CN108559635A - A kind of extraction process of perilla herb oil - Google Patents
A kind of extraction process of perilla herb oil Download PDFInfo
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- CN108559635A CN108559635A CN201810535059.9A CN201810535059A CN108559635A CN 108559635 A CN108559635 A CN 108559635A CN 201810535059 A CN201810535059 A CN 201810535059A CN 108559635 A CN108559635 A CN 108559635A
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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
- C11B9/025—Recovery by solvent extraction
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Abstract
The invention discloses a kind of extraction processes of perilla herb oil, belong to extraction of essential oil technical field, include the following steps：（1）Perilla leaf crushes, and obtains purple perilla powder；（2）Purple perilla powder is placed in extraction kettle, the digestion agent of 25 times of weight is added, is extracted using subcritical butane, obtains extract liquor；（3）Extract liquor carries out isolated solvent and purple perilla miscella, and solvent recovery enters solvent tank, collects purple perilla miscella and obtains perilla herb oil after further treatment.By improving extraction process, Fructus Perillae quintessence oil loss is few, and recovery rate is high.
Description
Technical field
The present invention relates to extraction of essential oil technical fields, more particularly, to a kind of extraction process of perilla herb oil.
Background technology
Purple perilla, property and flavor of peppery and warm have purple perilla fragrance, are mainly used for medicine and food industry.Wherein in perilla herb oil also
Containing abundant alpha-linolenic acid, there is significant health-care effect and medical efficacy to human body.Perilla herb oil in the prior art carries
Taking technique has cold pressing technique, supercritical fluid extraction technique etc..
China Patent Publication No. CN106135466A discloses a kind of perilla herb oil high efficiency extraction technique, includes the following steps：Step
Rapid 1：Through drying or drying after purple perilla seed harvesting, moisture content of kernels is made to be less than 8%；Picking of raw material is cleaned, seed cleanliness is made to reach
99% or more；Step 2：Single pressing extraction is carried out using double helix cold pressing expeller；Step 3：The crude oil that step 2 is obtained through precipitation,
It obtains once extracting oil product after refined filtration；Step 4：The grouts that step 2 obtains are crushed, 40 mesh sieve are crossed, into overcritical extraction
It takes system to carry out twice pressing to extract to obtain second extraction oil product；Step 5：By extracting twice, fat residue in grouts is obtained
Rate is less than 2%.The invention combines the advantage and disadvantage of cold-press and supercritical extraction processing technology, recovery rate can reach 98% with
On, but technics comparing is cumbersome, and cost is also relatively high.
Disclosed " response surface optimization of Fructus Perillae quintessence oil microwave extraction process and its change on the college journal of river river such as Lin Mengnan
Learn composition Study ", and the optimal processing parameter for specifically disclosing microwave abstracting is：Using hexamethylene as extractant, microwave power 329
W, 80 s of microwave time, solid-liquid ratio 1：6,56 min of soaking time, net yield 1.783% passes through gas-chromatography-mass spectrum
Combined instrument is analyzed, and 17 kinds of substances in Fructus Perillae quintessence oil is identified, wherein with the content highest of perillaldehyde, limonene.This method
The extractant used is hexamethylene, and the bigger constituents extraction of segment polarity does not come out, and recovery rate is relatively low.
Invention content
In view of this, in view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of extraction process of perilla herb oil, lead to
Improvement extraction process is crossed, Fructus Perillae quintessence oil loss is few, and recovery rate is high.
The technical scheme is that：
A kind of extraction process of perilla herb oil, includes the following steps：
（1）Perilla leaf crushes, and obtains purple perilla powder；
（2）Purple perilla powder is placed in extraction kettle, the digestion agent of 2-5 times of weight is added, is extracted, is obtained using subcritical butane
Extract liquor；
（3）Extract liquor carries out isolated solvent and purple perilla miscella, and solvent recovery enters solvent tank, collects purple perilla miscella,
After further treatment, perilla herb oil is obtained.
Further, the step（2）Middle digestion agent is soybean oil.
Further, the step（2）Middle digestion agent is petroleum ether：Ethyl alcohol：Soybean oil is by weight 1：1-3：9 mixing and
At.
Further, the step（2）In extraction temperature be 55-60 DEG C, extracting pressure 0.9-1.1MPa, when extraction
Between be 5-8h.
Further, the step（2）Middle extraction step is：When extraction kettle pressure rises to 0.9-1.1MPa, 1- is maintained
3min, then pressure release to normal pressure；Continue to boost to 0.9-1.1MPa later, extracts 5-8h.
Further, the step（1）The moisture of middle perilla leaf is 7-9%.
Further, the step（1）In crushing be at -50~-90 DEG C progress low-temperature grinding, the grain size after crushing
For 30-50 mesh.
Further, the step（1）In crushing be first to cool the temperature to -50~-90 DEG C, at the uniform velocity risen with 2 DEG C/min
It warms to room temperature, carries out low-temperature grinding at -50~-90 DEG C later, the grain size after crushing is 30-50 mesh.
Further, step（3）In be further processed include into grease add 0.1-0.2% ODO, obtain perilla herb oil
The beneficial effects of the invention are as follows：
1, the present invention discloses a kind of extraction process of perilla herb oil, is optimized by disintegrating process, extraction process, can be to greatest extent
Reduction essential oil loss, extraction process is simple, and the perilla herb oil that the application is finally prepared is Fructus Perillae quintessence oil（Extractive of perilla）With
The mixture of soybean oil is yellow oil, and the recovery rate of Fructus Perillae quintessence oil is 4.5-5.8%.
2, the perilla leaf disintegrating process of the application uses low-temperature grinding, and it is -50~-90 DEG C to crush temperature, can be to greatest extent
Reduction essential oil loss；On the other hand -50~-90 DEG C can be first cooled the temperature to, since the water content of purple perilla in the application is
7-9%, purple perilla tissue is interior to be more than surface moisture, organizes interior moisture to freeze at low temperature, forms a large amount of ice crystal grains, cause cell swollen
It is swollen, to damage cell wall；It is to slowly warm up to room temperature later, purple perilla surface temperature is higher than organization internal, in ice crystal fusion process
Pressure difference is formed, cell wall damage is further resulted in；It is crushed to 30-50 mesh at low temperature later, on the one hand can reduce essential oil loss,
On the other hand it can also reach broken wall effect, facilitate subsequent extracted.
When 3, extracting purple perilla using subcritical butane, when not adding soybean oil, final extract is thick grease, the application
Digestion agent is added in extraction, soybean oil is wherein contained in digestion agent, part lubricant component can incorporate soybean in one side purple perilla
In oil, increase the recovery rate of liposoluble constituent in essential oil, and in subsequent separation process, Fructus Perillae quintessence oil is dispersed in soybean oil,
Final products are fluid grease, facilitate subsequent processing；In addition petroleum ether may be used：Ethyl alcohol：Soybean oil is by weight 1：1-3：9
The mixed solvent mixed, since the main component in the Fructus Perillae quintessence oil of the application is olefines and aldehyde（Ketone）Alcohols, wherein
Olefines Polarity comparision is big, and aldehyde（Ketone）Alcohols Polarity comparision is big, and simple solvent extraction can all lead to the loss amount ratio of essential oil
Larger, the application uses petroleum ether：Ethyl alcohol：Soybean oil mixed solvent, can greatly improve in extraction process to polar component and
The recovery rate of nonpolarity element.
4, when extraction kettle pressure is first risen to 0.9-1.1MPa by the application in extraction process, 1-3min is maintained, is then let out
It is depressed into normal pressure, during boosting pressure release, solvent can immerse expansion dissolution in purple perilla tissue, lead to its tissue damaged, have
Help improve the mass transfer dissolution of follow-up derived essential oil.
5, to increase the stability of the application final products, quality is added in the miscella of soybean oil and extractive of perilla
Score is the ODO of 0.1-0.2%（Glycerin, mixed triester with caprylic acid capric acid）, product can be prevented to be layered, stability is more preferable.
Specific implementation mode
With reference to specific embodiment, the invention will be further described.
Embodiment 1
A kind of extraction process of perilla herb oil, includes the following steps：
（1）Perilla leaf low-temperature grinding under the conditions of -50 DEG C, grain size after crushing are 30 mesh, obtain purple perilla powder, wherein perilla leaf
Moisture is 7%；
（2）Purple perilla powder is placed in extraction kettle, the digestion agent soybean oil of 2 times of weight is added, impregnates 30min, vacuum pump is opened, waits for
Pressure in extraction kettle reaches -0.1Mpa, is injected by the solvent butane in the pressure official post solvent tank of extraction kettle and solvent tank
Extraction kettle, under conditions of extraction temperature is 55 DEG C, extracting pressure is 0.9MPa, after extracting 8h, extract liquor enters knockout drum
In；
（3）Extract liquor is in knockout drum, and precipitation detaches 5min, butane point under conditions of temperature is 55 DEG C, pressure is -0.1MPa
Solvent tank is returned to from after, purple perilla miscella is collected from knockout drum outlet valve, is perilla herb oil（The mixing of Fructus Perillae quintessence oil and soybean oil
Object）.
Step（2）Purple perilla powder and butane solid-liquid ratio are 1Kg in extraction process：5L.
The recovery rate of Fructus Perillae quintessence oil is（Perilla herb oil-soybean oil）/ perilla leaf * 100%, the recovery rate in the present embodiment are
4.5%。
Embodiment 2
A kind of extraction process of perilla herb oil, includes the following steps：
（1）Perilla leaf low-temperature grinding under the conditions of -70 DEG C, grain size after crushing are 40 mesh, obtain purple perilla powder, wherein perilla leaf
Moisture is 9%；
（2）Purple perilla powder is placed in extraction kettle, the digestion agent soybean oil of 3 times of weight is added, impregnates 30min, vacuum pump is opened, waits for
Pressure in extraction kettle reaches -0.1Mpa, is injected by the solvent butane in the pressure official post solvent tank of extraction kettle and solvent tank
Extraction kettle, under conditions of extraction temperature is 60 DEG C, extracting pressure is 1.0MPa, after extracting 7h, extract liquor enters knockout drum
In；
（3）Extract liquor is in knockout drum, and precipitation detaches 5min, butane point under conditions of temperature is 55 DEG C, pressure is -0.1MPa
Solvent tank is returned to from after, purple perilla miscella is collected from knockout drum outlet valve, is perilla herb oil（The mixing of Fructus Perillae quintessence oil and soybean oil
Object）.
Step（2）Purple perilla powder and butane solid-liquid ratio are 1Kg in extraction process：5L.
The recovery rate of Fructus Perillae quintessence oil is 4.7% in the present embodiment.
Embodiment 3
A kind of extraction process of perilla herb oil, includes the following steps：
（1）Perilla leaf low-temperature grinding under the conditions of -90 DEG C, grain size after crushing are 50 mesh, obtain purple perilla powder, wherein perilla leaf
Moisture is 8%；
（2）Purple perilla powder is placed in extraction kettle, the digestion agent of 3 times of weight is added, wherein digestion agent is petroleum ether：Ethyl alcohol：Soybean
Oil is by weight 1：1：9 mix, and impregnate 30min, open vacuum pump, and the pressure in kettle to be extracted reaches -0.1Mpa, passes through
Solvent butane in the pressure official post solvent tank of extraction kettle and solvent tank injects extraction kettle, is 65 DEG C, extracts pressure in extraction temperature
Under conditions of power is 1.1MPa, after extracting 5h, extract liquor enters in knockout drum；
（3）Extract liquor is in knockout drum, and precipitation detaches 5min, butane point under conditions of temperature is 55 DEG C, pressure is -0.1MPa
Solvent tank is returned to from after, purple perilla miscella is collected from knockout drum outlet valve, is perilla herb oil（The mixing of Fructus Perillae quintessence oil and soybean oil
Object）.
Step（2）Purple perilla powder and butane solid-liquid ratio are 1Kg in extraction process：5L.
The recovery rate of Fructus Perillae quintessence oil is 5.3% in the present embodiment.
Embodiment 4
A kind of extraction process of perilla herb oil, includes the following steps：
（1）Temperature is down to -60 DEG C before perilla leaf crushes, and room temperature is at the uniform velocity warming up to 2 DEG C/min, carries out low temperature at -60 DEG C later
It crushes, the grain size after crushing is 40 mesh, obtains purple perilla powder, and the wherein moisture of perilla leaf is 8%；
（2）Purple perilla powder is placed in extraction kettle, the digestion agent of 4 times of weight is added, wherein digestion agent is petroleum ether：Ethyl alcohol：Soybean
Oil is by weight 1：2：9 mix, and impregnate 30min, when kettle pressure to be extracted rises to 1.0MPa, maintain 3min, then pressure release
It it is later 60 DEG C in temperature, under the conditions of extracting pressure is 1.0MPa, subcritical butane extracts 7h, and extract liquor enters to normal pressure
In knockout drum；
（3）Extract liquor is in knockout drum, and precipitation detaches 5min, butane point under conditions of temperature is 55 DEG C, pressure is -0.1MPa
Solvent tank is returned to from after, and purple perilla miscella is collected from knockout drum outlet valve；
（4）Ethyl alcohol and petroleum ether are isolated in vacuum distillation, and then the ODO of addition 0.1% is to get perilla herb oil.
Step（2）Purple perilla powder and butane solid-liquid ratio are 1Kg in extraction process：5L.
The recovery rate of Fructus Perillae quintessence oil in the present embodiment is 5.8%.
Embodiment 5
A kind of extraction process of perilla herb oil, includes the following steps：
（1）Temperature is down to -70 DEG C before perilla leaf crushes, and room temperature is at the uniform velocity warming up to 2 DEG C/min, carries out low temperature at -70 DEG C later
It crushes, the grain size after crushing is 50 mesh, obtains purple perilla powder, and the wherein moisture of perilla leaf is 9%；
（2）Purple perilla powder is placed in extraction kettle, the digestion agent of 5 times of weight is added, wherein digestion agent is petroleum ether：Ethyl alcohol：Soybean
Oil is by weight 1：3：9 mix, and impregnate 30min, when kettle pressure to be extracted rises to 1.1MPa, maintain 3min, then pressure release
It it is later 65 DEG C in temperature, under the conditions of extracting pressure is 1.1MPa, subcritical butane extracts 7h, and extract liquor enters to normal pressure
In knockout drum；
（3）Extract liquor is in knockout drum, and precipitation detaches 5min, butane point under conditions of temperature is 55 DEG C, pressure is -0.1MPa
Solvent tank is returned to from after, and purple perilla miscella is collected from knockout drum outlet valve；
（4）Ethyl alcohol and petroleum ether are isolated in vacuum distillation, and then the ODO of addition 0.1% is to get perilla herb oil.
Step（2）Purple perilla powder and butane solid-liquid ratio are 1Kg in extraction process：5L.
The recovery rate of Fructus Perillae quintessence oil in the present embodiment is 5.7%.
Embodiment 6
A kind of extraction process of perilla herb oil, includes the following steps：
（1）Temperature is down to -90 DEG C before perilla leaf crushes, and room temperature is at the uniform velocity warming up to 2 DEG C/min, carries out low temperature at -90 DEG C later
It crushes, the grain size after crushing is 40 mesh, obtains purple perilla powder, and the wherein moisture of perilla leaf is 9%；
（2）Purple perilla powder is placed in extraction kettle, the digestion agent of 5 times of weight is added, wherein digestion agent is petroleum ether：Ethyl alcohol：Soybean
Oil is by weight 1：1：9 mix, and impregnate 30min, when kettle pressure to be extracted rises to 1.0MPa, maintain 3min, then pressure release
It it is later 60 DEG C in temperature, under the conditions of extracting pressure is 1.0MPa, subcritical butane extracts 6h, and extract liquor enters to normal pressure
In knockout drum；
（3）Extract liquor is in knockout drum, and precipitation detaches 5min, butane point under conditions of temperature is 55 DEG C, pressure is -0.1MPa
Solvent tank is returned to from after, and purple perilla miscella is collected from knockout drum outlet valve；
（4）Ethyl alcohol and petroleum ether are isolated in vacuum distillation, and then the ODO of addition 0.2% is to get perilla herb oil.
Step（2）Purple perilla powder and butane solid-liquid ratio are 1Kg in extraction process：5L.
The recovery rate of Fructus Perillae quintessence oil in the present embodiment is 5.6%.
Finally illustrate, the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, this field is common
Other modifications or equivalent replacement that technical staff makes technical scheme of the present invention, without departing from technical solution of the present invention
Spirit and scope, be intended to be within the scope of the claims of the invention.
Claims (9)
1. a kind of extraction process of perilla herb oil, it is characterised in that：Include the following steps：
（1）Perilla leaf crushes, and obtains purple perilla powder；
（2）Purple perilla powder is placed in extraction kettle, the digestion agent of 2-5 times of weight is added, is extracted, is obtained using subcritical butane
Extract liquor；
（3）Extract liquor carries out isolated solvent and purple perilla miscella, and solvent recovery enters solvent tank, collects purple perilla miscella,
After further treatment, perilla herb oil is obtained.
2. the extraction process of perilla herb oil according to claim 1, it is characterised in that：The step（2）Middle digestion agent is big
Soya-bean oil.
3. a kind of extraction process of perilla herb oil according to claim 1, it is characterised in that：The step（2）Middle digestion agent
For petroleum ether：Ethyl alcohol：Soybean oil is by weight 1：1-3：9 mix.
4. a kind of extraction process of perilla herb oil according to claim 1, it is characterised in that：The step（2）In extraction
Temperature is 55-60 DEG C, extracting pressure 0.9-1.1MPa, extraction time 5-8h.
5. a kind of extraction process of perilla herb oil according to claim 1, it is characterised in that：The step（2）Middle extraction step
Suddenly it is：When extraction kettle pressure rises to 0.9-1.1MPa, 1-3min, then pressure release to normal pressure are maintained；Continue to boost to 0.9- later
1.1MPa extracts 5-8h.
6. a kind of extraction process of perilla herb oil according to claim 1, it is characterised in that：The step（1）Middle perilla leaf
Moisture be 7-9%.
7. a kind of extraction process of perilla herb oil according to claim 1, it is characterised in that：The step（1）In crushing
It is progress low-temperature grinding at -50~-90 DEG C, the grain size after crushing is 30-50 mesh.
8. a kind of extraction process of perilla herb oil according to claim 1, it is characterised in that：The step（1）In crushing
It is first to cool the temperature to -50~-90 DEG C, room temperature is at the uniform velocity warming up to 2 DEG C/min, carries out low temperature powder at -50~-90 DEG C later
Broken, the grain size after crushing is 30-50 mesh.
9. a kind of extraction process of perilla herb oil according to claim 1, it is characterised in that：Step（3）In be further processed
Include the ODO for adding 0.1-0.2% into grease, obtains perilla herb oil.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111187671A (en) * | 2019-09-29 | 2020-05-22 | 郝兴群 | Extraction method of perilla leaf essential oil containing perilla flavone |
| CN114907910A (en) * | 2022-06-22 | 2022-08-16 | 中林油科技有限公司 | Extraction process for idesia polycarpa oil |
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| CN106135466A (en) * | 2016-06-29 | 2016-11-23 | 贵州省油菜研究所 | A kind of perilla oil high efficiency extraction technique |
| JP2017057178A (en) * | 2015-09-18 | 2017-03-23 | イビデン株式会社 | Extract of perilla frutescens var. crispa f. viridis. and production methods thereof |
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| JP2017057178A (en) * | 2015-09-18 | 2017-03-23 | イビデン株式会社 | Extract of perilla frutescens var. crispa f. viridis. and production methods thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111187671A (en) * | 2019-09-29 | 2020-05-22 | 郝兴群 | Extraction method of perilla leaf essential oil containing perilla flavone |
| CN114907910A (en) * | 2022-06-22 | 2022-08-16 | 中林油科技有限公司 | Extraction process for idesia polycarpa oil |
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