CN107418722A - Use supercritical CO2Extract Rosa roxburghii seed oil - Google Patents
Use supercritical CO2Extract Rosa roxburghii seed oil Download PDFInfo
- Publication number
- CN107418722A CN107418722A CN201710350524.7A CN201710350524A CN107418722A CN 107418722 A CN107418722 A CN 107418722A CN 201710350524 A CN201710350524 A CN 201710350524A CN 107418722 A CN107418722 A CN 107418722A
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- rosa roxburghii
- temperature
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- pressure
- seed oil
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Classifications
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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
-
- 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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Fats And Perfumes (AREA)
Abstract
One kind supercritical CO2Rosa roxburghii seed oil is extracted, takes the Rosa roxburghii seed after pulverizing and sieving to load supercritical CO2In extraction kettle, controlled by system, CO2It is driven into supercritical CO2In extraction kettle, extraction kettle and separating still temperature and pressure are controlled, starts the cycle over extraction, collects oil product.One kind supercritical CO is provided2The method for extracting Rosa roxburghii seed oil, it is determined that the process conditions such as pressure, temperature are to the yield of Rosa roxburghii seed oil and the influence of quality.Supercritical CO2Extraction has the advantages that the quality that technique is simple, extraction time is short, extraction temperature is low, oily is high, and this method also has the advantages of nonflammable explosive danger, noresidue solvent is green.
Description
Technical field
The present invention relates to the technical field of extraction separating and extracting Rosa roxburghii seed oil, more particularly to one kind supercritical CO2Extraction
Take Rosa roxburghii seed oil.
Background technology
Rosa roxburghii（Rosa Roxburghii Tratt）Also known as send the spring to return, be a kind of perennial fallen leaves bush of Qiang Wei sections,
The Southwest Mountainous Areas such as Yunnan, Sichuan, Guizhou mainly are grown on, it is especially the abundantest with Guizhou resource, and be the distinctive medicine food in China
Dual purpose plant.Rosa roxburghii seed is the seed that fruit of Grossularia burejensis Berger removes pulp.Contain abundant unrighted acid in Rosa roxburghii seed oil, no
It is only edible, also there is the value of medical treatment and health care well.The Rosa roxburghii seed in Rosa roxburghii slag after squeezing is often dropped, often
The harvest yield of year Rosa roxburghii seed is up to 10000t or so, the supercritical CO on Rosa roxburghii seed at present2Abstraction technique there is no document
Report.
The content of the invention
The problems such as developmental research is few, utilization rate is extremely low for Rosa roxburghii seed nutritional value height in above-mentioned background, the present invention
One kind supercritical CO is provided2Extract Rosa roxburghii seed oil.
The purpose of the present invention will be achieved through the following technical solutions：One kind supercritical CO2Rosa roxburghii seed oil is extracted, including
Following steps obtain：
（1）The Rosa roxburghii seed after pulverizing and sieving is taken, is loaded into SCF-CO 2 kettle, sets extraction kettle and separating still
I, separation reactor I I temperature；
（2）To extraction kettle, separation reactor I and separation reactor I I, heated or freezed to reach default temperature；
（3）When kettle, separating still and cold storage tank to be extracted respectively reach design temperature, gas cylinder is opened, CO2 is passed into extraction kettle
In separating still, control valve, extraction kettle and separating still pressure are controlled, when the pressure is reached preset value, close gas cylinder；
（4）Extraction is started the cycle over, stops extraction after certain time, collects product.
Preferably, the step（4）The temperature of middle extraction kettle is 35~50oC。
Preferably, the step（4）20~35MPa of pressure of middle extraction kettle.
Preferably, the step（4）Middle separation reactor I pressure and temperature is 12MPa and 50 DEG C respectively, the pressure of separating still II and
Temperature is 6MPa and 40 DEG C respectively.
Preferably, by the separation I of adjustment pressure, change in ratio of the oil in two separating stills, and separation I
Oleic acid value.
Preferably, by the separation I of adjustment temperature, change in ratio of the oil in two separating stills, and separation I
Oleic acid value.
Preferably, the step（4）In extracting pressure be 25MPa, extraction temperature 50oC, to obtain maximum receipts
Rate.
Preferably, the step（4）In separation I be 15MPa, separation I temperature is 60oC, to obtain maximum yield.
Brief description of the drawings
Fig. 1 is influence curve figure of the extraction temperature of the embodiment of the present invention with pressure dependence to yield value；
Fig. 2 is influence curve figure of the extracting pressure of the embodiment of the present invention with temperature relation to yield value；
Fig. 3 is that influence curve figure of the I pressure to yield is separated in the embodiment of the present invention；
Fig. 4 is that influence curve figure of the I temperature to yield is separated in the embodiment of the present invention；
Influence curve figure of Fig. 5 extracting pressures to oleic acid value；
Influence curve figure of Fig. 6 separation reactor Is pressure to acid number.
Embodiment
The following examples are that the present invention is described in further detail.
Embodiment 1
Supercritical CO2Extract the technological process of Rosa roxburghii seed oil：The Rosa roxburghii seed 200g after pulverizing and sieving is taken, is loaded into the super of 1L
Critical CO2In extraction kettle.Extraction kettle and separation reactor I, separation reactor I I temperature are set, and is heated or freezed to reach pre-
If temperature.When kettle, separating still and cold storage tank to be extracted respectively reach design temperature, gas cylinder, CO are opened2Through cold storage tank quilt
Squeeze into extraction kettle and separating still, control valve, control extraction kettle and separating still pressure, when the pressure is reached preset value, close
Gas cylinder, start the cycle over extraction.Stop extraction, collection material after certain time.
The yield calculation formula of Rosa roxburghii seed oil is as follows：
The quality of oil yield %=oil and grease extracting/Rosa roxburghii seed charge * 100
Extraction and influence of the separation condition to Rosa roxburghii seed oil acid number：Acid number in grease is also known as acid value, is grease deterioration journey
The index of degree.It represents to neutralize the potassium hydroxide in 1g greases needed for free fatty（KOH）Milligram number.In microorganism, enzyme
In the presence of heat, slowly hydrolysis occurs for grease, produces free fatty, and free fatty is dissolved in oil, causes acid value to raise.
In theory, the acid value of grease is more low-quality better.Therefore, the acid number of grease is also one of Optimized Extraction method condition foundation.
The investigation of Rosa roxburghii seed oil extracting process：Extracting pressure, extraction temperature, separation I pressure and separation I are chosen in this experiment
Temperature etc. is variable, using yield and acid number as evaluation index, carries out single factor exploration experiment.On the basis of experiment of single factor
On, using the method for orthogonal experiment, the supercritical extraction process of Rosa roxburghii seed oil is optimized.
The Rosa roxburghii seed oil supercritical extract single factor test table of table 1
Embodiment 2：Influence of the extracting pressure to oil yield
Different extraction temperatures have been investigated in this experiment（30oC、40oC、50oC）Under, influence of the extracting pressure to yield（Process conditions：
Feed intake 200g；Separation reactor I pressure 12MPa, temperature 50oC；Separation reactor I I pressure 6MPa, temperature 40oC）.As a result as shown in figure 1,
Under the conditions of extraction temperature is 30 DEG C and 40 DEG C, with the increase of pressure, yield gradually increases；It is 50 DEG C of bars in extraction temperature
Under part, when pressure is less than 30MPa, yield reduces with the increase of pressure, and after pressure increases to 30MPa, yield is with pressure
Amount of decrease increase.
Embodiment 3：Influence of the extraction temperature to oil yield
Different extracting pressures have been investigated in this experiment（20MPa、25MPa、30MPa）Under, influence of the extraction temperature to yield（Technique bar
Part：Feed intake 200g；Separation reactor I pressure 12MPa, temperature 50oC；Separation reactor I I pressure 6MPa, temperature 40oC）.As a result such as Fig. 2 institutes
Show, under the conditions of extracting pressure is 20MPa and 25MPa, extraction temperature is less than 45oDuring C, with the rise of temperature, yield be by
Gradually reduce, when extraction temperature reaches 45oAfter C, with the rise of temperature, yield gradually increases；When extracting pressure is 30MPa
Condition, yield shows first to raise with the rise of temperature to be reduced afterwards, then elevated trend again.
Embodiment 4：Influence of the separation reactor I pressure to oil yield
It is 40 that this experiment, which has been investigated in extraction temperature,oC, under the conditions of extracting pressure is 30MPa, shadow of the separation reactor I pressure to yield
Ring（Process conditions：Feed intake 200g；Separation reactor I temperature 50oC；Separation reactor I I pressure 6MPa, temperature 40oC）.As a result it is as shown in Figure 3：
With the increase of separation reactor I pressure, yield gradually reduces, and when reason is separation reactor I pressure rise, carbon dioxide is dividing
There is higher solvability from kettle I, prevent more oil from parsing, so from separation reactor I parse oil just compared with
It is few.
Embodiment 5：Influence of the separation reactor I temperature to oil yield
It is 40 that this experiment, which has been investigated in extraction temperature,oC, under the conditions of extracting pressure is 30MPa, shadow of the separation reactor I temperature to yield
Ring（Process conditions：Feed intake 200g；Separation reactor I pressure 12MPa；Separation reactor I I pressure 6MPa, temperature 40oC）.As a result such as Fig. 4 institutes
Show：With the rise of separation reactor I temperature, yield is to gradually rise, when temperature reaches 50oDuring C, yield reaches maximum, and temperature surpasses
Cross 50oAfter C, oil yield gradually lowers with the rise of temperature.When reason is that separation reactor I temperature is low, supercritical carbon dioxide
The density increase of fluid, its solubility to solute are big so that grease is not easy to parse from separation reactor I.When the temperature of separation reactor I
When spending high, supercritical carbon dioxide fluid is limited to the solvability of solute so that the grease of dissolving is less.Experimental data shows
Show, when separation reactor I temperature is 50oDuring C, the oil yield parsed is higher.
Embodiment 6：Influence of the extracting pressure to oleic acid value
This experimental study is under identical separation condition, extraction temperature 30oC、40oC、50oUnder the conditions of C, different extracting pressures
The influence for having acid number to separation reactor I.As a result as shown in figure 5, as seen from the figure, under the conditions of different extracting pressures, extraction is warm
Spend for 50oDuring C, acid number overall variation is little.It is 30 DEG C and 40 in extraction temperatureoUnder the conditions of C, separation reactor I pressure rises to 25MPa
Afterwards, the trend that acid number is gradually increasing with the rise presentation of pressure.
Embodiment 7：Influence of the separation reactor I pressure to acid number
Under this experimental study identical extraction conditions, influence of the different separation reactor I pressure to the oleic acid value of separation reactor I.By Fig. 6
Understand, the oleic acid value of separation reactor I raises with the increase of separation reactor I pressure.
Embodiment 8：The orthogonal test of supercritical extract
This experiment has investigated four extracting pressure, extraction temperature, separation reactor I pressure and separation reactor I temperature factors respectively at four
Orthogonal experiment is carried out under level conditions, investigates the supercritical CO of optimal Rosa roxburghii seed oil2Extraction process.As a result it is as shown in table 2.
Range analysis is as shown in table 3.As shown in Table 3, for yield：RD>RC>RB>RA, i.e. influence of four factors to yield be suitable
Sequence is：Extracting pressure>Extraction temperature>Separation reactor I pressure>Separation reactor I temperature；For acid number： RB>RC>RD>RA, i.e., four
Individual factor to acid number influence order be：Extracting pressure>Extraction temperature>Separation reactor I pressure>Separation reactor I temperature.Consider receipts
Rate and acid number, the optimum process condition of selection are：Extracting pressure 25PMa, extraction temperature 50oC, separation reactor I pressure 15PMa and point
From kettle I temperature 60oC。
The orthogonal test table of table 2
The range analysis table of table 3
Makings chromatography
Makings chromatography is carried out to the Rosa roxburghii seed oil under Optimal technique process in embodiment 8, method and result are as follows：
Analytical instrument：TRACE 1300-ISQ gas chromatography-mass spectrometries（U.S. Thermo Fisher Scientific are public
Department）；The phenyl polysilane elastic quartz capillary tube of TR-5MS types 5%（60m×0.25mm×0.25μm）.
Analysis condition：Post initial temperature 80oC, retain 2min, with 5oC/min heating rates rise to 200oC, retain 5min, with
1.5oC/min heating rates rise to 280oC, retain 10min.Injection port 280oC, split ratio 10：1, carrier gas is helium, flow velocity
1.0ml/min, the μ L of sample size 1.280 DEG C of transfer tube temperature；EI ion guns, 250 DEG C of ion source temperature；Full scan, scanning range：
m/z 28-650u。
Sample treatment：Take 200g oily, be placed in 25mL volumetric flask, add 2mL ether：N-hexane（2:1）Mixed solvent,
2mL absolute methanols are added, then add the methanol solution of 2mL 0.8mol/L potassium hydroxide,（Fat oil and all reagents
Anhydrous sodium sulfate drying is first used using preceding）, 10min is vibrated, adds water to scale, GC/MS points are carried out with syringe Aspirate supernatant
Analysis.Analysis result is as shown in table 4.
The GC-MS constituent analyses of table 4
As seen from the above table, the unrighted acid species in Rosa roxburghii seed oil is various, main unsaturated acids composition be palmitic acid,
Linoleic acid, leukotrienes.
Claims (8)
1. one kind supercritical CO2Extract Rosa roxburghii seed oil, it is characterised in that：Obtained by following steps：
1）Take the Rosa roxburghii seed after pulverizing and sieving, be loaded into SCF-CO 2 kettle, set extraction kettle and separation reactor I,
Separation reactor I I temperature；
2）To extraction kettle, separation reactor I and separation reactor I I, heated or freezed to reach default temperature；
3）When kettle, separating still and cold storage tank to be extracted respectively reach design temperature, gas cylinder is opened, CO2 is passed into extraction kettle
In separating still, control valve, extraction kettle and separating still pressure are controlled, when the pressure is reached preset value, close gas cylinder；
4）Extraction is started the cycle over, stops extraction after certain time, collects product.
2. use SCF-CO 2 Rosa roxburghii seed oil as claimed in claim 1, it is characterised in that：Extraction temperature be 35~
50oC。
3. use SCF-CO 2 Rosa roxburghii seed oil as claimed in claim 1, it is characterised in that：Extracting pressure be 30~
45MPa。
4. use SCF-CO 2 Rosa roxburghii seed oil as claimed in claim 1, it is characterised in that：Separate I pressure be 9~
15MPa。
5. use SCF-CO 2 Rosa roxburghii seed oil as claimed in claim 1, it is characterised in that：Separate I temperature be 40~
60oC。
6. use SCF-CO 2 Rosa roxburghii seed oil as claimed in claim 1, it is characterised in that：Separation reactor I pressure and temperature
It is 12MPa and 50 DEG C respectively, the pressure and temperature of separating still II is 6MPa and 40 DEG C respectively.
7. use SCF-CO 2 Rosa roxburghii seed oil as claimed in claim 1, it is characterised in that：Extraction time is 2h.
8. use SCF-CO 2 Rosa roxburghii seed oil as claimed in claim 1, it is characterised in that：Pass through the separation reactor I of adjustment
Pressure, change oil two separating stills ratio and quality, and oil two separating stills oleic acid value；Extracting pressure
25MPa, 50 DEG C of extraction temperature, to obtain maximum yield；Unrighted acid total amount in Rosa roxburghii seed oil is set to be no less than 80%,
Linolenic acid content is higher than more than 10%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108294969A (en) * | 2018-02-06 | 2018-07-20 | 浙江树人学院 | A kind of natural activity pears seed oil face cream and preparation method thereof |
| CN109329857A (en) * | 2018-11-28 | 2019-02-15 | 贵州宏财聚农投资有限责任公司 | A kind of preparation method of Rosa roxburghii Tratt essential oil |
| CN116590091A (en) * | 2023-05-11 | 2023-08-15 | 山东省葡萄研究院 | Grape seed oil extraction method and extraction device |
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| CN108294969A (en) * | 2018-02-06 | 2018-07-20 | 浙江树人学院 | A kind of natural activity pears seed oil face cream and preparation method thereof |
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Application publication date: 20171201 |