CN1490066A - Method for extracting effective components from natural materials - Google Patents
Method for extracting effective components from natural materials Download PDFInfo
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- CN1490066A CN1490066A CNA031341705A CN03134170A CN1490066A CN 1490066 A CN1490066 A CN 1490066A CN A031341705 A CNA031341705 A CN A031341705A CN 03134170 A CN03134170 A CN 03134170A CN 1490066 A CN1490066 A CN 1490066A
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Abstract
A process for extracting the active component from natural product features that the supercritical CO2 fluid extraction and the molecular distillation are combined for fully playing their roles.
Description
Technical field
The invention belongs to the field of chemical separation technology, its same food industry, pharmaceuticals industry are relevant with cosmetics industry.Specifically, it relates to and uses supercritical CO
2Fluid extraction technology and extract the method for active ingredient in the natural prodcuts with molecular distillation technique.Promptly the invention provides a kind of with supercritical CO
2Fluid extraction technology and molecular distillation technique are ingenious to combine, to extract the new method of active ingredient in the natural products.
Background technology
Supercritical liquid extraction technique is to utilize the fluid be in more than critical-temperature (Tc) and the critical pressure (Pc) to have the solvability of special growth and a kind of novel chemical separation technology of developing out.Because CO
2Its Tc=31.06 ℃; Pc=7.39MPa; And critical density ρ c=0.448 gram/cm
3, promptly its operating temperature is near room temperature, and operating pressure is comparatively moderate, and density is maximum in the common supercritical solvent, its solvability is also maximum, so adopt CO in supercritical liquid extraction technique
2Making active ingredient in the solvent extraction natural products is best selection.The supercritical fluid extraction system is mainly by extraction kettle and two parts of separating still and suitably be equipped with compression set and heat-exchange device constitutes.Its extraction process can reduce three kinds of isothermal method, equal-pressure method and absorption methods.The characteristics of isothermal method extraction process are extraction kettle and separating still isothermal, and the pressure of extraction kettle then is higher than separating still, CO
2Fluid under low pressure evaporates and separates with solute; The extraction kettle and the separating still of equal-pressure method are in uniform pressure, utilize not CO simultaneously of both temperature
2The difference of fluid solubility reaches the purpose of separation.And in the absorption method, extraction kettle and separating still pressure and temperature all equate, have just filled specific adsorbent in its separating still, by component and the CO of adsorbent with the desire separation
2Fluid is separated.The supercritical CO of natural products
2Extraction process generally is the mixture length that adopts isothermal method and equal-pressure method, and is main separation means with change pressure.As the method and the disclosed new technology of from artemisia annua, extracting qinghaosu of LZ93106143.1 of the disclosed supercritical extraction Seabuckthorn Oil of ZL87103942.9, all be merely to adopt the isothermal method supercritical CO
2Fluid extraction technology, and isolate active ingredient in the natural products with the method for a step step-down.ZL91103477.3 discloses a kind of overcritical (or fluid) carbon dioxide abstraction and refined wheat embryo oil technology, and this technology is improved to progressively step-down with aforesaid " a step voltage drop method " and regulates " the multistep analytic method " of temperature, has obtained preferable effect.
Be as chemical separation technology equally, and be particularly suitable for the molecular distillation technique that liquid-liquid separates, it utilizes the molecule effective diameter difference of each active ingredient in the natural products, and the principle that the mean free path of its molecular motion is different under identical temperature, pressure is separated.Molecular distillation technique is to carry out under high vacuum state and the condition far below the boiling point of material.Compare with traditional method, have that cost is low, energy consumption is little and the high tangible advantage of product quality with distillation and distillation technology parting liquid phase mixture.Be broadly divided into two classes in industrial its structure of molecular still of applying at present, i.e. scraped film type and centrifugal molecular distillator.For multi-component liquid mixture, in order to obtain multiple combination product or to be the purity that improves product, all right multiple-grade molecular distillation device of composite design in a device.ZL88100406.5 discloses nutraceutical methods such as extracting vitamin E from corn oil.Because it is with saponification process corn oil to be handled earlier, and carries out molecular clock again through after the vacuum dehydration.The vitamin E loss is bigger in process of production, and content of vitamin E is also lower in the composite nutrient capsule and pill that Gu Qisuo produces.ZL98111424.5 discloses a kind of supercritical fluid extraction and has combined with rectifying and separate the method for wheat-germ oil, it is characterized in that the supercritical fluid that will flow out and be dissolved with embryo oil from extraction kettle sends into a distillation column, utilize in the distillation column along short transverse Temperature Distribution difference, make the component in the embryo oil separated by the size of its solubility.Because this patent adopts and is still traditional rectification process, and is directly the supercritical fluid that contains embryo oil that flows out in the extraction kettle to be carried out fractionation, so its CO
2Fluid and energy resource consumption are all bigger, and separating effect is also not as effective with molecular distillation technique.
Summary of the invention
The objective of the invention is for seek a kind of more economical, from natural products, extract the method for its active ingredient efficiently.The main points of invention are supercritical CO
2Fluid extraction technology and molecular distillation technique combine dexterously, bring into play the advantage of these two chemical separation technologies fully, active ingredient with in this combination technique extraction natural products can obtain unprecedented, unexpected good result.
The invention provides a kind of method of extracting active ingredient in the natural products, it is characterized in that: supercritical CO
2Fluid extraction technology and molecular distillation technique combine, and make both be connected in series operation, and wherein (1) separating still is in series by plural pressure vessel, and each pressure vessel in the series connection is mounted with independently temperature adjustment, voltage-regulating system respectively; (2) each pressure vessel is equipped with independently solute drain valve, and they are connected respectively to more than one molecular still; (3) each pressure vessel series connection, pressure vessel foremost is connected with extraction kettle with filter by pressure-reducing valve, and the CO of the pressure vessel of least significant end by settling on it
2Return valve inserts compressor or heat-exchange system.
Independently temperature adjustment, the voltage-regulating system settled on said each pressure vessel among the present invention, its temperature regulating range can be 0 ℃--100 ℃, the adjustable range of pressure can be 2--30MPa.Between each pressure vessel, temperature raises one by one, and pressure reduces one by one.
The solute drain valve of said each pressure vessel of the present invention can be parallel with the connection of molecular still, also can be in-line structure.Adopt which type of connected mode to depend primarily on the coupling of the saturated vapour pressure and the interior pressure of molecular still of discharging solute, this point will be paid special attention to when separating multi-component material.
The said molecular still of the present invention can be scraped film type molecular still or centrifugal molecular distillator, also can be multistage combined molecular still.
The said molecular still of the present invention can be that the plural vacuum tank that is equipped with the controlled vacuum system of pressure is in series, and is equipped with heater in each vacuum tank and collects the cold-trap device that separates the back solute.Its adjustable range of pressure in each vacuum tank is 10
2--10
-4Pa.
In method implementation process of the present invention, under malleation (promptly greater than atmospheric pressure), carried out before this, that flow this moment in the device loop mainly is CO
2Fluid.Through supercritical CO
2The active ingredient that fluid extraction comes out, quality and purity are not up to standard usually; Subsequently, with same solvent (CO
2Fluid) solute molecule mean free path or the saturated vapour pressure by each component under negative pressure (being high vacuum) after the separation isolated finished product once more.Different any harmful, the noxious materials of product contact in whole process of production, and this can guarantee product quality and purity.So method of the present invention is very important for the production of food and medicine.
Method of the present invention is particularly suitable for the extraction of Chinese herbal medicine effective ingredients, yet under indivedual occasions, as the extraction of natural capsanthin pigment and pungent element, the extraction of odorless garlic oil also must add certain and guide and support agent or do certain and give processing.In to different natural products in the leaching process of active ingredient, the distribution of pressure is an important technical parameter very in the adjusting of temperature and pressure and each container, these parameters will be determined by the physical and chemical index of each component in the natural products, however can not exceed in general the present invention given adjustable extent.
Description of drawings
Fig. 1 is a process chart of the present invention.
Fig. 2 is the device schematic diagram of method of the present invention.
In Fig. 2, represented parts of each label and device are as follows: 1. extraction kettle; 2. high pressure filter; 3. valve; 4. give hot device; 5. separating still; 6. low-pressure filter; 7. solvent seasoning device; 8.CO
2Storage tank; 9. solvent circulating pump; 10. molecular still; 11. refrigeration system; 12. cold-trap; 13. diffusion pump; 14. oil-sealed rotary pump; 15. steam the excess basin; 16. steam thing (product) basin.As an example, this installation drawing only draw two separating stills and two-stage molecular still, and in an embodiment can have more than two separating still with more than the molecular still of two-stage, this fully will be according to material composition, and many-sided combined factors analysis such as target level of product quality is determined.
Specific embodiments
The method of active ingredient in the extraction natural products provided by the present invention because its application surface is very wide, so specific embodiments is also many, below in conjunction with the discussion of several embodiment so that content of the present invention is further elaborated.
Embodiment 1, the separating of the extraction of wheat-germ oil and natural VE
Wheat embryo accounts for the 2%--3% of whole wheat quality, wherein contains the quality plant fat of 8%--12%, comprises the unrighted acid of a large amount of needed by human such as linoleic acid.And containing 300 milligrams of natural VEs approximately in per 100 gram wheat-germ oils, content is the highest in each vegetable oil.Extract wheat-germ oil with traditional handicraft and not only have the residual solvent problem, also must be again through coming unstuck, purification step such as decolouring, depickling, deodorization just can obtain commodity wheat-germ oil.As for wanting separating natural vitamin E then very difficult especially.
The present invention uses supercritical CO earlier
2Fluid extraction technology extracts wheat tooth oil from wheat embryo.---filter---pressure-reducing valve---plural separator---CO that is by extraction kettle of the system that adopts
2---heat exchanger---force (forcing) pump---(extraction kettle) constitutes return valve.Temperature is 10 ℃ in the extraction kettle--60 ℃, pressure is 10--30MPa; And temperature is 0 ℃ in the separating still--60 ℃, and pressure is reduced to 7MPa by 20MPa step by step, specifically is distributed as: 20MPa (pressure-reducing valve)---15MPa (first separating still)---9MPa (second separating still)---7MPa (heat exchanger).The wheat-germ oil that extracts from separating still is separable and concentrate out natural VE with molecular distillation technique again.The present invention adopts three grades of molecules to distill separating natural vitamin E, and promptly the solute drain valve of separating still is connected to molecular still or three-stage combined molecular still of three series connection respectively.One-level molecular clock actuator temperature is: 140 ℃--200 ℃, pressure is: 10--15Pa; Secondary molecular clock actuator temperature is 200 ℃--250 ℃, pressure is 1-5Pa; The three-stage distillation actuator temperature is 230 ℃--270 ℃, pressure is 5 * 10
-2--5 * 10
-1Pa.What distillation back obtained from cold-trap is concentrated natural vitamin E, and what emit from the molecular still outlet is the wheat-germ oil colourless, that odorless is pure.The single-stage molecular still can be scraped film type or centrifugal molecular distillator.
Embodiment 2, and natural capsanthin pigment separates with the pungent element
Capsicum red pigment is a kind of natural red colouring matter that extracts in the capsicum skin after the maturation because its lovely luster, nontoxic, heat endurance is good, is a kind of desirable food color.And being material---the pungent element of pungent in the capsicum, it can not only promote appetite, and is aid digestion, and also has the effect of dissolved fat, fat-reducing as the raw material of medicine.Because the physicochemical property of capsicum red pigment and pungent element is close, makes both separating difficulties very big; And the quality of separating back two kinds of products can be greatly improved, and economic worth is very big.
Adopt method of the present invention to use supercritical CO earlier
2Fluid extraction contains the capsicum red pigment of pungent element, and the ethanol that can add some is guided and supported agent, also can give processing to chilli with ethanol, during extraction, and 30 ° of extraction kettle temperature--60 ℃.Pressure is 25--35MPa, and the first separating still temperature is 30 °--60 ℃, pressure is 10--14MPa, and the second separating still temperature is 30 °--and 60 ℃.Pressure is 3--5MPa, and this moment, total recovery rate of capsicum red pigment and pungent element can reach more than 98%, and capsicum red pigment account for wherein 40%.Then, the product after the above-mentioned extraction through the two-stage molecular clock, is therefrom separated the pungent element, just can be obtained pure natural capsanthin pigment and pungent element.Temperature, the pressure intensity parameter of its molecular still are as follows: 150 ° of one-level distillations--and 180 ℃, 1--5Pa; 180 ° of secondary distillations--230 ℃, 0.1--0.5Pa.
Sea-buckthorn is a kind of wild plant, and the fructus hippophae edible also can be used as medicine.Seabuckthorn Oil contains abundant nutrition and multiple bioactive ingredients to the human body beneficial, has the effect and the protective effect on cancer risk of extremely strong sterilization, pain relieving, promotion regeneration.Be rich in alpha-linolenic acid in the Seabuckthorn Oil, carry out basic, the most original material in the process and alpha-linolenic acid is a life, however it in human body, but can not synthesize, can only from food, absorb.By China abundant sea buckthorn resources is arranged, and another directly failing utilized well in the past, so refining its meaning of the extraction of exploitation Seabuckthorn Oil and alpha-linolenic acid is just very great.
Adopt supercritical CO
2Fluid extraction technology extracts Seabuckthorn Oil, and its device can be made up of the separating still of an extraction kettle and three series connection, makes raw material with seabuckthorn seeds and the broken fruit of sea-buckthorn, the extraction kettle temperature is 30 °--50 ℃, pressure is 20--30MPa, and first order separating still temperature is 30--50 ℃, and pressure is 15--20MPa; Second level separating still temperature is 30 °--50 ℃, pressure is 10--16MPa; Second level separating still temperature is 30 °--50 ℃, pressure is 6--10MPa.Recovery rate through above-mentioned technology extraction back Seabuckthorn Oil can reach more than 90%, at this moment C in the oil
16Constituent content is about 11%, and C
18Component then reaches 88%, and wherein alpha-linolenic acid can reach about 30%.Then can adopt two to three grades of molecule distillers to finish by refining alpha-linolenic acid in the Seabuckthorn Oil after the extraction, an also available combined type three-stage molecular still is finished.Three grades of molecule distil process parameters are that its temperature and pressure adjustable range are as follows: the temperature of one-level is 140 °--160 ℃, pressure is 5--10Pa; The temperature of secondary is 180 °--200 ℃, pressure is 0.1--1Pa, and three grades temperature is 220 °--and 240 ℃, pressure 1 * 10
-2--1 * 10
-1Pa.
Highly unsaturated fatty acid mainly contains eicosapentaenoic acid (EPA) and DHA (DHA); they have functions such as reducing blood lipid, preventing thrombosis, protection blood vessel and enhancing blood flow, are acknowledged as the active drug of the control cardiovascular and cerebrovascular disease of a new generation.Natural EPA and DHA mainly are present in marine animal and the marine phytoplankton, but mainly are to extract from ocean fish (as cod) oil at present.Technology from fish oil separation and Extraction EPA and DHA of the present invention is taked two step combined methods.The first step is used supercritical CO earlier
2Fluid extraction technology extracts fish oil ethyl ester from fish oil, the temperature of its extraction kettle is 50 °--and 80 ℃, pressure is 20--30MPa; The temperature of separating still is 40 °--60 ℃, pressure is 12--18MPa.Second step then adopted tandem multiple-grade molecular distillation technology to separate from fish oil ethyl ester and the content of concentrated EPA and DHA.Generally speaking, molecular clock technology can the branch Pyatyi be carried out, and temperature and pressure intensity parameter in its distillers at different levels are as follows: the first order is 110 °--120 ℃, and 15--25Pa; The second level is 115 °--125 ℃, and 2--5Pa; The third level is 130 °--150 ℃, and 1--3Pa; The fourth stage is 150 °--170 ℃, and 0.5--2Pa; Level V is 160 °--180 ℃, and 0.1--0.5Pa.Can be through the EPA in its final products after the Pyatyi molecular clock and DHA total amount greater than 80%, and fishlike smell is extremely light, is favored very much.
Its technical characterictic of method of the present invention just is supercritical CO
2Fluid extraction technology and molecular distillation technique combine, bring into play both advantages fully, to obtain beyond thought effect, with method of the present invention the needed various active ingredients of people can be proposed from many animal and plant and microorganism, it can be widely used in food, medicine and cosmetics industry, thereby create good social benefit and economic benefit.
Claims (8)
1, a kind of method of extracting active ingredient in the natural products is characterized in that: with supercritical CO
2Fluid extraction technology and molecular distillation technique combine, and make both be connected in series operation, wherein:
(1) separating still is in series by plural pressure vessel, and each pressure vessel in the series connection is mounted with independently temperature adjustment, voltage-regulating system respectively;
(2) each pressure vessel is equipped with independently solute drain valve, and they are connected respectively to more than one molecular still;
(3) each pressure vessel series connection, pressure vessel foremost is connected with extraction kettle with filter by pressure-reducing valve, and the CO of the pressure vessel of least significant end by settling on it
2Return valve inserts compressor or heat-exchange system.
2, press the method for active ingredient in the described extraction natural products of claim 1, it is characterized in that independently temperature adjustment, the voltage-regulating system settled on said each pressure vessel, its temperature regulating range can be 0 ℃--100 ℃, the adjustable range of pressure can be 2--30MPa.
3, by the method for active ingredient in the described extraction natural products of claim 1, it is characterized in that the solute drain valve of said each pressure vessel can be parallel with the connection of molecular still, also can be in-line structure.
4, by the method for active ingredient in the described extraction natural products of claim 1, it is characterized in that said molecular still can be scraped film type molecular still or centrifugal molecular distillator.
5, by the method for active ingredient in the described extraction natural products of claim 1, it is characterized in that said molecular still can be multistage combined molecular still.
6, press the method for active ingredient in the described extraction natural products of claim 1, it is characterized in that said distiller can be to be in series by the plural vacuum tank that is equipped with the controlled vacuum system of pressure, be equipped with heater in each vacuum tank and collect the cold-trap device that separates the back solute.
7, by the method for active ingredient in claim 4, the 5 described extraction natural products, it is characterized in that pressure adjustable range at different levels in the said molecular still is 10
2--10
-4Pa.
8, by the method for active ingredient in the described extraction natural products of claim 6, it is characterized in that the pressure adjustable range in said each vacuum tank is 10
2--10
-4Pa.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102061129A (en) * | 2009-11-13 | 2011-05-18 | 天津市食品研究所有限公司 | Method for extracting clove oil resin from clove |
| CN102349994A (en) * | 2011-10-21 | 2012-02-15 | 深圳市巨方生物技术有限公司 | Alligator oil hair restoring cream and preparation method thereof |
| CN102888280A (en) * | 2012-10-16 | 2013-01-23 | 九三粮油工业集团有限公司 | Method for extracting lilac essential oil |
| CN103205314A (en) * | 2013-03-21 | 2013-07-17 | 红云红河烟草(集团)有限责任公司 | Rosemary extract and application thereof in cigarettes |
| CN104194925A (en) * | 2014-07-31 | 2014-12-10 | 濮阳市天行健生物科技有限公司 | Method for extracting abelmoschus manihot L.Medic. oil with supercritical CO2 |
| CN104194924A (en) * | 2014-07-31 | 2014-12-10 | 濮阳市天行健生物科技有限公司 | Method for extracting linseed oil with supercritical CO2 |
| CN105597367A (en) * | 2016-03-14 | 2016-05-25 | 青岛利和萃取股份有限公司 | Method for separating ginger essential oil from gingerol-rich oleoresin ginger through low-pressure supercritical CO2 extraction |
| CN107828512A (en) * | 2017-11-01 | 2018-03-23 | 广州市浩立生物科技有限公司 | A kind of agalloch eaglewood Edgeworthia chrysantha extraction separation method and equipment |
| CN107858197A (en) * | 2017-11-01 | 2018-03-30 | 广东金妮宝科技发展有限公司 | A kind of production and processing method of low acid value high-quality edible oil tea-seed oil |
| CN108219922A (en) * | 2018-01-16 | 2018-06-29 | 广州市金妮宝食用油有限公司 | A kind of tea seed ready-mixed oil with healthcare function and preparation method thereof |
| CN108283221A (en) * | 2018-01-19 | 2018-07-17 | 广州市金妮宝食用油有限公司 | A kind of tea seed nourishing flavored oils and preparation method thereof rich in DHA |
-
2003
- 2003-08-27 CN CNA031341705A patent/CN1490066A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102061129A (en) * | 2009-11-13 | 2011-05-18 | 天津市食品研究所有限公司 | Method for extracting clove oil resin from clove |
| CN102349994A (en) * | 2011-10-21 | 2012-02-15 | 深圳市巨方生物技术有限公司 | Alligator oil hair restoring cream and preparation method thereof |
| CN102888280A (en) * | 2012-10-16 | 2013-01-23 | 九三粮油工业集团有限公司 | Method for extracting lilac essential oil |
| CN103205314A (en) * | 2013-03-21 | 2013-07-17 | 红云红河烟草(集团)有限责任公司 | Rosemary extract and application thereof in cigarettes |
| CN104194925A (en) * | 2014-07-31 | 2014-12-10 | 濮阳市天行健生物科技有限公司 | Method for extracting abelmoschus manihot L.Medic. oil with supercritical CO2 |
| CN104194924A (en) * | 2014-07-31 | 2014-12-10 | 濮阳市天行健生物科技有限公司 | Method for extracting linseed oil with supercritical CO2 |
| CN105597367A (en) * | 2016-03-14 | 2016-05-25 | 青岛利和萃取股份有限公司 | Method for separating ginger essential oil from gingerol-rich oleoresin ginger through low-pressure supercritical CO2 extraction |
| CN105597367B (en) * | 2016-03-14 | 2017-08-25 | 青岛利和萃取股份有限公司 | Low-pressure supercritical CO2Extract and separate ginger essential oil and the method rich in gingerol oleoresin ginger |
| CN107828512A (en) * | 2017-11-01 | 2018-03-23 | 广州市浩立生物科技有限公司 | A kind of agalloch eaglewood Edgeworthia chrysantha extraction separation method and equipment |
| CN107858197A (en) * | 2017-11-01 | 2018-03-30 | 广东金妮宝科技发展有限公司 | A kind of production and processing method of low acid value high-quality edible oil tea-seed oil |
| CN108219922A (en) * | 2018-01-16 | 2018-06-29 | 广州市金妮宝食用油有限公司 | A kind of tea seed ready-mixed oil with healthcare function and preparation method thereof |
| CN108283221A (en) * | 2018-01-19 | 2018-07-17 | 广州市金妮宝食用油有限公司 | A kind of tea seed nourishing flavored oils and preparation method thereof rich in DHA |
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