CN110747060A - Method for extracting melaleuca alternifolia essential oil by ultrasonic-assisted solvent-free microwave - Google Patents
Method for extracting melaleuca alternifolia essential oil by ultrasonic-assisted solvent-free microwave Download PDFInfo
- Publication number
- CN110747060A CN110747060A CN201911002794.4A CN201911002794A CN110747060A CN 110747060 A CN110747060 A CN 110747060A CN 201911002794 A CN201911002794 A CN 201911002794A CN 110747060 A CN110747060 A CN 110747060A
- Authority
- CN
- China
- Prior art keywords
- melaleuca alternifolia
- distillation
- microwave
- ultrasonic
- oil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
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)
- Medicines Containing Plant Substances (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a method for extracting melaleuca alternifolia essential oil by ultrasonic-assisted solvent-free microwave, which combines the modern processing technologies such as an ultrasonic technology, a solvent-free microwave technology, a gravity collection technology, a molecular distillation purification technology and the like to realize the extraction and purification of high-purity melaleuca alternifolia essential oil, achieves the purposes of high-efficiency extraction, no solvent pollution, no impurity in separation and high product purity, and has the advantages of simple operation process, short extraction time, greenness, no pollution, low cost and improvement on the extraction rate.
Description
Technical Field
The invention belongs to the technical field of natural plant essential oil extraction, and particularly relates to a method for extracting melaleuca alternifolia essential oil by ultrasonic-assisted solvent-free microwave.
Background
Melaleuca alternifolia (Melaleuca alternifolia) is a plant of Melaleuca (Melaleuca) of Myrtaceae (Myrtle), long green small tree or shrub. Native to Australia and part of New Zealand, China has formed large-scale planting in Fujian, Guangdong, Guangxi, Hainan, Yunnan and other places. The melaleuca alternifolia essential oil has pharmacological activities of resisting bacteria, fungi, corrosion, inflammation, tumors and the like, can resist viruses, oxidation, inflammation and parasites and promote wound healing, is an excellent natural antibacterial agent capable of replacing antibiotics, and is non-toxic and nuisanceless. The method is widely applied to industries such as basic medicine, daily necessities, fresh keeping, pharmacy, food spice, beauty treatment and the like. Therefore, it is very important to develop an efficient extraction method of melaleuca alternifolia essential oil.
The traditional techniques such as steam distillation, solvent extraction and the like, and the emerging new techniques such as supercritical fluid extraction, microwave-assisted extraction, ultrasonic-assisted extraction and the like are applied to the extraction of essential oil. CN103146473A discloses a method for simultaneously extracting australian tea tree essential oil and flavonoid glycoside: adding entrainer into dried Australia tea tree raw material, performing supercritical fluid extraction with carbon dioxide, and performing three-stage separation to obtain Australia tea tree flavonoid glycoside and Australia tea tree essential oil simultaneously. The supercritical extraction equipment has large investment, poor recovery rate and high system pressure, and is difficult to extract substances with strong polarity and macromolecular mass. CN109135929A discloses an extraction method of melaleuca alternifolia essential oil: selecting fresh stem leaves of melaleuca alternifolia, removing impurities, and pulverizing; mixing a certain amount of solvents with different polarities according to a certain proportion to obtain a mixed solvent, wetting tea tree stems and leaves, and standing for a period of time; heating, refluxing and extracting the mixture after standing, and filtering; and (4) carrying out reduced pressure distillation on the filtered mixed solution, and recovering the solvent and the tea tree essential oil. The extraction rate and purity of the essential oil are low, solvent residue is easy to occur, the quality of aroma is easy to destroy after long-time hot reflux, and the use of a large amount of solvent has danger.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for extracting melaleuca alternifolia essential oil by using ultrasonic-assisted solvent-free microwave.
The technical scheme of the invention is as follows:
a method for extracting melaleuca alternifolia essential oil by ultrasound-assisted solvent-free microwave comprises the following steps:
(1) removing impurities and soil from freshly picked melaleuca alternifolia leaves with water, draining, and pulverizing to 20-40 mesh to obtain crushed melaleuca alternifolia leaves;
(2) placing the crushed melaleuca alternifolia leaves in an oval glass extraction container, adding no solvent, keeping the inverted mode, placing the container in an ultrasonic-assisted microwave extraction instrument, controlling the ultrasonic power to be 45-210W, the ultrasonic treatment time to be 10-35min, the microwave power to be 280-860W, the microwave frequency to be 1-7 times, the microwave time to be 2-12min each time, the intermediate pause time to be 1-6min, the temperature to be 45-100 ℃, and the oil seeping from the cracked oil glands of the crushed melaleuca alternifolia leaves, flowing downwards through a condensing device under the action of gravity, and collecting the oil in a collecting container at the bottom of a condenser of the ultrasonic-assisted microwave extraction instrument to prepare primary melaleuca alternifolia oil;
(3) adding the primary melaleuca alternifolia crude oil into a molecular distiller for molecular distillation, and collecting light components in a first stage, wherein the distillation pressure of the molecular distillation is 95-210Pa, and the distillation temperature is 48-62 ℃;
(4) and (3) adding the light components in the first stage into a molecular distiller for molecular distillation, and collecting the heavy components in the second stage to obtain the melaleuca alternifolia essential oil, wherein the distillation pressure of the molecular distillation is 380-620Pa, and the distillation temperature is 33-47 ℃.
In a preferred embodiment of the present invention, in the step (2), the ultrasonic power is 50 to 200W, and the ultrasonic treatment time is 10 to 30 min.
In a preferred embodiment of the present invention, in the step (2), the microwave power is 300-.
In a preferred embodiment of the present invention, the distillation pressure of the molecular distillation in the step (3) is 100-200Pa, and the distillation temperature is 50-60 ℃.
In a preferred embodiment of the present invention, the distillation pressure of the molecular distillation in the step (4) is 400-600Pa, and the distillation temperature is 35-45 ℃.
The invention has the beneficial effects that:
1. the method adopts a microwave-assisted solvent-free microwave extraction technology to extract the melaleuca alternifolia essential oil, combines an ultrasonic technology with the microwave extraction technology, avoids the use of an organic solvent, greatly shortens the extraction time, improves the extraction rate, accords with a green chemical concept, and has innovativeness of technology and application. Overcomes the defects of long extraction time, complex process and solvent residue in the traditional process, prepares and obtains the melaleuca alternifolia essential oil with high quality and high purity, and the process accords with the concept of green development.
2. The method adopts a gravity-assisted solvent-free microwave extraction technology to extract the melaleuca alternifolia essential oil, the essential oil seeps from the cracked oil glands, flows downwards through a condenser under the action of gravity, and is collected in a collection container at the bottom of a condenser. Avoiding the chemical property change caused by long-time heating in the extraction tank and improving the extraction efficiency.
3. The invention refines the melaleuca alternifolia essential oil by applying a secondary molecular distillation technology, removes plant wax and pigment from the melaleuca alternifolia essential oil product prepared in the first stage, removes the discordant and pungent smell in the top aroma of the melaleuca alternifolia essential oil product prepared in the second stage, and combines the two stages to improve the aroma and the quality of the melaleuca alternifolia essential oil, the distillation temperature is far lower than the boiling point, the vacuum degree is high, the heat-sensitive components can be effectively protected from being heated and oxidized, and other organic solvents are not introduced, so that the green development concept is met.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
Example 1
(1) Pretreatment of melaleuca alternifolia leaves: washing freshly picked melaleuca alternifolia leaves with water to remove impurities and soil, draining, pulverizing to 20-40 mesh to obtain crushed melaleuca alternifolia leaves, and placing in a refrigerator at-20 deg.C for later use;
(2) ultrasonic-assisted solvent-free microwave extraction: placing the crushed melaleuca alternifolia leaves in an elliptical glass extraction container, adding no solvent, and keeping an inverted mode. Placing into CW-2000 type ultrasonic assisted microwave extraction apparatus (Shanghai New Tuo analytical instruments science and technology Co., Ltd.), controlling ultrasonic power at 50W, ultrasonic processing time at 30min, microwave power at 300W, microwave frequency at 3 times, microwave time at each time at 3min, intermediate pause time at 5min, temperature at 100 deg.C, oil exuding from ruptured oil gland, flowing downwards through condenser under gravity, and collecting in collecting container at the bottom of condenser to obtain primary Melaleuca alternifolia crude oil;
(3) separating melaleuca alternifolia essential oil: adding primary Melaleuca alternifolia crude oil into YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.) at a distillation pressure of 200Pa and a distillation temperature of 60 deg.C; performing molecular distillation, and collecting light components in the first stage;
(4) the light components in the first stage are filled into a feeding bottle of a YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.), molecular distillation is carried out under the set distillation pressure of 600Pa and the set distillation temperature of 45 ℃, and the heavy components in the second stage are collected and separated into melaleuca alternifolia essential oil products. The total yield of melaleuca alternifolia essential oil was 7.03%.
Example 2
(1) Pretreatment of melaleuca alternifolia leaves: washing freshly picked melaleuca alternifolia leaves with water to remove impurities and soil, draining, pulverizing to 20-40 mesh to obtain crushed melaleuca alternifolia leaves, and placing in a refrigerator at-20 deg.C for later use;
(2) ultrasonic-assisted solvent-free microwave extraction: placing the crushed melaleuca alternifolia leaves in an elliptical glass extraction container, adding no solvent, and keeping an inverted mode. Placing into CW-2000 type ultrasonic assisted microwave extraction apparatus (Shanghai New Tuo analytical instruments science and technology Co., Ltd.), controlling ultrasonic power at 50W, ultrasonic processing time at 30min, microwave power at 300W, microwave frequency at 5 times, each time at 3min, middle intermittent time at 5min, temperature at 100 deg.C, oil exuding from cracked oil gland, flowing downwards through condenser under gravity, and collecting in a collecting container at the bottom of condenser to obtain primary Melaleuca alternifolia crude oil;
(3) separating melaleuca alternifolia essential oil: adding primary Melaleuca alternifolia crude oil into YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.) at a distillation pressure of 200Pa and a distillation temperature of 60 deg.C; performing molecular distillation, and collecting light components in the first stage;
(4) the first stage light components were filled in a feed bottle of a YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.), molecular distillation was carried out with a distillation pressure of 600Pa and a distillation temperature of 45 ℃ set, and the second stage heavy components were collected and separated into melaleuca alternifolia essential oil products. The total yield of melaleuca alternifolia essential oil was 7.59%.
Example 3
(1) Pretreatment of melaleuca alternifolia leaves: washing freshly picked melaleuca alternifolia leaves with water to remove impurities and soil, draining, pulverizing to 20-40 mesh to obtain crushed melaleuca alternifolia leaves, and placing in a refrigerator at-20 deg.C for later use;
(2) ultrasonic-assisted solvent-free microwave extraction: placing the crushed melaleuca alternifolia leaves in an elliptical glass extraction container, adding no solvent, and keeping an inverted mode. Placing into CW-2000 type ultrasonic assisted microwave extraction apparatus (Shanghai New Tuo analytical instruments science and technology Co., Ltd.), controlling ultrasonic power at 50W, ultrasonic processing time at 30min, microwave power at 500W, microwave frequency at 3 times, microwave time at each time at 3min, intermediate pause time at 5min, temperature at 100 deg.C, oil exuding from ruptured oil gland, flowing downwards through condenser under gravity, and collecting in collecting container at the bottom of condenser to obtain primary Melaleuca alternifolia crude oil;
(3) separating melaleuca alternifolia essential oil: adding primary Melaleuca alternifolia crude oil into YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.) at a distillation pressure of 200Pa and a distillation temperature of 60 deg.C; performing molecular distillation, and collecting light components in the first stage;
(4) the first stage light components were filled in a feed bottle of a YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.), molecular distillation was carried out with a distillation pressure of 600Pa and a distillation temperature of 45 ℃ set, and the second stage heavy components were collected and separated into melaleuca alternifolia essential oil products. The total yield of melaleuca alternifolia essential oil was 8.17%.
Example 4
(1) Pretreatment of melaleuca alternifolia leaves: washing freshly picked melaleuca alternifolia leaves with water to remove impurities and soil, draining, pulverizing to 20-40 mesh to obtain crushed melaleuca alternifolia leaves, and placing in a refrigerator at-20 deg.C for later use;
(2) ultrasonic-assisted solvent-free microwave extraction: placing the crushed melaleuca alternifolia leaves in an elliptical glass extraction container, adding no solvent, and keeping an inverted mode. Placing into CW-2000 type ultrasonic assisted microwave extraction apparatus (Shanghai New Tuo analytical instruments science and technology Co., Ltd.), controlling ultrasonic power at 200W, ultrasonic processing time at 30min, microwave power at 300W, microwave frequency at 3 times, microwave time at each time at 3min, intermediate pause time at 5min, temperature at 100 deg.C, oil exuding from ruptured oil gland, flowing downwards through condenser under gravity, and collecting in collecting container at the bottom of condenser to obtain primary Melaleuca alternifolia crude oil;
(3) separating melaleuca alternifolia essential oil: adding primary Melaleuca alternifolia crude oil into YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.) at a distillation pressure of 200Pa and a distillation temperature of 60 deg.C; performing molecular distillation, and collecting light components in the first stage;
(4) the first stage light components were filled in a feed bottle of a YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.), molecular distillation was carried out with a distillation pressure of 600Pa and a distillation temperature of 45 ℃ set, and the second stage heavy components were collected and separated into melaleuca alternifolia essential oil products. The total yield of melaleuca alternifolia essential oil was 7.65%.
Example 5
(1) Pretreatment of melaleuca alternifolia leaves: washing freshly picked melaleuca alternifolia leaves with water to remove impurities and soil, draining, pulverizing to 20-40 mesh to obtain crushed melaleuca alternifolia leaves, and placing in a refrigerator at-20 deg.C for later use;
(2) ultrasonic-assisted solvent-free microwave extraction: placing the crushed melaleuca alternifolia leaves in an elliptical glass extraction container, adding no solvent, and keeping an inverted mode. Placing into CW-2000 type ultrasonic assisted microwave extraction apparatus (Shanghai New Tuo analytical instruments science and technology Co., Ltd.), controlling ultrasonic power at 200W, ultrasonic processing time at 30min, microwave power at 500W, microwave frequency at 5 times, microwave time at each time at 5min, intermediate pause time at 5min, temperature at 100 deg.C, oil exuding from ruptured oil gland, flowing downwards through condenser under gravity, and collecting in a collecting container at the bottom of condenser to obtain primary Melaleuca alternifolia crude oil;
(3) separating melaleuca alternifolia essential oil: adding primary Melaleuca alternifolia crude oil into YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.) at a distillation pressure of 200Pa and a distillation temperature of 60 deg.C; performing molecular distillation, and collecting light components in the first stage;
(4) the first stage light components were filled in a feed bottle of a YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.), molecular distillation was carried out with a distillation pressure of 600Pa and a distillation temperature of 45 ℃ set, and the second stage heavy components were collected and separated into melaleuca alternifolia essential oil products. The total yield of melaleuca alternifolia essential oil is 9.05%.
Example 6
(1) Pretreatment of melaleuca alternifolia leaves: washing freshly picked melaleuca alternifolia leaves with water to remove impurities and soil, draining, pulverizing to 20-40 mesh to obtain crushed melaleuca alternifolia leaves, and placing in a refrigerator at-20 deg.C for later use;
(2) ultrasonic-assisted solvent-free microwave extraction: placing the crushed melaleuca alternifolia leaves in an elliptical glass extraction container, adding no solvent, and keeping an inverted mode. Placing into CW-2000 type ultrasonic assisted microwave extraction apparatus (Shanghai New Tuo analytical instruments science and technology Co., Ltd.), controlling ultrasonic power at 50W, ultrasonic processing time at 30min, microwave power at 300W, microwave frequency at 4 times, each time at 3min, middle intermittent time at 5min, temperature at 100 deg.C, oil exuding from ruptured oil gland, flowing downwards through condenser under gravity, and collecting in a collecting container at the bottom of condenser to obtain primary Melaleuca alternifolia crude oil;
(3) separating melaleuca alternifolia essential oil: adding primary Melaleuca alternifolia crude oil into YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.) at a distillation pressure of 200Pa and a distillation temperature of 60 deg.C; performing molecular distillation, and collecting light components in the first stage;
(4) the first stage light components were filled in a feed bottle of a YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.), molecular distillation was carried out with a distillation pressure of 600Pa and a distillation temperature of 45 ℃ set, and the second stage heavy components were collected and separated into melaleuca alternifolia essential oil products. The total yield of melaleuca alternifolia essential oil was 7.29%.
Example 7
(1) Pretreatment of melaleuca alternifolia leaves: washing freshly picked melaleuca alternifolia leaves with water to remove impurities and soil, draining, pulverizing to 20-40 mesh to obtain crushed melaleuca alternifolia leaves, and placing in a refrigerator at-20 deg.C for later use;
(2) ultrasonic-assisted solvent-free microwave extraction: placing the crushed melaleuca alternifolia leaves in an elliptical glass extraction container, adding no solvent, and keeping an inverted mode. Placing into CW-2000 type ultrasonic assisted microwave extraction apparatus (Shanghai New Tuo analytical instruments science and technology Co., Ltd.), controlling ultrasonic power at 150W, ultrasonic processing time at 30min, microwave power at 800W, microwave frequency at 3 times, microwave time at each time at 3min, middle intermittent time at 8min, temperature at 60 deg.C, oil exuding from ruptured oil gland, flowing downwards through condenser under gravity, and collecting in collecting container at the bottom of condenser to obtain primary Melaleuca alternifolia crude oil;
(3) separating melaleuca alternifolia essential oil: adding primary Melaleuca alternifolia crude oil into YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.) at a distillation pressure of 200Pa and a distillation temperature of 60 deg.C; performing molecular distillation, and collecting light components in the first stage;
(4) the first stage light components were filled in a feed bottle of a YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.), molecular distillation was carried out with a distillation pressure of 600Pa and a distillation temperature of 45 ℃ set, and the second stage heavy components were collected and separated into melaleuca alternifolia essential oil products. The total yield of melaleuca alternifolia essential oil was 9.24%.
Example 8
(1) Pretreatment of melaleuca alternifolia leaves: washing freshly picked melaleuca alternifolia leaves with water to remove impurities and soil, draining, pulverizing to 20-40 mesh to obtain crushed melaleuca alternifolia leaves, and placing in a refrigerator at-20 deg.C for later use;
(2) ultrasonic-assisted solvent-free microwave extraction: placing the crushed melaleuca alternifolia leaves in an elliptical glass extraction container, adding no solvent, and keeping an inverted mode. Placing into CW-2000 type ultrasonic assisted microwave extraction apparatus (Shanghai New Tuo analytical instruments science and technology Co., Ltd.), controlling ultrasonic power at 100W, ultrasonic processing time at 30min, microwave power at 700W, microwave frequency at 4 times, each time at 3min, middle intermittent time at 5min, temperature at 100 deg.C, oil exuding from ruptured oil gland, flowing downwards through condenser under gravity, and collecting in a collecting container at the bottom of condenser to obtain primary Melaleuca alternifolia crude oil;
(3) separating melaleuca alternifolia essential oil: adding primary Melaleuca alternifolia crude oil into YMD-060 type molecular distillation system (Shanghai Yuanhua industry Co., Ltd.), performing molecular distillation at distillation pressure of 400Pa and distillation temperature of 60 deg.C, and collecting light components in the first stage;
(4) the first stage light components were filled in a feed bottle of a YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.), molecular distillation was carried out with a distillation pressure of 600Pa and a distillation temperature of 45 ℃ set, and the second stage heavy components were collected and separated into melaleuca alternifolia essential oil products. The total yield of melaleuca alternifolia essential oil was 9.23%.
Example 9
(1) Pretreatment of melaleuca alternifolia leaves: washing freshly picked melaleuca alternifolia leaves with water to remove impurities and soil, draining, pulverizing to 20-40 mesh to obtain crushed melaleuca alternifolia leaves, and placing in a refrigerator at-20 deg.C for later use;
(2) ultrasonic-assisted solvent-free microwave extraction: placing the crushed melaleuca alternifolia leaves in an elliptical glass extraction container, adding no solvent, and keeping an inverted mode. Placing into CW-2000 type ultrasonic assisted microwave extraction apparatus (Shanghai New Tuo analytical instruments science and technology Co., Ltd.), controlling ultrasonic power at 200W, ultrasonic processing time at 30min, microwave power at 400W, microwave frequency at 5 times, each time at 2min, middle intermittent time at 5min, temperature at 100 deg.C, oil exuding from ruptured oil gland, flowing downwards through condenser under gravity, and collecting in a collecting container at the bottom of condenser to obtain primary Melaleuca alternifolia crude oil;
(3) separating melaleuca alternifolia essential oil: adding primary Melaleuca alternifolia crude oil into YMD-060 type molecular distillation system (Shanghai Yuanhua industry Co., Ltd.), performing molecular distillation at a distillation pressure of 200Pa and a distillation temperature of 60 ℃, and collecting light components in a first stage;
(4) the first stage light components were filled in a feed bottle of a YMD-060 type molecular distillation system (Shanghai Yuanhua industries, Ltd.), molecular distillation was carried out with a distillation pressure of 600Pa and a distillation temperature of 45 ℃ set, and the second stage heavy components were collected and separated into melaleuca alternifolia essential oil products. The total yield of melaleuca alternifolia essential oil was 8.69%.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (5)
1. A method for extracting melaleuca alternifolia essential oil by ultrasound-assisted solvent-free microwave is characterized by comprising the following steps: the method comprises the following steps:
(1) removing impurities and soil from freshly picked melaleuca alternifolia leaves with water, draining, and pulverizing to 20-40 mesh to obtain crushed melaleuca alternifolia leaves;
(2) placing the crushed melaleuca alternifolia leaves in an oval glass extraction container, adding no solvent, keeping the inverted mode, placing the container in an ultrasonic-assisted microwave extraction instrument, controlling the ultrasonic power to be 45-210W, the ultrasonic treatment time to be 10-35min, the microwave power to be 280-860W, the microwave frequency to be 1-7 times, the microwave time to be 2-12min each time, the intermediate pause time to be 1-6min, the temperature to be 45-100 ℃, and the oil seeping from the cracked oil glands of the crushed melaleuca alternifolia leaves, flowing downwards through a condensing device under the action of gravity, and collecting the oil in a collecting container at the bottom of a condenser of the ultrasonic-assisted microwave extraction instrument to prepare primary melaleuca alternifolia oil;
(3) adding the primary melaleuca alternifolia crude oil into a molecular distiller for molecular distillation, and collecting light components in a first stage, wherein the distillation pressure of the molecular distillation is 95-210Pa, and the distillation temperature is 48-62 ℃;
(4) and (3) adding the light components in the first stage into a molecular distiller for molecular distillation, and collecting the heavy components in the second stage to obtain the melaleuca alternifolia essential oil, wherein the distillation pressure of the molecular distillation is 380-620Pa, and the distillation temperature is 33-47 ℃.
2. The method of claim 1, wherein: in the step (2), the ultrasonic power is 50-200W, and the ultrasonic treatment time is 10-30 min.
3. The method of claim 1, wherein: in the step (2), the microwave power is 300-850W, the microwave frequency is 1-5 times, the microwave time is 2-10min each time, the intermediate pause time is 2-5min, and the temperature is 50-100 ℃.
4. The method of claim 1, wherein: the distillation pressure of the molecular distillation in the step (3) is 100-200Pa, and the distillation temperature is 50-60 ℃.
5. The method of claim 1, wherein: the distillation pressure of the molecular distillation in the step (4) is 400-600Pa, and the distillation temperature is 35-45 ℃.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911002794.4A CN110747060A (en) | 2019-10-21 | 2019-10-21 | Method for extracting melaleuca alternifolia essential oil by ultrasonic-assisted solvent-free microwave |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911002794.4A CN110747060A (en) | 2019-10-21 | 2019-10-21 | Method for extracting melaleuca alternifolia essential oil by ultrasonic-assisted solvent-free microwave |
Publications (1)
Publication Number | Publication Date |
---|---|
CN110747060A true CN110747060A (en) | 2020-02-04 |
Family
ID=69279281
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201911002794.4A Pending CN110747060A (en) | 2019-10-21 | 2019-10-21 | Method for extracting melaleuca alternifolia essential oil by ultrasonic-assisted solvent-free microwave |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110747060A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114558145A (en) * | 2022-03-30 | 2022-05-31 | 诗玮雅(青岛)生物制药有限公司 | Plant essential oil pharmaceutic adjuvant as well as preparation method and application thereof |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1994026853A1 (en) * | 1993-05-11 | 1994-11-24 | Archimex | Method and plant for solvent-free microwave extraction of natural products |
CN104711121A (en) * | 2015-02-28 | 2015-06-17 | 湖北中烟工业有限责任公司 | Method for extracting chrysanthemum indicum essential oil in ultrasonic-assisted solvent-free microwave extraction manner |
CN105647649A (en) * | 2016-03-31 | 2016-06-08 | 李颖 | Preparation method and device using microwave and gravity to extract natural plant essential oil and hydrolat |
CN106010792A (en) * | 2016-06-27 | 2016-10-12 | 福建澳树佳生物科技有限公司 | Method for extracting melaleuca alternifolia and tea tree essence oil |
-
2019
- 2019-10-21 CN CN201911002794.4A patent/CN110747060A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1994026853A1 (en) * | 1993-05-11 | 1994-11-24 | Archimex | Method and plant for solvent-free microwave extraction of natural products |
CN104711121A (en) * | 2015-02-28 | 2015-06-17 | 湖北中烟工业有限责任公司 | Method for extracting chrysanthemum indicum essential oil in ultrasonic-assisted solvent-free microwave extraction manner |
CN105647649A (en) * | 2016-03-31 | 2016-06-08 | 李颖 | Preparation method and device using microwave and gravity to extract natural plant essential oil and hydrolat |
CN106010792A (en) * | 2016-06-27 | 2016-10-12 | 福建澳树佳生物科技有限公司 | Method for extracting melaleuca alternifolia and tea tree essence oil |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114558145A (en) * | 2022-03-30 | 2022-05-31 | 诗玮雅(青岛)生物制药有限公司 | Plant essential oil pharmaceutic adjuvant as well as preparation method and application thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101905091B (en) | Equipment and method for extracting biologically active ingredients from subcritical fluid | |
CN103045371B (en) | A kind of preparation method of purify from the wild Du Xiang in Daxing'an Mountainrange essential oil and ursolic acid | |
CN107400563A (en) | For extracting the process units and its production method of fragrant plant composition | |
CN107686773B (en) | Method for extracting rosemary essential oil and antioxidant from rosemary | |
CN103113980A (en) | Efficient extraction and purification method of mandarin peel oil | |
CN106318642A (en) | Preparation method of high-purity essential oil by low-temperature distillation extraction | |
CN109504540A (en) | A kind of agilawood essential oil extracting method | |
CN102100875B (en) | Process method for microwave assistant supercritical extraction of active ingredients of curcuma | |
CN104830538A (en) | Method of extracting tea tree essential oil from tea trees | |
CN102617655A (en) | Method for subcritical water extraction of oleuropein | |
CN105062686A (en) | Method for extracting lavender essential oil | |
CN105199853A (en) | Extraction method of raw ginger essential oil | |
CN108949363A (en) | A kind of Solventless Extraction Process of industrial hemp floral leaf essential oil | |
CN104726201A (en) | Preparation method of agilawood essential oil | |
CN105622777A (en) | Technology for extracting pectin from premna microphylla turca | |
CN110818456A (en) | Preparation method of pyroligneous foliar fertilizer | |
CN102040579A (en) | Method for extracting luteolin from peanut roots, stems, leaves and shells | |
CN110747060A (en) | Method for extracting melaleuca alternifolia essential oil by ultrasonic-assisted solvent-free microwave | |
CN103349850B (en) | A kind of method for extracting active ingredient in wax-apple | |
CN108503510B (en) | Green natural borneol refining method | |
CN105559003A (en) | Preparation method of sweet-scented osmanthus medicinal extract | |
CN106376912A (en) | Preparation method for red date extract | |
CN104844683A (en) | Method for extracting peony saponin from peony seed meal | |
CN111944604A (en) | Method for preparing oil by separating sea buckthorn and prepared oil | |
CN105272824A (en) | Preparation method of natural cinnamomum camphora aromatic material |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200204 |