out enzymatic liquefaction and obtain starch fluid, temperature during enzymatic liquefaction controls at 85 DEG C-110 DEG C, the time of enzymatic liquefaction is 60min-120min, wherein diastatic vigor is 20000u/ml-40000u/ml, amylase can be α-amylase, beta amylase or α-1,6 key debranching enzymes；Preferably by α-amylase, and vigor is preferably 40000u/ml, its enzymatic liquefaction best results；Wherein diastatic consumption is according to 8u/g-12u/g starch, it is preferred to 10u/g starch；
S4, saccharifying: the starch fluid temperature of post liquefaction is down to 60 DEG C-65 DEG C, starch fluid adds saccharifying enzyme saccharifying 20min-60min and obtains converted mash, wherein the vigor of saccharifying enzyme is 80000u/ml-120000u/ml, saccharifying enzyme can be α-1, 4-glucose hydrolysis enzyme or beta-glucosidase, preferably, saccharifying enzyme is α-1, 4-glucose hydrolysis enzyme, vigor is preferably 100000u/ml, by α-1, the hydrolysis to starch fluid of the 4-glucose hydrolysis enzyme, not only hydrolysis effect good and obtain converted mash contribute to following step utilize yeast wine zymocyte carry out biofermentation and distillation obtain ethanol；Wherein the consumption of saccharifying enzyme is according to 100u/g-200u/g starch, it is preferred to 150u/g starch；
S5, fermentation: in converted mash, add yeast wine zymocyte carry out biofermentation, obtain karusen, wherein yeast wine zymocyte is that the zymogenic interpolation mass ratio of yeast wine is 10-15% by being deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center and Wine brewing yeast strain amplification culture that preserving number is CGMCCNo.9518 obtains；The temperature that converted mash carries out fermenting controls at 28 DEG C-36 DEG C, and fermentation time is 40h-72h；The CO produced in sweat2Reclaim processing and can be used for the field such as food and machine-building；
Wherein Wine brewing yeast strain is trained the zymogenic method of yeast wine: 1. the formula of strain cultures is: Dioscorea zingiberensis sugar liquid 450ml-550ml, MgSO40.01g-0.02g, Co (NH2)20.17g-0.18g, (NH4)2HPO40.12g-0.13g, agar powder is 9-11g；2. the cultivation of bacterial strain preserves: heated by strain cultures, agar powder injects in culture dish and test tube after dissolving, cooling after 120 DEG C of-130 DEG C of autoclavings 30-120 minute, make flat board and slant tube, aseptically, by inoculation to plating medium, cultivate 3-4 days at 28-32 DEG C, the bigger colony inoculation of picking, to slant tube, was cultivated then through 3-4 days, and slant tube puts into cold compartment of refrigerator cryopreservation；3. the formula of yeast wine culture fluid is: Dioscorea zingiberensis sugar liquid 450ml-550ml, MgSO40.01g-0.02g, Co (NH2)20.17g-0.18g, (NH4)2HPO40.12g-0.13g；4. the bacterial strain of preservation is aseptically inoculated in the liquid tube equipped with 10ml yeast wine culture fluid, when 30-32 DEG C, after cultivating 10-16 hour, then is transferred in the liquid tube equipped with 10ml yeast wine culture fluid and continues cultivation 10-16 hour；5. with yeast wine for seed by the continuous amplification culture step by step of inoculum concentration 8%-15%, until required yeast wine zymocyte consumption.
S6, separation: karusen is carried out solid-liquid separation and obtains fermentation liquid and fermentation residue, wherein fermentation residue is continued to employ, by centrifugal mode, karusen can be carried out solid-liquid separation and obtain fermentation liquid and fermentation residue, it is also possible to karusen is carried out solid-liquid separation and obtains fermentation liquid and fermentation residue by the mode filtered by filter.
S7, distillation: fermentation liquid is carried out distillation and prepares an ethanol, distillation column can be selected to distill for producing in enormous quantities, can distilling with equipment such as rotary evaporators for small lot batch manufacture, the technique wherein distilling ethanol is prior art, no longer repeats in detail here；
S8, extraction: by the fermentation residue obtained in step S6 dry to moisture be 10%-15%, add water that to be adjusted to containing concentration of alcohol be the ethanol-water of 50%-80% by step S7 distills the ethanol obtained, wherein the concentration of ethanol is volume ratio, utilize ethanol-water that the fermentation residue after drying is carried out mixed extraction, obtaining Saponin extracting solution and crude fibre, fermentation residue per ton uses the consumption of ethanol-water to be 5000L-12000L；
S9, concentration: Saponin extracting solution is concentrated by concentration tank, concentrate at 60 DEG C-85 DEG C, obtain concentrated solution and secondary ethanol, and secondary ethanol can continue reclaim circulation and make ethanol-water for adding water in S8 step by recovery tower concentration to 90-95% (v/v)；
S10, acid hydrolysis: add in concentrated solution acid that concentration is 0.3mol/L-0.6mol/L 126 DEG C-136 DEG C, 0.2MPa-0.3MPa when carry out acid hydrolysis 2h-3h and obtain hydrolyzate, wherein in concentrated solution, every 20g-25g Saponin correspondence adds 100ml acid, hydrolyzate is carried out filter pressing and obtains filter cake, and add alkali and be neutralized washing, hydrolysis dried object is obtained after drying, this hydrolysis dried object is the crude product of diosgenin, and the waste water of washing is up to state standards after biochemical treatment and discharges；Wherein acid is hydrochloric acid or sulphuric acid, naturally it is also possible to for other strong acid or weak acid, all within protection scope of the present invention；Alkali is can be that the highly basic such as lime cream, sodium hydroxide, weak base are all within protection scope of the present invention, it is preferred to lime cream, and lime cream is prone to make a big purchase in large quantities and cheap, simultaneously because corrosivity is relatively weak, it is possible to reduce or avoid the probability of personal injury；
S11, extraction: hydrolysis dried object (i.e. the crude product of diosgenin) obtains the sterling of diosgenin with the organic solvent extraction such as petroleum ether, gasoline, dry the diosgenin got product after pulverizing.
Further, also include step S12,, remaining vinasse after distillation ethanol in step S7 is evaporated 6h-12h under 60 DEG C of-85 DEG C of conditions, the residual underflow that water content is 40%-60% is obtained after evaporation and concentration, the extraction leftover remaining with after extraction in step S11 by this residual underflow and step S8 extract the crude fibre merging of residual after separating and make biomass fuel, improve the comprehensive utilization ratio of raw material, it is to avoid waste resource.
Present invention process utilizes biofermentation technique, and starch is completely converted into ethanol and CO by the yeast wine zymocyte cultivated with programmed screening (by being deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center and preserving number is the Wine brewing yeast strain of CGMCCNo.9518)2, and utilize the ethanol self produced to extract, reduce energy consumption, greatly reduce cost, improve the comprehensive utilization ratio of raw material Dioscorea zingiberensis；Efficiently separate, extract the Saponin thing entrance acidolysis making finally to only have dry substance mixture 10%, greatly reduce acid, organic solvent oil and other power consumption, reduce contaminated wastewater, reduce the cost of environmental protection treatment, add added value of product, it is achieved comprehensive utilization of resources；After distillation, extraction and extraction being separated, residuals twice laid is made for biomass fuel, further increases the comprehensive utilization ratio of resource, and namely Dioscorea zingiberensis is utilized to the fullest, it does not have cause any loss and waste, greatly saves cost.
It is specifically described below by multiple embodiments.
Embodiment 1:
null2.5 tons of Dioscorea zingiberensis are cleaned，Carry out remove impurity simultaneously，Washings use through natural sedimentation Posterior circle，To clean、Dioscorea zingiberensis pulverizer after remove impurity is pulverized，Add water and grind to form the slurry of granularity 2mm，Wherein the solid content of slurry is 20% by weight percentage，The vigor of adding slurry into is that the α-amylase of 30000u/ml carries out enzymatic liquefaction and obtains starch fluid，The consumption of α-amylase is 10u/g starch，Temperature during enzymatic liquefaction controls at 100 DEG C，The time of enzymatic liquefaction is 90min，The starch fluid temperature of post liquefaction is down to 60 DEG C，In starch fluid, addition vigor is the α-1 of 100000u/ml,4-glucose hydrolysis enzyme glycolysis 40min obtains converted mash，Wherein α-1,4-glucose hydrolysis enzyme dosage is 150u/g starch，Converted mash adds yeast wine zymocyte and carries out biofermentation，Obtain karusen，This yeast wine zymocyte is cultivated obtain by being deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center and Wine brewing yeast strain that preserving number is CGMCCNo.9518，The zymogenic interpolation mass ratio of yeast wine is 10%，The temperature that converted mash carries out fermenting controls at 30 DEG C，Fermentation time is 60h，Karusen is carried out solid-liquid separation by centrifugal mode and obtains fermentation liquid and fermentation residue，Fermentation liquid therein is carried out distillation by distillation column and prepares an ethanol，Add water the ethanol-water that volume by volume concentration is 60% made containing ethanol by an ethanol，Stand-by，The fermentation residue drying above-mentioned separation obtained is 10% to moisture，Add above-mentioned ethanol-water to carry out extracting and separating，Obtain Saponin extracting solution and crude fibre，Wherein fermentation residue per ton uses 6000L ethanol-water，Saponin extracting solution is pumped in precipitation concentration tank and concentrates，Concentrate at 60 DEG C，Obtain concentrated solution and secondary ethanol，And secondary ethanol carries out reclaiming and be concentrated into 90% (v/v) concentration，It is cycled to used in above-mentioned extraction process，Adding concentration in concentrated solution is that the hydrochloric acid of 0.5mol/L is at 136 DEG C、Carry out acid hydrolysis 2h when 0.25MPa and obtain hydrolyzate，In concentrated solution, every 20g Saponin correspondence adds 100ml hydrochloric acid，Hydrolyzate is carried out filter pressing and obtains filter cake，And add lime cream and be neutralized washing，The crude product of hydrolysis dried object diosgenin is obtained after drying，The waste water of washing is up to state standards after biochemical treatment and discharges，The crude product 120# gasoline extraction of diosgenin is obtained the sterling of diosgenin，Dry the diosgenin got product after pulverizing.By vinasse remaining after distillation ethanol under 85 DEG C of conditions, obtaining, after evaporation 6h concentration, the residual underflow that water content is 50%, the crude fibre produced after remaining extraction leftover after this residual underflow, extraction and extraction being separated merges makes biomass fuel.
Embodiment 2:
null4 tons of Dioscorea zingiberensis are carried out，Carry out remove impurity simultaneously，Washings use through natural sedimentation Posterior circle，To clean、Dioscorea zingiberensis pulverizer after remove impurity is pulverized，Add water and grind to form the slurry of granularity 1mm，Wherein the solid content of slurry is 30% by weight percentage，The vigor of adding slurry into is that the beta amylase of 40000u/ml carries out enzymatic liquefaction and obtains starch fluid，The consumption of beta amylase is 12u/g starch，Temperature during enzymatic liquefaction controls at 85 DEG C，The time of enzymatic liquefaction is 110min，The starch fluid temperature of post liquefaction is down to 65 DEG C，In starch fluid, addition vigor is that the beta-glucosidase enzyme glycolysis 60min of 110000u/ml obtains converted mash，Wherein beta-glucosidase enzyme dosage is 200u/g starch，Converted mash adds yeast wine zymocyte and carries out biofermentation，Obtain karusen，This yeast wine zymocyte is cultivated obtain by being deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center and Wine brewing yeast strain that preserving number is CGMCCNo.9518，The zymogenic interpolation mass ratio of yeast wine is 15%，The temperature that converted mash carries out fermenting controls at 34 DEG C，Fermentation time is 72h，Karusen is carried out solid-liquid separation by the mode of filtering with microporous membrane and obtains fermentation liquid and fermentation residue，Wherein the aperture of microporous filter membrane is 0.45 μm，Fermentation liquid therein is carried out distillation by rotary evaporator and prepares an ethanol，Add water the ethanol-water that volume by volume concentration is 80% made containing ethanol by an ethanol，Stand-by，The fermentation residue drying above-mentioned separation obtained is 15% to moisture，Add above-mentioned ethanol-water carry out mixed extraction and separate，Obtain Saponin extracting solution and crude fibre，Wherein fermentation residue per ton uses 5000L ethanol-water，Saponin extracting solution is pumped in concentration tank and concentrates，Concentrate at 70 DEG C，Obtain concentrated solution and secondary ethanol，And secondary ethanol can be concentrated into 95% concentration and continue to reclaim circulation and for above-mentioned extraction process，Adding concentration in concentrated solution is that the sulphuric acid of 0.3mol/L is at 126 DEG C、Carry out acid hydrolysis 3h when 0.2MPa and obtain hydrolyzate，In concentrated solution, every 25g Saponin correspondence adds 100ml sulphuric acid，Hydrolyzate is carried out filter pressing and obtains filter cake，And add sodium hydroxide and be neutralized washing，The crude product of hydrolysis dried object diosgenin is obtained after drying，The waste water of washing discharges after being up to state standards again，The crude product petroleum ether extraction of diosgenin is obtained the sterling of diosgenin，Dry the diosgenin got product after pulverizing.The vinasse of residual after distillation ethanol is evaporated 10h under 60 DEG C of conditions, obtaining the residual underflow that water content is 60% after evaporation and concentration, the crude fibre produced after remaining extraction leftover after this residual underflow, extraction and extraction being separated merges makes biomass fuel.
Embodiment 3:
null10 tons of Dioscorea zingiberensis are carried out，Carry out remove impurity simultaneously，Washings use through natural sedimentation Posterior circle，To clean、Dioscorea zingiberensis pulverizer after remove impurity is pulverized，Add water and grind to form the slurry of granularity 1.5mm，Wherein the solid content of slurry is 15% by weight percentage，The vigor of adding slurry into is the α-1 of 20000u/ml，6 key debranching enzymes carry out enzymatic liquefaction and obtain starch fluid，α-1，The consumption of 6 key debranching enzymes is 8u/g starch，Temperature during enzymatic liquefaction controls at 110 DEG C，The time of enzymatic liquefaction is 120min，The starch fluid temperature of post liquefaction is down to 63 DEG C，In starch fluid, addition vigor is the α-1 of 120000u/ml,4-glucose hydrolysis enzyme glycolysis 20min obtains converted mash，α-1,The consumption of 4-glucose hydrolysis enzyme is 100u/g starch，Converted mash adds yeast wine zymocyte and carries out biofermentation，Obtain karusen，This yeast wine zymocyte is cultivated obtain by being deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center and Wine brewing yeast strain that preserving number is CGMCCNo.9518，The zymogenic adding proportion of yeast wine is 13%，The temperature that converted mash carries out fermenting controls at 36 DEG C，Fermentation time is 40h，Fermentation liquid is easily separated by chromatography gel post and obtains fermentation liquid and fermentation residue，Fermentation liquid therein is carried out distillation by distillation column and prepares an ethanol，Add water the ethanol-water that volume by volume concentration is 50% made containing ethanol by an ethanol，Stand-by，The fermentation residue drying above-mentioned separation obtained is 12% to moisture，Add above-mentioned ethanol-water carry out mixed extraction and separate，Obtain Saponin extracting solution and crude fibre，Wherein fermentation residue per ton uses 8000L ethanol-water，Saponin extracting solution is pumped in concentration tank and concentrates at 85 DEG C，Obtain concentrated solution and secondary ethanol，And secondary ethanol can be concentrated into 93% concentration and continue to reclaim circulation and for above-mentioned extraction process，Adding concentration in concentrated solution is that the sulphuric acid of 0.6mol/L is at 130 DEG C、Carry out acid hydrolysis 2.2h when 0.3MPa and obtain hydrolyzate，In concentrated solution, every 22.5g Saponin correspondence adds 100ml sulphuric acid，Hydrolyzate is carried out filter pressing and obtains filter cake，And add sodium hydroxide and be neutralized washing，The crude product of hydrolysis dried object diosgenin is obtained after drying，The waste water of washing discharges after being up to state standards again，The crude product gasoline extraction of diosgenin is obtained the sterling of diosgenin，Dry the diosgenin got product after pulverizing.The vinasse of residual after distillation ethanol is evaporated 12h under 70 DEG C of conditions, obtaining the residual underflow that water content is 40% after evaporation and concentration, the crude fibre produced after remaining extraction leftover after this residual underflow, extraction and extraction being separated merges makes biomass fuel.
Embodiment 4:
null40 tons of Dioscorea zingiberensis are carried out，Carry out remove impurity simultaneously，Washings use through natural sedimentation Posterior circle，To clean、Dioscorea zingiberensis pulverizer after remove impurity is pulverized，Add water and grind to form the slurry of granularity 1.8mm，Wherein the solid content of slurry is 23% by weight percentage，The vigor of adding slurry into is that the α-amylase of 40000u/ml carries out enzymatic liquefaction and obtains starch fluid，The consumption of α-amylase is 12u/g starch，Temperature during enzymatic liquefaction controls at 105 DEG C，The time of enzymatic liquefaction is 60min，The starch fluid temperature of post liquefaction is down to 62 DEG C，In starch fluid, addition vigor is the α-1 of 80000u/ml,4-glucose hydrolysis enzyme glycolysis 30min obtains converted mash，Wherein α-1,4-glucose hydrolysis enzyme dosage is 150u/g starch，Converted mash adds yeast wine zymocyte and carries out biofermentation，Obtain karusen，This yeast wine zymocyte is cultivated obtain by being deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center and Wine brewing yeast strain that preserving number is CGMCCNo.9518，The zymogenic interpolation mass ratio of yeast wine is 14%，The temperature that converted mash carries out fermenting controls at 28 DEG C，Fermentation time is 70h，Karusen is easily separated by centrifuge and obtains fermentation liquid and fermentation residue，Fermentation liquid therein is carried out distillation by distillation column and prepares an ethanol，Add water the ethanol-water that volume by volume concentration is 70% made containing ethanol by an ethanol，Stand-by，The fermentation residue drying above-mentioned separation obtained is 14% to moisture，Add above-mentioned ethanol-water carry out mixed extraction and separate，Obtain Saponin extracting solution and crude fibre，Wherein fermentation residue per ton uses 12000L ethanol-water，Saponin extracting solution is pumped in precipitation concentration tank and concentrates，Concentrate at 75 DEG C，Obtain concentrated solution and secondary ethanol，And secondary ethanol can be concentrated into 95% concentration and continue to reclaim circulation and for above-mentioned extraction process，Adding concentration in concentrated solution is that the hydrochloric acid of 0.4mol/L is at 133 DEG C、Carry out acid hydrolysis 2.5h when 0.28MPa and obtain hydrolyzate，In concentrated solution, every 24g Saponin correspondence adds 100ml hydrochloric acid，Hydrolyzate is carried out filter pressing and obtains filter cake，And add lime cream and be neutralized washing，The crude product of hydrolysis dried object diosgenin is obtained after drying，The waste water of washing discharges after being up to state standards again，The crude product petroleum ether extraction of diosgenin is obtained the sterling of diosgenin，Dry the diosgenin got product after pulverizing.The vinasse of residual after distillation ethanol is evaporated 8h under 75 DEG C of conditions, obtaining the residual underflow that water content is 550% after evaporation and concentration, the crude fibre produced after remaining extraction leftover after this residual underflow, extraction and extraction being separated merges makes biomass fuel.
Present invention process utilizes biofermentation technique that starch is completely converted into ethanol and CO2, and utilize the ethanol self produced to extract, reduce energy consumption, greatly reduce cost, improve the comprehensive utilization ratio of raw material Dioscorea zingiberensis；Utilize isolation technics that crude fibre is made for biomass fuel, and effective degraded separates the Saponin thing entrance acidolysis making finally to only have dry substance mixture 10%, greatly reduce hydrochloric acid, solvent naphtha and other power consumption, add added value of product, it is achieved comprehensive utilization of resources.This technique is adopted to be advantageous in that:
(1) through biofermentation (special yeast wine zymocyte), the starch in raw material is made to be completely converted into ethanol and CO2, wherein ethanol can be autonomous for extracting diosgenin process, improves comprehensive utilization ratio, saves cost, CO2Processing can be reclaimed for the field such as food and machine-building, produce added value；
(2) adopt isolation technics, before distillation, fermentation liquid is separated with filtering residue, utilize without slag distillation technique, decrease the thermal energy consumption of ethanol distillation；
(3) biomass fuel is made in the crude fibre merging that the vinasse after distilling ethanol, the extraction leftover after extraction diosgenin and extraction remain after separating, and makes raw material be fully used, improves comprehensive utilization ratio further；
(4) salt acid consumption is only the 10-15% of tradition prevailing technology, and the comprehensive wastewater of water consumption and generation for neutralizing washing is reduced to 1/30, and environmental protection treatment cost reduces and is easily achieved qualified discharge；
(5) invalid components finally entering gasoline extraction reduces, fuel consumption, coal consumption, greatly reducing of extraction time, and enterprise operation cost reduces, and production efficiency significantly improves.
In sum, the present invention not only diosgenin prepares response rate height, and energy consumption is low, active substance can high efficiency separation, farthest by resource conversion utilize.
It should be appreciated that for those of ordinary skills, it is possible to being improved according to the above description or convert, all these improve or convert within the protection domain that all should belong to claims of the present invention.
Claims (10)
1. the method that a clean environment firendly produces diosgenin, it is characterised in that comprise the following steps that
A, liquefaction: by Dioscorea zingiberensis by using amylase to liquefy, heating enzymolysis obtains starch fluid；
B, saccharifying: starch fluid cooling liquefaction obtained, add saccharifying enzyme in described starch fluid and obtain converted mash；
C, fermentation: cooled down by converted mash, add yeast wine zymocyte in described converted mash and carry out biofermentation, obtain karusen and CO2；
D, separation: described karusen is carried out solid-liquid separation and obtains fermentation liquid and fermentation residue；
E, distillation: described fermentation liquid is carried out distillation and prepares an ethanol；
F, extraction: the fermentation residue obtained by step D is dried, add the ethanol-water formed by the ethanol prepared in water and step E, described fermentation residue extracted and separated, obtains Saponin extracting solution and crude fibre；
G, concentration: concentrated by described Saponin extracting solution, obtain concentrated solution and secondary ethanol；
H, acid hydrolysis: add acid in described concentrated solution and be hydrolyzed and obtain hydrolyzate, carry out filter pressing and obtain filter cake described hydrolyzate, and add alkali and be neutralized washing, obtains hydrolysis dried object after drying；
I, extraction: described hydrolysis dried object organic solvent extraction is obtained diosgenin.
2. the method that clean environment firendly according to claim 1 produces diosgenin, it is characterized in that, in step E, after distillation ethanol, also remain vinasse, described vinasse is evaporated under 60 DEG C of-85 DEG C of conditions 6h-12h, after evaporation and concentration, obtains the residual underflow that water content is 40%-60%；In step I, after extraction, also remain extraction leftover；
Clean environment firendly produces the method for diosgenin and also includes step J: is merged by the described crude fibre of residual after extraction in described residual underflow, extraction leftover and step F and makes biomass fuel.
3. the method that clean environment firendly according to claim 1 produces diosgenin, it is characterized in that, before step A, also include step KET broken: Dioscorea zingiberensis pulverized, add water and grind to form slurry, described slurry is milled to granularity 2mm, and the solid content of described slurry is 15%-30%.
4. the method that clean environment firendly according to claim 1 produces diosgenin, it is characterized in that, in step, after heating, temperature during enzymatic liquefaction controls at 85 DEG C-110 DEG C, the time of enzymatic liquefaction is 60min-120min, described diastatic vigor is 20000u/ml-40000u/ml, and described diastatic consumption is according to 8u/g-12u/g starch.
5. the method that clean environment firendly according to claim 1 produces diosgenin, it is characterized in that, in stepb, the starch fluid that liquefaction obtains is cooled to 60 DEG C-65 DEG C, and saccharificatinn period is 20min-60min, the vigor of described saccharifying enzyme is 80000u/ml-120000u/ml, and the consumption of described saccharifying enzyme is according to 100u/g-200u/g starch.
6. the method that clean environment firendly according to claim 1 produces diosgenin, it is characterized in that, in step C, described yeast wine zymocyte is that the zymogenic interpolation mass ratio of described yeast wine is 10-15% by being deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center and Wine brewing yeast strain that preserving number is CGMCCNo.9518 is cultivated and obtained.
7. the method that clean environment firendly according to claim 1 produces diosgenin, it is characterised in that in step C, described converted mash being cooled to 28 DEG C-36 DEG C and ferments, fermentation time is 40h-72h.
8. the method that clean environment firendly according to claim 1 produces diosgenin, it is characterized in that, in step F, moisture after the drying of described fermentation residue is 10%-15%, described ethanol-water concentration by volume is 50%-80%, and described fermentation residue per ton uses the consumption of ethanol-water to be 5000L-12000L.
9. the method that clean environment firendly according to claim 1 produces diosgenin, it is characterized in that, in step G, temperature when being concentrated by described Saponin extracting solution controls at 60 DEG C-85 DEG C, wherein the secondary ethanol obtained in step H is reclaimed and be concentrated into 90-95% concentration, be cycled to used in step F and prepare ethanol-water.
10. the method that clean environment firendly according to claim 1 produces diosgenin, it is characterised in that in steph, described acid is hydrochloric acid or the sulphuric acid of 0.3mol/L-0.6mol/L concentration, in wherein said concentrated solution, every 20g-25g Saponin adds the acid of 100ml；Acid-hydrolyzed condition is: temperature is 126 DEG C-136 DEG C, and pressure is 0.2MPa-0.3MPa, and the time is 2h-3h.
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