CN1450082A - Process for extracting dioscin from yellow ginger and Rhizoma Dioscoreae Nipponicae and producing organic fertilizer using residue of same - Google Patents
Process for extracting dioscin from yellow ginger and Rhizoma Dioscoreae Nipponicae and producing organic fertilizer using residue of same Download PDFInfo
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- CN1450082A CN1450082A CN03127944A CN03127944A CN1450082A CN 1450082 A CN1450082 A CN 1450082A CN 03127944 A CN03127944 A CN 03127944A CN 03127944 A CN03127944 A CN 03127944A CN 1450082 A CN1450082 A CN 1450082A
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- diosgenin
- yellow ginger
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/20—Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The method for extracting dioscorea saponin from yellow ginger and Japanese dioscorea includes the following steps: washing yield ginger and Japanese dioscorea, breaking them, adding clear water and uniformly stirring them, ultrasonic wave treatment, placing them into cracking tank, adding concentrated hydrochloric acid or sulfuric acid, cracking under the condition of a certain concentration and pressure, adopting sodium hydroxide and potassium hydroxide to neutralize crackate to neutrality, distilling crackate mixture, when the water content is up to 15-40%, discharging material, drying to control water content in 3-8%, and using supercritical Co2 extraction process to obtain dioscorea saponin, and utilizing waste dregs produced after extraction to produce biological organic fertilizer for improving soil structure.
Description
(1) technical field
The present invention relates to a kind ofly extract the method for diosgenin and with its waste residue production biological organic fertilizer by yellow ginger, Ningpo Yam Rhizome.
(2) background technology
Yellow ginger is a Dioscoreaceae plant Rhizome of Peltate Yam rhizome, and Ningpo Yam Rhizome is a Dioscoreaceae plant Dioscorea nipponica Mak. Ningpo Yam Rhizome rhizome, and diosgenin is the important source material of synthesizing steroid hormone medicine.The plant saponin at present still can not chemosynthesis, can only extract from minority plants such as yellow ginger, Ningpo Yam Rhizome, and yellow ginger is the highest plant of saponin content in the world.China has become the big producing country of diosgenin, and the saponin of wherein extracting from yellow ginger accounts for more than 70% of total amount.Because yellow ginger has good cultivation, is suitable for large-scale planting, all there is plantation in provinces such as China Shaanxi, Hubei, Hunan, Sichuan, Yunnan, Guizhou.
Traditional diosgenin extraction process has acid-hydrolysis method and water mill enzymolysis process, and 1 ton of saponin of every production is approximately used hydrochloric acid 15-18 ton, water 260-500 ton, and the saponin yield is only about 2%.Fermentation time is long in the production process, causes easily and goes mouldy, and it is not thorough to ferment, and the product fusing point is reduced, and yield descends; Adopt the strong acid catalytic pyrolysis, or with Ye Huamei and saccharifying enzyme enzymolysis, the glucosyl group of dioscin and the molecular linkage of diosgenin are disconnected, glucosyl group, starch and other chemical substances are stayed in the lysate, these materials are discharged with hydrochloric acid in water washing process, and environment and water source are caused severe contamination.
In recent years, because the yellow ginger plantation is persistently overheating, yellow ginger processing has become the local economy mainstay industry, and the investment construction of Waste Water Treatment can not be supporting with it, the phenomenon of random effluent is still very serious, it is imperative, very urgent to change traditional yellow ginger extraction process, and this problem has caused showing great attention to of local government.At present, the existing technology that adopts the supercritical carbon dioxide extraction diosgenin, its preamble still adopts the strong acid catalytic pyrolysis, just change gasoline extraction into supercritical carbon dioxide extraction, shortened extraction time, the saponin yield increases, and has eliminated the hidden danger of using gasoline to bring simultaneously, but the waste liquid of strong acid catalytic pyrolysis process discharging still causes severe contamination to environment and water source.
(3) summary of the invention
The technical problem that the present invention mainly solves is that raw material has shortened technological process without fermentative processing in the diosgenin extraction process; Waste liquid behind the employing strong acid catalytic pyrolysis does not discharge, and has eliminated environmental pollution, has reduced production cost; Waste residue behind the extraction diosgenin can fully utilize, and produces biological organic fertilizer.
Technical solution of the present invention is: yellow ginger, Ningpo Yam Rhizome are placed in the container through washing, pulverizing, add clear water according to 1: 0.5～3 and stir; Adopt ultrasonication 0.5～3h, make plant cell wall breaking, help the effective constituent stripping: with yellow ginger, the Ningpo Yam Rhizome that ultrasonication is crossed, put in the crack tank, add concentrated hydrochloric acid or sulfuric acid, concentration is at 1mol～5mol, at 0.5Kg～5Kg/cm
2Pressure under, cracking 1～6 hour; Lysate adopts liquefied ammonia, aqua ammonia, calcium hydroxide, lime carbonate, calcium oxide, salt of wormwood, sodium bicarbonate, yellow soda ash, sodium hydroxide, potassium hydroxide or bicarbonate of ammonia that lysate is carried out neutralization reaction to neutral before or after being diverted to still kettle, distill, discharging when the cleavage mixture water content reaches 15～40%, dry, moisture controlled is 3～8%; Cleavage mixture after the oven dry is passed through CO
2The supercritical extraction diosgenin, the waste residue after the extraction is used to produce biological organic fertilizer.
The add-on of above-mentioned neutralization reaction is calculated according to the material that participates in reaction, and this technology has been saved the discharging that is washed to neutral process and waste liquid in the traditional technology.
Above-mentioned cleavage mixture is diverted in the still kettle, by the mixing liquid that condenser distills, handles with ultrasonic wave or ozone, and the liquid after the processing can be done cooling water circulation use.
Above-mentioned cleavage mixture is diverted in the still kettle, not by condenser, by improving the temperature of still kettle, also can make water content reach discharging in 15～40% o'clock, dries after the discharging.
The preparation technology that waste residue behind the extraction diosgenin is produced biological organic fertilizer is: waste residue and chicken manure, cottonseed cake or soya-bean cake behind the extraction diosgenin, mixed according to waste residue 15～35%, chicken manure 35～48%, cottonseed cake or soya-bean cake 20～30%, calcium superphosphate 5% is even, add microbial strains 2% fermentation about 10 days, mix, the cold wind granulation promptly can be made into biological organic fertilizer.
Microbial strains of the present invention is thermophilic sporotrichum (SporotrichumThermophile), and culture presevation is in CGMCC.
Adopt diosgenin extraction process raw material provided by the invention without fermentative processing, technological process can shorten more than 48 hours, had improved the fusing point and the yield of diosgenin; Waste liquid behind the employing strong acid catalytic pyrolysis does not discharge, and has eliminated environmental pollution, and the water-soluble saponin of discharging in the traditional technology is also reclaimed, and has significantly reduced production cost; Waste residue behind the extraction diosgenin can fully utilize, and produces the green bio fertilizer, helps improving Soil structure, and elimination is hardened, and increases fertilizer efficiency.
(4) embodiment
Embodiment 1: get 1000 kilograms of raw material cadmium yellow ginger, washing, pulverizing are placed in the container, add clear water according to 1: 2 and stir: adopt ultrasonication 1h, make plant cell wall breaking; The yellow ginger of handling is put in the crack tank, added 300 kilograms of hydrochloric acid, at 2Kg/cm
2Pressure under, cracking 2 hours; Add 396 kilograms in sodium hydroxide, make lysate carry out neutralization reaction to neutral; Cleavage mixture is diverted in the still kettle, distill, the mixing liquid that comes out by condenser condenses enters retrieving arrangement, discharging when the cleavage mixture water content reaches 30%, dry, moisture controlled is 3～8%: the cleavage mixture after the oven dry is passed through CO
2The supercritical extraction diosgenin can get 10 kilograms of diosgenins, and the saponin yield is 4%.
Embodiment 2: get 1000 kilograms of the bright Ningpo Yam Rhizomes of raw material, washing, pulverizing are placed in the container, and added clear water according to 1: 3 and stir: adopt ultrasonication 1.5h, make plant cell wall breaking: the Ningpo Yam Rhizome that will handle is put in the crack tank, add 100 kilograms in sulfuric acid, at 3Kg/cm
2Pressure under, cracking 4 hours; Cleavage mixture is diverted in the still kettle, adds 110 kilograms in yellow soda ash, make lysate carry out neutralization reaction to neutral, not by condenser,, make the cleavage mixture water content reach discharging in 25% o'clock by improving the temperature of still kettle, dry, moisture controlled is 3～8%; Cleavage mixture after the oven dry is passed through CO
2The supercritical extraction diosgenin can get 8 kilograms of diosgenins, and the saponin yield is 3.7%.
Cell wall breaking technology among above-mentioned two embodiment also can adopt fermentation and bulking process to handle.
Embodiment 3:
The waste residue that 1000 kilograms of cadmium yellow ginger are extracted behind the diosgenin is a 120 kg, produce biological organic fertilizer according to preparation technology provided by the invention: waste residue and chicken manure, cottonseed cake or soya-bean cake behind the extraction diosgenin, mixed according to waste residue 30%, chicken manure 43%, cottonseed cake or soya-bean cake 20%, calcium superphosphate 5% is even, add microbial strains thermophilic sporotrichum 2% fermentation about 10 days, mix, the cold wind granulation can produce 400 kilograms of biological organic fertilizers.
Claims (6)
1, a kind of method by yellow ginger, Ningpo Yam Rhizome extraction diosgenin is characterized in that yellow ginger, Ningpo Yam Rhizome are placed in the container through washing, pulverizing, adds clear water according to 1: 0.5～3 and stirs; Adopt ultrasonication 0.5～3h, make plant cell wall breaking; With yellow ginger, the Ningpo Yam Rhizome that ultrasonication is crossed, put in the crack tank, add concentrated hydrochloric acid or sulfuric acid, concentration is at 1mol～5mol, at 0.5Kg～5Kg/cm
2Pressure under, cracking 1～6 hour; Lysate adopts liquefied ammonia, aqua ammonia, calcium hydroxide, lime carbonate, calcium oxide, salt of wormwood, sodium bicarbonate, yellow soda ash, sodium hydroxide, potassium hydroxide or bicarbonate of ammonia that lysate is carried out neutralization reaction to neutral before or after being diverted to still kettle, distill, discharging when the cleavage mixture water content reaches 15～40%, dry, moisture controlled is 3～8%; Cleavage mixture after the oven dry is passed through CO
2The supercritical extraction diosgenin, the waste residue after the extraction is used to produce biological organic fertilizer.
2, the method for extracting diosgenin by yellow ginger, Ningpo Yam Rhizome according to claim 1, it is characterized in that above-mentioned cleavage mixture is diverted in the still kettle, by the mixing liquid that condenser distills, to handle with ultrasonic wave or ozone, the liquid after the processing can be done cooling water circulation use.
3, the method for extracting diosgenin by yellow ginger, Ningpo Yam Rhizome according to claim 1, it is characterized in that above-mentioned cleavage mixture is diverted in the still kettle, not by condenser, by improving the temperature of still kettle, also can make water content reach discharging in 15～40% o'clock, dry after the discharging.
4, the method by yellow ginger, Ningpo Yam Rhizome extraction diosgenin according to claim 1 is characterized in that yellow ginger, Ningpo Yam Rhizome after washing, pulverizing, and plant cell wall breaking also can adopt bulking process, zymotechnique to handle.
5, a kind of waste residue that extracts behind diosgenin preparation technology of producing biological organic fertilizer, it is characterized in that extracting waste residue and chicken manure, cottonseed cake or soya-bean cake behind the diosgenin, mixed according to waste residue 15～35%, chicken manure 35～48%, cottonseed cake or soya-bean cake 20～30%, calcium superphosphate 5% is even, add microbial strains 2% fermentation about 10 days, mix, the cold wind granulation promptly can be made into biological organic fertilizer.
6, the waste residue behind the extraction diosgenin according to claim 1 is produced the preparation technology of biological organic fertilizer, it is characterized in that the microbial strains of being adopted is a thermophilic sporotrichum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031279449A CN1233653C (en) | 2003-04-25 | 2003-04-25 | Process for extracting dioscin from yellow ginger and Rhizoma Dioscoreae Nipponicae and producing organic fertilizer using residue of same |
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| CNB031279449A CN1233653C (en) | 2003-04-25 | 2003-04-25 | Process for extracting dioscin from yellow ginger and Rhizoma Dioscoreae Nipponicae and producing organic fertilizer using residue of same |
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| CN1450082A true CN1450082A (en) | 2003-10-22 |
| CN1233653C CN1233653C (en) | 2005-12-28 |
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| CNB031279449A Expired - Fee Related CN1233653C (en) | 2003-04-25 | 2003-04-25 | Process for extracting dioscin from yellow ginger and Rhizoma Dioscoreae Nipponicae and producing organic fertilizer using residue of same |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304414C (en) * | 2005-05-10 | 2007-03-14 | 浙江工业大学 | Process for extracting yam saponin from yellow ginger hydrolysate |
| CN101134625B (en) * | 2006-03-03 | 2011-06-08 | 倪文斌 | Method for wastewater comprehensive utilization of saponin production |
| CN102161691A (en) * | 2011-04-11 | 2011-08-24 | 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 |
| CN102659910A (en) * | 2012-05-08 | 2012-09-12 | 四川省荣桓科技有限责任公司 | High-efficiency extraction and cleaning production process for diosgenin |
| CN104355762A (en) * | 2014-12-01 | 2015-02-18 | 吴晖 | Lettuce nutrient |
| CN104387199A (en) * | 2014-12-01 | 2015-03-04 | 吴晖 | Method for preparing lettuce nutrient |
| CN104945128A (en) * | 2015-06-18 | 2015-09-30 | 广西大学 | Synsepalum dulcificum special fertilizer and preparation method thereof |
| CN106008658A (en) * | 2016-05-30 | 2016-10-12 | 铜陵东晟生态农业科技有限公司 | Method for purifying diosgenin in Discorea nipponica Makino |
| CN108623373A (en) * | 2017-10-28 | 2018-10-09 | 陕西永春生态科技有限公司 | A method of preparing fertilizer by raw material of yellow ginger |
| CN108623372A (en) * | 2017-10-28 | 2018-10-09 | 陕西永春生态科技有限公司 | A method of preparing microbial manure using yellow ginger hydrolyzate and waste residue |
| CN108623374A (en) * | 2017-10-28 | 2018-10-09 | 陕西永春生态科技有限公司 | A method of preparing microbial manure by raw material of yellow ginger |
| CN108840900A (en) * | 2018-07-25 | 2018-11-20 | 江苏黄河药业股份有限公司 | A method of extracting zingiberensis newsaponin |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659909B (en) * | 2012-04-26 | 2014-06-18 | 湘西自治州奥瑞克医药化工有限责任公司 | Method for separating dioscin hydrolysate |
-
2003
- 2003-04-25 CN CNB031279449A patent/CN1233653C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304414C (en) * | 2005-05-10 | 2007-03-14 | 浙江工业大学 | Process for extracting yam saponin from yellow ginger hydrolysate |
| CN101134625B (en) * | 2006-03-03 | 2011-06-08 | 倪文斌 | Method for wastewater comprehensive utilization of saponin production |
| CN102161691A (en) * | 2011-04-11 | 2011-08-24 | 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 |
| 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 |
| CN102659910A (en) * | 2012-05-08 | 2012-09-12 | 四川省荣桓科技有限责任公司 | High-efficiency extraction and cleaning production process for diosgenin |
| CN104355762A (en) * | 2014-12-01 | 2015-02-18 | 吴晖 | Lettuce nutrient |
| CN104387199A (en) * | 2014-12-01 | 2015-03-04 | 吴晖 | Method for preparing lettuce nutrient |
| CN104945128A (en) * | 2015-06-18 | 2015-09-30 | 广西大学 | Synsepalum dulcificum special fertilizer and preparation method thereof |
| CN106008658A (en) * | 2016-05-30 | 2016-10-12 | 铜陵东晟生态农业科技有限公司 | Method for purifying diosgenin in Discorea nipponica Makino |
| CN108623373A (en) * | 2017-10-28 | 2018-10-09 | 陕西永春生态科技有限公司 | A method of preparing fertilizer by raw material of yellow ginger |
| CN108623372A (en) * | 2017-10-28 | 2018-10-09 | 陕西永春生态科技有限公司 | A method of preparing microbial manure using yellow ginger hydrolyzate and waste residue |
| CN108623374A (en) * | 2017-10-28 | 2018-10-09 | 陕西永春生态科技有限公司 | A method of preparing microbial manure by raw material of yellow ginger |
| CN108840900A (en) * | 2018-07-25 | 2018-11-20 | 江苏黄河药业股份有限公司 | A method of extracting zingiberensis newsaponin |
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| CN1233653C (en) | 2005-12-28 |
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