CN105597367B - Low-pressure supercritical CO2Extract and separate ginger essential oil and the method rich in gingerol oleoresin ginger - Google Patents
Low-pressure supercritical CO2Extract and separate ginger essential oil and the method rich in gingerol oleoresin ginger Download PDFInfo
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- CN105597367B CN105597367B CN201610144470.4A CN201610144470A CN105597367B CN 105597367 B CN105597367 B CN 105597367B CN 201610144470 A CN201610144470 A CN 201610144470A CN 105597367 B CN105597367 B CN 105597367B
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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 present invention relates to a kind of low-pressure supercritical CO2Extract and separate ginger essential oil and the method rich in gingerol oleoresin ginger, by first with high pressure low temperature CO2Fluid is extracted in relatively low extracting pressure with a temperature of to ginger powder, and the first time CO for being dissolved with effective components of ginger is made2Extract；Again by the first time CO2Extract carries out directly carrying out the oleoresin ginger that the full component extract containing ginger is made in separation after heat exchange heating；Afterwards using the oleoresin ginger of the full component extract containing ginger as being extracted successively, exchange heat heating, rectifying, separating treatment, high-purity ginger essential oil is finally obtained respectively and rich in gingerol oleoresin ginger, realizes efficiently separating for two kinds of active ingredient；The method of the invention is while effectively reduction extraction temperature and extracting pressure so that two kinds of active ingredient gingerol class oleoresin gingers and ginger essential oil are effectively separated in ginger, and high-purity ginger essential oil and the oleoresin ginger rich in gingerol is finally made.
Description
Technical field
The invention belongs to the extraction and separation technology field of natural products, and in particular to a kind of low-pressure supercritical CO2Extraction point
From ginger essential oil and the method rich in gingerol oleoresin ginger.
Background technology
Ginger be Zingiber ginger ginger (Zingiber officinale Rosc.) rhizome, traditional Chinese medicine think Jiang Xin,
Heat；Returns spleen, stomach, the heart, lung channel, with warming spleen and stomach for dispelling cold, Back to Yang Tongmai, effect of eliminating dampness dissolving phlegm, for wrist abdomen crymodynia, vomiting is let out
Rush down, cold weak pulse of limb, the disease such as sputum cough, modern pharmacological research shows, ginger have antipyretic, analgesia, anti-inflammatory, anti-heart failure, it is antibacterial,
Town is told, promotes choleresis, and protection Myocytes Anoxia, which lacks sugar, to be damaged, the pharmacological activity such as platelet aggregation-against.Ginger is also one
Kind is liked deeply, widely used natural pungent Fragrant food flavoring, is typical medical and edible dual purpose plant.
Most important chemical composition is that volatile oil-ginger essential oil (Essential oil of ginger) and ginger are peppery in ginger
Plain class-oleoresin ginger (Oleoresin of ginger).
Ginger essential oil typically refers to the volatile oil extracted from ginger rhizome with the method for steam distillation, hardly
Composition containing higher boiling, with strong aromatic odor, is mainly used in perfuming and the seasoning of food and beverage.Ginger essential oil be it is transparent,
It is pale yellow to arrive orange flowable liquid, it is a kind of complicated mixture.Because ginger essential oil gives off a strong fragrance, there is the tool of pleasant fresh
The fragrance of flower feature, slightly lemon, taste warm, perfume is not pungent, pungent, is mainly used in food and cosmetics.Such as be used for food,
Beverage, the perfuming without alcohol cold drink and special sweet wine, seasoning, are natural food flavors；For cosmetics particularly man
With the preferable natural essence raw material of perfume.Ginger essential oil also has long history as medicinal, there is dispelling cold and dehumidification, wind dispelling analgesic, temperature
Through dredging collateral, prevent and cure Car-sickness, the motion sickness, also anti-aging effects such as ship, aircraft.It has recently been demonstrated that the terpenes in ginger essential oil
Compound has a protection gastric mucosa and antiulcer action, and ginger essential oil Central nervous system has an inhibitory action, ginger essential oil also have compared with
Good antiinflammatory action.
Oleoresin ginger refers to, with organic solvent extraction ginger rhizome, then reclaim organic solvent, remaining comparison is sticky
Semi-fluid substance, the nonvolatile fat constituent not possessed containing essential oil.Oleoresin ginger contains as ginger flavoring intensely processed products
There are very important volatile oil on sense organ, gingerol composition and fat oil, brown eleostearic acid, resin and carbohydrate, its
Middle gingerol is the main composition of the flavour and oleoresin ginger local flavor that determine ginger.As flavoring, oleoresin ginger contains ginger
Whole fragrance and taste, therefore can be substituted as the concentration flavoring of high-quality traditional natural spicy materials be applied to food processing and
Culinary art, particularly it contain main flavor composition-gingerol of ginger, research is confirmed, gingerol have cardiac stimulant, decompression, reducing blood lipid,
The extensive pharmacological action such as hypoglycemic, antiplatelet, anti-oxidant, antitumor, anti-inflammatory analgesic, and make with important bioactivity
With having important use in field of medicaments.
Supercritical fluid extraction, particularly supercritical CO2Fluid extraction technology, is a kind of new chemical separating unit skill
Art, integrates extraction separation process, and technological process is short, and extraction temperature is low, and extraction efficiency is high, and no solvent residue is particularly suitable for
Nonpolar or low pole material-extraction such as fat-soluble volatile effective component is separated in natural products.
However, utilizing supercritical CO in the prior art2The method of extracting and separating effective components of ginger is, it is necessary in higher extraction
Extraction is carried out at pressure power 7MPa~45MPa, 32 DEG C -88 DEG C of higher extraction temperature extract is made, carry out many fractions again afterwards
From obtained gingerol class-oleoresin ginger and ginger essential oil, finally gingerol content is relatively low in obtained gingerol class-oleoresin ginger, only
For 11-14wt%, and because the extraction temperature of use is higher, heat-sensitive ingredients in natural products are caused damage, so as to influence
The yield and purity of active ingredient.Further, since extracting system needs to bear high pressure, equipment manufacturing cost is expensive, invests huge, typically
Enterprise is difficult to bear；And extracting system overall size is typically smaller, it is difficult to realize extensive extraction.
The content of the invention
In order to solve the above mentioned problem of prior art presence, the invention provides one kind in effectively reduction extraction temperature and extraction
Active ingredient yield and the low-pressure supercritical CO of purity are improved while pressure power2Extract and separate ginger essential oil and rich in gingerol ginger
The method of oleoresin.
The technical solution adopted in the present invention is：
A kind of low-pressure supercritical CO2Extract and separate ginger essential oil and the method rich in gingerol oleoresin ginger, including following step
Suddenly：
(S1) extract for the first time：Utilize the high pressure low temperature CO that pressure is 8-12MPa, temperature is 7-28 DEG C2Fluid is to ginger
Powder is extracted, and the first time CO for being dissolved with effective components of ginger is made2Extract；This is due to above-mentioned extracting pressure 8-
12MPa is slightly above CO2Critical pressure (7.4MPa), 7-28 DEG C of extraction temperature then be less than CO2Critical-temperature (31 DEG C), herein
Under the conditions of, CO2In liquid, viscosity is low, with preferable permeability, diffusivity, and density is high, with stronger solvability, warp
The present inventor's research discovery, the CO under the conditions of this2The dissolving power of fluid equivalent to 45 DEG C, 27MPa pressure above it is overcritical
CO2, so as to carry out fully dissolving and extracting to the active ingredient in ginger powder；
(S2) heat exchange heating for the first time：By the first time CO for being dissolved with effective components of ginger described in step (S1)2Extraction
Liquid carries out heat exchange heating, forms the first time CO of supercriticality2Extract；
(S3) separate for the first time：It is described to step (S2) super to face under conditions of pressure is 6-8MPa, 35-45 DEG C of temperature
The CO of boundary's state2Extract is separated, and obtains the oleoresin ginger and low-pressure supercritical CO of the full component extract containing ginger2Fluid；
(S4) second of extraction：Utilize the high pressure low temperature CO that pressure is 8-12MPa, temperature is 7-28 DEG C2Fluid is to step
(S3) oleoresin ginger of the full component extract containing ginger described in is extracted, and be dissolved with effective components of ginger second is made
CO2Extract；
(S5) second of heat exchange heating：By second of CO for being dissolved with effective components of ginger described in step (S4)2Extraction
Liquid carries out heat exchange heating, forms second of CO of supercriticality2Extract；
(S6) rectifying：Under conditions of pressure is 8-12MPa, 35-45 DEG C of temperature, to second of the supercriticality
CO2Extract carry out rectifying, obtain rich in gingerol oleoresin ginger and with volatility light component；
(S7) second of separation：Under conditions of pressure is 6-8MPa, 35-45 DEG C of temperature, by the volatility light component
Separated, obtain ginger essential oil and low-pressure supercritical CO2Fluid.This is due to：The volatility light component formed after rectifying includes
Ginger essential oil and supercritical CO2Fluid, ginger essential oil is with supercritical CO2Fluid enters relatively low pressure environment (less than initial extraction pressure
Power 8-12MPa) after, ginger essential oil is separated out, while so that low-pressure supercritical CO2Fluid is separated.
In step (S1), the particle diameter of the ginger powder is 2-3 ㎜.
In step (S2), the first time CO of the supercriticality2The temperature of extract is 31-45 DEG C.
In step (S5), second of CO of the supercriticality2The temperature of extract is 31-45 DEG C.
The low-pressure supercritical CO that step (S3) and step (S7) are obtained2Fluid cooled down successively, be pressurized after shape
Into the high pressure low temperature CO described in step (S1)2Fluid, is recycled.This is because, the low pressure after being separated with ginger essential oil surpasses
Critical CO2Fluid, through cooling to 31 DEG C of critical-temperature, does not undergo phase transition, directly pressurized rear formation high pressure low temperature
CO2Fluid is recycled as extractant, and due to no heat of transformation, is more saved.
It is a kind of implement methods described system, along technique distance set gradually including：
Extraction equipment, the top of the extraction equipment sets extract outlet, and bottom sets CO2Fluid-infusing port；
Exchange heat heat riser, and the top of the heat exchange heat riser connects setting with the extract outlet；
Rectifying column, the bottom of the rectifying column is connected by the first connecting tube with the bottom of the heat exchange heat riser and set
Put, the first valve is set in first connecting tube；
Knockout tower, the top of the knockout tower sets CO respectively2Extract import and volatility light component import, top is set
Put supercritical CO2Fluid discharge outlet, bottom sets material outlet；The CO2Extract import and the heat exchange heat riser
Bottom is connected by the second connecting tube and set, and the second valve is set in second connecting tube；The volatility light component import
Connected with the top of the rectifying column by the 3rd connecting tube and the 3rd valve is set in setting, the 3rd connecting tube.
The rectifying column sets gradually the first rectification cell, the second rectification cell, the 3rd rectification cell and from the bottom to top
Four rectification cells, first rectification cell, the second rectification cell, the rectification temperature of the 3rd rectification cell and the 4th rectification cell
It is incremented by successively.
Also include surge tank, the top of the surge tank and the supercritical CO of the knockout tower2Fluid discharge outlet connection is set
Put, the bottom of the surge tank and the CO of the extraction equipment2Fluid-infusing port is connected by the 4th connecting tube and set, and described the
Force (forcing) pump is set in four connecting tubes.
Beneficial effects of the present invention are：
Low-pressure supercritical CO of the present invention2Extract and separate ginger essential oil and the method rich in gingerol oleoresin ginger, lead to
Cross first with high pressure low temperature CO2Fluid is at relatively low extracting pressure 8-12MPa and 7-28 DEG C relatively low of extraction temperature to ginger
Powder is extracted, and the first time CO for being dissolved with effective components of ginger is made2Extract；Again by the first time CO2Extract is carried out
The oleoresin ginger that the full component extract containing ginger is made in separation is directly carried out after heat exchange heating；The full constituents extraction of ginger will be contained afterwards
The oleoresin ginger of thing is extracted under specific control condition successively, exchange heat heating, rectifying, separating treatment, is finally obtained respectively
High-purity ginger essential oil and rich in gingerol oleoresin ginger, realizes efficiently separating for two kinds of active ingredient；Data display, present invention side
The high purity more than 99% of the ginger essential oil is made in method, is substantially free of gingerol；It is simultaneously described to be rich in gingerol oleoresin ginger
Middle gingerol content is up to 52.4wt%, and supercritical CO is significantly larger than used in the prior art2It is peppery that ginger is made in extraction separating method
Gingerol content is only 11-14wt% in plain class-oleoresin ginger.In summary, the method for the invention is in effective reduction extraction
While temperature and extracting pressure so that two kinds of active ingredient gingerol class-oleoresin gingers and ginger essential oil carry out effective in ginger
Separation, is finally made high-purity ginger essential oil and the oleoresin ginger rich in gingerol.
Brief description of the drawings
Fig. 1 is the low-pressure supercritical CO that the embodiment of the present invention 1 is provided2Extract and separate ginger essential oil and rich in gingerol ginger oil tree
The structural representation of fat system；
Fig. 2 is the low-pressure supercritical CO that the embodiment of the present invention 2 is provided2Extract and separate ginger essential oil and rich in gingerol ginger oil tree
The structural representation of fat system.
In figure：1- extraction equipments, 2- heat exchange heat risers, the valves of 3- first, 4- rectifying columns, the valves of 5- the 3rd, 6- second
Valve, 7- knockout towers, 8- surge tanks, 9- high-pressure plunger pumps.
Embodiment
With reference to 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 rich in gingerol ginger oil
The system of resin, sets gradually including extraction equipment 1, heat exchange heat riser 2, rectifying column 4, knockout tower 7 along technique distance.
The top of the extraction equipment 1 sets extract outlet, and bottom sets CO2Fluid-infusing port；
The top of the heat exchange heat riser 2 connects setting with the extract outlet；
The bottom of the rectifying column 4 by the first connecting tube connects setting with the bottom of the heat exchange heat riser 2, described
First valve 3 is set in first connecting tube；
The top of the knockout tower 7 sets CO respectively2Extract import and volatility light component import, top set super face
Boundary CO2Fluid discharge outlet, bottom sets material outlet；The CO2Extract import and the bottom of the heat exchange heat riser 2
Connected and set by the second connecting tube, the second valve 6 is set in second connecting tube；The volatility light component import and institute
The top for stating rectifying column 4 connects the 3rd valve 5 of setting in setting, the 3rd connecting tube by the 3rd connecting tube.
Low-pressure supercritical CO based on the system2Extract and separate ginger essential oil and the method rich in gingerol oleoresin ginger,
Comprise the following steps：
(S1) Feedstock treating：The rhizoma zingiberis 1888g that water content≤18wt%, gingerol content are 1.47wt% is weighed, is crushed
It is 2mm to particle diameter, is fitted into the extraction equipment 1；
(S2) extract for the first time：From the bottom of the extraction equipment 1 injection pressure be 8MPa, the height that temperature is 7 DEG C forces down
Warm CO2Fluid, utilizes the high pressure low temperature CO2Fluid carries out extraction 2h to ginger powder, is made and is dissolved with the of effective components of ginger
CO2Extract；
(S3) heat exchange heating for the first time：By the first time CO for being dissolved with effective components of ginger described in step (S2)2Extraction
Liquid is passed through the heat exchange heat riser 2 and carries out heat exchange heating, forms the first time CO for the supercriticality that temperature is 31 DEG C2Extraction
Liquid；
(S4) separate for the first time：The first valve 3 and the 3rd valve 5 are closed, the second valve 6 is opened, by step (S3) Suo Shu
The CO of supercriticality2Extract is passed through knockout tower 7, to the supercritical state under conditions of pressure is 6MPa, 35 DEG C of temperature
The CO of state2Extract is separated, and obtains the oleoresin ginger and low-pressure supercritical CO of the full component extract containing ginger2Fluid；
(S5) second of extraction：The oleoresin ginger of the full component extract containing ginger step (S4) Suo Shu is loaded into extraction equipment
1, from the bottom of the extraction equipment 1 injection pressure be 8MPa, the high pressure low temperature CO that temperature is 7 DEG C2Fluid, utilizes the high pressure
Low temperature CO2Fluid carries out extraction 2.5h to the oleoresin ginger of the full component extract containing ginger, is made and is dissolved with ginger and has
Imitate second of CO of composition2Extract；
(S6) second of heat exchange heating：By second of CO for being dissolved with effective components of ginger described in step (S5)2Extraction
Liquid is passed through the heat exchange heat riser 2 and carries out heat exchange heating, forms second of CO of the supercriticality that temperature is 31 DEG C2Extraction
Liquid；
(S7) rectifying：The second valve 6 is closed, the first valve 3 and the 3rd valve 5 is opened, step (S6) is described overcritical
Second of CO of state2Extract is passed through rectifying column 4, under conditions of pressure is 12MPa, temperature 45 C, to described overcritical
Second of CO of state2Extract carries out rectifying, obtains being rich in gingerol oleoresin ginger and volatility light component and other are few
Impure fraction is measured, impure fraction is the compositions such as wax, the phosphatide in oleoresin ginger, pungent is neither contributed in the product nor is contributed
Fragrance, is directly discarded；
(S8) second of separation：Step (S7) the volatility light component is passed through knockout tower 7, is 6MPa, temperature in pressure
Under conditions of 35 DEG C of degree, the volatility light component is separated, ginger essential oil and low-pressure supercritical CO is obtained2Fluid.
Detected according to ISO 13685, the extracting rate rich in gingerol oleoresin ginger is that 1.64wt% (obtains richness
The quality of the oleoresin ginger containing gingerol accounts for the mass fraction of rhizoma zingiberis quality), it is described to contain rich in gingerol in gingerol oleoresin ginger
Measure as 52.4wt%, (quality for obtaining ginger essential oil accounts for the quality point of rhizoma zingiberis quality to the extracting rate 2.86wt% of the ginger essential oil
Number), the purity of the ginger essential oil is higher, after testing, and the amount containing gingerol is only 8.87wt% in the ginger essential oil.
Embodiment 2
As shown in Fig. 2 the present embodiment provides another low-pressure supercritical CO2Extract and separate ginger essential oil and rich in gingerol ginger
The system of oleoresin, sets gradually including extraction equipment 1, heat exchange heat riser 2, rectifying column 4, knockout tower 7, slow along technique distance
Rush tank 8.
The top of the extraction equipment 1 sets extract outlet, and bottom sets CO2Fluid-infusing port；
The top of the heat exchange heat riser 2 connects setting with the extract outlet；
The bottom of the rectifying column 4 by the first connecting tube connects setting with the bottom of the heat exchange heat riser 2, described
First valve 3 is set in first connecting tube；The rectifying column 4 sets gradually the first rectification cell, the second rectifying list from the bottom to top
Member, the 3rd rectification cell and the 4th rectification cell, first rectification cell, the second rectification cell, the 3rd rectification cell and the
The rectification temperature of four rectification cells is incremented by successively；
The top of the knockout tower 7 sets CO respectively2Extract import and volatility light component import, top set super face
Boundary CO2Fluid discharge outlet, bottom sets material outlet；The CO2Extract import and the bottom of the heat exchange heat riser 2
Connected and set by the second connecting tube, the second valve 6 is set in second connecting tube；The volatility light component import and institute
The top for stating rectifying column 4 connects the 3rd valve 5 of setting in setting, the 3rd connecting tube by the 3rd connecting tube；
The top of the surge tank 8 and the supercritical CO of the knockout tower 72Fluid discharge outlet connection is set, the buffering
The bottom of tank 8 and the CO of the extraction equipment 12Fluid-infusing port is connected by the 4th connecting tube and set, the 4th connecting tube
Upper setting high-pressure plunger pump 9.
Low-pressure supercritical CO based on the system2Extract and separate ginger essential oil and the method rich in gingerol oleoresin ginger,
Comprise the following steps：
(S1) Feedstock treating：The rhizoma zingiberis 1888g that water content≤18wt%, gingerol content are 1.47wt% is weighed, is crushed
It is 2mm to particle diameter, is fitted into the extraction equipment 1；
(S2) extract for the first time：From the bottom of the extraction equipment 1 injection pressure be 12MPa, the high pressure that temperature is 28 DEG C
Low temperature CO2Fluid, utilizes the high pressure low temperature CO2Fluid carries out extraction 2.5h to ginger powder, is made and is dissolved with effective components of ginger
First time CO2Extract；
(S3) heat exchange heating for the first time：By the first time CO for being dissolved with effective components of ginger described in step (S2)2Extraction
Liquid is passed through the heat exchange heat riser 2 and carries out heat exchange heating, forms the first time CO for the supercriticality that temperature is 45 DEG C2Extraction
Liquid；
(S4) separate for the first time：The first valve 3 and the 3rd valve 5 are closed, the second valve 6 is opened, by step (S3) Suo Shu
The CO of supercriticality2Extract is passed through knockout tower 7, under conditions of pressure is 12MPa, temperature 45 C, to described overcritical
The CO of state2Extract is separated, and obtains the oleoresin ginger and low-pressure supercritical CO of the full component extract containing ginger2Fluid；Will
The low-pressure supercritical CO2Fluid cooled down successively, be pressurized after form high pressure low temperature CO2Fluid re-injects the extraction dress
1 bottom is put to be recycled；
(S5) second of extraction：The oleoresin ginger of the full component extract containing ginger step (S4) Suo Shu is loaded into extraction equipment
1, from the bottom of the extraction equipment 1 injection pressure be 12MPa, the high pressure low temperature CO that temperature is 28 DEG C2Fluid, utilizes the height
Force down warm CO2Fluid carries out extraction 2.5h to the oleoresin ginger of the full component extract containing ginger, is made and is dissolved with ginger
Second of CO of active ingredient2Extract；
(S6) second of heat exchange heating：By second of CO for being dissolved with effective components of ginger described in step (S5)2Extraction
Liquid is passed through the heat exchange heat riser 2 and carries out heat exchange heating, forms second of CO of the supercriticality that temperature is 45 DEG C2Extraction
Liquid；
(S7) rectifying：The second valve 6 is closed, the first valve 3 and the 3rd valve 5 is opened, step (S6) is described overcritical
Second of CO of state2Extract is passed through rectifying column 4, under conditions of pressure is 12MPa, temperature 45 C, to described overcritical
Second of CO of state2Extract carries out continuous 4 rectifying from top to bottom, the temperature of 4 rectifying be followed successively by 38 DEG C, 35 DEG C, 48
DEG C, 45 DEG C, finally give rich in gingerol oleoresin ginger and volatility light component other a small amount of impure fractions, impure fraction is ginger
The compositions such as wax, phosphatide in oleoresin, neither contribute pungent nor contribute fragrance, directly discard in the product；
(S8) second of separation：Step (S7) the volatility light component is passed through knockout tower 7, is 8MPa, temperature in pressure
Under conditions of 45 DEG C of degree, the volatility light component is separated, ginger essential oil and low-pressure supercritical CO is obtained2Fluid；By institute
State low-pressure supercritical CO2Fluid cooled down successively, be pressurized after form high pressure low temperature CO2Fluid re-injects the extraction equipment 1
Bottom is to be recycled.
Detected according to ISO 13685, the extracting rate rich in gingerol oleoresin ginger is that 1.64wt% (obtains richness
The quality of the oleoresin ginger containing gingerol accounts for the mass fraction of rhizoma zingiberis quality), it is described to contain rich in gingerol in gingerol oleoresin ginger
Measure as 52.4wt%, (quality for obtaining ginger essential oil accounts for the quality point of rhizoma zingiberis quality to the extracting rate 2.86wt% of the ginger essential oil
Number), the purity of the ginger essential oil is higher, after testing, and the amount containing gingerol is only 8.87wt% in the ginger essential oil.
The present invention is not limited to above-mentioned preferred forms, and anyone can show that other are various under the enlightenment of the present invention
The product of form, however, make any change in its shape or structure, it is every that there is skill identical or similar to the present application
Art scheme, is within the scope of the present invention.
Claims (9)
1. a kind of low-pressure supercritical CO2Extract and separate ginger essential oil and the method rich in gingerol oleoresin ginger, it is characterised in that bag
Include following steps：
(S1) extract for the first time：Utilize the high pressure low temperature CO that pressure is 8-12MPa, temperature is 7-20 DEG C2Fluid is carried out to ginger powder
Extraction, is made first time CO2Extract；
(S2) heat exchange heating for the first time：By the first time CO for being dissolved with effective components of ginger described in step (S1)2Extract is carried out
Heat exchange heating, forms the first time CO of supercriticality2Extract；
(S3) separate for the first time：Under conditions of pressure is 6-8MPa, 35-45 DEG C of temperature, to step (S2) supercritical state
The CO of state2Extract is separated, and obtains oleoresin ginger crude product and low-pressure supercritical CO2Fluid；
(S4) second of extraction：Utilize the high pressure low temperature CO that pressure is 8-12MPa, temperature is 7-20 DEG C2Fluid is to step (S3) institute
The oleoresin ginger crude product stated is extracted, and second of CO is made2Extract；
(S5) second of heat exchange heating：By second of CO described in step (S4)2Extract carries out heat exchange heating, is formed overcritical
Second of CO of state2Extract；
(S6) rectifying：Under conditions of pressure is 8-12MPa, 35-45 DEG C of temperature, to second of CO of the supercriticality2Extraction
Take liquid to carry out rectifying, obtain oleoresin ginger and volatility light component rich in gingerol；
(S7) second of separation：Under conditions of pressure is 6-8MPa, 35-45 DEG C of temperature, the volatility light component is carried out
Separation, obtains ginger essential oil and low-pressure supercritical CO2Fluid.
2. low-pressure supercritical CO according to claim 12Extract and separate ginger essential oil and the side rich in gingerol oleoresin ginger
Method, it is characterised in that in step (S1), the particle diameter of the ginger powder is 2-3 ㎜.
3. low-pressure supercritical CO according to claim 12Extract and separate ginger essential oil and the side rich in gingerol oleoresin ginger
Method, it is characterised in that in step (S2), the first time CO of the supercriticality2The temperature of extract is 31-45 DEG C.
4. low-pressure supercritical CO according to claim 12Extract and separate ginger essential oil and the side rich in gingerol oleoresin ginger
Method, it is characterised in that in step (S5), second of CO of the supercriticality2The temperature of extract is 31-45 DEG C.
5. low-pressure supercritical CO according to claim 12Extract and separate ginger essential oil and the side rich in gingerol oleoresin ginger
Method, it is characterised in that the low-pressure supercritical CO for obtaining step (S3) and step (S7)2Fluid is cooled down, increased successively
High pressure low temperature CO after pressure described in forming step (S1)2Fluid, is recycled.
6. a kind of system for implementing any one of claim 1-4 methods described, it is characterised in that set gradually bag along technique distance
Include extraction equipment (1), heat exchange heat riser (2), rectifying column (4), knockout tower (7)；
The top of the extraction equipment (1) sets extract outlet, and bottom sets CO2Fluid-infusing port；
The top of the heat exchange heat riser (2) connects setting with the extract outlet；
The bottom of the rectifying column (4) by the first connecting tube connects setting with the bottom of the heat exchange heat riser (2), described
First valve (3) is set in the first connecting tube；
The top of the knockout tower (7) sets CO respectively2Extract import and volatility light component import, top set overcritical
CO2Fluid discharge outlet, bottom sets material outlet；The CO2Extract import and the bottom of the heat exchange heat riser (2)
Connected and set by the second connecting tube, the second valve (6) is set in second connecting tube；The volatility light component import with
The top of the rectifying column (4) is connected by the 3rd connecting tube and set, and the 3rd valve (5) is set in the 3rd connecting tube.
7. system according to claim 6, it is characterised in that the rectifying column (4) sets gradually the first essence from the bottom to top
Evaporate unit, the second rectification cell, the 3rd rectification cell and the 4th rectification cell, first rectification cell, the second rectification cell,
The rectification temperature of 3rd rectification cell and the 4th rectification cell is incremented by successively.
8. system according to claim 6, it is characterised in that also including surge tank (8), the top of the surge tank (8)
With the supercritical CO of the knockout tower (7)2Fluid discharge outlet connection is set, and the bottom of the surge tank (8) is filled with the extraction
Put the CO of (1)2Fluid-infusing port is connected by the 4th connecting tube and set, and force (forcing) pump is set in the 4th connecting tube.
9. system according to claim 8, it is characterised in that the force (forcing) pump is high-pressure plunger pump (9).
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| CN106083548B (en) * | 2016-06-22 | 2018-11-30 | 湖南科技学院 | A kind of method of microwave auxiliary extraction rhizoma zingiberis gingerol |
| CN107663475A (en) * | 2017-09-28 | 2018-02-06 | 江永百润福天然植物科技发展有限公司 | A kind of preparation method and ginger essential oil that ginger essential oil is extracted from ginger |
| CN107699353B (en) * | 2017-09-29 | 2020-07-03 | 晨光生物科技集团股份有限公司 | Continuous distillation process |
| CN109693289A (en) * | 2019-01-22 | 2019-04-30 | 常州双元职业技能培训中心 | A kind of preparation method of mildew preventing agent for wood |
| CN109762662B (en) * | 2019-03-13 | 2021-12-28 | 陈世湘 | Physical method for extracting oleoresin by using natural essential oil of the same type as plant to be extracted to replace chemical solvent |
| 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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