CN108795563A - A kind of supercritical CO2The method of extraction of oil from grape seeds - Google Patents
A kind of supercritical CO2The method of extraction of oil from grape seeds Download PDFInfo
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- CN108795563A CN108795563A CN201810697790.1A CN201810697790A CN108795563A CN 108795563 A CN108795563 A CN 108795563A CN 201810697790 A CN201810697790 A CN 201810697790A CN 108795563 A CN108795563 A CN 108795563A
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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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
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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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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- Engineering & Computer Science (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The invention belongs to supercritical extraction technique field, a kind of supercritical CO2The method of extraction of oil from grape seeds.This method includes：(1) prepare：Grape pip is placed in extraction kettle, setting extraction temperature is 30-40 DEG C and extracting pressure is 25Mpa；After opening the white fog of bus-bar discharge, by CO2Gas passes through the condenser of bus-bar, clarifier, temperature no more than 10 DEG C, main pump, mixer, is passed into the extraction kettle successively；(2) static extracting：The temperature and pressure of kettle to be extracted reach setting value to it is constant when, carry out static extracting 2h；(3) dynamic extraction：After step (2), opening and sequentially connected first separating still of extraction kettle and the second separating still, and the first separating still is connected to bus-bar, carry out dynamic extraction 0.5h.This method has environmentally friendly, energy saving, safe；The yield for the grape seed oil being obtained by extraction by this method is high, environmentally protective, purity is high.
Description
Technical field
The invention belongs to supercritical extraction technique fields, specifically, being related to a kind of supercritical CO2Extraction of oil from grape seeds
Method.
Background technology
Grape is most of all to apply in liquor industry other than directly being eaten by people as fruit.As people live
Level is continuously improved, and Grape Wine Industry is grown rapidly, and people are continuously increased the demand of grape wine, if Portugal is made by an enterprise
The annual production capacity of grape wine has reached 150,000, will just have 2.25 ten thousand tons of skin slag every year, and grape pip is brewing industry residue
Main component be not only a kind of pollution to environment, more if equally disposed these by-products as common rubbish
It is a kind of waste to resource.It is gradually exploited with the researching value of grape pip, grape pip is considered as by more and more scholars
The resource mislayed is also gradually being unfolded for extracting the research of active ingredient of grape pip.Moreover, grape seed oil is eating
Product, health care and beauty industry can all be applied.Therefore, the active ingredient in grape pip is carried out adequately extracting and processing profit
Meaning is very great, and the contradiction of grease oil plant shortage is not only enable effectively to solve in this way, at the same also avoid waste and
Pollution.Therefore, extraction of oil from grape seeds has very high significance.
In the prior art, mechanical pressing method or extraction method are mostly used to extract grape seed oil.However, passing through squeezing
Method leads gained oil plant original comprehensive resource utilization rate.In extraction method, easily there is dissolvent residual in product, during recycling design
The ingredient of grape seed oil may be destroyed, easily loss oil is natural flavour mountaineous, destroys unsaturated fatty acid, influences yield, return simultaneously
That receives is costly, influences economic benefit, dissolvent residual pollution problem is also inevitable, and there is also some security risks for solvent.
Invention content
For deficiency above-mentioned in the prior art, the first object of the present invention is the provision of a kind of supercritical CO2Extraction
The method of grape seed oil；This method has environmentally friendly, energy saving, safe；Pass through the production for the grape seed oil that this method is obtained by extraction
Rate is high, environmentally protective, purity is high.
In order to achieve the above object, the solution that the present invention uses is：
A kind of supercritical CO2The method of extraction of oil from grape seeds, including：
(1) prepare：Grape pip is placed in extraction kettle, setting extraction temperature is 30-40 DEG C and extracting pressure is 25Mpa；
After opening the white fog of bus-bar discharge, by CO2Gas passes through the condensation that bus-bar, clarifier, temperature are not more than 10 DEG C successively
Device, mixer, is passed into the extraction kettle main pump；(2) static extracting：The temperature and pressure of kettle to be extracted reach setting value
When extremely constant, static extracting 2h is carried out；(3) dynamic extraction：After step (2), open and extraction kettle sequentially connected first
Separating still and the second separating still, and the first separating still is connected to bus-bar, carry out dynamic extraction 0.5h.
A kind of supercritical CO provided by the invention2The advantageous effect of the method for extraction of oil from grape seeds is：
Supercritical CO provided by the invention2The method of extraction of oil from grape seeds, is extracted using supercritical carbon dioxide extraction method
Take the grape seed oil containing unsaturated fatty acid.This method has the following advantages：Pass through the adjusting to extraction temperature, extracting pressure
So as to obtain higher grape seed oil extraction yield.Whole process is environmentally friendly, energy saving, safe.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Below to a kind of supercritical CO provided in an embodiment of the present invention2The method of extraction of oil from grape seeds is specifically described.
A kind of supercritical CO2The method of extraction of oil from grape seeds, including：
(1) prepare：The valve on all entire extracting systems is closed, by addition than being 3-50g：The grape pip of 200ml
And entrainer, it is further 40g：200ml is placed in extraction kettle.It should be noted that in the present embodiment, entrainer energy
Enough improve the selectivity of solute；Change the critical parameters of solvent；Solute solubility is improved to temperature, the sensitivity of pressure；It carries
Height is intended to solubility of the extract in supercritical fluid.In the present embodiment, it is 2-4 that entrainer, which includes further mass ratio,：
The acetone and water of 6-8；Further it is 3：7, it is matched using this kind, gained yield higher.It should be noted that grape pip exists
By crushing before being put into extraction kettle, to reach better effect of extracting.
Inventor creatively has found that the solvability of supercritical fluid is directly proportional to density, in Near The Critical Point, pressure
It varies slightly, density will generate relatively large variation.Thus, the extract in most liquid or solid is come
It says, if extract can not reach infinitely dissolve with solvent, then proves that the solvability of supercritical fluid and pressure have
Larger contact.Meanwhile being changed with the change of extract by the range of pressure influence.Furthermore, it is necessary to examine rate to it is many because
Element, for example keep the safety in production, the tolerance situation etc. of cost and equipment.It therefore, cannot be in order to improve in actual production operation
Yield should consider the resource of whole device parameter and product without the raising reaction pressure of limitation.In this reality
It applies in example, further, setting extracting pressure is 25Mpa.In the present embodiment, the temperature of extraction also can cause shadow to yield
It rings, in the present embodiment, further, setting extraction temperature is 30-40 DEG C, is further 35 DEG C.Then bus-bar is opened
The white high pressure fog of discharge, can be confirmed that equipment is ready, by CO at this time2Gas passes through bus-bar, net successively from gas cylinder
Change the condenser of device, temperature no more than 10 DEG C, main pump, mixer, be passed into extraction kettle.
(2) static extracting：The temperature and pressure of kettle to be extracted reach setting value to it is constant when, carry out static extracting 2h.
(3) dynamic extraction：The constant-flux pump being connect with mixer is opened after step (2), makes entrainer and CO2Gas exists
Fluid-mixing is mixed to form in mixer；Then fluid-mixing is in CO2Extraction kettle is entered back under gas effect to carry out grape pip
Supercritical extract；It opens and sequentially connected first separating still of extraction kettle and the second separating still；By adjusting the first separating still
Switch size adjusts the pressure in the first separating still to stabilization；Fluid-mixing enters entrainment of extract in the first separating still,
And CO is made by cooling and decompression wherein2Nominal gas is reverted to, so that entrainer is reverted to liquid, extract is with liquid
Entrainer stay among the first separating still；At this point, adjusting the second separating still by adjusting the switch size of the second separating still
In pressure to stabilization；Without detaching complete CO in the first separating still2Gas and the liquid solvent for having carried extract secretly, into
Enter into the second separating still and be kept completely separate, the first separating still is connected to bus-bar, carries out dynamic extraction 0.5h.
(4) it detaches：Extract taking-up in first separating still and the second separating still is put into round-bottomed flask, to round-bottomed flask
It is heated, entrainer connects by being reached after the still head, condenser pipe, reception pipe that are sequentially connected to round-bottomed flask in a gaseous form
It receives bottle to be received, remaining in round-bottomed flask is then the grape seed oil after separation.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1-3
Present embodiments provide a kind of supercritical CO2The method of extraction of oil from grape seeds, including：
(1) prepare：Grape pip is placed in extraction kettle, setting extraction temperature is respectively 30 DEG C, 35 DEG C, 40 DEG C and extraction pressure
Power is 25Mpa；After opening the white fog of bus-bar discharge, by CO2Gas passes through bus-bar, clarifier, temperature and is not more than successively
10 DEG C of condenser, mixer, is passed into the extraction kettle main pump；(2) static extracting：The temperature and pressure of kettle to be extracted
Reach setting value to it is constant when, carry out static extracting 2h；(3) dynamic extraction：After step (2), open with extraction kettle successively
The first separating still and the second separating still of connection, and the first separating still is connected to bus-bar, carry out dynamic extraction 0.5h.
Embodiment 4-6
Present embodiments provide a kind of supercritical CO2The method of extraction of oil from grape seeds, including：
(1) prepare：By addition than being 40g：The grape pip and entrainer of 200ml is placed in extraction kettle, and extraction temperature is arranged
Respectively 35 DEG C are 25Mpa with extracting pressure；Entrainer includes that mass ratio is respectively 2：8,3：7,4：6 acetone and water；It opens
After the white fog of bus-bar discharge, by CO2Gas passes through the condenser of bus-bar, clarifier, temperature no more than 10 DEG C, master successively
Pump, is passed into extraction kettle mixer；(2) static extracting：The temperature and pressure of kettle to be extracted reach setting value to it is constant when,
Carry out static extracting 2h；(3) dynamic extraction：The constant-flux pump that is connect with mixer is opened after step (2), make entrainer and
CO2Gas is mixed to form fluid-mixing in a mixer；Then fluid-mixing is in CO2Extraction kettle is entered back into Portugal under gas effect
Grape seed carries out supercritical extract；It opens and sequentially connected first separating still of extraction kettle and the second separating still；By adjusting first
The switch size of separating still adjusts the pressure in the first separating still to stabilization；Fluid-mixing enters first point entrainment of extract
From in kettle, and CO is made by cooling and decompression wherein2Revert to nominal gas, entrainer made to revert to liquid, extract with
The entrainer for liquid stays among the first separating still；At this point, adjusting second by adjusting the switch size of the second separating still
Pressure in separating still is to stabilization；Without detaching complete CO in the first separating still2Gas and the liquid for having carried extract secretly
Solvent is entered in the second separating still and is kept completely separate, and the first separating still is connected to bus-bar, carries out dynamic extraction
0.5h；(4) it detaches：By in the first separating still and the second separating still extract taking-up be put into round-bottomed flask, to round-bottomed flask into
Row heating, entrainer are received by being reached after the still head, condenser pipe, reception pipe that are sequentially connected to round-bottomed flask in a gaseous form
Bottle is received, and remaining in round-bottomed flask is then the grape seed oil after separation.
Comparative example 1
This comparative example provides a kind of supercritical CO2The method of extraction of oil from grape seeds, including：
(1) prepare：Grape pip is placed in extraction kettle, setting extraction temperature is respectively 25 DEG C and extracting pressure is 25Mpa；
After opening the white fog of bus-bar discharge, by CO2Gas passes through the condensation that bus-bar, clarifier, temperature are not more than 10 DEG C successively
Device, mixer, is passed into the extraction kettle main pump；(2) static extracting：The temperature and pressure of kettle to be extracted reach setting value
When extremely constant, static extracting 2h is carried out；(3) dynamic extraction：After step (2), open and extraction kettle sequentially connected first
Separating still and the second separating still, and the first separating still is connected to bus-bar, carry out dynamic extraction 0.5h.
Comparative example 2-3
Present embodiments provide a kind of supercritical CO2The method of extraction of oil from grape seeds, including：
(1) prepare：Grape pip is placed in extraction kettle, setting extraction temperature be 35 DEG C and extracting pressure be respectively 15Mpa,
20Mpa；After opening the white fog of bus-bar discharge, by CO2Gas passes through bus-bar, clarifier, temperature and is not more than 10 DEG C successively
Condenser, main pump, mixer, be passed into the extraction kettle；(2) static extracting：The temperature and pressure of kettle to be extracted reach
Setting value to it is constant when, carry out static extracting 2h；(3) dynamic extraction：After step (2), opening is sequentially connected with extraction kettle
The first separating still and the second separating still, and the first separating still is connected to bus-bar, carries out dynamic extraction 0.5h.
Comparative example 4-8
This comparative example provides a kind of supercritical CO2The method of extraction of oil from grape seeds, including：
(1) prepare：By addition than being 40g：The grape pip and entrainer of 200ml is placed in extraction kettle, and extraction temperature is arranged
Respectively 35 DEG C are 25Mpa with extracting pressure；Entrainer includes that mass ratio is respectively 0：1,1：9,5：5,6：4,7：3 acetone and
Water；After opening the white fog of bus-bar discharge, by CO2It is cold no more than 10 DEG C that gas passes through bus-bar, clarifier, temperature successively
Condenser, mixer, is passed into extraction kettle main pump；(2) static extracting：The temperature and pressure of kettle to be extracted reach setting value extremely
When constant, static extracting 2h is carried out；(3) dynamic extraction：The constant-flux pump being connect with mixer is opened after step (2), makes folder
Band agent and CO2Gas is mixed to form fluid-mixing in a mixer；Then fluid-mixing is in CO2Extraction is entered back under gas effect
Kettle carries out supercritical extract to grape pip；It opens and sequentially connected first separating still of extraction kettle and the second separating still；Pass through tune
The switch size of the first separating still is saved to adjust the pressure in the first separating still to stabilization；Fluid-mixing enters entrainment of extract
In first separating still, and CO is made by cooling and decompression wherein2Nominal gas is reverted to, entrainer is made to revert to liquid, is extracted
Object is taken to be stayed among the first separating still with the entrainer of liquid；At this point, being adjusted by adjusting the switch size of the second separating still
Pressure in the second separating still is saved to stabilization；Without detaching complete CO in the first separating still2Gas and extract is carried secretly
Liquid solvent, enter in the second separating still and be kept completely separate, the first separating still is connected to bus-bar, into Mobile state extract
Take 0.5h；(4) it detaches：Extract taking-up in first separating still and the second separating still is put into round-bottomed flask, to round-bottomed flask
It is heated, entrainer connects by being reached after the still head, condenser pipe, reception pipe that are sequentially connected to round-bottomed flask in a gaseous form
It receives bottle to be received, remaining in round-bottomed flask is then the grape seed oil after separation.
Comparative example 9
This comparative example provides a kind of supercritical CO2The method of extraction of oil from grape seeds, including：
(1) prepare：By addition than being 40g：The grape pip and entrainer of 200ml is placed in extraction kettle, and extraction temperature is arranged
Respectively 35 DEG C are 25Mpa with extracting pressure；Entrainer includes that mass ratio is respectively 3：7 ethyl ketone and water；Open bus-bar row
After going out white fog, by CO2Gas passes through the condenser of bus-bar, clarifier, temperature no more than 10 DEG C, main pump, mixing successively
Device is passed into extraction kettle；(2) static extracting：The temperature and pressure of kettle to be extracted reach setting value to it is constant when, carry out static
Extract 2h；(3) dynamic extraction：The constant-flux pump being connect with mixer is opened after step (2), makes entrainer and CO2Gas exists
Fluid-mixing is mixed to form in mixer；Then fluid-mixing is in CO2Extraction kettle is entered back under gas effect to carry out grape pip
Supercritical extract；It opens and sequentially connected first separating still of extraction kettle and the second separating still；By adjusting the first separating still
Switch size adjusts the pressure in the first separating still to stabilization；Fluid-mixing enters entrainment of extract in the first separating still,
And CO is made by cooling and decompression wherein2Nominal gas is reverted to, so that entrainer is reverted to liquid, extract is with liquid
Entrainer stay among the first separating still；At this point, adjusting the second separating still by adjusting the switch size of the second separating still
In pressure to stabilization；Without detaching complete CO in the first separating still2Gas and the liquid solvent for having carried extract secretly, into
Enter into the second separating still and be kept completely separate, the first separating still is connected to bus-bar, carries out dynamic extraction 0.5h；(4) divide
From：Extract taking-up in first separating still and the second separating still is put into round-bottomed flask, round-bottomed flask is heated, is carried secretly
Agent is received by reaching receiving bottle after the still head, condenser pipe, reception pipe that are sequentially connected to round-bottomed flask in a gaseous form,
Remaining in round-bottomed flask is then the grape seed oil after separation.
Experimental example 1
Experimental method：Embodiment 1-3 and comparative example 1 are set to experimental group 1-4, by the grape pip of experimental group 1-4 through dividing
Analysis balance measurement obtains M1, and the grape seed oil assay balance measurement of experimental group 1-4 is obtained M2, calculates yield V (%)=(M1-
M2)/M1, is shown in Table 1；
The yield of 1 experimental group 1-4 of table
| Group number | 1 | 2 | 3 | 4 |
| M1(g) | 40 | 40 | 40 | 40 |
| M2(g) | 4.2 | 5.15 | 3.73 | 2.49 |
| V (%) | 10.5 | 13 | 9.33 | 6.23 |
From the data in table 1, it can be seen that under the same extracting pressure, with the raising of temperature, the extraction of grape seed oil takes the lead in increasing
It is reduced after adding, at 35 DEG C, extraction yield reaches maximum.It is dual that this, which is primarily due to influence of the temperature to extraction yield,.One side
Face, temperature raising can cause molecular thermalmotion speed to be accelerated, improve supercritical CO2Frequency is contacted with the active principle in material
Rate contributes to solute to spread, to make extraction progress faster, extraction yield increase；Meanwhile temperature raising can also increase substance
Vapour pressure, steam can make supercritical CO after increasing2The solubility of fluid increases, and the solubility of fluid increases, to improve pair
The extraction degree of substance.On the other hand, as the temperature increases, supercritical CO can be caused2Fluid density declines, and in general, surpasses
The bigger dissolving of density of critical fluids is bigger, therefore temperature raising also results in solubility reduction, hinders the progress of extraction, from
And extraction yield is reduced, and temperature is too high may destroy some active materials, can also increase energy consumption and production cost.
Experimental example 2
Experimental method：Embodiment 2 and comparative example 2-3 are set to experimental group 1-3, by the grape pip of experimental group 1-3 through dividing
Analysis balance measurement obtains M1, and the grape seed oil assay balance measurement of experimental group 1-3 is obtained M2, calculates yield V (%)=(M1-
M2)/M1, is shown in Table 2；
The yield of 2 experimental group 1-3 of table
From the data in table 2, it can be seen that when extraction temperature is constant, with the increase of pressure, extraction yield is also increasing.This is because
In one timing of temperature, supercritical fluid is close with the increase of pressure can also increase, this can reduce the mass transfer distance between molecule, carry
Height passs efficiency, keeps intermolecular movement more active, improves the contact rate between molecule, solvent is enable more fully to contact
To solute, the extraction yield of entire extraction process is made to increase, but then, although supercritical CO2Dissolubility with liquid, but
As density enhances, supercritical CO2The viscosity of fluid will increase, and mass transfer speed declines between making molecule, can reduce supercritical CO2Stream
The liquid dissolubility and supercritical CO for the liquid that body has2The selectivity of fluid, causes extracting power to decline.But it on the whole, presses
Power increases, and extraction yield gradually increases.But the variation of the two is not linear relationship.When pressure is relatively low, pressure has increased slightly, extraction
Rate becomes apparent.This is because when low pressure, density is more sensitive to the variation of pressure, and pressure has increased slightly, and density will be notable
Increase, increase so as to cause solute solubility, extraction yield increases；When pressure continues, the increased amplitude of density is then gradually reduced,
The increased amplitude of extraction yield is also gradually reduced.And pressure is too big, can be higher for equipment requirement, it is produced into increase
This, so, it is not that the pressure the high good.
Experimental example 3
Experimental method：It sets embodiment 4-6 and comparative example 4-8 to experimental group 1-8, the grape pip of experimental group 1-8 is passed through
Assay balance measurement obtains M1, and the grape seed oil assay balance measurement of experimental group 1-8 is obtained M2, calculate yield V (%)=
(M1-M2)/M1, is shown in Table 3；
The yield of 3 experimental group 1-8 of table
| Group number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 |
| M1(g) | 40 | 40 | 40 | 40 | 40 | 40 | 40 | 40 |
| M2(g) | 7.72 | 10.91 | 6.90 | 4.99 | 6.95 | 6.67 | 5.70 | 5.10 |
| V (%) | 19.30 | 27.28 | 17.25 | 12.48 | 17.38 | 16.68 | 14.25 | 12.75 |
From the data in table 3, it can be seen that in extraction temperature and constant pressure, extraction yield is first increased with entrainer ratio and is reduced afterwards,
With the mass ratio of acetone and water for 3：7 yield is best.This is because a small amount of addition of entrainer can substantially change SCF systems
Phase behavior increases solubility of the Cucumber in SCF.In general, entrainer influences solute overcritical in terms of two
Solubility in fluid and selectivity：First, the density of solvent；Second is that the interaction between solute and entrainment agent molecule.Entrainment
A small amount of addition of agent is little to the Effects of Density of supercritical fluid, or even can also make the reduction of supercritical solvent density, works as entrainer
After ratio reaches certain value, solubility of the solute in supercritical fluid and selectivity can significantly improve；After entrainer is added, mix
The critical point of bonding solvent will produce variation, and the solubility of solute is influenced to increased in degree by temperature, pressure change,
To make extraction yield increase.Increasing with the ratio of acetone, extraction yield is begun to decline, this is because some existing alcohol are molten
Property impurity or the strong ingredient stripping quantity of close matter increase, and grape seed oil forms combination of the competitive relation with alcohol-water molecule,
Decline so as to cause extraction yield.Although the use of entrainer can improve extraction yield, its addition can remain some entrainers
Ingredient needs to increase equipment when increasing the entrainer in separating step, or even recycling residue, increases energy consumption in extract.
Experimental example 4
Experimental method：Embodiment 5 and comparative example 9 are set to experimental group 1-2, by the grape pip of experimental group 1-2 through analysis
Balance measurement obtains M1, and the grape seed oil assay balance measurement of experimental group 1-2 is obtained M2, calculates yield V (%)=(M1-
M2)/M1, is shown in Table 4；
The yield of 4 experimental group 1-2 of table
| Group number | 1 | 2 |
| M1(g) | 40 | 40 |
| M2(g) | 10.91 | 5.96 |
| V (%) | 27.28 | 14.90 |
It can be obtained by table 1, under the ratio of identical ethyl alcohol and acetone, the yield that entrainer is done using acetone is higher than
Ethyl alcohol does the ratio of entrainer.
Experimental example 5
Experimental method：The grape pip that will be obtained using embodiment 2, embodiment 5, comparative example 9, squeezing method and extraction method
Oil is set as experimental group 1-5, and the oil yield of experimental group 1-5 is shown in Table 5；
The yield of 5 experimental group 1-5 of table
| Group number | 1 | 2 | 3 | 4 | 5 |
| Oil yield (%) | 13 | 27.28 | 14.90 | 5.10 | 7.12 |
It can be obtained by table 5, the oil yield of traditional extraction method is significantly lower than supercritical CO2Extraction, and traditional extraction
Taking method, there is also problem of solvent residual.In the presence of having entrainer simultaneously, the extraction yield of grape seed oil significantly improves.
In conclusion using supercritical CO provided by the invention2The method of extraction of oil from grape seeds：This method have environmental protection,
It is energy saving, safe；The yield for the grape seed oil being obtained by extraction by this method is high, environmentally protective, purity is high.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of supercritical CO2The method of extraction of oil from grape seeds, it is characterised in that：Including：
(1) prepare：Grape pip is placed in extraction kettle, setting extraction temperature is 30-40 DEG C and extracting pressure is 25Mpa；It opens
After the white fog of bus-bar discharge, by CO2Gas is not more than 10 DEG C of condensation by the bus-bar, clarifier, temperature successively
Device, mixer, is passed into the extraction kettle main pump；
(2) static extracting：When the temperature of the extraction kettle and pressure reach setting value to it is constant when, carry out static extracting 2h；
(3) dynamic extraction：After step (2), opening is detached with sequentially connected first separating still of the extraction kettle and second
Kettle, and first separating still is connected to the bus-bar, carry out dynamic extraction 0.5h.
2. supercritical CO according to claim 12The method of extraction of oil from grape seeds, it is characterised in that：Step (1) further includes
Entrainer is added in the extraction kettle；The addition of the grape pip and the entrainer is compared for 3-5g：200ml；The entrainment
Agent includes that mass ratio is 2-4：The acetone and water of 6-8.
3. supercritical CO according to claim 22The method of extraction of oil from grape seeds, it is characterised in that：Step (3) further includes：
Before opening first separating still and second separating still, the constant-flux pump being connect with the mixer is opened, the folder is made
Band agent and CO2Gas is mixed to form fluid-mixing in the mixer；Then the fluid-mixing is in CO2Under gas effect again
Supercritical extract is carried out to grape pip into the extraction kettle；Described the is adjusted by adjusting the switch size of the first separating still
Pressure in one separating still is to stabilization；The fluid-mixing enters entrainment of extract in first separating still, and wherein
By cooling and decompression, make CO2Revert to nominal gas, the entrainer made to revert to liquid, extract with liquid institute
Entrainer is stated to stay among first separating still；At this point, adjusting described the by adjusting the switch size of the second separating still
Pressure in two separating stills is to stabilization；Without detaching complete CO in first separating still2Gas and extract is carried secretly
Liquid solvent, enter in second separating still and be kept completely separate.
4. supercritical CO according to claim 32The method of extraction of oil from grape seeds, it is characterised in that：Further include：(4) divide
From：Extract taking-up in first separating still and second separating still is put into round-bottomed flask, to the round-bottomed flask
It is heated, the entrainer passes through the still head, condenser pipe, reception pipe for being sequentially connected to the round-bottomed flask in a gaseous form
It reaches receiving bottle afterwards to be received, remaining in the round-bottomed flask is then the grape seed oil after separation.
5. supercritical CO according to claim 22The method of extraction of oil from grape seeds, it is characterised in that：The entrainer includes
Mass ratio is 3：7 acetone and water.
6. supercritical CO according to claim 12The method of extraction of oil from grape seeds, it is characterised in that：The extraction temperature is
35℃。
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| CN111484897A (en) * | 2020-05-21 | 2020-08-04 | 浙江师范大学 | Method for circularly extracting grape seed oil by carbon dioxide expansion ethanol |
| CN112410117A (en) * | 2020-11-11 | 2021-02-26 | 海南省粮油科学研究所 | Extraction method of green cumquat seed oil |
| CN112450308A (en) * | 2020-10-22 | 2021-03-09 | 洛阳红牡丹产业科技发展有限公司 | Method for preparing peony seed oil filled chocolate candy |
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