CN1242416A - Method for obtg. Wheat-germ oil using supercritical extraction combined with rectification - Google Patents
Method for obtg. Wheat-germ oil using supercritical extraction combined with rectification Download PDFInfo
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- CN1242416A CN1242416A CN 98111424 CN98111424A CN1242416A CN 1242416 A CN1242416 A CN 1242416A CN 98111424 CN98111424 CN 98111424 CN 98111424 A CN98111424 A CN 98111424A CN 1242416 A CN1242416 A CN 1242416A
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- rectifying column
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Abstract
The present invention using supercritical CO2 as solvent to extract germ oil from wheat germ is characterized by that the supercritical fluid in which the germ oil is dissolved flows out from extractor, and enters into a rectification column, then passed through said rectification column, so that the germ oil components can be accurately separated according to the solubility so as to implement concentration of object components of vitamin E, etc..
Description
The present invention relates to the vegetables oil field of chemical aspect, mainly be applicable to the concentrating and separating of vegetables oil active principle.It is that a kind of supercritical fluid extraction and rectifying are combined separated the method for wheatgerm oil.
Wheatgerm is the byproduct in the wheat flour milling process, accounts for 2～3% of wheat.Contain about 10% the grease of having an appointment in the plumule.Wheatgerm oil contains abundant biologically active substance, comprises 50～60% linolic acid, the vitamin-E of 200～400mg/100g and the 28 carbon alcohol about 100ppm.The process for purification of wheatgerm oil and the separation of biologically active substance are the keys that the good quality wheat germ oil is produced.
Supercritical liquid extraction technique is a high-new isolation technique.In recent years there are many use supercritical liquid extraction techniques that wheatgerm oil is extracted and the purified bibliographical information.For example, the mouth of a valley grade just of Japan in 1984 has been reported the wheatgerm oil supercritical CO
2The research of (40 ℃, 20MPa) extraction has been done test to the percentage extraction of germ oil under the different condition, and the physical and chemical index of this method and organic solvent method gained wheatgerm oil has been compared.Further tested in 1985, they studies show that, adopt the grease color of this method gained light, phospholipids content seldom.The clear 60-58498 of Japanese Patent had introduced and has used supercritical CO in 1985
2(30～60 ℃, 70～300kg/cm
3) method of extraction wheatgerm oil, propose to use a separating still that the wheatgerm oil that extracts is separated, to collect successively by the priority that extracts, carbonic acid gas does not recycle.The shortcoming of this method is that the grease of gained also needs further processing, and carbonic acid gas does not reclaim, this technology apply difficulty.Chinese patent CN1066874A in 1992 have reported the method for a kind of overcritical (or liquid) carbon dioxide abstraction and refined wheat germ oil.This method is by using two (or many) separating stills, substep reduces pressure and changes separation temperature, germ oil can be separated out from carbonic acid gas by its character substep, can make grease obtainedly on purity, to improve, but not relate to the further isolating problem of physiologically active substance in the wheatgerm oil (as vitamin-E).Liu Chongyi in 1994 etc. have reported the research of supercritical carbon dioxide extraction wheatgerm oil, and the solubleness of wheatgerm oil is tested, and it adopts single-stage separation processes method, the spissated problem of not mentioned physiologically active substance.
The objective of the invention is supercritical fluid extraction and rectifying combined makes the biologically active substance in the wheatgerm oil be separated by the size of its solubleness, and target components (for example vitamin-E) is concentrated.
The object of the present invention is achieved like this: its principle is to use supercritical CO
2(pressure is greater than 70kg/cm
2, temperature is greater than 31 ℃) and extraction during wheatgerm oil from wheatgerm, utilize the solubleness of some effective constituents of wheatgerm oil in rectifying column rising gradually and descend and feature that the decline degree is different makes V with temperature under the pressure of 7～35MPa
EConcentrated etc. target components.Its implementation is: the supercritical CO that is dissolved with wheatgerm oil
2After extraction kettle flows out, through a rectifying column.Rectifying column along short transverse from top to bottom temperature rise gradually, bottom temp is not less than 15 ℃, head temperature is not higher than 95 ℃.Along with the rising of temperature, the component that solubleness is little in the wheatgerm oil can be eliminated formation gradually and be refluxed in rectifying column.
The present invention makes the supercritical CO that is dissolved with wheatgerm oil
2Enter rectifying column with following dual mode: I, enter rectifying column from the bottom of rectifying column; II, enter rectifying column from the middle part of rectifying column.When the bottom enters, enter a separating still again from the effusive fluid in rectifying column top and separate, because the wash-out effect of rectifying column phegma causes bigger first being taken out of of component of solubleness such as vitamin-E, taken out of after all the other components.The pressure of rectifying column equals extracting pressure.When the middle part enters, the position that enters is positioned at about 1/5～1/3 place of rectifying column near the bottom, and the less component of solubleness is separated out to flow downward, and forms to reflux, and accumulates in the bottom of rectifying column, is emitted off and on; The component that solubleness such as vitamin-E are bigger continues to be retained in supercritical CO
2In, entering separating still in the lump thereupon, pressure falls and ends below the 7.5MPa in separating still, discharges all components.The pressure of rectifying column is selected between 8～30MPa.Two kinds of feeding manners have all been realized the concentrating and separating of vitamin-E.
Need to fill filler in the rectifying column.The specification and the loading level of the height of rectifying column, temperature distribution and the filler that uses can be according to target components V
EThe purity that needs is determined.
The present invention also is applicable to the extraction and the rectifying of liquid starting material.
Concrete grammar of the present invention is provided by following examples and accompanying drawing.
Fig. 1 is actually operating figure of the present invention.
Label among Fig. 1 is: 1CO
2Steel cylinder, 2 strainers, 3 liquefaction grooves, 4 boost equipment, 5 gas holders, 6 pressure regulator valves, 7 preheaters, 8 check valves, 9 extraction kettles, 10 reducing valve, 11 stopping valve, 12 rectifying columns, 13 reducing valve, 14 separating stills, 15 stopping valve, 16 stopping valve.
Method disclosed by the invention is described in detail as follows:
The extraction kettle 9 of at first wheat embryo being packed into is opened CO then2Steel cylinder 1, CO2Through filtering Device 2 enters liquefaction groove 3, enters subsequently the equipment of boosting 4, is forced into the pressure (greater than 70MPa) that needs After be admitted to gas tank 5, enter preheater 7 by gas tank 5 through pressure-regulating valve 6. CO2By pre-Heat enters extraction kettle 9 through check valve 8 insulations and extracts to operating temperature (greater than 31 ℃). Molten The CO that wheat-germ oil is arranged2To enter rectifying column 12 from extraction kettle 9 outflows. Enter from the bottom if select Rectifying column then needs shut off valve 10, opens valve 11. The fluid that flows out from the rectifying column top is through pressure-reducing valve 13 decompressions, CO in separating still 142Separate out extract. CO subsequently2Circulation enters filter 2, Carry out next one circulation. If select to enter rectifying column from the middle part, then need shut off valve 11, open valve 10. The component that solubility is little in rectifying column " is eliminated ", and backflow flows downward in the gathering formation; The big component of solubility is with CO2Reduce to separating pressure via pressure-reducing valve 13 together, and enter separating still 14. In separating still 14, CO2Solvability descends, and discharges all components. CO subsequently2Follow Ring enters filter 2, carries out next one circulation. The component that solubility is big is passed through valve 15 from separating still 14 The bottom is intermittently emitted, and the component that solubility is little is intermittently emitted from rectifying column 12 bottoms by valve 16.
Embodiment of the method rectifying column disclosed by the invention adopts axial four sections heating water baths, the height of rectifying column Degree 2.0m, internal diameter 9mm.
Compared with prior art, advantage of the present invention is once to feed intake to obtain different two kinds of quality Embryo oil is effectively concentrated the target components vitamin E.
Embodiment one (middle part charging)
Charging 500g, extraction kettle pressure 30MPa, 35 ℃ of extraction kettle temperature, the temperature distribution of rectifying column is: 35 ℃ (end), 40 ℃, 45 ℃, 50 ℃ (top), separating still pressure 5MPa, 20 ℃ of separating still temperature.From the effusive germ oil 18.34g in rectifying column bottom, color and luster is darker, content of vitamin E 180mg/100g; The effusive germ oil 30.21g from the separating still top, color and luster is light, content of vitamin E 392mg/100g.
Embodiment two (middle part charging)
Charging 500g, extraction kettle pressure 36MPa, 35 ℃ of extraction kettle temperature, the pressure 20MPa of rectifying column, the temperature distribution of rectifying column is: 35 ℃ (end), 45 ℃, 55 ℃, 65 ℃ (top), separating still pressure 5MPa, 20 ℃ of separating still temperature.From the effusive germ oil 20.31g in rectifying column bottom, color and luster is darker, content of vitamin E 162mg/100g; The effusive germ oil 28.04g from the separating still top, color and luster is light, content of vitamin E 416mg/100g.
Embodiment three (bottom feed)
Charging 200g, extraction kettle pressure 35MPa, 40 ℃ of extraction kettle temperature, the pressure of rectifying column equals extraction kettle pressure, and the temperature distribution of rectifying column is: 40 ℃ (end), 50 ℃, 61 ℃, 70 ℃ (top), separating still pressure 5MPa, 25 ℃ of separating still temperature.From the extract 3.0g that separating still is collected earlier, its content of vitamin E 501mg/100g.
Claims (4)
1. a supercritical fluid extraction combines with rectifying and separates the method for wheatgerm oil, it is that solvent extracts germ oil with the supercritical co from wheatgerm, it is characterized in that: make the supercutical fluid that flows out and be dissolved with germ oil from extraction kettle, enter a rectifying column.
2. method according to claim 1, it is characterized in that the supercutical fluid that is dissolved with germ oil enters rectifying column with following dual mode: I, enter rectifying column from the bottom of rectifying column, then the component in the germ oil flows out from the rectifying column top by the descending order of solubleness; II, enter rectifying column from the middle part of rectifying column, then the component that solubleness is little in the germ oil flows out from the rectifying column bottom, and the component that solubleness is big flows out from the rectifying column top.
3. method according to claim 1 is characterized in that rectifying column along short transverse temperature distribution difference, and pressure is constant along short transverse.
4. method according to claim 3, the temperature that it is characterized in that rectifying column temperature from top to bottom rises gradually, and bottom temp is not less than 15 ℃, and head temperature is not higher than 95 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98111424 CN1242416A (en) | 1998-07-20 | 1998-07-20 | Method for obtg. Wheat-germ oil using supercritical extraction combined with rectification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98111424 CN1242416A (en) | 1998-07-20 | 1998-07-20 | Method for obtg. Wheat-germ oil using supercritical extraction combined with rectification |
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|---|---|
| CN1242416A true CN1242416A (en) | 2000-01-26 |
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|---|---|---|---|
| CN 98111424 Pending CN1242416A (en) | 1998-07-20 | 1998-07-20 | Method for obtg. Wheat-germ oil using supercritical extraction combined with rectification |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7524522B2 (en) | 2006-08-18 | 2009-04-28 | Mor Technology, Llc | Kernel fractionation system |
| US7612220B2 (en) | 2006-08-18 | 2009-11-03 | Mor Technology, Llc | Carbon dioxide extraction of corn germ oil from corn germ |
| CN102406049A (en) * | 2011-10-25 | 2012-04-11 | 江苏江大源生态生物科技有限公司 | Joint preparation method of wheat germ oil and wheat germ protein |
| US8227012B2 (en) | 2006-08-18 | 2012-07-24 | Mor Technology, Llc | Grain fraction extraction material production system |
| US8747931B2 (en) | 2007-10-24 | 2014-06-10 | Mor Supercritical, Llc | Super critical fluid extraction and fractionation of bran extraction materials |
| US10486083B2 (en) | 2016-04-06 | 2019-11-26 | Kiinja Corporation | Separator for fractional separation of supercritical carbon dioxide extracts |
| US11305212B2 (en) | 2016-04-06 | 2022-04-19 | Kiinja Corporation | Multifunctional vessels for extraction and fractionation of extracts from biomass |
-
1998
- 1998-07-20 CN CN 98111424 patent/CN1242416A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7524522B2 (en) | 2006-08-18 | 2009-04-28 | Mor Technology, Llc | Kernel fractionation system |
| US7612220B2 (en) | 2006-08-18 | 2009-11-03 | Mor Technology, Llc | Carbon dioxide extraction of corn germ oil from corn germ |
| US8747106B2 (en) | 2006-08-18 | 2014-06-10 | Mor Technology, Llc | Power production using grain fractionation products |
| US8227012B2 (en) | 2006-08-18 | 2012-07-24 | Mor Technology, Llc | Grain fraction extraction material production system |
| US8551553B2 (en) | 2006-08-18 | 2013-10-08 | Mor Technology, Llc | Grain endosperm extraction system |
| US8603328B2 (en) | 2006-08-18 | 2013-12-10 | Mor Supercritical, Llc | Carbon dioxide corn germ oil extraction system |
| US8747931B2 (en) | 2007-10-24 | 2014-06-10 | Mor Supercritical, Llc | Super critical fluid extraction and fractionation of bran extraction materials |
| CN102406049A (en) * | 2011-10-25 | 2012-04-11 | 江苏江大源生态生物科技有限公司 | Joint preparation method of wheat germ oil and wheat germ protein |
| US10486083B2 (en) | 2016-04-06 | 2019-11-26 | Kiinja Corporation | Separator for fractional separation of supercritical carbon dioxide extracts |
| US10625175B2 (en) | 2016-04-06 | 2020-04-21 | Kiinja Corporation | Extractor for high pressure extraction of a matrix |
| US11235261B2 (en) | 2016-04-06 | 2022-02-01 | Kiinja Corporation | Separator for fractional separation of supercritical carbon dioxide extracts |
| US11305212B2 (en) | 2016-04-06 | 2022-04-19 | Kiinja Corporation | Multifunctional vessels for extraction and fractionation of extracts from biomass |
| US11478726B2 (en) | 2016-04-06 | 2022-10-25 | Kiinja Corporation | Extractor for high pressure extraction of a matrix |
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