CN100432095C - Waste-water-free production method for diosgenin - Google Patents
Waste-water-free production method for diosgenin Download PDFInfo
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- CN100432095C CN100432095C CNB2006100177878A CN200610017787A CN100432095C CN 100432095 C CN100432095 C CN 100432095C CN B2006100177878 A CNB2006100177878 A CN B2006100177878A CN 200610017787 A CN200610017787 A CN 200610017787A CN 100432095 C CN100432095 C CN 100432095C
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Abstract
The present invention relates to a method for producing diosgenin without wastewater, which comprises: by using a pressurization and decomposition method, after coarse crushing, dioscorea raw materials, such as yellow ginger, dioscorea nipponica, yellow yam, etc., are put in a thermal decomposition device to be pressurized and decomposed, the temperature in the device is controlled between 0 and 200 DEG C, the pressure in the device is controlled between 0.8 and 40MPa, and the retention time is controlled between 5 minutes and 8 hours; after the decomposed material is dried, diosgenin is extracted by a conventional method. In the process of production, the present invention has improvement on raw material treatment processes, acid and base are not used in the whole process of production, and the step of acid hydrolysis in the traditional extraction method is completely eliminated. Thereby, the generation of a large amount of wastewater is avoided, and the extraction effect is obvious. The extracted materials can be used as raw materials for fermenting alcohol, and can be used as raw materials for producing feed and fertilizer or activated carbon. The present invention has the advantages of simple production process, short production period and low production cost, and can satisfy the requirements of environmental protection.
Description
Technical field:
The present invention relates to a kind of method of extracting diosgenin, particularly relate to and a kind ofly from yam tuberous roots such as yellow ginger, Ningpo Yam Rhizome, Dioscorea panthaica Prain et Burkill, extract the diosgenin non-wastewater production method of (also claiming diosgenin), belong to diosgenin extraction separation field.
Background technology:
Traditional production technique of extracting diosgenin (also claiming diosgenin) from yams such as yellow ginger, Ningpo Yam Rhizome, Dioscorea panthaica Prain et Burkill comprises: hydrolysis is cut off glycoside bond, is slightly put forward steps such as glucoside unit, recrystallize, and wherein hydrolysis process is the committed step of decision yield.Hydrolysis process mainly comprises chemical hydrolysis (directly acid hydrolysis, pre-fermentation-acid hydrolysis) and biological hydrolysis process (enzymolysis or microbial fermentation), adopts operations such as filtration, extraction, recrystallize to obtain diosgenin after the hydrolysis then.Except that containing a small amount of sapogenin, also have Mierocrystalline cellulose that content reaches 40% starch and 50% in the Chinese yam because the biological hydrolysis process condition is relatively gentleer, sapogenin yield height not only, and help the comprehensive utilization of starch and cellulose resource, thereby more rising; But because chemical hydrolysis equipment is simple relatively, study comparatively ripely, the present stage practical application is more general.At present, it is solvent that extraction process generally adopts organic solvents such as gasoline, alcohol, sherwood oil, hexane, chloroform, benzene, and the energy consumption height has inflammable and explosive danger, also environment has been caused pollution.Simultaneously, organic solvent causes foreign matter content height in the extract to the dissolving poor selectivity of diosgenin, needs decolouring to reach repeatedly recrystallization, and purification step is many, and yield is low; Supercritical CO
2(Supercritical CO
2, SC-CO
2) abstraction technique is the new technology that development in recent years is got up, just extensively be studied and progressively obtaining some application aspect the active skull cap components extraction.
Conventional acid-hydrolysis method is (to adopt hydrochloric acid or aqueous sulfuric acid) directly medicinal material coarse powder to be hydrolyzed in acidic solution more, makes dioscin be hydrolyzed to glucoside unit, with lipophilic solvent glucoside unit is extracted again.In hydrolytic process, what have carries out under normal pressure, and what have carries out under pressurized state.Under pressurized state the time of hydrolysis shorter, productive rate is higher.But thisly have at the industrial direct acid-hydrolysis method that generally adopts that hydrolysis is incomplete, yield rate is low (yield is generally about 1.7%), starch can not be by comprehensive utilization, work in-process are a large amount of during big, the washing of water consumption in extracting runs off and problem such as serious environment pollution.
Conventional biological hydrolysis process is to stir adding water after the pulverizing such as yellow ginger, Ningpo Yam Rhizome, after spontaneous fermentation, is hydrolyzed with diluted acid, and neutralization is filtered, and further extracts with organic solvent behind the filtration cakes torrefaction, and crystallization goes out finished product; Or size mixing adding water after the pulverizing such as cadmium yellow ginger, Ningpo Yam Rhizome, add α-Dian Fenmei earlier and liquefies, adding saccharifying enzyme then carries out saccharification, till saccharification to iodine liquid indication is not blueness.Make enzyme-deactivating, the filtrate behind the suction filtration is further handled to extract and is obtained glucose; Filter residue is hydrolyzed with diluted acid, uses organic solvent extraction again, condensing crystal, and oven dry obtains finished product; Or, add a certain amount of enzyme and water logging bubble with after the pulverizing such as yellow ginger, Ningpo Yam Rhizome, carry out enzymatic hydrolysis and fermentation and handle, wash suction filtration then, filter residue diluted acid back hydrolysis, neutralization is filtered, carry out extracting with organic solvent behind the filtration cakes torrefaction, condensing crystal, the recrystallize oven dry obtains finished product.
No matter chemical hydrolysis or biological hydrolysis process, extracting in the diosgenin process all needs to be hydrolyzed, and the filtrate treatment process after the hydrolysis has two kinds: a kind of method is that filtrate is discharged as waste water, but does the damage ratio of environment more serious like this.Another kind method is through improvement, and the further processing of filtrate can be got glucose product.If handle reclaiming filtrate, recyclable saponin significantly reduces the discharging of waste water.If do not handle to reclaiming filtrate, press the yellow ginger production statistics of artificial growth, 1 ton of saponin of every production needs 130～180 tons of cadmium yellow ginger, 15～20 tons of technical hydrochloric acids (volume fraction 35%) (or volume fraction 98% sulfuric acid 7～8 tons) produce 400～500 tons of waste water.In the comprehensive wastewater, because of the directly discharging of unemployed starch, sugar part, cause survey the COD value up to 30000mg/L about (about the about 8000mg/L of BOD), pH value 1.0～2.5, NH
3The about 300mg/L of-N.In addition, 1 ton of saponin of every production also produces the yellow ginger slag about 10 tons.Because yellow ginger processing needs a large amount of waters, so most of enterprise build the place near the water source in, but the acidolysis waste water that produces in saponin producing process is called as the king of waste water, and the black liquor that produces with papermaking equally is difficult to handle.Many enterprises have spent money on treatment facility, because cost of water treatment is very high, can only not have a tame manufacturing enterprise can accomplish discharged wastewater met the national standard at present as ornaments, and a large amount of efflux wastewaters of producer of producing diosgenin bring pollution for these water sources, form huge threat.Therefore, be badly in need of a kind of need not and carry out the no waste water production technique appearance that acid hydrolysis just can extract diosgenin, satisfy environmental protection requirement.
Summary of the invention:
The objective of the invention is: in order to overcome the problem that needs in the diosgenin production process to carry out acid hydrolysis and produce a large amount of waste water, provide a kind of acid hydrolysis that need not to carry out, just can extract the non-wastewater production method of diosgenin.
The objective of the invention is to be achieved through the following technical solutions:
A kind of non-wastewater production method of diosgenin, its concrete steps are:
A. coarse crushing: dioscorea raw materials is removed silt, is ground into the bulk of 0.5～5cm size;
B. pressurization is decomposed: the raw material after the coarse crushing is placed on the decomposition of pressurizeing in the thermal decomposer, and the temperature in the control device is 0～200 ℃, and pressure is 0.8～40MPa, and the hold-time is 5min～8h, blowing then;
C. dry: the material after will decomposing carries out drying treatment, and drying temperature is less than 150 ℃, and material moisture is less than 10%.
D. extract: dried material is adopted organic solvent extraction, or adopt supercritical CO
2Extraction promptly obtains needed diosgenin, and the optional diosgenin that obtains is adopted adds an amount of charcoal absorption and decolour and make with extra care.
Bulk in the described step " a " is between 0.5～3cm; Drying temperature in the described step " c " is between 70～100 ℃.
Described thermal decomposer is medium pressure vessel or high pressure vessel, and (vessel) class is decided according to concrete pressure, when pressure is lower than 10MPa, is medium pressure vessel, when pressure is higher than 10MPa, is high pressure vessel.
In the described thermal decomposer, the medium that produces pressure is CO
2, N
2, in the air, water vapor a kind of, two or more.
When adopting organic solvent extraction, total consumption of organic solvent is 8～30 times of degradation production volume, and temperature remains on 80～95 ℃, refluxing extraction 0.5～8 hour, and filtered while hot is collected filtrate, concentrates then to reclaim organic solvent.
Described employing supercritical CO
2Extraction process in, add an amount of ethanol as entrainment agent.
Described dioscorea raw materials is the tuberous root of yellow ginger, Ningpo Yam Rhizome or Dioscorea panthaica Prain et Burkill.
Material after the extraction uses as the raw material of fermentation alcohol.
Material after the extraction uses as the raw material of producing feed, fertilizer or gac.
Positive beneficial effect of the present invention:
1. the non-wastewater production method of diosgenin of the present invention in process of production, improves the treatment process of raw material, and having abandoned fully needs in the traditional extraction process to carry out acid-hydrolyzed step, has avoided the generation of a large amount of waste water.Need not to use acid, alkali in whole process of production, also do not have waste water and produce, Production Flow Chart is simple, and the production cycle can shorten greatly, and production cost significantly reduces, and extraction effect is remarkable, satisfies environmental requirement.
2. the non-wastewater production method of diosgenin of the present invention extracts the raw material use that the back material that is produced can be used as fermentation alcohol; Also can be used as the raw material of producing feed, fertilizer or gac and use, greatly utilized resource, saved cost.
Embodiment:
Embodiment 1: a kind of non-wastewater production method of diosgenin, and its concrete steps are: bright raw material 10kg is removed silt, carries out coarse crushing, form the bulk of 1cm～5cm size; Raw material after the coarse crushing is placed on the decomposition of pressurizeing in the hot high pressure decomposer, adopts CO
2For the medium of pressure is provided, the temperature in the control device is 120 ℃, and pressure is 20MPa, the 6h that keep-ups pressure, blowing then; Material after the thermolysis is cooled off, and drying promptly can be used for extracting diosgenin; Extract diosgenin with sherwood oil as organic solvent; The consumption of sherwood oil (volume) is 10 times (with the 10g raw material are example, add the 100mL sherwood oil and carry out refluxing extraction) of quality of material, and extracting temperature is 85 ℃, backflow 4h, and filtered while hot is collected filtrate; In filtrate, add the 0.2g gac, backflow 0.5h, filtered while hot is collected filtrate, and filtrate is concentrated into 20ml under normal pressure, pour out, and is placed on that 12h can obtain needed diosgenin in the stink cupboard.
Bright raw material recited above is the bright raw material of yam tuberous roots such as yellow ginger, Ningpo Yam Rhizome, Dioscorea panthaica Prain et Burkill.
Embodiment 2: a kind of non-wastewater production method of diosgenin, and its concrete steps are: dried raw material 10kg is removed silt, carries out coarse crushing, form the bulk of 1cm～5cm size; Raw material after the coarse crushing is soaked 2h in clear water, be placed on the decomposition of pressurizeing in the hot high pressure decomposer then, adopt CO
2For the medium of pressure is provided, the temperature in the control device is 150 ℃, and pressure is 30MPa, the 4h that keep-ups pressure, blowing then.Material after the thermolysis is cooled off, and drying promptly can be used for extracting diosgenin.
Use supercritical CO
2The extraction diosgenin extracts as entrainment agent with ethanol; Raw material 200g after heat-obtaining decomposes is in extraction kettle, and extracting pressure is 35MPa, and extraction temperature is 45 ℃, and the extraction time is 2h, CO
2Flow is 10kg/h, and separating still 1 and 2 pressure are 5.0MPa, and the product after the extraction is emitted by separating still, can obtain needed diosgenin.
Dried raw material recited above is the dried raw material of yam tuberous roots such as yellow ginger, Ningpo Yam Rhizome, Dioscorea panthaica Prain et Burkill.
Embodiment 3: a kind of non-wastewater production method of diosgenin, its concrete steps are: bright raw material 5kg is removed silt, carries out coarse crushing, form the bulk of 1cm～2cm size.Raw material after the coarse crushing is placed on the decomposition of pressurizeing in the thermal decomposer, adopts CO
2For the medium of pressure is provided, the temperature in the control device is a normal temperature, and pressure is 30MPa, the 3h that keep-ups pressure, blowing then.Material after the thermolysis is carried out drying treatment, as the raw material that extracts diosgenin.
Extract diosgenin with methyl alcohol as organic solvent.The consumption of methyl alcohol (volume) is 10 times of quality of material, promptly gets the 10g raw material, adds 100ml methyl alcohol and carries out refluxing extraction, and extracting temperature is 85 ℃, backflow 6h, and filtered while hot is collected filtrate; In filtrate, add the 0.2g gac, backflow 0.5h, filtered while hot is collected filtrate, and filtrate is concentrated into 20ml under normal pressure, pour out, and is placed on that 12h can obtain needed diosgenin in the stink cupboard.
Bright raw material recited above is the bright raw material of yam tuberous roots such as yellow ginger, Ningpo Yam Rhizome, Dioscorea panthaica Prain et Burkill.
Embodiment 4: a kind of non-wastewater production method of diosgenin, its concrete steps are: dried raw material 100kg is removed silt, carries out coarse crushing, form the bulk of 1cm～5cm size.Raw material after the coarse crushing is placed on the decomposition of pressurizeing in the thermal decomposer, adopts steam for the medium of pressure is provided, the pressure in the control device is 1MPa, the 0.5h that keep-ups pressure, blowing then.Material after the thermolysis is cooled off, and drying promptly can be used for extracting diosgenin.
Extract diosgenin with ethanol as organic solvent.Consumption of ethanol (volume) is 15 times of quality of material, promptly gets the 10g raw material, adds 150ml ethanol and carries out refluxing extraction, and extracting temperature is 90 ℃, backflow 6h, and filtered while hot is collected filtrate; In filtrate, add the 0.2g gac, backflow 0.5h, filtered while hot is collected filtrate, and filtrate is concentrated into 30ml under normal pressure, pour out, and is placed on that 12h can obtain needed diosgenin in the stink cupboard.
Dried raw material recited above is the dried raw material of yam tuberous roots such as yellow ginger, Ningpo Yam Rhizome, Dioscorea panthaica Prain et Burkill.
Claims (9)
1. the non-wastewater production method of a diosgenin, its concrete steps are:
A. coarse crushing: dioscorea raw materials is removed silt, is ground into the bulk of 0.5～5cm size;
B. pressurization is decomposed: the raw material after the coarse crushing is placed on the decomposition of pressurizeing in the thermal decomposer, and the temperature in the control device is 0～200 ℃, and pressure is 0.8～40MPa, and the hold-time is 5min～8h, blowing then;
C. dry: the material after will decomposing carries out drying treatment, and drying temperature is less than 150 ℃, and material moisture is less than 10%;
D. extract: dried material is adopted organic solvent extraction, or adopt supercritical CO
2Extraction promptly obtains needed diosgenin, and the optional diosgenin that obtains is adopted adds an amount of charcoal absorption and decolour and make with extra care.
2. according to the non-wastewater production method of the described diosgenin of claim 1, it is characterized in that: the bulk in the described step " a " is between 0.5～3cm; Drying temperature in the described step " c " is between 70～100 ℃.
3. according to the non-wastewater production method of the described diosgenin of claim 1, it is characterized in that: described thermal decomposer is medium pressure vessel or high pressure vessel, and (vessel) class is decided according to concrete pressure, when pressure is lower than 10MPa, be medium pressure vessel, when pressure is higher than 10MPa, be high pressure vessel.
4. according to the non-wastewater production method of the described diosgenin of claim 3, it is characterized in that: in the described thermal decomposer, the medium that produces pressure is CO
2, N
2, in the air, water vapor a kind of, two or more.
5. according to the non-wastewater production method of the described diosgenin of claim 1, it is characterized in that: when adopting organic solvent extraction, total consumption of organic solvent is 8～30 times of degradation production volume, temperature remains on 80～95 ℃, refluxing extraction 0.5～8 hour, filtered while hot is collected filtrate, concentrates then to reclaim organic solvent.
6. according to the non-wastewater production method of the described diosgenin of claim 1, it is characterized in that: described employing supercritical CO
2Extraction process in, add an amount of ethanol as entrainment agent.
7. according to the non-wastewater production method of the described diosgenin of claim 1, it is characterized in that: described dioscorea raw materials is the tuberous root of yellow ginger, Ningpo Yam Rhizome or Dioscorea panthaica Prain et Burkill.
8. according to the non-wastewater production method of each described diosgenin of claim 1～7, it is characterized in that: the material after the extraction uses as the raw material of fermentation alcohol.
9. according to the non-wastewater production method of each described diosgenin of claim 1～7, it is characterized in that: the material after the extraction uses as the raw material of producing feed, fertilizer or gac.
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| CN101830965B (en) * | 2010-05-13 | 2013-01-16 | 金凤燮 | Method for catalyzing and hydrolyzing natural nucleoside compound by metal ion |
| CN103183718A (en) * | 2011-12-28 | 2013-07-03 | 十堰市秦岭中地生物科技有限公司 | Hydrolysis method for production of saponin from turmeric |
| CN104126782B (en) * | 2014-07-29 | 2015-10-21 | 桂林实力科技有限公司 | A kind of momordica grosvenori sweetening agent and preparation method thereof |
| CN107936082B (en) * | 2017-12-01 | 2019-08-27 | 广东丰绿源生物医药科技有限公司 | The method of microwave and hot pressing decomposition technique combination production Chinese yam saponin |
| 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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| CN1111250A (en) * | 1994-05-03 | 1995-11-08 | 厦门同安皂素厂 | Method of extracting dioscorea saponin from dioscorea plant |
| CN1243834A (en) * | 1999-06-27 | 2000-02-09 | 中国科学院昆明植物研究所 | Process for preparing yam saponin |
| CN1442484A (en) * | 2003-04-01 | 2003-09-17 | 田成国 | Production method of diosgenin |
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2006
- 2006-05-16 CN CNB2006100177878A patent/CN100432095C/en not_active Expired - Fee Related
Patent Citations (3)
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|---|---|---|---|---|
| CN1111250A (en) * | 1994-05-03 | 1995-11-08 | 厦门同安皂素厂 | Method of extracting dioscorea saponin from dioscorea plant |
| CN1243834A (en) * | 1999-06-27 | 2000-02-09 | 中国科学院昆明植物研究所 | Process for preparing yam saponin |
| CN1442484A (en) * | 2003-04-01 | 2003-09-17 | 田成国 | Production method of diosgenin |
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