CN1255549C - Method for extracting diosgenin for joint production of starch suger by prehy drolysis of yellow ginger by multienzyme process - Google Patents
Method for extracting diosgenin for joint production of starch suger by prehy drolysis of yellow ginger by multienzyme process Download PDFInfo
- Publication number
- CN1255549C CN1255549C CN 200310111250 CN200310111250A CN1255549C CN 1255549 C CN1255549 C CN 1255549C CN 200310111250 CN200310111250 CN 200310111250 CN 200310111250 A CN200310111250 A CN 200310111250A CN 1255549 C CN1255549 C CN 1255549C
- Authority
- CN
- China
- Prior art keywords
- saponin
- yellow ginger
- saccharification
- concentration
- slurry
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Saccharide Compounds (AREA)
Abstract
The present invention provides a saponin extraction method for joint production of starch sugar by pre-hydrolyzing yellow ginger by a multienzyme method. The method comprises the steps: firstly, washing yellow ginger, and wearing to slurry; then, adding alpha amylase and liquefying; adding amylase and saccharifying; then, warming and inactivating; subsequently, obtaining filter cakes and starch sugar by saccharifying material through centrifugation; separating the sugar solution by using ultrafiltration membrane with catch molecular weight of 1000 to 10000 daltons pore diameters or micro filtration membrane of 100 to 200 nm to obtain a starch sugar solution; mixing filter residues into the centrifuged filter cakes to obtain sugar residues; hydrolyzing the sugar residues by adding hydrochloric acid or sulfuric acid, and obtaining a saponin product by hydrolysate through filtration, washing, drying and solvent extraction. The present invention adopts the multienzyme method for producing sugar by amylolysis and a membrane separation technique before acid hydrolysis, and has the advantages of acid hydrolysis material total reduction, more sufficient saponin hydrolyzation, high yield of the saponin, small waste water quantity and low chemical oxygen demand. The method can also be used for extracting diosgenin of starch sugar by joint production with dioscorea nipponica.
Description
Technical field
The present invention relates to utilize saponin (sapogenin) extracting method of Rhizome of Peltate Yam-yellow ginger through multi-enzyme method prehydrolysis coproduction Dian Fentang.
Background technology
The method of domestic production saponin is to take yellow ginger direct acidolysis after pulverizing, fermenting in advance to produce the technology of saponin mostly at present, and mainly there is following problem in this method:
1, the starch component of yellow ginger does not obtain utilizing.Starch-containing in the cadmium yellow ginger 〉=18%, dried yellow ginger is starch-containing 〉=and 45%, from waste water, discharge after the acidolysis, cause the waste of resource.
2, waste water complicated component, quantity discharged is big, and is seriously polluted.Saponin waste discharge 450-500M per ton
3, COD value 30000～110000mg/L wherein; PH value: 0.2-1.5.
3, saponin yield is lower, and raw material consumption is big, and cadmium yellow ginger saponin yield is 0.6-0.8%, and dried turmeric saponin yield is 1.8-2.0%.
Recently the someone proposes to separate earlier Mierocrystalline cellulose and the starch in the yellow ginger, and starch is produced alcohol, and the method for saponin is produced in the vinasse acidolysis.There is following shortcoming in this method: in order to guarantee saponin yield, yellow ginger is carried out repeatedly defibrination and washing when 1, the separated fiber element is with starch, cause starch concentration low; 2, because yellow ginger institute soluble-containing starch is many, granularity is little, the separation difficulty of starch and water, the ethanol concn of being produced is low, and the energy consumption of defibrination and alcohol distillation is big; 3, from mash, separate when containing the schlempe of saponin,, filter very difficult because zymic exists; 4.Complex process, investment is big, and the waste water generation is big.
Summary of the invention
The objective of the invention is to overcome the shortcoming of aforesaid method, a kind of saponin (sapogenin) extracting method of multi-enzyme method prehydrolysis yellow ginger coproduction Dian Fentang is provided, particularly adopt saponin and sapogenin in micro-filtration (MF) or ultrafiltration (UF) the separation multi-enzyme method saccharification liquid., this method consumes low, the yield height, and technology is simple, and wastewater flow rate is little,
The saponin extracting method of a kind of multi-enzyme method prehydrolysis yellow ginger coproduction Dian Fentang of the present invention the steps include:
1, washing is pulverized: yellow ginger removes silt particle through washing, and the pulverising mill form slurry generally is ground into granularity＜2mm, wears into granularity＜1mm slurry, solid content 15-30% (quality) in the slurry;
2, liquefaction: add αDian Fenmei (E.C.3.2.1.1 under with) and liquefy in the slurry that step 1 obtains, reaction conditions is that temperature 80-100 ℃, pH value 6.0-7.0, enzyme concentration are that concentration is the αDian Fenmei liquid 0.5-1.5L/M of 18000U/L
3Slurry, liquefying time 2-4 hour;
3, saccharification: add saccharifying enzyme (same under the E.C.3.2.1.3) saccharification in the liquefier that step 2 obtains, the saccharification condition is temperature 50-60 ℃, and pH value 4.0-5.0, enzyme concentration are that concentration is the saccharifying enzyme liquid 0.5-1.5L/M of 18000U/L
3Liquefier saccharification time 6-10 hour, is warmed up to 90 ℃ of deactivations then:
4, the slag sugar is from saccharification material that step 3 is obtained, earlier through centrifugation, get filter cake and Dian Fentang solution, in the Dian Fentang solution except that starch-containing sugared 5-10%, also contain small-particle saponin and solubility saponin, with Dian Fentang solution molecular weight cut-off is that ultrafiltration (UF) film in 1000-10000daltons aperture or micro-filtration (MF) membrane sepn of 100-200nm obtain clean Dian Fentang solution, and filter residue is sneaked into and got sugared slag in the centrifugal filter cake;
5, the sugared pulp water that step 4 is obtained is separated: the concentration of pressing 0.6-3N in the sugared slag adds hydrochloric acid or sulfuric acid, under the condition of 0.05-0.12MPa (gauge pressure) and 100-115 ℃ hydrolysis 2-6 hour, hydrolyzate after filtration, washing, dry, industrial naptha or sherwood oil extracting get the saponin product.
Used αDian Fenmei is a warm amylase among commercially available α alpha-amylase or the α.Used saccharifying enzyme is commercially available saccharifying enzyme.Used microfiltration membrane is the zirconium oxide film of aperture 100nm or is the pellumina of aperture 200nm.Used ultrafiltration (UF) film is a tubular fibre UF film.
Because the present invention before acidolysis, has adopted multi-enzyme method starch hydrolysis sugar refining and membrane separation technique, has reduced acidolysis thing total amount, the hydrolysis of saponin is more abundant, and saponin yield obtains bigger raising, and the chemical oxygen demand of hydrolyzed waste water has decline by a relatively large margin.The present invention also can be used for the diosgenin extraction of Dioscorea nipponica Mak. Ningpo Yam Rhizome through multi-enzyme method prehydrolysis coproduction Dian Fentang.
Embodiment
Below with embodiment the present invention is elaborated:
Embodiment 1
Cadmium yellow ginger 1000g was soaked in water under the normal temperature 6 hours, after it is cleaned, pulverized with Universalpulverizer, obtained the slurry of the about 1mm of particle diameter, added water in cadmium yellow ginger at 1: 2.5 with the ratio of water and mixed; Place the 5000ml beaker to be warmed up to 90-95 ℃ rapidly in slurry, add the commercially available α alpha-amylase of 2.0ml (enzyme liquid concentration 18000U/L down with), under agitation in 90-95 ℃ of enzymolysis 2.5 hours; When treating that temperature drops to 55 ℃, add the commercially available saccharifying enzyme of 3.5ml (enzyme liquid concentration 18000U/L down with), under 55-60 ℃ and pH4-5 reaction 8 hours the saccharification material; The centrifugation of saccharification material gets filter cake and sugar soln, and saccharification liquid is used tubular fibre UF membrane filtration down at 40-50 ℃; Centrifugal filter cake and membrane filtration slag are merged, add the hydrochloric acid soln of concentration 30% (weight), concentration of hydrochloric acid is 2.0N in the water conditioned reaction thing, and in 100-105 ℃, normal pressure refluxes down and got hydrolyzate in 5 hours; Hydrolyzate gets saponin 12.2g through No. 120 industrial naptha extractings, 196 ℃ of its fusing points through vacuum filtration, washing, neutralization, the dry dried hydrolyzate 72g that gets moisture 4.5% (weight).The COD value of hydrolysis filtrate is 18200mg/L, and the COD value of mixing washing lotion is 8800mg/L.
Embodiment 2
Be soaked in water 10 hours under dried fresh ginger slice 400g (moisture content 10%) normal temperature, it cleaned, pulverize, obtain the powder of the about 4mm of particle diameter with Universalpulverizer, with powder in the yellow ginger and the ratio of water be mix at 1: 6.5, defibrination, must particle diameter 0.5-1mm slurry; Place the 5000ml beaker to be warmed up to 85 ℃ rapidly in slurry, add warm amylase among the commercially available α of 3ml (enzyme liquid concentration 18000U/L down with), under agitation in 80-90 ℃ of enzymolysis 2 hours; When treating that temperature drops to 55 ℃, add the commercially available saccharifying enzyme of 4.5ml, under 55-60 ℃ and pH4-5 reaction 10 hours saccharification liquid; The centrifugation of saccharification liquid, its filtrate is down the zirconium oxide film filtration of 100nm with the aperture at 40-50 ℃; Merge centrifugal filter cake and membrane filtration slag, add the hydrochloric acid soln of concentration 30% (weight), concentration of hydrochloric acid is 1.5N in the water conditioned reaction thing, and under 100-105 ℃, normal pressure refluxes down and got hydrolyzate in 6 hours; Hydrolyzate gets saponin 14.2g through No. 120 industrial naptha extractings, 194.5 ℃ of its fusing points through vacuum filtration, washing, neutralization, the dry dried hydrolyzate 69.5g that gets moisture 3.8% (weight).The COD value of hydrolysis filtrate is 17600mg/L, and the COD value of mixing washing lotion is 6500mg/L.
Embodiment 3
Cadmium yellow ginger 1000g was soaked in water under the normal temperature 8 hours, and it is cleaned, and pulverized with Universalpulverizer, obtained the powder of particle diameter 2-3mm, its powder in yellow ginger and the ratio of water be mix at 1: 2, defibrination, must particle diameter 0.5-1mm slurry; Place the 5000ml beaker to be warmed up to 95 ℃ rapidly in slurry, add the commercially available α alpha-amylase of 4ml, under agitation in 95-100 ℃ of enzymolysis 3 hours; When treating that temperature drops to 60 ℃, add the commercially available saccharifying enzyme of 2.0ml, under 55-60 ℃ and pH4-5 reaction 6 hours saccharification liquid; The centrifugation of saccharification liquid, its filtrate is down the pellumina filtration of 200nm with the aperture at 40-50 ℃; Merge centrifugal filter cake and membrane filtration slag, add water 500ml filter wash slag, add the hydrochloric acid soln of concentration 30% (weight), concentration of hydrochloric acid is 0.8N in the water conditioned reaction thing, must hydrolyzate in 105-110 ℃ and 0.10MPa (gauge pressure) pressurized hydrolysis 2.5 hours; Hydrolyzate is through vacuum filtration, washing, neutralization, the dry dried hydrolyzate 75g that gets moisture 4.5% (weight), and dried hydrolyzate gets saponin 13.5g, 195 ℃ of its fusing points with the sherwood oil extracting saponin of 80-90.The COD value of hydrolysis filtrate is 12500mg/L, and the COD value of washing lotion is 4500mg/L.
Embodiment 4
Dried fresh ginger slice 400g (moisture content 8%) was soaked in water under the normal temperature 12 hours, and it is cleaned, pulverize with Universalpulverizer, obtain the powder of the about 2mm of particle diameter, its powder in the yellow ginger and the ratio of the affination pulp water of embodiment 3 be mix at 1: 6.5, defibrination, the about 1mm slurry of particle diameter; Place the 5000ml beaker to be warmed up to 95 ℃ rapidly in its slurry, add the commercially available α alpha-amylase of 3.5ml, under agitation in 95-100 ℃ of enzymolysis 2.5 hours; When treating that temperature drops to 60 ℃, add the commercially available saccharifying enzyme of 3.0ml, under 55-60 ℃ and pH4-5 reaction 10 hours saccharification liquid; Saccharification liquid filters with 30 eye mesh screens, uses the 600ml water washing respectively 4 times, and sieve liquid down is down the zirconium oxide film filtration of 100nm with the aperture at 40-50 ℃; Add the sulfuric acid of concentration 98% (weight) in the trapped substance, sulfuric acid concentration is 0.6N in the conditioned reaction thing, and hydrolysis 2.5 hours must hydrolyzate under the pressure of 110-115 ℃ and 0.12MPa (gauge pressure); Hydrolyzate is through vacuum filtration, washing, neutralization, the dry dried hydrolyzate 44g that gets moisture 5% (weight), and dried hydrolyzate gets saponin 14.8g through No. 120 industrial naptha extractings, 196 ℃ of its fusing points.The COD value of hydrolysis filtrate is 14500mg/L, and the COD value of washing lotion is 6600mg/L.
Claims (3)
1. the saponin extracting method of a multi-enzyme method prehydrolysis yellow ginger coproduction Dian Fentang is characterized in that step is:
1) the yellow ginger washing is pulverized: yellow ginger removes silt particle through washing, pulverizes, and wears into slurry, solid content 15-30% (quality) in the slurry;
2) in the slurry that step 1 obtains, add αDian Fenmei (E.C.3.2.1.1) liquefaction, get liquefier;
3) in the liquefier that step 2 obtains, add saccharifying enzyme (E.C.3.2.1.3) saccharification, obtain the saccharification material;
4) the saccharification material that step 3 is obtained, earlier through centrifugation, get filter cake and Dian Fentang solution, the ultra-filtration membrane that its Dian Fentang solution molecular weight cut-off is the 1000-10000daltons aperture or the microfiltration membrane of 100-200nm are separated and are obtained clean Dian Fentang solution, hold back filter residue sneak in the centrifugal filter cake sugared slag;
5) the sugared pulp water that step 4 is obtained is separated: the concentration of pressing 0.6-3N in the sugared slag adds hydrochloric acid or sulfuric acid, under the condition of 0.05-0.12MPa (gauge pressure) and 100-115 ℃ hydrolysis 2-6 hour, hydrolyzate after filtration, washing, dry, industrial naptha or sherwood oil extracting get the saponin product;
Wherein said αDian Fenmei is a warm amylase among α alpha-amylase or the α; Described liquefaction reaction condition is that temperature 80-100 ℃, pH value 6.0-7.0, enzyme concentration are that concentration is the αDian Fenmei liquid 0.5-1.5L/M of 18000U/L
3Slurry, liquefying time 2-4 hour; Described saccharification condition is temperature 50-60 ℃, and pH value 4.0-5.0, enzyme concentration are that concentration is the saccharifying enzyme liquid 0.5-1.5L/M of 18000U/L
3Liquefier saccharification time 6-10 hour, is warmed up to the saccharification material that 90 ℃ of deactivations obtain then.
2, the method for claim 1 is characterized in that described microfiltration membrane is the zirconium oxide film of aperture 100nm or the pellumina of aperture 200nm.
3, the method for claim 1 is characterized in that described ultra-filtration membrane is a hollow fiber ultrafiltration membrane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310111250 CN1255549C (en) | 2003-10-20 | 2003-10-20 | Method for extracting diosgenin for joint production of starch suger by prehy drolysis of yellow ginger by multienzyme process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310111250 CN1255549C (en) | 2003-10-20 | 2003-10-20 | Method for extracting diosgenin for joint production of starch suger by prehy drolysis of yellow ginger by multienzyme process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1528913A CN1528913A (en) | 2004-09-15 |
| CN1255549C true CN1255549C (en) | 2006-05-10 |
Family
ID=34304763
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310111250 Expired - Fee Related CN1255549C (en) | 2003-10-20 | 2003-10-20 | Method for extracting diosgenin for joint production of starch suger by prehy drolysis of yellow ginger by multienzyme process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1255549C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304594C (en) * | 2005-05-19 | 2007-03-14 | 陕西科技大学 | Biological process for extracting yellow ginger saponin |
| CN100364604C (en) * | 2005-05-23 | 2008-01-30 | 中国地质大学（武汉） | Method for producing health caring syrup using enzymolysis sugar solution as byproduct during the production of saponin from turmeric |
| CN1332691C (en) * | 2005-05-23 | 2007-08-22 | 中国地质大学（武汉） | Medication for treating cardiovascular diseases prepared from byproduct of solution from 'Huangjiang' in producing saponin |
| CN102021218B (en) * | 2009-09-18 | 2013-04-10 | 张晖 | Dioscin degradation catalyst |
| CN102485900A (en) * | 2010-12-06 | 2012-06-06 | 竹溪创艺皂素有限公司 | Method for separating dioscorea zingiberensis enzymolysis sugar solution by using metal membrane |
| CN102106875A (en) * | 2010-12-06 | 2011-06-29 | 浙江工业大学 | Method for extracting water-soluble alpha-glucosidase inhibitor |
| CN108192779A (en) * | 2017-12-30 | 2018-06-22 | 高产明 | A kind of skin care scented soap and preparation method thereof |
-
2003
- 2003-10-20 CN CN 200310111250 patent/CN1255549C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1528913A (en) | 2004-09-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101077182B (en) | Technology for preparing functional dietary fiber through myrica ruba marc enzymolysis | |
| US20140053829A1 (en) | Method of and system for producing oil and valuable byproducts from grains in dry milling systems with a back-end dewater milling unit | |
| CN108383886B (en) | Method for extracting hesperidin from immature bitter orange by continuous countercurrent method and hesperidin obtained by extraction | |
| CN101255453A (en) | Method for extracting purple sweet potato anthocyanin pigments by employing invoice process | |
| CN105418781A (en) | Ultrasonic extraction method of ganoderan | |
| CN102203297A (en) | Process for the production of alcohol | |
| CN1255549C (en) | Method for extracting diosgenin for joint production of starch suger by prehy drolysis of yellow ginger by multienzyme process | |
| CN103087143A (en) | Method for extracting tigogenin from squeezed juice of sisal residue | |
| CN104026706B (en) | A kind of preparation method of red bamboo liquid | |
| WO2009094418A2 (en) | Corn wet milling process | |
| CN109549038A (en) | The technique for comprehensively utilizing sweet potato multistage coproduction starch and juice being concentrated | |
| CN105907801A (en) | Method of continuously producing dietary fibers, alcohol and single-cell protein with potato residue | |
| CN1962686A (en) | Method for cleanly producing saponin by integrated utilization of yam | |
| CN103897074B (en) | A kind of method utilizing membrane process separation and purification curdlan | |
| CN106432529B (en) | A kind of preparation method of high-purity rice bran polysaccharide | |
| CN1834106B (en) | Fermenting free hydralysis process for extracting saporin from yellow ginger | |
| CN101333552B (en) | Process for producing yam saponin and co-producing glucose by acid-enzyme method prehydrolyzing turmeric | |
| CN102925516A (en) | Xylo-oligosaccharide preparation method | |
| CN102464700B (en) | Hydrolysis extraction process for yam diosgenin | |
| CN107252117A (en) | A kind of method that oligopeptide, polysaccharide and dietary fiber are produced by raw material of peanut meal | |
| CN101333551B (en) | Cleaning production process for extracting saponin from turmeric | |
| CN105087149A (en) | Comprehensive utilization method of silkworm chrysalis | |
| CN104041904B (en) | A kind of preparation method of red bamboo liquid | |
| CN1844162A (en) | Process for preparing high purity pectin by using apple pomace | |
| CN101885750B (en) | Method for circularly processing and utilizing rhizome in dioscorea |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20060510 Termination date: 20111020 |