CN1315873C - Solvent extraction production technology of pullulanose - Google Patents
Solvent extraction production technology of pullulanose Download PDFInfo
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- CN1315873C CN1315873C CNB200510042016XA CN200510042016A CN1315873C CN 1315873 C CN1315873 C CN 1315873C CN B200510042016X A CNB200510042016X A CN B200510042016XA CN 200510042016 A CN200510042016 A CN 200510042016A CN 1315873 C CN1315873 C CN 1315873C
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- organic solvent
- pullulanose
- pulullan
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- ethanol
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Abstract
The present invention relates to a solvent extraction producing technique of pullulanose, particularly to a producing technique of the pullulanose product. The present invention has the technical scheme that (1) pullulanose fermentation liquid is dehydrated by using organic solvents, such as alcohol, isopropyl alcohol, etc. as a dewatering agent, and simultaneously, the product is decolorized and desalted; (2) a layering overflow mode is used for the solid-liquid separation after the pullulanose is mixed with the organic solvents; (3) the organic solvents are used many times for extracting the product in a multi-dehydrating mode. The present invention adopts the organic solvent method to produce pullulanose products, and the extraction yield is larger than 90%. Moreover, the present invention has low cost, and additionally, the continuity and the automation are realized in the production processes of the present invention. Thus, the present invention provides the source of raw pullulanose materials for health foods.
Description
Technical field
The present invention relates to the suitability for industrialized production technology of chemical field pulullan, specifically adopt organic solvent method to extract the production technique of pulullan product.
Background technology
Pulullan is the higher Microbial exopolysaccharides of a kind of using value, and by α-1, the trisaccharide maltose repeating unit that the 4-glycosidic link connects is through α-1, the straight chain shape polysaccharide that the 6-glycosidic link is polymerized.But because the difference of bacterial strain uses therefor, the trisaccharide maltose unit in the polysaccharide chain once in a while also can be by the minute quantity maltotetrose, and maltose or glucosyl residue replace, and also occur branched structure under the individual cases.The molecular weight of pulullan is generally 5.0 * 10
4-5.0 * 10
6Between the daltons; Its molecular weight size is subjected to the influence of culture condition bigger.The control fermentation condition can be fixed its molecular weight in certain scope.As the organic solvent method that adopts existing other polysaccharide is when extracting, with there are the following problems, the one, owing to the not thorough mutual anchoring effect that causes of pulullan dehydration, as adopt pulullan centrifugal or that the filter type precipitation separation gets off, can cause the pulullan bonding to become one, can't carry out suitability for industrialized production; The 2nd, organic solvent is not applied mechanically during owing to dehydration, thereby the consumption of leaching process organic solvent is big, the production cost height.
Summary of the invention
The object of the present invention is to provide a kind of production technique that adopts organic solvent method to extract the pulullan product, adopt this operational path to produce pulullan, product yield height, cost is low, and production process has realized serialization and automatization.
Technical scheme of the present invention is: the solvent extraction production technology of this pulullan is characterized in that comprising the steps:
(1), as dewatering agent the pulullan fermented liquid is dewatered, and simultaneously to product decolouring and desalination with alcohol or Virahol class organic solvent;
(2), after the pulullan fermented liquid adds the heat extraction thalline, clear filtrate is pumped into the water knockout from basin, in jar, add 80%-95% ethanol v/v or 80%-99% Virahol v/v, stir, standing demix, opening surplus valve outflow lower concentration organic solvent is supernatant liquor;
(3), dewatering type extracts product to adopt the multipass organic solvent to apply mechanically several times, the supernatant liquor that water knockout overflows for the first time carries out the solvent distillation and reclaims, and in water knockout, add 80%-95% ethanol v/v or 80%-99% Virahol v/v once more, stir, standing demix, opening surplus valve outflow low concentration organic solvent is supernatant liquor; The organic solvent that these organic solvents add for the first time as the next batch fermented liquid.
For technique scheme of the present invention:
Described organic solvent can be small molecule alcohols such as ethanol, Virahol, utilize pulullan soluble in water and be insoluble to the characteristic of small molecule alcohol material, with organic solvent and pulullan fermentation liquid-phase mixing, thereby pulullan is precipitated in organic solvent.
The mode that the present invention adopts the layering overflow to carry out solid-liquid separation can be: mixing different heights installation series of valves gate discharge supernatant liquor on the tank skin, also can be to adopt siphon principle to draw supernatant liquor; The dehydrated organic solvent that in mixing tank, adds (small molecule alcohol) concentration: ethanol (80%-95%) (v/v), Virahol (80%-99%) is (v/v).
The method that employing multipass organic solvent of the present invention is applied mechanically the product of dewatering type extraction several times can be: the supernatant liquor that water knockout overflows for the first time (lower concentration organic solvent) carries out the solvent distillation and reclaims, and in water knockout, add once more ethanol (80%-95%) (v/v) or Virahol (80%-99%) (v/v), stir, standing demix is opened surplus valve and is flowed out low concentration organic solvent (supernatant liquor); The organic solvent that these organic solvents add for the first time as the next batch fermented liquid.
The present invention compared with prior art has following beneficial effect:
1, adopts layering overflow mode to carry out solid-liquid separation and can solve the mutual anchoring effect that pulullan does not thoroughly cause owing to dehydration, supernatant liquor is separated smoothly with the pulullan that precipitates, and can make the pulullan that has precipitated keep rarefaction, non-caked agglomerating, the smoothness of assurance abstraction process.
2, the method that adopts the multipass organic solvent to apply mechanically the product of dewatering type extraction several times can reduce the consumption of pulullan leaching process organic solvent greatly, saves production cost.
3, adopt this operational path to produce pulullan, extract yield is greater than 90%, and cost is low, and production process has realized serialization and automatization.
Description of drawings
Figure is a process flow diagram of the present invention
Embodiment
In conjunction with the accompanying drawings the processing method of invention is further specified below by example:
1. at 7m
3Adorn 1.5m in the water knockout
3Removed the clarified broth of thalline, to water knockout, slowly added 3m from circulation ethanol basin
3About 86% (v/v) ethanol, stir, standing demix is opened the surplus valve of dehydration tank skin successively from top to down, this part low-concentration ethanol is flowed into needs distillatory ethanol basin, stays the bottom settlings thing and dewaters once more.
2. to water knockout, slowly add 1.5m from tank deck
395% (v/v) ethanol, and open to stir simultaneously, after ethanol adds, stir standing demix, the surplus valve of the tank skin of unlatching dehydration from top to down successively, with this part lower concentration (about 86%) (v/v) ethanol flow into circulation ethanol basin, use to get batch fermentation liquid ready; Staying the bottom settlings thing dewaters once more.
3. to water knockout, slowly add 1.5m from tank deck
395% (v/v) ethanol, and open to stir simultaneously, after ethanol adds, stir, the product pump that mixes is gone into the sheet frame filter filters, filtrate partly enters circulation ethanol basin, uses to get batch fermentation liquid ready; The solid materials drying obtains the 90Kg sample.Extract yield is 96.5%.
4. after super-dry, usual method is pulverized, packing, gets product.
Claims (1)
1, the solvent extraction production technology of pulullan is characterized in that comprising the steps:
(1), the pulullan fermented liquid is dewatered as dewatering agent with alcohol or Virahol organic solvent, and decolouring and desalination simultaneously: after the pulullan fermented liquid adds the heat extraction thalline, clear filtrate is pumped into the water knockout from basin, in jar, add 80%-95% ethanol v/v or 80%-99% Virahol v/v, stir, standing demix, opening surplus valve outflow lower concentration organic solvent is supernatant liquor;
(2), dewatering type extracts to adopt the multipass organic solvent to apply mechanically several times: the supernatant liquor that water knockout overflows for the first time carries out the solvent distillation and reclaims, and in water knockout, add 80%-95% ethanol v/v or 80%-99% Virahol v/v once more, stir, standing demix, opening surplus valve outflow low concentration organic solvent is supernatant liquor; The organic solvent that these organic solvents add for the first time as the next batch fermented liquid gets product after solid materials drying, the pulverizing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510042016XA CN1315873C (en) | 2005-01-11 | 2005-01-11 | Solvent extraction production technology of pullulanose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510042016XA CN1315873C (en) | 2005-01-11 | 2005-01-11 | Solvent extraction production technology of pullulanose |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1651467A CN1651467A (en) | 2005-08-10 |
| CN1315873C true CN1315873C (en) | 2007-05-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200510042016XA Expired - Fee Related CN1315873C (en) | 2005-01-11 | 2005-01-11 | Solvent extraction production technology of pullulanose |
Country Status (1)
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| CN (1) | CN1315873C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10568839B2 (en) | 2011-01-11 | 2020-02-25 | Capsugel Belgium Nv | Hard capsules |
| US11878079B2 (en) | 2017-04-14 | 2024-01-23 | Capsugel Belgium Nv | Pullulan capsules |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100465191C (en) * | 2006-11-03 | 2009-03-04 | 天津市工业微生物研究所 | Drying method of bearing blue polysaccharide |
| CN103570842A (en) * | 2013-11-07 | 2014-02-12 | 镇江东方生物工程设备技术有限责任公司 | Extracting method of pullulan |
| CN103626885A (en) * | 2013-11-14 | 2014-03-12 | 江南大学 | Clean production method of Pulullan |
| BR112019021396A2 (en) | 2017-04-14 | 2020-04-28 | Capsugel Belgium Nv | pullulan manufacturing process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05331202A (en) * | 1991-10-16 | 1993-12-14 | Shinetsu Bio Inc | High-molecular pullulan and its production |
| CN1216781A (en) * | 1997-11-05 | 1999-05-19 | 中国科学院微生物研究所 | Method for producing pullulan from fermentation liquor |
-
2005
- 2005-01-11 CN CNB200510042016XA patent/CN1315873C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05331202A (en) * | 1991-10-16 | 1993-12-14 | Shinetsu Bio Inc | High-molecular pullulan and its production |
| EP0812919A1 (en) * | 1991-10-16 | 1997-12-17 | SHIN-ETSU BIO, Inc. | High molecular weight pullulan and method for its production |
| CN1216781A (en) * | 1997-11-05 | 1999-05-19 | 中国科学院微生物研究所 | Method for producing pullulan from fermentation liquor |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10568839B2 (en) | 2011-01-11 | 2020-02-25 | Capsugel Belgium Nv | Hard capsules |
| US11878079B2 (en) | 2017-04-14 | 2024-01-23 | Capsugel Belgium Nv | Pullulan capsules |
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| Publication number | Publication date |
|---|---|
| CN1651467A (en) | 2005-08-10 |
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| 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 | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Tonghua Bio Technology Co., Ltd. Assignor: Su Li Contract record no.: 2011370000241 Denomination of invention: Solvent extraction production technology of pullulanose Granted publication date: 20070516 License type: Exclusive License Open date: 20050810 Record date: 20110603 |
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| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070516 Termination date: 20140111 |