CN107858207A - A kind of supercritical CO of golden flower tea essential oils2Extracting process - Google Patents
A kind of supercritical CO of golden flower tea essential oils2Extracting process Download PDFInfo
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- CN107858207A CN107858207A CN201711188917.9A CN201711188917A CN107858207A CN 107858207 A CN107858207 A CN 107858207A CN 201711188917 A CN201711188917 A CN 201711188917A CN 107858207 A CN107858207 A CN 107858207A
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- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
-
- 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
- C11B9/022—Refining
Landscapes
- 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)
Abstract
The invention discloses a kind of supercritical CO of golden flower tea essential oils2Extracting process, comprise the following steps：(1) drained away the water after golden camellia tea to be extracted is cleaned up, then carry out microwave drying, wherein moisture is dropped to less than 10%；(2) golden camellia tea is crushed, sieved with 40 60 mesh sieve, it is expanded；(3) supercritical CO2Refining：The golden camellia tea is sent into supercritical CO2In device, after first time extraction and second extract, extract is collected, obtains Camellia nitidissima crude oil；(4) refrigerated centrifuge, Camellia nitidissima crude oil after extraction is positioned in 8 11 DEG C of environment, freeze 30 35 minutes, the Camellia nitidissima crude oil after freezing is positioned in high speed freezing centrifuge again and centrifuged 20 30 minutes, remove impurity, temperature is put into as 45 50 DEG C, vacuum distillation purifying condensation, golden flower tea essential oils are made.The yield of the present invention is high, does not have any dissolvent residual rapidly and efficiently, does not pollute by extracting material.
Description
Technical field
The present invention relates to oil extraction technical field, and in particular to a kind of supercritical CO of golden flower tea essential oils2Extraction side
Method.
Background technology
Camellia nitidissima [Camellia chrysantha (Hu) Tuyama] category Theaceae, Camellia, Camellia Section Chrysantha.
Nineteen sixty finds first in Guangxi, due to its floral wax matter is golden yellow, golden valve jade stamen, the pretty cause of floridity, the famous plant in nineteen sixty-five China
Scholar Hu Xian doctors Jiasu are named as Camellia nitidissima.A kind of Camellia nitidissima plant resources rare as world (is only distributed in Guangxi
With the band of Vietnam border one), local always by as Traditional Folk Chinese herbal medicine, for treating sphagitis, dysentery, hypertension, pre-
Preventing tumor, have blood in stool, the disease such as irregular menstruation [woods Hua Juan, waits food science and technologies, 2010,35 (10):88-91].By authoritative department and
Scientific research institution's detection shows that golden camellia tea contains more than 400 kinds of nutriment, rich in a variety of natural nutrition compositions.Golden camellia tea is institute
There is general flavone content highest in tealeaves.Golden camellia tea is obvious because having containing active skull cap components such as abundant flavonoids
Anti-aging, immunity of organism, atherosclerosis are improved, suppresses tumour growth, reduce cholesterol, lowering blood pressure and blood fat
Deng effect.
Essential oil, also known as volatile oil, English name essential oil, it is that the one kind contained in plant has aromatic odor
Oily composition general name.It is mixture, and specific comparison of ingredients is complicated, primary fat compounds of group and aromatic compound,
Including alcohols, esters, phenols, ethers, terpenes etc..
Scientific research finds that plant-derived essential oil mostly has calm nerves, calmness, antibacterial bacteriostatic, beauty, treatment disease
And other effects, widely used in medical science, food, essence and flavoring agent industry.For example, Rosa Damascana has, anti-melancholy, alleviation are nervous,
Spirit is improved, makes one excited, body circulation is assisted, capilary can be shunk, have antiinflammation to cholecystitis, conjunctivitis, ophthalmia, can be with
Purify the blood, sharp spleen, stomach invigorating, mend body, anti-nausea etc..Peppermint essential oil throat-clearing throat-moistening, to eliminate halitosis it is fine the effect of, micro- blood can be shunk
Pipe, vivotoxin is excluded, improve eczema, tinea, releive and itch, inflammation and burn, soft skin, eliminate blackhead, be beneficial to
Oily hair and skin quality, also releive body and mind the effect of.
Derived essential oil is the essence of plant, and content is few, and extraction yield is nor very high, and therefore, price general charged is expensive.At present
Essential oil extracting process mainly have steam distillation, microwave-assisted, ultrasound-assisted extraction method, overcritical, sub- face
Boundary's extraction etc..
Supercritical CO2Fluid has the selectivity of height；Its extract and separate efficiency high, good product quality.Can also be simultaneously complete
Into extracting and 2 processes of distillation, the organic mixture of difficult separation is separated, the fractionation especially for homologue refined has more
Characteristic, for some special separation processes, it is difficult to handle with other separation methods, and utilizes supercritical CO2Fluid can then obtain
To gratifying result.Such as in the technique of coffee bean removing caffeine, supercritical CO2The advantage of extraction is not destroy coffee
The original flavor of coffee, and be difficult to accomplish this point with other method.And for the extraction of natural perfume material, using supercritical CO2Extraction
Technology is taken, there is higher oxygenatedchemicals and relatively low monoterpene olefin(e) centent, and contain more head perfume (or spice) composition in extract
With more bottom note compositions, show to be more nearly natural true fragrance.
Compared with conventional method, oil yield made from traditional milling process is low；When carrying oil with organic solvent extractionprocess, though
The yield of right grease greatly improves, but the problems such as dissolvent residual in solvent recovery and product be present.And supercritical carbon dioxide extraction
Obtained oil product high income, impurity content is low, lighter color, and can save the refining steps such as follow-up vacuum distillation and deodorization.
At present, a kind of supercritical CO of the high golden flower tea essential oils of yield is lacked2Extracting process.
The content of the invention
To solve the above problems, the shortcomings that it is an object of the invention to provide being to overcome prior art, there is provided one kind production
The supercritical CO of the high golden flower tea essential oils of rate2Extracting process.
To realize above-mentioned technical purpose, the technical solution adopted by the present invention is as follows：A kind of golden flower tea essential oils of the present invention
Supercritical CO2Extracting process, comprise the following steps：
(1) drained away the water after golden camellia tea to be extracted is cleaned up, then carry out microwave drying, make wherein moisture drop
To less than 10%；
(2) golden camellia tea is crushed, sieved with 40-60 mesh sieve, it is expanded；
(3) supercritical CO2Refining：The golden camellia tea is sent into supercritical CO2In device, through first time extraction and second
After secondary extraction, extract is collected, obtains Camellia nitidissima crude oil；
(4) refrigerated centrifuge, the Camellia nitidissima crude oil after extraction is positioned in 8-11 DEG C of environment, freezes 30-35 minutes, then
Camellia nitidissima crude oil after freezing is positioned in the high speed freezing centrifuge that rotating speed is 8000-10000r/min and centrifuges 20-30 points
Clock, impurity is removed, be put into temperature as 45-50 DEG C, vacuum distillation purifying condensation, golden flower tea essential oils are made.It is evaporated in vacuo herein
It can make it that essential oil is purer, purity is higher.
Further, in step (1), the frequency of the microwave drying is 800-1000MHz, drying time 2-
4min。
Further, in step (2), the parameter of the screw extrusion processing is：Screw speed 180-220r/
Min, 115-145 DEG C of extrusion temperature, charging rate 15-25r/min；Airflow puffing technical finesse parameter is：Operation temperature 60-
80 DEG C, bulking pressure difference is 200-400kPa, puffing time 50-75min；Microwave bulking technical parameter is：Microwave power
1000-2000W, processing time 2-4min.
Further, in step (3), CO2Supercritical extract, extract for the first time：Fluid extraction pressure is 30-
40MPa, 35-40 DEG C of extraction temperature, CO2Fluid flow is 700-800L/h, extraction time 30-60min.
Further, in step (3), second of extraction：Fluid extraction pressure is 45-55MPa, extraction temperature 45-50
DEG C, CO2Fluid flow is 800-900L/h, extraction time 60-120min.
Further, in step (4), the vacuum distillation uses alembic, and the pressure inside the tank of the alembic is
0.06MPa, vacuum 60-70MPa.
Beneficial effect：The yield of the present invention is high, does not have any dissolvent residual rapidly and efficiently, does not pollute by extract
Matter.Whole technical process is simple, and separation is thorough, green.
The present invention compared with prior art, has the following advantages that：
(1) expanding treatment technology is utilized, under the synergy of other techniques so that the eucaryotic cell structure of plant material becomes
Loosely, cell wall rupture, be advantageous to the extraction of follow-up derived essential oil, improve the yield of golden flower tea essential oils.
(2) essential oil product is adapted to select airflow puffing and supercritical CO2Extracting refining.Microwave drying ratio faster, is dried
Effect is good.
Embodiment
The present invention is further illustrated by the following examples.It should be understood that these embodiments are the explainations of the present invention
And citing, the scope of the present invention is not limited in any form.
Embodiment 1
A kind of supercritical CO of golden flower tea essential oils of the present invention2Extracting process, comprise the following steps：
(1) drained away the water after golden camellia tea to be extracted is cleaned up, then carry out microwave drying, make wherein moisture drop
To less than 10%；The frequency of the microwave drying is 800MHz, drying time 4min.
(2) golden camellia tea is crushed, sieved with 40 mesh sieve；It is expanded；The parameter of screw extrusion processing is：Spiral shell
Bar rotating speed 180r/min, 135 DEG C of extrusion temperature, charging rate 15r/min；Airflow puffing technical finesse parameter is：Operation temperature
60 DEG C of degree, bulking pressure difference is 200kPa, puffing time 65min；Microwave bulking technical parameter is：Microwave power 1000W, place
Manage time 2min.
(3) supercritical CO2Refining：The golden camellia tea is sent into supercritical CO2In device, through first time extraction and second
After secondary extraction, extract is collected, obtains Camellia nitidissima crude oil；CO2Supercritical extract, extract for the first time：Fluid extraction pressure is
30MPa, 40 DEG C of extraction temperature, CO2Fluid flow is 700L/h, extraction time 30min.Second of extraction：Fluid extraction pressure
Power is 45MPa, 50 DEG C of extraction temperature, CO2Fluid flow is 800L/h, extraction time 60min.
(4) refrigerated centrifuge, the Camellia nitidissima crude oil after extraction is positioned in 8 DEG C of environment, freezed 33 minutes, then will freezing
Camellia nitidissima crude oil afterwards is positioned in the high speed freezing centrifuge that rotating speed is 8000r/min and centrifuged 20 minutes, removes impurity, is put into
Temperature is 50 DEG C, and vacuum tank vacuumizes 4 hours, and golden flower tea essential oils are made.
Embodiment 2
The difference of embodiment 2 and embodiment 1 is：
A kind of supercritical CO of golden flower tea essential oils of the present invention2Extracting process, comprise the following steps：
(1) drained away the water after golden camellia tea to be extracted is cleaned up, then carry out microwave drying, make wherein moisture drop
To less than 10%；The frequency of the microwave drying is 900MHz, drying time 2min.
(2) golden camellia tea is crushed, sieved with 60 mesh sieve；It is expanded；The parameter of screw extrusion processing is：Spiral shell
Bar rotating speed 220r/min, 115 DEG C of extrusion temperature, charging rate 20r/min；Airflow puffing technical finesse parameter is：Operation temperature
70 DEG C of degree, bulking pressure difference is 400kPa, puffing time 75min；Microwave bulking technical parameter is：Microwave power 2000W, place
Manage time 4min.
(3) supercritical CO2Refining：The golden camellia tea is sent into supercritical CO2In device, through first time extraction and second
After secondary extraction, extract is collected, obtains Camellia nitidissima crude oil；CO2Supercritical extract, extract for the first time：Fluid extraction pressure is
35MPa, 35 DEG C of extraction temperature, CO2Fluid flow is 760L/h, extraction time 60min.Second of extraction：Fluid extraction pressure
Power is 50MPa, 45 DEG C of extraction temperature, CO2Fluid flow is 900L/h, extraction time 100min.
(4) refrigerated centrifuge, the Camellia nitidissima crude oil after extraction is positioned in 11 DEG C of environment, freezed 35 minutes, then will be cold
Camellia nitidissima crude oil after jelly is positioned in the high speed freezing centrifuge that rotating speed is 9000r/min and centrifuged 30 minutes, removes impurity, puts
Enter temperature for 48 DEG C, vacuum tank vacuumizes 5 hours, and golden flower tea essential oils are made.
Embodiment 3
The difference of embodiment 3 and embodiment 1 is：
A kind of supercritical CO of golden flower tea essential oils of the present invention2Extracting process, comprise the following steps：
(1) drained away the water after golden camellia tea to be extracted is cleaned up, then carry out microwave drying, make wherein moisture drop
To less than 10%；The frequency of the microwave drying is 1000MHz, drying time 3min.
(2) golden camellia tea is crushed, sieved with 50 mesh sieve, it is expanded；The parameter of screw extrusion processing is：Spiral shell
Bar rotating speed 200r/min, 145 DEG C of extrusion temperature, charging rate 25r/min；Airflow puffing technical finesse parameter is：Operation temperature
80 DEG C of degree, bulking pressure difference is 300kPa, puffing time 50min；Microwave bulking technical parameter is：Microwave power 1800W, place
Manage time 3min.
(3) supercritical CO2Refining：The golden camellia tea is sent into supercritical CO2In device, through first time extraction and second
After secondary extraction, extract is collected, obtains Camellia nitidissima crude oil；CO2Supercritical extract, extract for the first time：Fluid extraction pressure is
40MPa, 38 DEG C of extraction temperature, CO2Fluid flow is 800L/h, extraction time 50min.Second of extraction：Fluid extraction pressure
Power is 55MPa, 48 DEG C of extraction temperature, CO2Fluid flow is 870L/h, extraction time 120min.
(4) refrigerated centrifuge, the Camellia nitidissima crude oil after extraction is positioned in 10 DEG C of environment, freezed 30 minutes, then will be cold
Camellia nitidissima crude oil after jelly is positioned in the high speed freezing centrifuge that rotating speed is 10000r/min and centrifuged 25 minutes, removes impurity,
Temperature is put into as 45 DEG C, vacuum tank vacuumizes 6 hours, and golden flower tea essential oils are made.
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, the present invention
Claimed scope is by appended claims, specification and its equivalent thereof.
Claims (6)
- A kind of 1. supercritical CO of golden flower tea essential oils2Extracting process, it is characterised in that comprise the following steps：(1) drained away the water after golden camellia tea to be extracted is cleaned up, then carry out microwave drying, drop to wherein moisture Less than 10%；(2) golden camellia tea is crushed, sieved with 40-60 mesh sieve, it is expanded；(3) supercritical CO2Refining：The golden camellia tea is sent into supercritical CO2In device, extract through first time extraction and second After taking, extract is collected, obtains Camellia nitidissima crude oil；(4) refrigerated centrifuge, the Camellia nitidissima crude oil after extraction is positioned in 8-11 DEG C of environment, freezes 30-35 minutes, then will be cold Camellia nitidissima crude oil after jelly is positioned in the high speed freezing centrifuge that rotating speed is 8000-10000r/min and centrifuges 20-30 minutes, removes Decontamination, temperature is put into as 45-50 DEG C, vacuum distillation purifying condensation, golden flower tea essential oils are made.
- 2. the supercritical CO of golden flower tea essential oils according to claim 12Extracting process, it is characterised in that：In step (1) In, the frequency of the microwave drying is 800-1000MHz, drying time 2-4min.
- 3. the supercritical CO of golden flower tea essential oils according to claim 12Extracting process, it is characterised in that：In step (2) In, the parameter of the screw extrusion processing is：Screw speed 180-220r/min, 115-145 DEG C of extrusion temperature, charging speed Spend for 15-25r/min；Airflow puffing technical finesse parameter is：60-80 DEG C of operation temperature, bulking pressure difference is 200-400kPa, Puffing time is 50-75min；Microwave bulking technical parameter is：Microwave power 1000-2000W, processing time 2-4min.
- 4. the supercritical CO of golden flower tea essential oils according to claim 12Extracting process, it is characterised in that：In step (3) In, CO2Supercritical extract, extract for the first time：Fluid extraction pressure is 30-40MPa, 35-40 DEG C of extraction temperature, CO2Fluid flow For 700-800L/h, extraction time 30-60min.
- 5. the supercritical CO of golden flower tea essential oils according to claim 12Extracting process, it is characterised in that：In step (3) In, second of extraction：Fluid extraction pressure is 45-55MPa, 45-50 DEG C of extraction temperature, CO2Fluid flow is 800-900L/ H, extraction time 60-120min.
- 6. the supercritical CO of golden flower tea essential oils according to claim 12Extracting process, it is characterised in that：In step (4) In, the vacuum distillation uses alembic, and the pressure inside the tank of the alembic is 0.06MPa, vacuum 60-70MPa.
Priority Applications (1)
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| CN108434306A (en) * | 2018-06-26 | 2018-08-24 | 张宗杰 | A kind of department of general surgery's burn and scald treatment Chinese medicine composition and preparation method thereof |
| CN108456594A (en) * | 2018-05-07 | 2018-08-28 | 南召留山岭南艾叶制品有限公司 | A kind of extracting method of high yield wormwood essential oil |
| CN109810789A (en) * | 2018-07-25 | 2019-05-28 | 上海药辰生物科技有限公司 | A kind of extracting method of ginkgo essential oil |
| CN110029013A (en) * | 2019-04-10 | 2019-07-19 | 浙江工业大学 | A kind of method of ultrasonic wave added aqueous enzymatic extraction cape jasmine oil |
| CN111040867A (en) * | 2019-12-17 | 2020-04-21 | 河南省农业科学院 | Preparation method of sesame oil by water substitution method |
| CN113416607A (en) * | 2021-06-07 | 2021-09-21 | 浙江邦宁尔制药有限公司 | Extraction system who contains supercritical fluid extraction cauldron |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108456594A (en) * | 2018-05-07 | 2018-08-28 | 南召留山岭南艾叶制品有限公司 | A kind of extracting method of high yield wormwood essential oil |
| CN108434306A (en) * | 2018-06-26 | 2018-08-24 | 张宗杰 | A kind of department of general surgery's burn and scald treatment Chinese medicine composition and preparation method thereof |
| CN109810789A (en) * | 2018-07-25 | 2019-05-28 | 上海药辰生物科技有限公司 | A kind of extracting method of ginkgo essential oil |
| CN110029013A (en) * | 2019-04-10 | 2019-07-19 | 浙江工业大学 | A kind of method of ultrasonic wave added aqueous enzymatic extraction cape jasmine oil |
| CN111040867A (en) * | 2019-12-17 | 2020-04-21 | 河南省农业科学院 | Preparation method of sesame oil by water substitution method |
| CN113416607A (en) * | 2021-06-07 | 2021-09-21 | 浙江邦宁尔制药有限公司 | Extraction system who contains supercritical fluid extraction cauldron |
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