CN103242418A - Clean production process of diosgenin - Google Patents
Clean production process of diosgenin Download PDFInfo
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- CN103242418A CN103242418A CN201310144472XA CN201310144472A CN103242418A CN 103242418 A CN103242418 A CN 103242418A CN 201310144472X A CN201310144472X A CN 201310144472XA CN 201310144472 A CN201310144472 A CN 201310144472A CN 103242418 A CN103242418 A CN 103242418A
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Abstract
The invention discloses a clean production process of diosgenin. By utilizing the technology of saccharification, membrane separation and ultrasonic extraction, the process comprises the following steps: fermenting, liquefying and saccharifying the cleaned and smashed yellow ginger, thereby obtaining saccharified mash; spirally squeezing and screening the saccharified mash, thereby obtaining fibrous residues and a filtrate; performing membrane separation on the filtrate, thereby obtaining a membrane concentrate and a sugar liquor; drying the fibrous residues and performing ultrasonic extraction, thereby obtaining an extracted concentrate; performing acid hydrolysis on the membrane concentrate and the extracted concentrate, thereby obtaining a saponin hydrolysate; and extracting the saponin from the saponin hydrolysate by utilizing gasoline. According to the process, the starch and the fibers in the yellow ginger are effectively separated from material systems before the acid hydrolysis is performed, so that the acid hydrolysis condition can be controlled more easily; and the acid hydrolysis process can be performed more finely. Therefore, the generation of wastewater during the diosgenin production is reduced greatly while the diosgenin yield is ensured; and the starch sugar liquor as a by-product is obtained. As a result, the comprehensive utilization of resources is realized.
Description
Technical field
The present invention relates to the former medicine manufacturing technology of pharmaceutical chemicals field, be specifically related to a kind of cleaning manufacturing technique method of turmeric saponin.
Background technology
From yellow ginger, can extract saponin, be that raw material can be produced a series of medicine intermediate and final production goes out steroid hormone class medicine with the saponin.The discovery of steroid hormone and application have been one of major progresses of pharmaceutical field since over half a century, and types of drugs reaches 292 kinds more than, clinically at home and abroad pharmaceutically widely use, and be the requisite medicine class of medical field.
In China, the plant that contains diosgenin mainly contains yellow ginger and Dioscorea nipponica Mak. Ningpo Yam Rhizome etc.The Dioscorea nipponica Mak. Ningpo Yam Rhizome saponin content has only half of yellow ginger, and growth cycle is longer than yellow ginger.Therefore, yellow ginger becomes the topmost medicine source plant resource that China produces the steroid hormone medicine.
The traditional processing technology of turmeric saponin ferments after earlier yellow ginger being cleaned and crush, and directly with sulfuric acid or hydrochloric acid heating hydrolysis, the hydrolyzate that obtains is washed with water to neutrality to the material after the fermentation, with the hydrolyzate drying, obtains saponin with gasoline extraction at last again.Its flow process is: yellow ginger-cleaning-pulverizing-fermentation-acid hydrolysis-washing-drying-extraction-crystallization-saponin.The traditional processing technology operation of turmeric saponin is fairly simple, but because the material after the fermentation has all participated in acid hydrolytic reaction, make traditional technology have three subject matters: 1) seriously polluted, one ton of saponin of every production produces 800-1000 ton waste water, and the waste strength height, the COD mean concns of its waste water is up to 30000-50000mg/L; 2) sour consumption is big, and the ton saponin consumes sulfuric acid 15-20 ton; 3) comprehensive utilization of resources rate is low, and a large amount of starch that contain in the yellow ginger are not utilized.
Some useful explorations have been carried out in domestic cleaner production and comprehensive utilization of resources etc. with regard to turmeric saponin at present, have also accumulated a large amount of experiences.
Plant proposes " partition method is produced the diosgenin novel process " to the northwest, Shaanxi, its key step is elder generation's separating starch slurry from yellow ginger, carries out dilute acid hydrolysis again and makes mashing, obtains liquid glucose and sugared slag after the separation, the sugar slag is used for extracting saponin, and liquid glucose is used for the fermentative production saponin(e.The loss of this technology saponin in the starch washing separates can influence the saponin yield, and the water treatment amount is big, does not obtain yet at present promoting but according to the literature.
Hubei Fangtong Drug Industry Co., Ltd has applied for " microwave broken wall and alcohol extracting and oil are put forward the processing method that diosgenin is produced in the technology coupling ", and the material after this method will be pulverized carries out microwave exposure, when making temperature of charge reach 100 ℃, continues radiation 30-40 minute; With weight of material 2-3 methyl alcohol or ethanol doubly feed back was extracted 6-8 hour again; Discard filter residue after the filtration, filtrate is concentrated near doing, get alcohol extract; Alcohol extract added amylase enzymolysis 72-120 hour; Enzymolysis solution is carried out acid hydrolysis, obtain the saponin crude product; In the saponin crude product, add the gasoline extraction saponin at last.This method energy consumption is higher relatively, the equipment requirements height, and solvent-oil ratio is big, and technico-economical comparison is unsatisfactory during suitability for industrialized production.
The someone proposes the starch partition method in addition, adopts physical method for separation to obtain starch and fiber before hydrolysis, and it exists saponin to run off, the pre-treatment energy consumption is big, leaching requirement big, the saponin(e layer concentrates deficiencies such as difficulty.
In a word, although at present in the part link of turmeric saponin cleaner production some researchs and report have been arranged, exist not enough mostly.At present, it is open that Shang Weijian utilizes the relevant technology of the separation of saccharification binding film and ultrasonic extraction turmeric saponin.
Summary of the invention
The object of the present invention is to provide a kind of cleaning manufacturing technique method of turmeric saponin.This processing method is utilized saccharification, membrane sepn and ultrasonic extraction technology, can significantly reduce the waste water generation, reduces the sulfuric acid consumption, improves saponin yield and comprehensive utilization of resources rate simultaneously.
To achieve these goals, technical scheme of the present invention is: a kind of cleaning manufacturing technique method of turmeric saponin is characterized in that step is as follows:
1) cadmium yellow ginger or dried yellow ginger are cleaned removal of impurities after, be broken to below the particle diameter 5mm with pigment, fermented 48-72 hour between be incubated 45-60 ℃;
2) the yellow ginger slurry that will finish after the fermentation liquefies, and liquefaction temperature is controlled at 90 ~ 100 ℃, adds the high temperature resistant α-Dian Fenmei that accounts for amount of slurry 0.02 ~ 0.05% weight part, enzyme activity 20000u/mL, liquefaction 90min; After finishing liquefaction, when liquefied fermented glutinous rice is cooled to 60 ± 2 ℃, add the saccharifying enzyme that accounts for liquefied fermented glutinous rice 0.03 ~ 0.06% weight part, enzyme activity 100000u/mL, insulation saccharification 4 ~ 5h obtains converted mash;
3) with step 2) converted mash that obtains carries out pre-separation by 60 ~ 100 purpose vibratory screening apparatuss and expeller, obtains fibrous residue and filtrate;
4) filtrate that step 3) is obtained is carried out membrane sepn by mineral membrane, and the membrane sepn temperature is controlled at 65-75 ℃, obtains membrane concentration liquid and liquid glucose;
5) fibrous residue that step 3) is obtained defeated by drying machine drying to water ratio less than after 10%, deliver in the feeding unit of continuous countercurrent ultrasonic extractor, beginning charging the time is that the ratio of 1:1-1.5 is input in the extraction tube by the deslagging end of continuous countercurrent ultrasonic extractor according to the ratio of yellow ginger weight kilogram and ethanol volume liter with the methyl alcohol of 75%-85% or alcohol solvent, at normal temperatures and pressures, carry out the continuous countercurrent ultrasonic extraction 90-120 minute, and obtained fibrous residue extract remainder and extraction liquid;
6) in the step 5) extraction after finishing the fibrous residue extract remainder carry out solvent recuperation by the solvent recovering system that slag-drip opening enters the continuous countercurrent ultrasonic extractor;
7) extraction liquid that obtains in the step 5) is transported to the 10%-20% that concentration tank is concentrated into original volume after the slag liquid/gas separator separates, and obtains being rich in the extraction concentrated solution of saponin(e, reclaims ethanol simultaneously;
8) membrane concentration liquid that the extraction concentrated solution that step 7) is obtained and step 4 obtain carries out acid-catalyzed hydrolysis after mixing together, and hydrolysising condition is: system acid concentration 0.6 ~ 1.0mol/L, 120 ~ 130 ℃ of temperature of reaction (0.2 ~ 0.3MPa), hydrolysis time 2-3h; The hydrolyzate that obtains filters, and the filter cake that obtains adopts tap water or soda lye wash to neutral, carries out drying again and obtains saponin hydrolysate;
9) saponin hydrolysate that step 8) is obtained adopts No. 120 gasoline extraction, after the extract drying, obtains saponin.
The invention has the beneficial effects as follows:
By the converted mash behind the yellow ginger fermentation liquefying-saccharifying is carried out membrane sepn and ultrasonic extraction, make and before acid hydrolysis, the starch in the yellow ginger and the fiber overwhelming majority are isolated the material system, the membrane concentration liquid that only membrane sepn is obtained and ultrasonic extraction obtain extracting concentrated solution and carry out acid hydrolysis, reduced participating in acid-hydrolyzed inventory significantly, thereby subdued the generation of pollutent in the source; By the yellow ginger after the fermentation is carried out liquefying-saccharifying and membrane sepn, but the liquid glucose direct production alcohol that obtains, or as the raw materials for production of lactic acid, citric acid and yeast extract etc., resource is fully utilized effectively; Only fibrous residue is carried out ultrasonic extraction, compare with whole yellow ginger materials abstractions, significantly reduced the consumption of solvent; Utilize ultrasonic auxiliary extraction, make the extraction time significantly shorten; The minimizing of acid hydrolysis inventory makes acid consumption reduce, and hydrolysising condition is easier to control simultaneously, and hydrolytic process is meticulousr, is conducive to the raising of saponin yield; Use membrane sepn and ultrasonic extraction technology, when significantly reducing the pollutent generation, saponin(e does not run off, and saponin yield is guaranteed.
Embodiment
Embodiment 1:
A kind of cleaning manufacturing technique method of turmeric saponin, step is as follows:
1) 1000kg cadmium yellow ginger (Yunxi County, Hubei Province) is adopted the rotating cage ginger washing machine clean removal of impurities, get clean yellow ginger 850kg, add water 630kg again and be crushed to below the particle diameter 5mm with pulverizer, squeezed in the fermentor tank between 35-60 ℃ of the insulation fermentation 72 hours;
2) the yellow ginger slurry that will finish after the fermentation liquefies, and liquefaction temperature is controlled at 90 ~ 100 ℃, adds the high temperature resistant α-Dian Fenmei 0.5kg of enzyme activity 20000u/mL, liquefaction 90min; When finishing liquefied fermented glutinous rice after the liquefaction and being cooled to 60 ± 2 ℃, add the saccharifying enzyme 0.5kg of enzyme activity 100000u/mL, insulation saccharification 4h obtains converted mash;
3) with step 2) converted mash that obtains carries out pre-separation by expeller and 60 purpose vibratory screening apparatuss, obtains fibrous residue and filtrate;
4) filtrate that step 3) is obtained is carried out membrane sepn by mineral membrane, and the membrane sepn temperature is controlled at 65-72 ℃, obtains membrane concentration liquid and liquid glucose;
5) fibrous residue that step 3) is obtained is defeated be 5% by drying machine drying to water ratio after, deliver in the feeding unit of continuous countercurrent ultrasonic extractor (Jining Sinobest Construction Machinery Co., Ltd), beginning charging the time is that the ratio of 1:1 is input in the extraction tube by the deslagging end of continuous countercurrent ultrasonic extractor according to the ratio of yellow ginger weight kilogram and ethanol volume liter with 75% ethanol, at normal temperatures and pressures, carry out the continuous countercurrent ultrasonic extraction 40 minutes, and obtained fibrous residue extract remainder and extraction liquid;
6) in the step 5) extraction after finishing the fibrous residue extract remainder carry out solvent recuperation by the solvent recovering system that slag-drip opening enters the continuous countercurrent ultrasonic extractor;
7) extraction liquid that obtains in the step 5) is transported to concentration tank and is concentrated into 25% of original volume after the slag liquid/gas separator separates, and obtains being rich in the extraction concentrated solution of saponin(e, reclaims ethanol simultaneously;
8) the membrane concentration liquid that the extraction concentrated solution that step 7) is obtained and step 4 obtain carries out acid-catalyzed hydrolysis after mixing together, and hydrolysising condition is: system acid concentration 0.9mol/L, 120 ℃ of temperature of reaction, hydrolysis time 2h; The hydrolyzate that obtains filters, and the filter cake that obtains adopts tap water or soda lye wash to neutral, carries out drying again and obtains saponin hydrolysate;
9) saponin hydrolysate that step 8) is obtained adopts No. 120 gasoline extraction, after the extract drying, obtains saponin.
Finally, get saponin 8.1kg, saponin yield 0.81%, 195 ℃ of saponin fusing points, the starch liquid sugar 850kg of by-product concentration of reduced sugar 8.5%, wastewater flow rate 480kg, COD value 50000mg/L.
Embodiment 2:
A kind of cleaning manufacturing technique method of turmeric saponin is characterized in that step is as follows:
1) 1000kg cadmium yellow ginger (Shanyang County, Hubei Province) is adopted the rotating cage ginger washing machine clean removal of impurities, get clean yellow ginger 880kg, be crushed to below the particle diameter 5mm with pulverizer again, squeezed in the fermentor tank between 35-60 ℃ of the insulation fermentation 72 hours;
2) the yellow ginger slurry that will finish after the fermentation liquefies, and liquefaction temperature is controlled at 90 ~ 100 ℃, adds the high temperature resistant α-Dian Fenmei 0.5kg of enzyme activity 20000u/mL, liquefaction 90min; When finishing liquefied fermented glutinous rice after the liquefaction and being cooled to 60 ± 2 ℃, add the saccharifying enzyme 0.5kg of enzyme activity 100000u/mL, insulation saccharification 4h obtains converted mash;
3) with step 2) converted mash that obtains carries out pre-separation by expeller and 60 purpose vibratory screening apparatuss, obtains fibrous residue and filtrate;
4) filtrate that step 3) is obtained is carried out membrane sepn by mineral membrane, and the membrane sepn temperature is controlled at 65-72 ℃, obtains membrane concentration liquid and liquid glucose;
5) fibrous residue that step 3) is obtained is defeated be 5% by drying machine drying to water ratio after, deliver in the feeding unit of continuous countercurrent ultrasonic extractor (Jining Sinobest Construction Machinery Co., Ltd), beginning charging the time is that the ratio of 1:1 is input in the extraction tube by the deslagging end of continuous countercurrent ultrasonic extractor according to the ratio of yellow ginger weight kilogram and ethanol volume liter with 75% ethanol, at normal temperatures and pressures, carry out the continuous countercurrent ultrasonic extraction 40 minutes, and obtained fibrous residue extract remainder and extraction liquid;
6) in the step 5) extraction after finishing the fibrous residue extract remainder carry out solvent recuperation by the solvent recovering system that slag-drip opening enters the continuous countercurrent ultrasonic extractor;
7) extraction liquid that obtains in the step 5) is transported to concentration tank and is concentrated into 25% of original volume after the slag liquid/gas separator separates, and obtains being rich in the extraction concentrated solution of saponin(e, reclaims ethanol simultaneously;
8) the membrane concentration liquid that the extraction concentrated solution that step 7) is obtained and step 4 obtain carries out acid-catalyzed hydrolysis after mixing together, and hydrolysising condition is: system acid concentration 0.9mol/L, 120 ℃ of temperature of reaction, hydrolysis time 2h; The hydrolyzate that obtains filters, and the filter cake that obtains adopts tap water or soda lye wash to neutral, carries out drying again and obtains saponin hydrolysate;
9) saponin hydrolysate that step 8) is obtained adopts No. 120 gasoline extraction, after the extract drying, obtains saponin.
Finally, get saponin 8.5kg, saponin yield 0.85%, 195 ℃ of saponin fusing points, the starch liquid sugar 900kg of by-product concentration of reduced sugar 8.8%, wastewater flow rate 450kg, COD value 50000mg/L.
Claims (1)
1. the cleaning manufacturing technique method of a turmeric saponin is characterized in that step is as follows:
1) cadmium yellow ginger or dried yellow ginger are cleaned removal of impurities after, be broken to below the particle diameter 5mm with pigment, fermented 48-72 hour between be incubated 45-60 ℃;
2) the yellow ginger slurry that will finish after the fermentation liquefies, and liquefaction temperature is controlled at 90 ~ 100 ℃, adds the high temperature resistant α-Dian Fenmei that accounts for amount of slurry 0.02 ~ 0.05% weight part, enzyme activity 20000u/mL, liquefaction 90min; After finishing liquefaction, when liquefied fermented glutinous rice is cooled to 60 ± 2 ℃, add the saccharifying enzyme that accounts for liquefied fermented glutinous rice 0.03 ~ 0.06% weight part, enzyme activity 100000u/mL, insulation saccharification 4 ~ 5h obtains converted mash;
3) with step 2) converted mash that obtains carries out pre-separation by 60 ~ 100 purpose vibratory screening apparatuss and expeller, obtains fibrous residue and filtrate;
4) filtrate that step 3) is obtained is carried out membrane sepn by mineral membrane, and the membrane sepn temperature is controlled at 65-75 ℃, obtains membrane concentration liquid and liquid glucose;
5) fibrous residue that step 3) is obtained defeated by drying machine drying to water ratio less than after 10%, deliver in the feeding unit of continuous countercurrent ultrasonic extractor, beginning charging the time is that the ratio of 1:1-1.5 is input in the extraction tube by the deslagging end of continuous countercurrent ultrasonic extractor according to the ratio of yellow ginger weight kilogram and ethanol volume liter with the methyl alcohol of 75%-85% or alcohol solvent, at normal temperatures and pressures, carry out the continuous countercurrent ultrasonic extraction 90-120 minute, and obtained fibrous residue extract remainder and extraction liquid;
6) in the step 5) extraction after finishing the fibrous residue extract remainder carry out solvent recuperation by the solvent recovering system that slag-drip opening enters the continuous countercurrent ultrasonic extractor;
7) extraction liquid that obtains in the step 5) is transported to the 10%-20% that concentration tank is concentrated into original volume after the slag liquid/gas separator separates, and obtains being rich in the extraction concentrated solution of saponin(e, reclaims ethanol simultaneously;
8) membrane concentration liquid that the extraction concentrated solution that step 7) is obtained and step 4 obtain carries out acid-catalyzed hydrolysis after mixing together, and hydrolysising condition is: system acid concentration 0.6 ~ 1.0mol/L, 120 ~ 130 ℃ of temperature of reaction (0.2 ~ 0.3MPa), hydrolysis time 2-3h;
The hydrolyzate that obtains filters, and the filter cake that obtains adopts tap water or soda lye wash to neutral, carries out drying again and obtains saponin hydrolysate;
9) saponin hydrolysate that step 8) is obtained adopts No. 120 gasoline extraction, after the extract drying, obtains saponin.
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| CN105348357A (en) * | 2015-12-03 | 2016-02-24 | 中国科学院过程工程研究所 | Lepidium meyenii saponin as well as preparation method and application thereof |
| CN108058423A (en) * | 2017-12-15 | 2018-05-22 | 海宁永欣科技咨询有限公司 | The extracting process and its pressing device of plant petals |
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Application publication date: 20130814 |