CN105597367A - Method for separating ginger essential oil from gingerol-rich oleoresin ginger through low-pressure supercritical CO2 extraction - Google Patents
Method for separating ginger essential oil from gingerol-rich oleoresin ginger through low-pressure supercritical CO2 extraction Download PDFInfo
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- CN105597367A CN105597367A CN201610144470.4A CN201610144470A CN105597367A CN 105597367 A CN105597367 A CN 105597367A CN 201610144470 A CN201610144470 A CN 201610144470A CN 105597367 A CN105597367 A CN 105597367A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D2011/007—Extraction using a solvent in the gas phase
Abstract
The invention relates to a method for separating ginger essential oil from gingerol-rich oleoresin ginger through low-pressure supercritical CO2 extraction. The method comprises the steps of extracting ginger powder with high-pressure low-temperature CO2 fluid under low extraction pressure and at low temperature to prepare first CO2 extract liquid in which effective ingredients of ginger are dissolved; performing heat exchange and heating on the first CO2 extract liquid and separating directly to obtain oleoresin ginger resin containing extracts of full ingredients of ginger; carrying out extraction, heat exchange and heating, rectification and separation on the oleoresin ginger resin containing extracts of full ingredients of ginger sequentially to obtain high-purity ginger essential oil and gingerol-rich oleoresin ginger respectively, thereby achieving effective separation of the two effective ingredients. According to the method, while the extraction temperature and the extraction pressure are effectively reduced, the two effective ingredients, gingerol-based oleoresin ginger and ginger essential oil, in ginger are effectively separated, and finally, high-purity ginger essential oil and gingerol-rich oleoresin ginger are prepared.
Description
Technical field
The invention belongs to the extraction and separation technology field of natural products, be specifically related to a kind of low-pressure supercritical CO2Extract and separate ginger essential oil and the method that is rich in gingerol oleoresin ginger.
Background technology
Ginger is the rhizome of Zingiber ginger ginger (ZingiberofficinaleRosc.), and traditional Chinese medicine is thought gingerPungent, hot; Return spleen, stomach, the heart, lung channel, have warming spleen and stomach for dispelling cold, Hui Yang promotes blood circulation, effect of eliminating dampness dissolving phlegm,For wrist abdomen crymodynia, vomiting is had loose bowels, the cold weak pulse of limb, and phlegm and retained fluid is breathed with cough and is waited disease, and modern pharmacological research shows, gives birth toThat ginger has is antipyretic, analgesia, anti-inflammatory, anti-heart failure, antibacterial, tell in town, promote choleresis, and protection cardiac muscle is thinThe damage of born of the same parents' Anoxia, the pharmacologically actives such as platelet aggregation-against. Ginger is also that one is deeply liked, extensively madeWith natural pungent Fragrant food flavoring, be typical medicine food dual purpose plant.
In ginger, most important chemical composition is that volatile oil-Jiang essential oil (Essentialoilofginger) and ginger are pepperyElement class-oleoresin ginger (Oleoresinofginger).
Ginger essential oil typically refers to the volatility oil content that the steam distilled method of water extracts from ginger rhizome,Containing higher boiling composition, there is strong aromatic odor hardly, be mainly used in perfuming and the tune of food and beverageTaste. Ginger essential oil is transparent, pale yellow to orange flowable liquid, is a kind of mixture of complexity. Due to gingerEssential oil gives off a strong fragrance, and has the fragrance of the tool fresh flower feature of pleasant, lemon slightly, and taste is warm, fragrantPungent, not pungent, be mainly used in food and cosmetics. As for food, beverage, without alcohol cold drink and spyPerfuming, the seasoning of different sweet wine are natural food flavors; For the particularly reason of man's use perfume of cosmeticsThink natural essence raw material. Ginger essential oil also has long history as medicinal, has dispelling cold and dehumidification, wind dispelling pain relieving,Warming and activating meridian, the motion sicknesses such as prevent and cure Car-sickness, ship, aircraft, also have anti-aging effects. Nearest research shows,Terpene compound in ginger essential oil has protection gastric mucosa and antiulcer action, and ginger essential oil is to central nervous systemHave inhibitory action, ginger essential oil also has good antiinflammatory action.
Oleoresin ginger refers to organic solvent extraction ginger rhizome, then reclaims organic solvent, remaining comparisonThe semi-fluid substance of thickness, contains nonvolatile fat constituent that essential oil does not possess. Oleoresin ginger is adjusted as gingerTaste substance intensely processed products, contain very important volatility oil content, gingerol composition and fat oil on sense organ,Palm fibre eleostearic acid, resin and carbohydrate, wherein gingerol is to determine the flavour of ginger and oleoresin ginger local flavorMain composition. As flavoring, whole fragrance and taste that oleoresin ginger contains ginger, therefore can be used as heightThe concentrated flavoring of quality substitutes traditional natural spicy materials and is applied to food processing and culinary art, and particularly it contains gingerMain flavor components-gingerol, studies confirm that, gingerol have cardiac stimulant, step-down, reducing blood lipid, hypoglycemic,The pharmacological actions widely such as antiplatelet, anti-oxidant, antitumor, anti-inflammatory analgesic, and there is important biologyActive function, has important use at field of medicaments.
Supercritical fluid extraction, particularly supercritical CO2Fluid extraction technology is a kind of new chemical separatingMonotechnics, integrates and extracts separation process, and technological process is short, and extraction temperature is low, and extraction efficiency is high,No solvent residue, is particularly suitable for nonpolar in natural products or low pole material-as effective in fat-soluble volatilityThe extraction of composition separates.
But, in prior art, utilize supercritical CO2The method of extracting and separating effective components of ginger, need to beAt 32 DEG C-80 DEG C of higher extracting pressure 7Mpa～45Mpa, higher extraction temperature, extract and make extractionThing, carries out afterwards multi-stage separation again and makes gingerol class-oleoresin ginger and ginger essential oil, finally makes gingerol classIn-oleoresin ginger, gingerol content is lower, is only 11-14wt%, and because the extraction temperature adopting is higher,Heat-sensitive ingredients in natural products is caused damage, thereby affect yield and the purity of active ingredient. In addition, byNeed to bear high pressure in extracting system, equipment manufacturing cost costliness, invests hugely, and general enterprises is difficult to bear; AndAnd extracting system overall size is generally smaller, be difficult to realize extensive extraction.
Summary of the invention
The problems referred to above that exist in order to solve prior art, the invention provides a kind of in effective extraction temperature that reducesWhen degree and extracting pressure, improve the low-pressure supercritical CO of active ingredient yield and purity2Extract and separate ginger essenceOil and the method that is rich in gingerol oleoresin ginger.
The technical solution adopted in the present invention is:
A kind of low-pressure supercritical CO2Extract and separate ginger essential oil and the method that is rich in gingerol oleoresin ginger, compriseFollowing steps:
(S1) extraction for the first time: utilize the high pressure low temperature CO that pressure is 7-20 DEG C for 8-12MPa, temperature2Fluid extracts ginger powder, makes the CO for the first time that is dissolved with effective components of ginger2Extract; This isBecause above-mentioned extracting pressure 8-12MPa is a little more than CO2Critical pressure (7.4MPa), extraction temperature 7-20 DEG CLower than CO2Critical-temperature (31 DEG C), with this understanding, CO2Be liquid, viscosity is low, has betterPermeability, diffusivity, density is high, has stronger solvability, studies discovery through the inventor, thisCO under individual condition2The dissolving power of fluid is equivalent to 45 DEG C, the supercritical CO of the above pressure of 27MPa2, fromAnd can the active ingredient in ginger powder fully be dissolved and be extracted;
(S2) heat exchange for the first time heats up: will step (S1) Suo Shu, be dissolved with first of effective components of gingerInferior CO2Extract carries out heat exchange intensification, forms the CO for the first time of supercriticality2Extract;
(S3) separate for the first time: be under the condition of 6-8MPa, temperature 35-45 DEG C, to step (S2) at pressureThe CO of described supercriticality2Extract separates, and obtains the oleoresin ginger containing the full component extract of gingerWith low-pressure supercritical CO2Fluid;
(S4) extraction for the second time: utilize the high pressure low temperature CO that pressure is 7-20 DEG C for 8-12MPa, temperature2Fluid extracts the oleoresin ginger containing the full component extract of ginger step (S3) Suo Shu, makes dissolvingThere is the CO for the second time of effective components of ginger2Extract;
(S5) heat exchange for the second time heats up: will step (S4) Suo Shu, be dissolved with second of effective components of gingerInferior CO2Extract carries out heat exchange intensification, forms the CO for the second time of supercriticality2Extract;
(S6) rectifying: be under the condition of 8-12MPa, temperature 35-45 DEG C, to described overcritical shape at pressureThe CO for the second time of state2Extract carries out rectifying, obtain being rich in the oleoresin ginger of gingerol and with light group of volatilityPoint;
(S7) separate for the second time: be under the condition of 6-8MPa, temperature 35-45 DEG C at pressure, will described in waveThe property sent out light component separates, and obtains ginger essential oil and low-pressure supercritical CO2Fluid. This be due to: after rectifyingThe volatility light component forming comprises ginger essential oil and supercritical CO2Fluid, ginger essential oil is along with supercritical CO2StreamBody enters lower pressure environment (lower than initial extracting pressure 8-12MPa), and afterwards, ginger essential oil is separated out, withTime make low-pressure supercritical CO2Fluid is separated.
In step (S1), the particle diameter of described ginger powder is 2-3 ㎜.
In step (S2), the CO for the first time of described supercriticality2The temperature of extract is 31-45 DEG C.
In step (S5), the CO for the second time of described supercriticality2The temperature of extract is 31-45 DEG C.
The described low-pressure supercritical CO that step (S3) and step (S7) are obtained2That fluid carries out is successively cooling,After supercharging, form the described high pressure low temperature CO of step (S1)2Fluid, recycles. This be due to, with gingerLow-pressure supercritical CO after essential oil separates2Fluid, through cooling to critical-temperature below 31 DEG C, noUndergo phase transition, directly after pressurization, form high pressure low temperature CO2Fluid recycles as extractant, andAnd owing to there is no the heat of transformation, more energy-conservation.
Implement a system for described method, set gradually and comprise along technique distance:
Extraction equipment, the top of described extraction equipment arranges extract outlet, and bottom arranges CO2Fluid noteEntrance;
Heat exchange heat riser, the top of described heat exchange heat riser is communicated with setting with described extract outlet;
Rectifying column, the bottom of the bottom of described rectifying column and described heat exchange heat riser connects by the first tube connectorLogical setting, arranges the first valve on described the first tube connector;
Knockout tower, the top of described knockout tower arranges respectively CO2Extract import and the import of volatility light component,Top arranges supercritical CO2Fluid discharge outlet, bottom arranges material outlet; Described CO2Extract importBe communicated with setting with the bottom of described heat exchange heat riser by the second tube connector, on described the second tube connector, arrangeThe second valve; The import of described volatility light component is communicated with and is established by the 3rd tube connector with the top of described rectifying columnPut, on described the 3rd tube connector, the 3rd valve is set.
Described rectifying column sets gradually the first rectification cell, the second rectification cell, the 3rd rectifying list from the bottom to topUnit and the 4th rectification cell, described the first rectification cell, the second rectification cell, the 3rd rectification cell and the 4thThe rectification temperature of rectification cell increases progressively successively.
Also comprise surge tank, the top of described surge tank and the supercritical CO of described knockout tower2Fluid discharge outletBe communicated with and arrange, the bottom of described surge tank and the CO of described extraction equipment2Fluid inlet connects by the 4thPipe is communicated with setting, on described the 4th tube connector, force (forcing) pump is set.
Beneficial effect of the present invention is:
Low-pressure supercritical CO of the present invention2Extract and separate ginger essential oil and the side of being rich in gingerol oleoresin gingerMethod, by first utilizing high pressure low temperature CO2Fluid is in lower extracting pressure 8-12MPa and lower extraction temperatureAt spending 7-20 DEG C, ginger powder is extracted, make the CO for the first time that is dissolved with effective components of ginger2Extract;Again by described CO for the first time2Extract carries out directly separating to make containing the full composition of ginger after heat exchange intensification carryingGet the oleoresin ginger of thing; Afterwards using containing the oleoresin ginger of the full component extract of ginger as successively in specific controlUnder condition, extract, heat exchange intensification, rectifying, separating treatment, finally obtain respectively high-purity ginger essential oil and richnessContaining gingerol oleoresin ginger, realize effective separation of two kinds of active ingredients; Data show, the inventive methodMake the purity of described ginger essential oil up to more than 99%, substantially not containing gingerol; Simultaneously, be rich in gingerolIn oleoresin ginger, gingerol content is up to 52.4wt%, far away higher than using supercritical CO in prior art2ExtractionGetting separation method, to make in gingerol class-oleoresin ginger gingerol content be only 11-14wt%. In sum, originallyInvent described method in effectively reducing extraction temperature and extracting pressure, make two kinds of effective one-tenth in gingerPoint gingerol class-oleoresin ginger effectively separates with ginger essential oil, finally makes high-purity ginger essential oil and be rich in ginger pepperyThe oleoresin ginger of element.
Brief description of the drawings
Fig. 1 is the low-pressure supercritical CO that the embodiment of the present invention 1 provides2Extract and separate ginger essential oil and to be rich in ginger pepperyThe structural representation of element oleoresin ginger system;
Fig. 2 is the low-pressure supercritical CO that the embodiment of the present invention 2 provides2Extract and separate ginger essential oil and to be rich in ginger pepperyThe structural representation of element oleoresin ginger system.
In figure: 1-extraction equipment, 2-heat exchange heat riser, 3-the first valve, 4-rectifying column, 5-the 3rd valve,6-the second valve, 7-knockout tower, 8-surge tank, 9-high-pressure plunger pump.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
As shown in Figure 1, the present embodiment provides a kind of low-pressure supercritical CO2Extract and separate ginger essential oil and be rich in gingerThe system of Capsaicin oleoresin ginger, along technique distance set gradually comprise extraction equipment 1, heat exchange heat riser 2,Rectifying column 4, knockout tower 7.
The top of described extraction equipment 1 arranges extract outlet, and bottom arranges CO2Fluid inlet;
The top of described heat exchange heat riser 2 is communicated with setting with described extract outlet;
The bottom of described rectifying column 4 is communicated with and is established by the first tube connector with the bottom of described heat exchange heat riser 2Put, the first valve 3 is set on described the first tube connector;
The top of described knockout tower 7 arranges respectively CO2Extract import and the import of volatility light component, topSupercritical CO is set2Fluid discharge outlet, bottom arranges material outlet; Described CO2Extract import and instituteThe bottom of stating heat exchange heat riser 2 is communicated with and is arranged by the second tube connector, arranges the on described the second tube connectorTwo valves 6; The import of described volatility light component is communicated with by the 3rd tube connector with the top of described rectifying column 4Arrange, on described the 3rd tube connector, the 3rd valve 5 is set.
Low-pressure supercritical CO based on described system2Extract and separate ginger essential oil and be rich in gingerol oleoresin gingerMethod, comprise the steps:
(S1) raw material processing: the rhizoma zingiberis 1000g that to take water content≤18wt%, gingerol content be 1.47wt%,Being crushed to particle diameter is 2mm, packs in described extraction equipment 1;
(S2) extraction for the first time: be that 8MPa, temperature are 7 DEG C from the bottom injection pressure of described extraction equipment 1High pressure low temperature CO2Fluid, utilizes described high pressure low temperature CO2Fluid extracts 2h to ginger powder, makesBe dissolved with the CO for the first time of effective components of ginger2Extract;
(S3) heat exchange for the first time heats up: will step (S2) Suo Shu, be dissolved with first of effective components of gingerInferior CO2Extract passes into described heat exchange heat riser 2 and carries out heat exchange intensification, and formation temperature is super the facing of 31 DEG CThe CO for the first time of boundary's state2Extract;
(S4) separate for the first time: close the first valve 3 and the 3rd valve 5, open the second valve 6, will walkSuddenly the CO of (S3) described supercriticality2Extract passes into knockout tower 7, is 6MPa, temperature at pressureCO to described supercriticality under the condition of 35 DEG C2Extract separates, and obtains carrying containing the full composition of gingerGet oleoresin ginger and the low-pressure supercritical CO of thing2Fluid;
(S5) extraction for the second time: by the oleoresin ginger dress containing the full component extract of ginger step (S4) Suo ShuEntering extraction equipment 1, is that 8MPa, temperature are the high pressure of 7 DEG C from the bottom injection pressure of described extraction equipment 1Low temperature CO2Fluid, utilizes described high pressure low temperature CO2Fluid is to the described ginger containing the full component extract of gingerOleoresin extracts 2.5h, makes the CO for the second time that is dissolved with effective components of ginger2Extract;
(S6) heat exchange for the second time heats up: will step (S5) Suo Shu, be dissolved with second of effective components of gingerInferior CO2Extract passes into described heat exchange heat riser 2 and carries out heat exchange intensification, and formation temperature is super the facing of 31 DEG CThe CO for the second time of boundary's state2Extract;
(S7) rectifying: close the second valve 6, open the first valve 3 and the 3rd valve 5, by step (S6)The CO for the second time of described supercriticality2Extract passes into rectifying column 4, is 12MPa, temperature 45 C at pressureCondition under, to the CO for the second time of described supercriticality2Extract carries out rectifying, obtains being rich in gingerolOleoresin ginger and volatility light component and other a small amount of impurity cuts, impurity cut is the wax in oleoresin gingerThe composition such as matter, phosphatide neither contributes pungent also not contribute fragrance in product, directly discards;
(S8) separate for the second time: described step (S7) volatility light component is passed into knockout tower 7, pressingPower is under the condition of 35 DEG C of 6MPa, temperature, and described volatility light component is separated, and obtains ginger essential oilWith low-pressure supercritical CO2Fluid.
Detect according to ISO13685, described in be rich in gingerol oleoresin ginger go out rate be 1.64wt% (The quality that obtains being rich in gingerol oleoresin ginger accounts for the mass fraction of rhizoma zingiberis quality), described in be rich in gingerol ginger oilIn resin, gingerol content is 52.4wt%, and the rate 2.06wt% that goes out of described ginger essential oil (obtains the matter of ginger essential oilAmount accounts for the mass fraction of rhizoma zingiberis quality), the purity of described ginger essential oil is higher, after testing, in described ginger essential oil, containsThe amount of gingerol is only 0.87wt%.
Embodiment 2
As shown in Figure 2, the present embodiment provides another kind of low-pressure supercritical CO2Extract and separate ginger essential oil and being rich inThe system of gingerol oleoresin ginger, along technique distance set gradually comprise extraction equipment 1, heat exchange heat riser 2,Rectifying column 4, knockout tower 7, surge tank 8.
The top of described extraction equipment 1 arranges extract outlet, and bottom arranges CO2Fluid inlet;
The top of described heat exchange heat riser 2 is communicated with setting with described extract outlet;
The bottom of described rectifying column 4 is communicated with and is established by the first tube connector with the bottom of described heat exchange heat riser 2Put, the first valve 3 is set on described the first tube connector; Described rectifying column 4 sets gradually first from the bottom to topRectification cell, the second rectification cell, the 3rd rectification cell and the 4th rectification cell, described the first rectification cell,The rectification temperature of the second rectification cell, the 3rd rectification cell and the 4th rectification cell increases progressively successively;
The top of described knockout tower 7 arranges respectively CO2Extract import and the import of volatility light component, topSupercritical CO is set2Fluid discharge outlet, bottom arranges material outlet; Described CO2Extract import and instituteThe bottom of stating heat exchange heat riser 2 is communicated with and is arranged by the second tube connector, arranges the on described the second tube connectorTwo valves 6; The import of described volatility light component is communicated with by the 3rd tube connector with the top of described rectifying column 4Arrange, on described the 3rd tube connector, the 3rd valve 5 is set;
The supercritical CO of the top of described surge tank 8 and described knockout tower 72Fluid discharge outlet is communicated with setting,The CO of the bottom of described surge tank 8 and described extraction equipment 12Fluid inlet is communicated with by the 4th tube connectorArrange, on described the 4th tube connector, high-pressure plunger pump 9 is set.
Low-pressure supercritical CO based on described system2Extract and separate ginger essential oil and be rich in gingerol oleoresin gingerMethod, comprises the steps:
(S1) raw material processing: the rhizoma zingiberis 1000g that to take water content≤18wt%, gingerol content be 1.47wt%,Being crushed to particle diameter is 2mm, packs in described extraction equipment 1;
(S2) extraction for the first time: be that 12MPa, temperature are from the bottom injection pressure of described extraction equipment 1The high pressure low temperature CO of 20 DEG C2Fluid, utilizes described high pressure low temperature CO2Fluid extracts 2.5h to ginger powder,Make the CO for the first time that is dissolved with effective components of ginger2Extract;
(S3) heat exchange for the first time heats up: will step (S2) Suo Shu, be dissolved with first of effective components of gingerInferior CO2Extract passes into described heat exchange heat riser 2 and carries out heat exchange intensification, and formation temperature is super the facing of 45 DEG CThe CO for the first time of boundary's state2Extract;
(S4) separate for the first time: close the first valve 3 and the 3rd valve 5, open the second valve 6, will walkSuddenly the CO of (S3) described supercriticality2Extract passes into knockout tower 7, is 12MPa, temperature at pressureUnder the condition of 45 DEG C, to the CO of described supercriticality2Extract separates, and obtains containing the full composition of gingerThe oleoresin ginger of extract and low-pressure supercritical CO2Fluid; By described low-pressure supercritical CO2Fluid enters successivelyAfter cooling, the supercharging of row, form high pressure low temperature CO2Fluid re-injects described extraction equipment 1 bottom to followRing uses;
(S5) extraction for the second time: by the oleoresin ginger dress containing the full component extract of ginger step (S4) Suo ShuEntering extraction equipment 1, is that 12MPa, temperature are the height of 20 DEG C from the bottom injection pressure of described extraction equipment 1Force down warm CO2Fluid, utilizes described high pressure low temperature CO2Fluid to described containing the full component extract of gingerOleoresin ginger extracts 2.5h, makes the CO for the second time that is dissolved with effective components of ginger2Extract;
(S6) heat exchange for the second time heats up: will step (S5) Suo Shu, be dissolved with second of effective components of gingerInferior CO2Extract passes into described heat exchange heat riser 2 and carries out heat exchange intensification, and formation temperature is super the facing of 45 DEG CThe CO for the second time of boundary's state2Extract;
(S7) rectifying: close the second valve 6, open the first valve 3 and the 3rd valve 5, by step (S6)The CO for the second time of described supercriticality2Extract passes into rectifying column 4, is 12MPa, temperature 45 C at pressureCondition under, to the CO for the second time of described supercriticality2Extract carries out continuous 4 rectifying from top to bottom,The temperature of 4 rectifying is followed successively by 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, finally obtains being rich in gingerol ginger oil treeOther a small amount of impurity cuts of fat and volatility light component, impurity cut is wax, the phosphatide etc. in oleoresin gingerComposition neither contributes pungent also not contribute fragrance in product, directly discards;
(S8) separate for the second time: described step (S7) volatility light component is passed into knockout tower 7, pressingPower is under the condition of 8MPa, temperature 45 C, and described volatility light component is separated, and obtains ginger essential oilWith low-pressure supercritical CO2Fluid; By described low-pressure supercritical CO2That fluid carries out is successively cooling, shape after superchargingBecome high pressure low temperature CO2Fluid re-injects described extraction equipment 1 bottom to recycle.
Detect according to ISO13685, described in be rich in gingerol oleoresin ginger go out rate be 1.64wt% (The quality that obtains being rich in gingerol oleoresin ginger accounts for the mass fraction of rhizoma zingiberis quality), described in be rich in gingerol ginger oilIn resin, gingerol content is 52.4wt%, and the rate 2.06wt% that goes out of described ginger essential oil (obtains the matter of ginger essential oilAmount accounts for the mass fraction of rhizoma zingiberis quality), the purity of described ginger essential oil is higher, after testing, in described ginger essential oil, containsThe amount of gingerol is only 0.87wt%.
The present invention is not limited to above-mentioned preferred forms, and anyone can draw it under enlightenment of the present inventionHis various forms of products, no matter but in its shape or structure, do any variation, every have and the applicationIdentical or akin technical scheme, within all dropping on protection scope of the present invention.
Claims (9)
1. a low-pressure supercritical CO2Extract and separate ginger essential oil and the method that is rich in gingerol oleoresin ginger, itsBe characterised in that, comprise the steps:
(S1) extraction for the first time: utilize the high pressure low temperature CO that pressure is 7-20 DEG C for 8-12MPa, temperature2Fluid extracts ginger powder, makes CO for the first time2Extract;
(S2) heat exchange for the first time heats up: will step (S1) Suo Shu, be dissolved with first of effective components of gingerInferior CO2Extract carries out heat exchange intensification, forms the CO for the first time of supercriticality2Extract;
(S3) separate for the first time: be under the condition of 6-8MPa, temperature 35-45 DEG C, to step (S2) at pressureThe CO of described supercriticality2Extract separates, and obtains the thick product of oleoresin ginger and low-pressure supercriticalCO2Fluid;
(S4) extraction for the second time: utilize the high pressure low temperature CO that pressure is 7-20 DEG C for 8-12MPa, temperature2Fluid extracts the thick product of oleoresin ginger step (S3) Suo Shu, makes CO for the second time2Extract;
(S5) heat exchange for the second time heats up: by the CO for the second time step (S4) Suo Shu2Extract carries out heat exchangeHeat up, form the CO for the second time of supercriticality2Extract;
(S6) rectifying: be under the condition of 8-12MPa, temperature 35-45 DEG C, to described overcritical shape at pressureThe CO for the second time of state2Extract carries out rectifying, obtains being rich in oleoresin ginger and the volatility light component of gingerol;
(S7) separate for the second time: be under the condition of 6-8MPa, temperature 35-45 DEG C at pressure, will described in waveThe property sent out light component separates, and obtains ginger essential oil and low-pressure supercritical CO2Fluid.
2. low-pressure supercritical CO according to claim 12Extract and separate ginger essential oil and be rich in gingerol gingerThe method of oleoresin, is characterized in that, in step (S1), the particle diameter of described ginger powder is 2-3 ㎜.
3. low-pressure supercritical CO according to claim 12Extract and separate ginger essential oil and be rich in gingerol gingerThe method of oleoresin, is characterized in that, in step (S2), and the CO for the first time of described supercriticality2ExtractionThe temperature of getting liquid is 31-45 DEG C.
4. low-pressure supercritical CO according to claim 12Extract and separate ginger essential oil and be rich in gingerol gingerThe method of oleoresin, is characterized in that, in step (S5), and the CO for the second time of described supercriticality2ExtractionThe temperature of getting liquid is 31-45 DEG C.
5. low-pressure supercritical CO according to claim 12Extract and separate ginger essential oil and be rich in gingerol gingerThe method of oleoresin, is characterized in that, super the facing of described low pressure that step (S3) and step (S7) are obtainedThe CO of boundary2That fluid carries out is successively cooling, form the described high pressure low temperature CO of step (S1) after supercharging2Fluid,Recycle.
6. a system that implements the claims method described in 1-4 any one, is characterized in that, along technique roadJourney sets gradually and comprises extraction equipment (1), heat exchange heat riser (2), rectifying column (4), knockout tower (7);
The top of described extraction equipment (1) arranges extract outlet, and bottom arranges CO2Fluid inlet;
The top of described heat exchange heat riser (2) is communicated with setting with described extract outlet;
The bottom of the bottom of described rectifying column (4) and described heat exchange heat riser (2) is by the first tube connectorBe communicated with and arrange, the first valve (3) is set on described the first tube connector;
The top of described knockout tower (7) arranges respectively CO2Extract import and the import of volatility light component, topPortion arranges supercritical CO2Fluid discharge outlet, bottom arranges material outlet; Described CO2Extract import withThe bottom of described heat exchange heat riser (2) is communicated with and is arranged by the second tube connector, on described the second tube connector, establishesPut the second valve (6); The top of the import of described volatility light component and described rectifying column (4) connects by the 3rdTake over and be communicated with setting, the 3rd valve (5) is set on described the 3rd tube connector.
7. system according to claim 6, is characterized in that, described rectifying column (4) from the bottom to topSet gradually the first rectification cell, the second rectification cell, the 3rd rectification cell and the 4th rectification cell, described inThe rectification temperature of the first rectification cell, the second rectification cell, the 3rd rectification cell and the 4th rectification cell successivelyIncrease progressively.
8. system according to claim 6, is characterized in that, also comprises surge tank (8), described slowRush the top of tank (8) and the supercritical CO of described knockout tower (7)2Fluid discharge outlet is communicated with setting, described inThe CO of the bottom of surge tank (8) and described extraction equipment (1)2Fluid inlet connects by the 4th tube connectorLogical setting, arranges force (forcing) pump on described the 4th tube connector.
9. system according to claim 8, is characterized in that, described force (forcing) pump is high-pressure plunger pump (9).
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| CN115216366B (en) * | 2022-06-20 | 2023-09-15 | 福建仙芝楼生物科技有限公司 | Ganoderma extract with natural flavor |
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Address after: 266000, Qingdao District, Shandong City, Chengyang District, Hong Kong beach after the double lane road, 210 community Patentee after: Lihe flavor (Qingdao) Food Industry Co., Ltd Address before: 266000, Qingdao District, Shandong City, Chengyang District, Hong Kong beach after the double lane road, 210 community Patentee before: QINGDAO LIHE EXTRACT Co.,Ltd. |
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Denomination of invention: Separation of ginger essential oil and gingerol rich ginger oleoresin by low pressure supercritical CO2extraction Effective date of registration: 20201119 Granted publication date: 20170825 Pledgee: Bank of China Limited Longnan branch Pledgor: Lihe flavor (Qingdao) Food Industry Co., Ltd Registration number: Y2020370010048 |
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Date of cancellation: 20211221 Granted publication date: 20170825 Pledgee: Bank of China Limited Longnan branch Pledgor: Lihe flavor (Qingdao) Food Industry Co., Ltd Registration number: Y2020370010048 |