CN115449422A - Method for extracting magnolia flower oil - Google Patents
Method for extracting magnolia flower oil Download PDFInfo
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- CN115449422A CN115449422A CN202211115233.7A CN202211115233A CN115449422A CN 115449422 A CN115449422 A CN 115449422A CN 202211115233 A CN202211115233 A CN 202211115233A CN 115449422 A CN115449422 A CN 115449422A
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- tank
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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- 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
Abstract
The invention provides a method for extracting magnolia flower oil, which comprises the following steps of (1) selecting and preparing raw materials, selecting magnolia flower, cleaning and drying; (2) crushing and screening the dried magnolia flower powder; (3) placing the screened flos Magnoliae pollen powder into an extraction tank, introducing subcritical fluid into the extraction tank, and extracting flos Magnoliae oil; (4) and (5) after the separation is finished, collecting the magnolia flower oil from the extraction tank and the bottom of the separation tank, and recovering the subcritical fluid in the separation tank for recycling. The magnolia flower oil is extracted by subcritical fluid, the product quality is good, the production process is environment-friendly and pollution-free, and the extraction tank is preheated before extraction, so that the extraction transition time is effectively saved; compared with the existing supercritical carbon dioxide fluid extraction, the method has the advantages of low equipment pressure and low production cost, and is extremely suitable for large-scale industrial operation.
Description
Technical Field
The invention relates to the technical field of essential oil extraction, in particular to a method for extracting magnolia flower oil.
Background
Flos Magnoliae is also called Magnolia liliflora and Magnolia biondii, and is a plant of Magnoliaceae. Flos Magnoliae is a common Chinese medicine, and dried flower bud is used for medicine, and has effects of warming lung, inducing resuscitation, dispelling pathogenic wind, and dispelling cold. It can be used for treating wind-cold type common cold, sinusitis, toothache, headache, etc. Currently, most of the magnolia flowers are brewed and introduced, and the utilization efficiency is low, so that a method for improving the utilization efficiency of the magnolia flowers needs to be developed.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention provides a method for extracting magnolia flower oil to solve the problems of the prior art.
In order to solve the problems, the invention provides a method for extracting magnolia flower oil, which at least comprises the following processes:
(1) selecting and preparing raw materials, namely selecting magnolia flowers, cleaning with water to remove impurities, and draining; drying the cleaned flos Magnoliae at 50-80 deg.C for 2-7 hr until the water content of flos Magnoliae is less than 10%;
(2) pulverizing dried flos Magnoliae, and sieving with 20-25 mesh sieve to obtain flos Magnoliae powder with suitable size;
(3) preheating an extraction tank, placing screened flos Magnoliae pollen powder into the extraction tank after the extraction tank is preheated to the temperature close to the extraction temperature, vacuumizing the extraction tank, and enabling the vacuum degree to be 0-10MPa; introducing subcritical fluid into an extraction tank, wherein the material-liquid ratio of the magnolia flower powder to the subcritical fluid is 1.1-1;
(4) after extraction, introducing subcritical fluid in the extraction tank into a separation tank to separate with flos Magnoliae oil to extract effective components in flos Magnoliae granules, wherein the pressure in the separation tank is maintained at 0-10MPa, the pressure in the separation tank is less than the pressure in the extraction tank, and the temperature is maintained at 30-50 deg.C;
(5) repeating the separation procedure in (4), wherein the separation time of each time lasts for 45-90 minutes;
(6) after the separation is finished, the pressure in the tank is reduced to 0MPa, the magnolia flower oil is collected from the bottom of the extraction tank and the separation tank, and the subcritical fluid in the separation tank is recovered for recycling.
Further, the subcritical fluid medium introduced in (3) above includes one or a mixture of more of butane, tetrafluoroethane, propane, ethane and methane.
The invention also provides the magnolia flower oil which is prepared by the method for extracting the magnolia flower oil.
The invention also provides a magnolia flower oil product, which contains the magnolia flower oil, and the magnolia flower oil is prepared by the method for extracting the magnolia flower oil.
By implementing the subcritical fluid extraction method of magnolia flower oil provided by the invention, the following technical effects are achieved: the magnolia oil is extracted by subcritical fluid, the product quality is good, and the production process is environment-friendly and pollution-free; the extraction tank is preheated before extraction, so that the extraction transition time is effectively saved; compared with the existing supercritical carbon dioxide fluid extraction, the method has the advantages of low equipment pressure and low production cost, and is extremely suitable for large-scale industrial operation.
Drawings
The conception, specific structure and technical effects of the present invention will be further described in conjunction with the accompanying drawings to fully understand the purpose, characteristics and effects of the present invention.
FIG. 1 is a process flow chart of the subcritical fluid extraction method of magnolia flower oil according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The technical solution of the present invention is described in detail below using examples.
Based on the selection of the raw materials of the magnolia flower oil, the process for preparing the magnolia flower oil at least comprises the following working procedures:
the method comprises the following steps:
(1) selecting and preparing raw materials, namely selecting magnolia flower, cleaning with water to remove impurities, and draining; drying the cleaned flos Magnoliae at 50-80 deg.C for 2-7 hr until the water content of flos Magnoliae is less than 10%;
(2) pulverizing dried flos Magnoliae, and sieving with 20-25 mesh sieve to obtain flos Magnoliae powder with suitable size;
(3) preheating an extraction tank, placing screened flos Magnoliae pollen powder into the extraction tank after the extraction tank is preheated to the temperature close to the extraction temperature, vacuumizing the extraction tank, and keeping the vacuum degree to 0-10MPa; introducing subcritical fluid into an extraction tank, wherein the material-liquid ratio of the magnolia flower powder to the subcritical fluid is 1.1-1;
(4) after extraction, introducing subcritical fluid in the extraction tank into a separation tank to separate with flos Magnoliae oil to extract effective components in flos Magnoliae granule, wherein the pressure in the separation tank is maintained at 0-10MPa, the pressure in the separation tank is less than that in the extraction tank, and the temperature is maintained at 30-50 deg.C;
(5) repeating the separation procedure in (4), wherein the separation time of each time lasts for 45-90 minutes;
(6) after the separation is finished, the pressure in the tank is reduced to 0MPa, the magnolia flower oil is collected from the bottom of the extraction tank and the separation tank, and the subcritical fluid in the separation tank is recovered for recycling.
This scheme is further illustrated in the following examples:
example 1
Firstly, selecting 50g of magnolia flower, washing with water to remove impurities, and draining; drying the cleaned flos Magnoliae at 50-80 deg.C for 2-7 hr until the water content of flos Magnoliae is less than 10%;
secondly, crushing the dried magnolia flowers, and sieving the crushed magnolia flowers through a 20-mesh sieve to obtain magnolia flower powder with a proper size;
thirdly, preheating the extraction tank to 30 ℃, placing the screened flos magnoliae pollen powder into the extraction tank, vacuumizing the extraction tank, introducing subcritical fluid butane into the extraction tank from the liquid storage tank after the vacuum degree is 0.8MPa, setting the material-liquid ratio of the flos magnoliae powder to the subcritical fluid butane to be 1.1, setting the extraction temperature to be 35 ℃, setting the extraction time to be 12 hours, and extracting to obtain flos magnoliae oil;
fourthly, after extraction is finished, introducing subcritical fluid butane in the extraction tank into a separation tank to be separated from the magnolia flower oil, and keeping the pressure in the separation tank at 0.5MPa and the temperature at 30 ℃ to extract effective components in the magnolia flower particles;
fifthly, the separation procedure of the separation tank is repeated, and each separation is kept for 90 minutes;
and finally, collecting the separated magnolia flower oil from the bottoms of the extraction tank and the separation tank, and recovering subcritical fluid butane in the separation tank through a condensation tank for recycling.
The magnolia flower oil was collected and weighed 17g, and the oil yield was 34%.
The basic structure of the screen, the separating tank, the extracting tank, the liquid storage tank and the condensing tank used in the above steps can adopt the existing screen, separating tank, extracting tank, liquid storage tank and condensing tank, and will not be described in detail herein.
Example 2
Firstly, selecting 50g of magnolia flower, washing with water to remove impurities, and draining; drying the cleaned flos Magnoliae at 50-80 deg.C for 2-7 hr until the water content of flos Magnoliae is less than 10%;
secondly, crushing the dried magnolia flowers, and sieving the crushed magnolia flowers with a 25-mesh sieve to obtain magnolia flower powder with a proper size;
thirdly, preheating the extraction tank to 60 ℃, placing the screened flos magnoliae pollen powder into the extraction tank, vacuumizing the extraction tank, introducing subcritical fluid methane into the extraction tank from the liquid storage tank after the vacuum degree is 10MPa, setting the material-liquid ratio of the flos magnoliae powder to the subcritical fluid methane to be 1.8, setting the extraction temperature to be 65 ℃, setting the extraction time to be 10 hours, and extracting to obtain flos magnoliae oil;
fourthly, after extraction is finished, introducing subcritical fluid methane in the extraction tank into a separation tank to be separated from the magnolia flower oil, keeping the pressure in the separation tank at 8MPa and the temperature at 50 ℃ to extract effective components in the magnolia flower particles;
fifthly, the separation procedure of the separation tank is repeated, and each separation is kept for 45 minutes;
and finally, after the separation is finished, reducing the pressure in the extraction tank to 0MPa, collecting the separated magnolia flower oil from the bottoms of the extraction tank and the separation tank, and recovering the subcritical fluid methane in the separation tank through a condensation tank for recycling.
The weight of the collected magnolia flower oil was 18.6g, and the oil yield was 37.2%.
Example 3
Firstly, selecting 50g of magnolia flowers, washing with water to remove impurities, and draining; drying the cleaned flos Magnoliae at 50-80 deg.C for 2-7 hr until the water content of flos Magnoliae is less than 10%;
secondly, crushing the dried magnolia flowers, and sieving the crushed magnolia flowers through a 25-mesh sieve to obtain magnolia flower powder with a proper size;
thirdly, preheating the extraction tank to 40 ℃, placing the screened flos magnoliae pollen powder in the extraction tank, vacuumizing the extraction tank, introducing subcritical fluid ethane into the extraction tank from the liquid storage tank after the vacuum degree is 5MPa, setting the material-liquid ratio of the flos magnoliae powder to subcritical fluid methane to be 1.5, setting the extraction temperature to be 45 ℃, and setting the extraction time to be 10 hours;
fourthly, after extraction is finished, introducing subcritical fluid ethane in the extraction tank into a separation tank to be separated from the magnolia flower oil, keeping the pressure in the separation tank at 3MPa and the temperature at 45 ℃ to extract effective components in the magnolia flower particles;
fifthly, the separation procedure of the separation tank is repeated, and each separation is kept for 60 minutes;
and finally, after the separation is finished, reducing the pressure in the tank to 0MPa, collecting the separated magnolia flower oil from the bottoms of the extraction tank and the separation tank, and recovering subcritical fluid ethane in the separation tank through a condensation tank for recycling.
The weight of collected magnolia flower oil was 16.7g, and the oil yield was 33.4%.
Example 4
Firstly, selecting 50g of magnolia flowers, washing with water to remove impurities, and draining; drying the cleaned flos Magnoliae at 50-80 deg.C for 2-7 hr until the water content of flos Magnoliae is less than 10%;
secondly, crushing the dried magnolia flowers, and sieving the crushed magnolia flowers through a 25-mesh sieve to obtain magnolia flower powder with a proper size;
thirdly, preheating an extraction tank, preheating the extraction tank to 50 ℃, placing the granules manufactured by the granulator into the extraction tank, vacuumizing the extraction tank, introducing subcritical fluid propane into the extraction tank from a liquid storage tank after the vacuum degree is 10MPa, setting the material-liquid ratio of magnolia flower powder to subcritical fluid methane to be 1.7, setting the extraction temperature to be 55 ℃, and setting the extraction time to be 6 hours;
fourthly, after extraction is finished, introducing subcritical fluid propane in the extraction tank into a separation tank to be separated from the magnolia flower oil, and keeping the pressure in the separation tank at 8MPa and the temperature at 40 ℃ to extract effective components in the magnolia flower particles;
fifthly, the separation procedure of the separation tank is repeated, and each separation is kept for 40 minutes;
and finally, after the separation is finished, reducing the pressure in the extraction tank to 0MPa, collecting the separated magnolia flower oil from the bottoms of the extraction tank and the separation tank, and recovering subcritical fluid propane in the separation tank through a condensation tank for recycling.
The magnolia flower oil is collected and weighed as 17.9g, and the oil yield is 35.8%.
Example 5
Firstly, selecting 50g of magnolia flowers, washing with water to remove impurities, and draining; drying the cleaned flos Magnoliae at 50-80 deg.C for 2-7 hr until the water content of flos Magnoliae is less than 10%;
secondly, crushing the dried magnolia flowers, and sieving the crushed magnolia flowers with a 25-mesh sieve to obtain magnolia flower powder with a proper size;
thirdly, preheating an extraction tank, preheating the extraction tank to 50 ℃, placing the particles manufactured by the granulator into the extraction tank, vacuumizing the extraction tank, introducing subcritical fluid tetrafluoroethane into the extraction tank from a liquid storage tank after the vacuum degree reaches 10MPa, setting the material-liquid ratio of magnolia flower powder to subcritical fluid methane to be 1.2, setting the extraction temperature to be 60 ℃, and setting the extraction time to be 8 hours;
fourthly, after extraction is finished, introducing subcritical fluid tetrafluoroethane in the extraction tank into a separation tank to be separated from the magnolia flower oil, and keeping the pressure in the separation tank at 8MPa and the temperature at 35 ℃ to extract effective components in the magnolia flower particles;
fifthly, the separation procedure of the separation tank is repeated, and each separation is kept for 50 minutes;
and finally, after the separation is finished, reducing the pressure in the extraction tank to 0MPa, collecting the separated magnolia flower oil from the bottoms of the extraction tank and the separation tank, and recovering subcritical fluid tetrafluoroethane in the separation tank through a condensation tank for recycling.
The weight of the collected magnolia flower oil was 18.2g, and the oil yield was 36.4%.
Based on the above tests, the oil yield of the magnolia oil extracted by the extraction method is about 33-38%.
It should be noted that, unless otherwise defined, technical terms or scientific terms used herein should have the ordinary meaning as understood by those having ordinary skill in the art to which the present invention belongs.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This application is intended to cover any uses or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
It will be understood that the present invention is not limited to the structures that have been described above and shown in the drawings, and that various modifications and changes can be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.
Claims (4)
1. A method for extracting magnolia flower oil is characterized by at least comprising the following processes:
(1) selecting and preparing raw materials, namely selecting magnolia flower, cleaning with water to remove impurities, and draining; drying the cleaned flos Magnoliae at 50-80 deg.C for 2-7 hr until the water content of flos Magnoliae is less than 10%;
(2) pulverizing dried flos Magnoliae, and sieving with 20-25 mesh sieve to obtain flos Magnoliae powder with appropriate size;
(3) preheating an extraction tank, placing screened flos Magnoliae pollen powder into the extraction tank after the extraction tank is preheated to the temperature close to the extraction temperature, vacuumizing the extraction tank, and enabling the vacuum degree to be 0-10MPa; introducing subcritical fluid into an extraction tank, wherein the material-liquid ratio of the magnolia flower powder to the subcritical fluid is 1.1-1;
(4) after extraction, introducing subcritical fluid in the extraction tank into a separation tank to separate with flos Magnoliae oil to extract effective components in flos Magnoliae granules, wherein the pressure in the separation tank is maintained at 0-10MPa, the pressure in the separation tank is less than the pressure in the extraction tank, and the temperature is maintained at 30-50 deg.C;
(5) repeating the separation procedure in (4), wherein the separation time of each time lasts for 45-90 minutes;
(6) after the separation is finished, the pressure in the tank is reduced to 0MPa, the magnolia flower oil is collected from the bottom of the extraction tank and the separation tank, and the subcritical fluid in the separation tank is recovered for recycling.
2. The method for extracting magnolia oil according to claim 1, wherein the subcritical fluid medium introduced in (3) comprises one or more mixtures of butane, tetrafluoroethane, propane, ethane, and methane.
3. A Magnolia flower oil prepared by the method for extracting Magnolia flower oil according to claim 1 or 2.
4. A magnolia oil product comprising the magnolia oil of claim 3, prepared by the method for extracting the magnolia oil of claim 1 or claim 2.
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Citations (8)
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CN111777691A (en) * | 2020-08-04 | 2020-10-16 | 河南白云牧港生物科技有限公司 | Extraction method of magnolia flower polysaccharide |
CN113925901A (en) * | 2021-12-03 | 2022-01-14 | 周淑菲 | Essential oil composition for treating nasosinusitis and preparation method thereof |
CN114246925A (en) * | 2020-09-22 | 2022-03-29 | 香港科技大学 | Traditional Chinese medicine essential oil and application thereof |
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2022
- 2022-09-14 CN CN202211115233.7A patent/CN115449422A/en active Pending
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102919390A (en) * | 2012-11-05 | 2013-02-13 | 晨光生物科技集团股份有限公司 | Preparation method of cooked flavor spice seasoning oil |
CN104083441A (en) * | 2014-06-16 | 2014-10-08 | 南京泽朗医药科技有限公司 | Flos magnoliae volatile oil extraction method |
CN104357216A (en) * | 2014-10-22 | 2015-02-18 | 西安米亿生物科技有限公司 | Method for extracting essential oil from magnolia flower |
CN105815462A (en) * | 2016-04-15 | 2016-08-03 | 合肥珠光粮油贸易有限公司 | Portulaca oleracea and rice bran blend oil capable of improving eyesight and removing toxic substances |
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CN111777691A (en) * | 2020-08-04 | 2020-10-16 | 河南白云牧港生物科技有限公司 | Extraction method of magnolia flower polysaccharide |
CN114246925A (en) * | 2020-09-22 | 2022-03-29 | 香港科技大学 | Traditional Chinese medicine essential oil and application thereof |
CN113925901A (en) * | 2021-12-03 | 2022-01-14 | 周淑菲 | Essential oil composition for treating nasosinusitis and preparation method thereof |
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