CN113416605A - Hydrolat extraction method and hydrolat extraction device - Google Patents
Hydrolat extraction method and hydrolat extraction device Download PDFInfo
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Images
Classifications
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/003—Filters in combination with devices for the removal of liquids
- B01D36/008—Means to filter or treat the separated liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/025—Reverse osmosis; Hyperfiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/04—Feed pretreatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/08—Apparatus therefor
-
- 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
-
- 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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- 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
- C11B9/027—Recovery of volatiles by distillation or stripping
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Water Supply & Treatment (AREA)
- Nanotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a method and a device for concentrating hydrolat. The method comprises a hydrolat extraction system, a membrane separation and impurity removal system and a membrane concentration system. 1) Putting the plant raw materials into a distillation retort, distilling with steam, condensing the distilled steam into distilled water, and separating to obtain essential oil and low-concentration hydrolat, wherein the hydrolat is generated in the form of nearly colorless distilled water. 2) And filtering the low-concentration hydrolat through a ceramic membrane system, clarifying, removing impurities and sterilizing the low-concentration hydrolat by utilizing a ceramic membrane, and removing suspended matters, insoluble impurities and the like to obtain the ceramic membrane permeate of the low-concentration hydrolat. 3) And concentrating the ceramic membrane permeate through an organic membrane system to obtain a high-concentration hydrolat concentrated solution.
Description
Technical Field
The invention relates to a hydrolat extraction method and device, and belongs to the technical field of plant extraction.
Background
The hydrolat is called aromatic water or aromatic distilled water, such as rose hydrolat and lavender hydrolat. Most of plant essential oils have low solubility in water, and when the essential oils are prepared by steam distillation in actual production, a part of plant essential oils and some small-molecule aromatic substances are dissolved in water, for example, when the rose essential oils are prepared, the main aromatic component of phenethyl alcohol is partially dissolved in water, so that rose hydrosol is formed. The rose hydrosol is a pure natural product without any essence, humectant, preservative and the like, so the rose hydrosol is particularly mild and safe. The rose hydrosol contains a large amount of volatile aromatic components of roses, and the components of the rose hydrosol are particularly complex, more than about 300, and mainly comprise alcohol, aldehyde, acid, ester, ether and the like. The rose hydrosol has the functions of purifying skin, quickly diminishing inflammation, resisting allergy, relieving itching, resisting aging and the like.
A large amount of rose hydrosol is produced during industrial production of rose essential oil, and the rose hydrosol is generally directly discharged as production wastewater because the value of the rose hydrosol is ignored in the past. Nowadays, the rose hydrosol can be developed into toning lotion, skin disinfectant, air freshener and the like with certain effects. Compared with the rose essential oil product, the rose hydrosol has large market demand and high development value. The rose hydrosol product in the market has low concentration of aromatic substances, is only used as a rose essential oil byproduct, is not further concentrated generally, and has low additional value. The traditional rotary evaporation method has high energy consumption and long time consumption, and the newly developed advanced technologies such as supercritical extraction, molecular distillation and the like need to invest in expensive equipment, so the processing cost is high. Therefore, the cost of both the traditional method and the recent advanced technology is too high, and the seeking of a concentration method with simple and feasible process, small equipment investment and low cost is imperative.
Disclosure of Invention
The invention aims to provide a method and a device for concentrating hydrolat, which are particularly suitable for preparing rose hydrolat and can solve the problems of high energy consumption, high cost and long time consumption in the concentration of the rose hydrolat; the concentration method is stable and scientific, has higher automation degree and is more suitable for industrial production.
A first object of the present invention provides:
a hydrolat extraction method comprises the following steps:
and 4, concentrating the organic matters in the filtrate obtained in the step 3 by adopting an organic membrane, wherein the concentrated solution is hydrolat.
In one embodiment, the plant material includes, but is not limited to, cinnamon, lavender, thyme, jasmine, rosemary, tea, bay leaf, or an extract portion of wormwood.
In one embodiment, the extraction site is a petal, shoot or leaf.
In one embodiment, the method further comprises the step of subjecting the filtrate obtained in the step 3 to ethanol concentration conditions such that the concentration of ethanol in the filtrate is 2 to 5 vol%.
In one embodiment, the method further comprises the step of removing low boiling substances by evaporating the pure dew obtained in the step 4 under reduced pressure.
In one embodiment, the step 1, the extraction is steam extraction, evaporation extraction or water extraction.
In one embodiment, the operating parameters of the steam extraction are: introducing steam for 1-15 hr, and extracting for 1-5 times.
In one embodiment, the step 1 further comprises a step of condensing the extract obtained by the extraction.
In one embodiment, in the step 2, standing separation is adopted in the oil-water separation process, the upper layer is an oil phase, and the lower layer is a water phase.
In one embodiment, in the step 3, the filtration for impurity removal is performed by using a separation membrane.
In one embodiment, the separation membrane is a ceramic membrane having an average pore size of 8-2000nm and a channel diameter of 1-6 mm.
In one embodiment, the operating parameters of the ceramic membrane are: the operating pressure is 0.1-0.4MPa, and the concentration multiple is more than 5 times.
In one embodiment, in the step 4, the organic membrane is a nanofiltration membrane or a reverse osmosis membrane, and the molecular weight cut-off of the organic membrane is less than 200 Da.
A hydrolat extraction device comprising:
the extraction equipment is used for extracting essential oil in the plant raw materials;
the condenser is connected with the gas phase outlet of the extraction equipment and is used for condensing the steam obtained in the extraction equipment;
the layering tank is connected with the condenser and used for layering the condensate obtained by the condenser to obtain an oil layer and a water layer;
the solid-liquid separation membrane is connected with the layering tank and is used for filtering and removing impurities from the water layer obtained in the layering tank;
and the organic membrane is connected to the permeation side of the solid-liquid separation membrane and is used for concentrating organic matters in the permeation liquid obtained by the solid-liquid separation membrane to obtain the hydrolat.
In one embodiment, further comprising: and the ethanol adding tank is connected to the feed inlet of the organic membrane and is used for adding ethanol into the penetrating fluid obtained from the solid-liquid separation membrane.
In one embodiment, further comprising: and the reduced pressure evaporator is used for carrying out reduced pressure distillation on the hydrolat obtained from the organic membrane to remove the ethanol with low boiling point.
In one embodiment, the extraction apparatus is a distillation tank.
In one embodiment, the solid-liquid separation membrane is a ceramic membrane, the average pore diameter ranges from 8nm to 1200nm, and the diameter of a channel is 1 mm to 6 mm.
In one embodiment, the organic membrane is a nanofiltration membrane or a reverse osmosis membrane with a molecular weight cut-off of less than 200 Da.
Advantageous effects
The invention provides a method and a device for concentrating rose hydrosol. The membrane integration technology replaces the traditional concentration methods such as rotary evaporation, supercritical extraction and molecular distillation, the novel process avoids the problems of large equipment investment, high energy consumption, long time consumption and the like, simultaneously improves the product quality, has higher automation degree, shortens the production period and realizes the green, environment-friendly and energy-saving manufacture of the rose hydrosol.
In the method, the ceramic membrane is used for purifying the water phase after distillation extraction and oil-water separation, so that the water phase can be effectively suitable for concentration of the organic membrane, the volatile aromatic substances in the water phase are successfully concentrated, and the high-purity rose hydrosol is obtained.
In the invention, the ceramic membrane is purified by adding water for dialysis, so that the main components such as phenethyl alcohol and the like are effectively eluted and enter the permeation side of the ceramic membrane, and the concentration of the phenethyl alcohol in the final rose hydrosol is improved.
According to the invention, the concentration of ethanol in the penetrating fluid of the ceramic membrane is utilized to adjust, the ethanol can have the function of shrinking membrane pores on the polymer membrane of the organic membrane system, the retention rate of molecules such as phenethyl alcohol is improved, the component concentration in the product is improved, and the ethanol and the phenethyl alcohol with higher boiling point and the like can be separated in a reduced pressure distillation mode.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a diagram of the apparatus of the present invention;
FIG. 3 is a GC spectrum of the rose hydrosol obtained by extraction.
Wherein, 1, extracting equipment; 2. a condenser; 3. a layering tank; 4. a solid-liquid separation membrane; 5. an organic film; 6. adding ethanol into the tank; 7. a pressure reducing evaporator.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments. It will be understood by those skilled in the art that the following examples are illustrative of the present invention only and should not be taken as limiting the scope of the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
The recitation of values by ranges is to be understood in a flexible manner to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. For example, a "ceramic membrane filter element having a pore size in the range of 8 to 1200 nm" should be understood to include not only the specifically recited range of 8 to 1200nm, but also other pore sizes (e.g., 4nm, and 5 nm) and sub-ranges (e.g., 50 to 1200nm, 1 to 8nm, 20 to 500 nm) within the indicated range.
Reference throughout this specification to "one embodiment," "another embodiment," "an implementation," or the like, means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment described generally throughout this application. The appearances of the same phrase in various places in the specification are not necessarily all referring to the same embodiment. Further, when a particular feature, structure, or characteristic is described in connection with any embodiment, it is submitted that it is within the purview of this application to effect such feature, structure, or characteristic in connection with other ones of the embodiments.
The hydrosol to be concentrated in the invention is rose hydrosol, including but not limited to rose hydrosols such as cinnamon hydrosol, lavender hydrosol, thyme hydrosol, jasmine hydrosol, rosemary hydrosol, tea plant hydrosol, laurel leaf hydrosol, wormwood hydrosol and the like.
The extraction method of the invention is as follows:
step 1: putting the picked plant raw materials into a distillation retort, and distilling with steam; the purpose of this step is to extract the steam extractable cost of the plant material by distillation, which can be achieved with a corresponding essential oil cost. In the invention, rose petals can be used as raw materials, and corresponding rose essential oil extraction products can be obtained; similarly, the extract of cinnamon, lavender, thyme, jasmine, rosemary, tea, bay leaf or wormwood, which may be petals, branches or leaves, may be used. As preferred parameters for this step, steam distillation refers to two distillations, the parameters are: introducing water vapor, distilling for 5h for the first time, and stopping distilling and standing for 1 h. And introducing steam for the second time for distillation, wherein the distillation time is 3 h.
Step 2: introducing the distilled steam into a cooling system for condensation to obtain distillate; in this step, volatile extractable essential oil is obtained by condensing the components obtained in the distillation extraction mode. As the preferable parameters in the step, the cooling system is that normal-temperature or low-temperature tap water is introduced into a condensing pipe for cooling, and the distillate is condensed by utilizing temperature difference.
In addition, the hydrolat to be treated by the invention is mainly produced by a distillation method, and includes but is not limited to hydrolat produced by a distillation method, such as hydrolat, rotary evaporation and the like.
And 3, step 3: introducing distilled water into an oil-water separator. Under the condition of low temperature, the rose essential oil floats on the upper part and the distilled water is under the lower part due to different densities. Extracting rose essential oil into an essential oil storage container to obtain the low-concentration rose hydrosol. The purpose of this step is to allow the essential oil obtained to be separated from the water initially, but the water still contains a certain amount of volatile organic components, which need to be recycled again. The oil-water separator is a storage tank with a jacket, the storage tank can be filled with cooling water or chilled water for cooling, a discharge valve is arranged at the upper end of the storage tank, and a discharge valve is arranged at the bottom of the storage tank. The upper end valve is used for collecting rose essential oil, and the tank bottom valve is used for collecting low-concentration rose hydrosol.
And 4, step 4: clarifying, removing impurities and degerming the low-concentration rose hydrosol by a ceramic membrane system, and removing suspended matters, insoluble impurities and the like to obtain ceramic membrane permeate of the low-concentration rose hydrosol; the purpose of this step is to carry out preliminary membrane filtration purification to the hydrolat that obtains, can remove the suspended solid in the hydrolat effectively, and other colloid materials play the effect of preliminary treatment for subsequent membrane concentration process. The ceramic membrane system is a ceramic membrane filter element which adopts multi-channel strong acid, strong base and high temperature resistance and is incompatible with an organic solvent, the aperture of the ceramic membrane filter element is 8-1200 nm, more preferably 50nm, and the diameter of the channel is 1-6 mm. The operating pressure of the ceramic membrane system is 0.1-0.4Mpa, and the concentration multiple is more than 5 times.
And 5, step 5: and concentrating the ceramic membrane permeate by adopting an organic membrane system to obtain a high-concentration rose hydrosol concentrated solution. The purpose of this step is to concentrate the effective component of purified pure dew, and the organic membrane used here can be a nanofiltration membrane with small molecular weight cut-off or a reverse osmosis membrane. When a nanofiltration membrane is used, the cut-off molecular weight is preferably controlled to be less than 200 Da. When concentrating, as the preferred parameter, ethanol can be added into the hydrolat, and the ethanol content of the hydrolat is adjusted to 5-10 vol%, so that the polymer membrane material can be slightly swelled, and the retention effect on volatile aroma components can be effectively improved. For rose hydrosol, the main volatile aroma components are as follows: the beta-phenethyl alcohol, the citronellol, the geraniol, the eugenol, the linalool and the rose ether, and for the macromolecular alcohols which are main components, the retention and concentration rate of aroma components can be higher through the addition treatment of the ethanol, so that the purity of the finally obtained product is improved.
Based on the above steps, the apparatus provided by the present invention, as shown in fig. 2, includes:
the extraction equipment 1 is used for extracting essential oil in plant raw materials;
the condenser 2 is connected to the gas phase outlet of the extraction equipment 1 and is used for condensing the steam obtained in the extraction equipment 1;
the layering tank 3 is connected to the condenser 2 and used for layering the condensate obtained by the condenser 2 to obtain an oil layer and a water layer;
the solid-liquid separation membrane 4 is connected to the layering tank 3 and is used for filtering and removing impurities from the water layer obtained in the layering tank 3;
and an organic membrane 5 connected to the permeate side of the solid-liquid separation membrane 4, for concentrating organic substances in the permeate obtained by the solid-liquid separation membrane 4 to obtain a purified water.
In one embodiment, the extraction apparatus 1 is a distillation tank.
In one embodiment, the solid-liquid separation membrane 4 is a ceramic membrane, the average pore diameter ranges from 8nm to 1200nm, and the diameter of a channel is 1 mm to 6 mm.
In one embodiment, the organic membrane 5 is a nanofiltration membrane or a reverse osmosis membrane, and the molecular weight cut-off is less than 200 Da.
In one embodiment, further comprising: and the ethanol adding tank 6 is connected to a feed inlet of the organic membrane 5 and is used for adding ethanol into the penetrating fluid obtained in the solid-liquid separation membrane 4.
In one embodiment, further comprising: and a reduced pressure evaporator 7 for distilling the pure dew obtained in the organic film 5 under reduced pressure to remove ethanol with a low boiling point.
In the invention, the content of the obtained rose hydrosol is tested, the main components and the content of the rose hydrosol are analyzed by gas chromatography, and the chromatographic conditions are as follows: GC-14C gas chromatograph is adopted, an SPB-5 (30 mm multiplied by 0.25 mu m) capillary column is adopted, the carrier gas is nitrogen, and the split ratio is 70: 1, the temperature of the FID detector is 240 ℃, the temperature of the gasification chamber is 255 ℃, the heating rate is 4 ℃/min, and the sample injection amount is 1.0 mu L.
Example 1
1. Putting the picked rose petals into a distillation retort, introducing water vapor, distilling for 5h for the first time, and stopping distilling and standing for 1 h. And introducing steam for the second time for distillation, wherein the distillation time is 3 h.
2. And introducing the distilled steam into a cooling system for condensation to obtain distilled water.
3. Introducing distilled water into an oil-water separator. Under the condition of low temperature, the rose essential oil floats on the upper part and the distilled water is under the lower part due to different densities. Extracting rose essential oil into an essential oil storage container to obtain the low-concentration rose hydrosol.
4. And (3) clarifying, impurity removing and degerming the obtained low-concentration rose hydrosol by using a ceramic membrane system, removing suspended matters, insoluble impurities and the like, wherein the aperture of a ceramic membrane filter element is 50 nanometers, the diameter of a channel is 4 millimeters, the membrane surface flow rate is 4m/s, the system operation pressure is 0.3Mpa, and the concentration multiple is 10 times, so that the low-concentration rose hydrosol ceramic membrane permeate is obtained.
5. And (3) concentrating the obtained low-concentration rose hydrosol ceramic membrane permeate through an organic membrane system. The special organic membrane filter element is made of a high-molecular composite material, the molecular weight cut-off is about 100Da, the system operation pressure is 2.0Mpa, and the concentration multiple is 20 times, so that the high-concentration rose hydrosol concentrated solution is obtained.
Example 2
1. Putting the picked rose petals into a distillation retort, introducing water vapor, distilling for 5h for the first time, and stopping distilling and standing for 1 h. And introducing steam for the second time for distillation, wherein the distillation time is 3 h.
2. And introducing the distilled steam into a cooling system for condensation to obtain distilled water.
3. Introducing distilled water into an oil-water separator. Under the condition of low temperature, the rose essential oil floats on the upper part and the distilled water is under the lower part due to different densities. Extracting rose essential oil into an essential oil storage container to obtain the low-concentration rose hydrosol.
4. And (3) clarifying, impurity removing and degerming the obtained low-concentration rose hydrosol by using a ceramic membrane system, removing suspended matters, insoluble impurities and the like, wherein the aperture of a ceramic membrane filter element is 30 nanometers, the diameter of a channel is 4 millimeters, the membrane surface flow rate is 4m/s, the system operation pressure is 0.4Mpa, and the concentration multiple is 8 times, so that the low-concentration rose hydrosol ceramic membrane permeate is obtained.
5. And (3) concentrating the obtained low-concentration rose hydrosol ceramic membrane permeate through an organic membrane system. The organic membrane filter element is made of a high-molecular composite material, the molecular weight cut-off is about 100Da, the system operation pressure is 2.0Mpa, and the concentration multiple is 20 times, so that the high-concentration rose hydrosol concentrated solution is obtained.
Example 3
The difference from example 2 is that: and adding pure water for dialysis treatment in the ceramic membrane system treatment process.
1. Putting the picked rose petals into a distillation retort, introducing water vapor, distilling for 5h for the first time, and stopping distilling and standing for 1 h. And introducing steam for the second time for distillation, wherein the distillation time is 3 h.
2. And introducing the distilled steam into a cooling system for condensation to obtain distilled water.
3. Introducing distilled water into an oil-water separator. Under the condition of low temperature, the rose essential oil floats on the upper part and the distilled water is under the lower part due to different densities. Extracting rose essential oil into an essential oil storage container to obtain the low-concentration rose hydrosol.
4. And (3) clarifying, impurity removing and degerming the obtained low-concentration rose hydrosol through a ceramic membrane system, removing suspended matters, insoluble impurities and the like, wherein the aperture of a ceramic membrane filter element is 30 nanometers, the diameter of a channel is 4 millimeters, the flow rate of a membrane surface is 4m/s, the operating pressure of the system is 0.4Mpa, pure water dialysis is added when the concentration multiple is 8 times, and the addition is 2 times of that of the concentrated solution, so that the low-concentration rose hydrosol ceramic membrane permeate is obtained.
5. And (3) concentrating the obtained low-concentration rose hydrosol ceramic membrane permeate through an organic membrane system. The organic membrane filter element is made of high molecular material, the molecular weight cut-off is about 100Da, the system operation pressure is 2.0Mpa, and the concentration multiple is 20 times, so that the high-concentration rose hydrosol concentrated solution is obtained.
Example 4
The difference from example 3 is that: adjusting the permeation of the ceramic membrane, adding ethanol, and then delivering the ceramic membrane into an organic membrane system for concentration.
1. Putting the picked rose petals into a distillation retort, introducing water vapor, distilling for 5h for the first time, and stopping distilling and standing for 1 h. And introducing steam for the second time for distillation, wherein the distillation time is 3 h.
2. And introducing the distilled steam into a cooling system for condensation to obtain distilled water.
3. Introducing distilled water into an oil-water separator. Under the condition of low temperature, the rose essential oil floats on the upper part and the distilled water is under the lower part due to different densities. Extracting rose essential oil into an essential oil storage container to obtain the low-concentration rose hydrosol.
4. And (3) clarifying, impurity removing and degerming the obtained low-concentration rose hydrosol through a ceramic membrane system, removing suspended matters, insoluble impurities and the like, wherein the aperture of a ceramic membrane filter element is 30 nanometers, the diameter of a channel is 4 millimeters, the flow rate of a membrane surface is 4m/s, the operating pressure of the system is 0.4Mpa, pure water dialysis is added when the concentration multiple is 8 times, and the addition is 2 times of that of the concentrated solution, so that the low-concentration rose hydrosol ceramic membrane permeate is obtained.
5. And (3) adjusting the ethanol concentration of the obtained low-concentration rose hydrosol ceramic membrane permeate to 5 vol%, and concentrating by an organic membrane system. The organic membrane filter element is made of high molecular material, the molecular weight cut-off is about 100Da, the system operation pressure is 2.0Mpa, the concentration multiple is 20 times, high-concentration rose hydrosol concentrated solution is obtained, and the concentrated solution is distilled under the low-temperature condition to remove ethanol with low boiling point.
Comparative example 1
In contrast to example 1, no special organic membrane system was used for concentration during membrane system treatment.
1. Putting the picked rose petals into a distillation retort, introducing water vapor, distilling for 5h for the first time, and stopping distilling and standing for 1 h. And introducing steam for the second time for distillation, wherein the distillation time is 3 h.
2. And introducing the distilled steam into a cooling system for condensation to obtain distilled water.
3. Introducing distilled water into an oil-water separator. Under the condition of low temperature, the rose essential oil floats on the upper part and the distilled water is under the lower part due to different densities. Extracting rose essential oil into an essential oil storage container to obtain the low-concentration rose hydrosol.
4. And (3) clarifying, impurity removing and sterilizing the obtained low-concentration rose hydrosol by a ceramic membrane system, removing suspended matters, insoluble impurities and the like, wherein the aperture of a ceramic membrane filter element is 50 nanometers, the diameter of a channel is 4 millimeters, the membrane surface flow rate is 4m/s, the system operation pressure is 0.3Mpa, and the concentration multiple is 10 times, so that the rose hydrosol ceramic membrane permeate is obtained.
The main volatile components of the rose hydrosol obtained in the above steps were detected by gas chromatography, and the results are shown in the following table:
taking example 4 as an example, the gas chromatogram of the obtained rose essential oil is shown in fig. 3, wherein the main volatile components are: ethanol (peak 1), 1-bromobenzene (peak 2), linalool (peak 3), phenethyl alcohol (peak 4), citronellol (peak 5). Wherein the ethanol is mainly introduced from the previous steps, and part of ethanol is trapped after reduced pressure distillation.
As seen from the table, the main component is phenethyl alcohol, and the comparison between the example 1 and the comparative example 1 shows that the content of the phenethyl alcohol in the pure dew is increased from 900mg/L to 169900 mg/L after the concentration treatment of the organic membrane, which indicates that the organic membrane concentration method of the invention can effectively recover the effective components in the rose pure dew, improve the concentration of the phenethyl alcohol and obtain the high-purity product. It can be seen by comparing example 1 with example 2 that when the pore size of the ceramic membrane filter element is reduced, the main component beta-phenylethyl alcohol of rose hydrosol is trapped. It can be seen from the comparison between example 2 and example 3 that, when the ceramic membrane system is used for clarifying and removing impurities from distilled water, a certain proportion of pure water is added for dialysis and then the pure water is concentrated by the special organic membrane system, so that the rose hydrosol content can be increased. It can be seen from the comparison between example 3 and example 4 that when ethanol is applied to the feed liquid entering the organic membrane system, the shrinkage of the membrane pores of the organic membrane can be caused, and the retention rate of phenethyl alcohol is improved.
Claims (10)
1. The hydrolat extraction method is characterized by comprising the following steps:
step 1, extracting essential oil from plant raw materials;
step 2, performing oil-water separation on the crude essential oil obtained in the step 1;
step 3, filtering the water phase obtained in the step 2 to remove impurities;
and 4, concentrating the organic matters in the filtrate obtained in the step 3 by adopting an organic membrane, wherein the concentrated solution is hydrolat.
2. The method for extracting hydrolat according to claim 1, wherein the plant material includes but is not limited to extracted parts of cinnamon, lavender, thyme, jasmine, rosemary, tea tree, bay leaf or wormwood;
the extraction part is a petal, a branch or a leaf.
3. The method for extracting hydrolat according to claim 1, further comprising the step of subjecting the filtrate obtained in step 3 to ethanol concentration conditions such that the concentration of ethanol in the filtrate is 2-5 vol%;
further comprising the step of removing low-boiling-point substances by carrying out reduced pressure evaporation on the hydrolat obtained in the step 4;
in the step 1, the extraction adopts steam extraction, evaporation extraction or water extraction;
the operating parameters of the steam extraction are: introducing steam for 1-15 hr for 1-5 times;
the step 1 also comprises a step of condensing the extract obtained by extraction.
4. The method for extracting hydrolat according to claim 1, wherein in step 2, the oil-water separation process adopts standing separation, the upper layer is oil phase, and the lower layer is water phase.
5. The method for extracting hydrolat according to claim 1, wherein in step 3, the filtration and impurity removal are carried out by adopting a separation membrane;
the separation membrane is a ceramic membrane, the average pore diameter is 8-2000nm, and the separation membrane has a channel diameter of 1-6 mm;
the operating parameters of the ceramic membrane are as follows: the operating pressure is 0.1-0.4MPa, and the concentration multiple is more than 5 times.
6. The method for extracting the hydrolat as claimed in claim 1, wherein in the step 4, the organic membrane is a nanofiltration membrane or a reverse osmosis membrane, and the molecular weight cut-off of the organic membrane is less than 200 Da.
7. An apparatus for extracting hydrolat, comprising:
the extraction equipment (1) is used for extracting essential oil in plant raw materials;
the condenser (2) is connected to the gas phase outlet of the extraction equipment (1) and is used for condensing the steam obtained in the extraction equipment (1);
the layering tank (3) is connected to the condenser (2) and is used for layering the condensate obtained by the condenser (2) to obtain an oil layer and a water layer;
the solid-liquid separation membrane (4) is connected with the layering tank (3) and is used for filtering and removing impurities from the water layer obtained in the layering tank (3);
and an organic membrane (5) connected to the permeation side of the solid-liquid separation membrane (4) and used for concentrating organic matters in the permeation liquid obtained by the solid-liquid separation membrane (4) to obtain the hydrolat.
8. The apparatus for extracting hydrol as defined in claim 7, further comprising: the ethanol adding tank (6) is connected to a feed inlet of the organic membrane (5) and is used for adding ethanol into the penetrating fluid obtained in the solid-liquid separation membrane (4); in one embodiment, further comprising: and a reduced pressure evaporator (7) for distilling the pure dew obtained in the organic membrane (5) under reduced pressure to remove ethanol with low boiling point.
9. A hydrolat extraction device according to claim 7, characterized in that said extraction apparatus (1) is a distillation tank; the solid-liquid separation membrane (4) is a ceramic membrane, the average pore diameter ranges from 8nm to 1200nm, and the diameter of a channel is 1 mm to 6 mm.
10. The apparatus for extracting the purified dew as claimed in claim 7, wherein the organic membrane (5) is a nanofiltration membrane or a reverse osmosis membrane having a molecular weight cut-off of less than 200 Da.
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