CN111979050A - Extraction method for improving oil yield and quality of volatile plant essential oil - Google Patents
Extraction method for improving oil yield and quality of volatile plant essential oil Download PDFInfo
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- CN111979050A CN111979050A CN202010870161.1A CN202010870161A CN111979050A CN 111979050 A CN111979050 A CN 111979050A CN 202010870161 A CN202010870161 A CN 202010870161A CN 111979050 A CN111979050 A CN 111979050A
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- ultrafiltration membrane
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 58
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—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
- C11B9/027—Recovery of volatiles by distillation or stripping
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- 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)
- Separation Using Semi-Permeable Membranes (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides an extraction method for improving the oil yield and quality of volatile plant essential oil, which adopts a steam distillation extraction process and is additionally provided with a combined ultrafiltration membrane damping separator with obviously different surface properties and functions in an oil-water separation process of the extraction process. The method is characterized in that cold hydrazine is additionally arranged on a pipeline for communicating an oil-water separator with the outside, an ultrafiltration membrane damping separator with double hydrophobic surfaces is additionally arranged at an outlet of the cold hydrazine, an ultrafiltration membrane damping separator with oleophilic hydrophobic surface properties is arranged on one side, close to the oil-water separator, of a pipeline for leading an oil-water separator process to essential oil (or an essential oil receiver), an ultrafiltration membrane damping separator with hydrophilic oleophobic surface properties is additionally arranged on a pipeline for leading an oil-water separator process to a pure dew storage tank, an ultrafiltration membrane damping separator with hydrophilic oleophobic surface properties is additionally arranged on a pipeline for leading an oil-water separator process to a distillation kettle to enter a re-distillation process, and the combined ultrafiltration membrane damping separator is used for carrying out oil-water separation on essential oil extraction to the greatest extent according to different extraction processes.
Description
Technical Field
The invention relates to the technical field of essential oil extraction, in particular to an extraction method for improving the oil yield and quality of volatile plant essential oil.
Background
Plant essential oils such as rose essential oil, lavender essential oil, lemongrass essential oil, wormwood essential oil and the like all belong to secondary metabolites of plants, and are volatile oily liquids which exist in roots, stems, leaves, flowers and fruits of the plants, can be distilled along with steam and have certain odor. The extraction method of essential oil comprises steam distillation, supercritical extraction, organic solvent extraction, etc. The steam distillation method is mainly adopted for production at home and abroad at present due to the advantages of simple equipment, low price and easy availability of solvent, green and environment-friendly extraction process, easy large-scale production and the like.
The oil yield, composition and content of each component of natural plants vary greatly with plant species, extraction method, extraction process parameters, plant growth conditions, plant harvesting mode and storage mode. Natural plant essential oils contain a wide variety of components, for example, rose essential oils contain at least over 300 known or unknown components. The rose essential oil mainly comprises terpene and derivatives thereof, wherein the variety of monoterpene and derivatives thereof, sesquiterpene and derivatives thereof, diterpene and derivatives thereof is as high as hundreds, the proportion is 50-75%, and the rose essential oil also comprises alcohol, aldehyde, phenol, ketone, ester, ether, aromatic hydrocarbon, aliphatic hydrocarbon, heteropolycyclic compounds and the like.
The rose essential oil is taken as a rare natural spice extracted from fresh roses, has unique characteristics of elegant, soft, plump, mellow and smooth, elegant and elegant head fragrance, mellow and sweet tail fragrance and lasting fragrance, is always taken as a high-end spice for perfuming international first-line rare perfume and high-end cosmetics, is an indispensable raw material in the world spice industry, and has an extremely important position. Meanwhile, the natural rose essential oil also has multiple effects of resisting oxidation, whitening and fading spots, inhibiting bacteria and diminishing inflammation, resisting aging and wrinkles, soothing the nerves, resisting tumors and the like, and has great market potential. There are many varieties of natural rose essential oil at home and abroad, and the quality and the price are greatly different. Besides the difference of the rose variety and the planting method, the extraction and processing technology is also a key factor influencing the quality of the rose essential oil.
The total oil yield of the essential oil is very low, and even if the structures of a distillation kettle, a condenser and extraction parameters are fully optimized by taking a steam distillation extraction method as an example, the yield of the rose essential oil can only reach about three ten-thousandths. Therefore, the price of the pure natural essential oil is very expensive, and the consistency of the product is extremely difficult to control because the 'aroma' components of the pure natural essential oil are very complex.
Although the essential oil industry in China has a long history, the essential oil has unstable quality and low oil yield, so that the essential oil cannot occupy a place in the international market, and the essential oil industry has important significance in improving the oil yield of the rose essential oil and improving and stabilizing the quality of the essential oil.
The ultrafiltration membrane technology has been greatly developed and perfected in the twenty-first century, and the application range is rapidly expanded. The ultrafiltration technology is widely used in the fields of water purification treatment and oily sewage treatment. The use of ultrafiltration is also mentioned in some patents relating to essential oils. For example, patent application No. CN 103045364 a, "a perilla dehydration method capable of preparing perilla essential oil" refers to a method in which substances with molecular weight more than 1000 are removed by ultrafiltration membrane filtration, and components with molecular weight less than 1000 are permeated and then subjected to nanofiltration and reverse osmosis concentration steps, so as to obtain perilla essential oil and perilla distillate in the reverse osmosis concentration step. Patent application No. CN 103045367A "Lavender dehydration method capable of preparing Lavender essential oil at the same time" is also to use ultrafiltration membrane filtration step to remove substances with molecular weight more than 1000, and to pass components with molecular weight less than 1000 through nanofiltration and reverse osmosis concentration steps to obtain Lavender essential oil and Lavender essence in reverse osmosis concentration step. Both patents are used in the perilla (lavender) or drying process, the ultrafiltration technology is not directly used for oil-water separation of the perilla, but is used for removing components with molecular weight more than 1000 in condensate, and perilla essential oil and hydrolat both belong to components less than 1000 through the components with molecular weight less than 1000.
The patent application No. CN 105669800A 'a method for extracting essential oil, pectin, hesperidin, synephrine and limonin from citrus jointly' also uses an ultrafiltration technology, the patent utilizes an ultrafiltration method to separate to obtain pectin and permeate liquid passing through an ultrafiltration membrane, then the permeate liquid is extracted by ethanol reflux to obtain supernatant and filter residue, the filter residue is crystallized and freeze-dried to obtain the hesperidin; separating the supernatant with macroporous resin, and eluting with ethanol to obtain limonin.
Disclosure of Invention
The invention provides an extraction method for improving the oil yield and quality of volatile plant essential oil, solves the problems of low oil yield of the essential oil, low product quality and poor product consistency and stability, and provides a method for improving the oil yield of the essential oil and improving and stabilizing the quality of the essential oil.
The technical scheme for realizing the invention is as follows:
an extraction method for improving the oil yield and quality of volatile plant essential oil adopts a steam distillation extraction process, and a combined ultrafiltration membrane damping separator with remarkably different surface properties and functions is additionally arranged in an oil-water separation process of the extraction process. The single ultrafiltration membrane damping separator has different separation effects due to different surface properties, and can improve the oil-water separation effect in a specific process even if being used independently. The combined ultrafiltration membrane damping separator can carry out oil-water separation on essential oil extraction to the utmost extent and most effectively according to different extraction processes.
The oil-water separation process comprises an oil-water separator, wherein an external communicating pipeline, an essential oil pipeline and a pure dew pipeline are arranged on the oil-water separator, cold hydrazine is additionally arranged on the pipeline communicated with the outside of the oil-water separator, and an ultrafiltration membrane damping separator with double hydrophobic surfaces is additionally arranged at an outlet of the cold hydrazine. The ultrafiltration membrane can adopt an organic ultrafiltration membrane and an inorganic ultrafiltration membrane. Preferably, an organic polymer ultrafiltration membrane is used. Preferably, the ultrafiltration membrane is a hydrophobic and oleophobic surface modified double-hydrophobic type macromolecule ultrafiltration membrane. The ultrafiltration membrane damping separator can adopt a laminated, tubular, rolled and hollow fiber membrane. Preferably, a three-stage series laminated structure can be adopted, the laminated structure is placed in parallel, and a detachable easy-cleaning structure is adopted.
An ultrafiltration membrane damping separator with hydrophilic and oleophobic surface properties is additionally arranged on a pipeline leading to a pure dew storage tank in an oil-water separator process and close to one side of the oil-water separator, and has the remarkable effect of furthest preventing rose essential oil from being carried in rose pure dew leading to the rose pure dew storage tank. The ultrafiltration membrane can adopt an organic ultrafiltration membrane and an inorganic ultrafiltration membrane. Preferably, an organic polymer ultrafiltration membrane is used. Preferably, the ultrafiltration membrane is a hydrophilic oleophobic surface modified polymeric ultrafiltration membrane. The ultrafiltration membrane damping separator can adopt a laminated, tubular, rolled and hollow fiber membrane. Preferably, a two-stage series laminated structure can be adopted, the laminated structure is placed in parallel, and a detachable easy-to-clean structure is adopted.
An ultrafiltration membrane damping separator with oleophylic and hydrophobic surface properties is arranged on one side, close to the oil-water separator, of a pipeline leading to the essential oil (or an essential oil receiver) in the oil-water separator process. The essential oil product has the obvious effect of filtering out water phase (pure dew phase) and other impurities in the crude essential oil to the maximum extent to obtain the essential oil product. The ultrafiltration membrane can adopt an organic ultrafiltration membrane and an inorganic ultrafiltration membrane. Preferably, an organic polymer ultrafiltration membrane is used. Preferably, the ultrafiltration membrane is a polymer ultrafiltration membrane subjected to oleophilic hydrophobic surface modification. The ultrafiltration membrane damping separator can adopt a laminated, tubular, rolled and hollow fiber membrane. Preferably, a two-stage series laminated structure can be adopted, the laminated structure is placed in parallel, and a detachable easy-to-clean structure is adopted.
The oil-water separator is also provided with a re-distillation pipeline, and the re-distillation pipeline is provided with an ultrafiltration membrane damping separator with hydrophilic and oleophobic surface properties.
The ultrafiltration membrane damping separator adopts a polymer ultrafiltration membrane subjected to hydrophilic and oleophobic surface modification.
The invention has the beneficial effects that: the invention takes the rose essential oil as an example, and the specific part of the oil-water separator of the rose essential oil extraction equipment is combined with the ultrafiltration membrane damping separator with completely different surface properties, so that the rose essential oil and the rose hydrosol are separated and refined to the maximum extent, the essential oil yield is obviously improved, the fragrance quality of the essential oil is obviously improved, and the consistency of essential oil products is obviously improved. Compared with the prior art, the content of the main fragrance components of the rose essential oil extracted by additionally arranging the combined ultrafiltration membrane damping separator, including citronellol, geraniol, linalool and the like, is remarkably improved. The quality of the rose essential oil product is improved, the original prickling sense is obviously reduced, the faint scent and fresh fragrance sense are increased, and the consistency and the stability of the rose essential oil product are obviously improved.
Due to the organic combination use of the ultrafiltration membrane damping separators with completely different surface properties, the yield and the efficiency of all oil-water separation processes are obviously improved, the volatilization loss of light components in the rose essential oil, particularly in the main fragrance component, is reduced to the maximum extent, and the yield of the rose essential oil is obviously improved. The content of the main fragrant components of the rose essential oil, including citronellol, geraniol, linalool and other components, in the essential oil product is remarkably improved, the fragrance quality of the rose essential oil is remarkably improved, and the consistency and the stability of the rose essential oil product are also remarkably improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of a process flow of extracting rose essential oil by steam distillation without a re-distillation process.
FIG. 2 is a schematic diagram of a process for extracting rose essential oil by steam distillation including a re-distillation process.
FIG. 3 is a comparison of GC-MS total ion flow diagrams of rose essential oils obtained in example 19 and example 20, and the method file used in example 20 is the same as that of example 19.
FIG. 4 is a comparison of GC-MS total ion flow graphs of a total of 6 batches of rose essential oil product from example 21 using the same recipe file as in example 19.
FIG. 5 is a comparison of GC-MS total ion flow graphs of a total of 2 batches of lavender essential oil product of example 24, using the same recipe file as in example 19.
FIG. 6 is a comparison of GC-MS total ion flow graphs of 2 batches of lavender essential oil product of example 27, using the same recipe file as in example 19.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood 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 obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Taking rose as an example, the rose essential oil extraction process by steam distillation comprises the working procedures of distillation, condensation, oil-water separation and the like.
Example 1
As shown in figure 1, for the process of extracting rose essential oil by steam distillation without a re-distillation process, 1#, 2#, and 3# ultrafiltration membrane damping separators are additionally arranged on an oil-water separator.
The 1# ultrafiltration membrane damping separator is arranged on a pipeline of the oil-water separator and communicated with the outside, and is close to one side of the oil-water separator, a filter membrane in the 1# ultrafiltration membrane damping separator is a hydrophobic and oleophobic surface modified double-hydrophobic high polymer ultrafiltration membrane, and the 1# ultrafiltration membrane can adopt a laminated, tubular, rolled and hollow fiber membrane. Preferably, the No. 1 filter membrane adopts a 2-stage series laminated structure, is placed in parallel and adopts a detachable easy-to-clean structure.
The damping separator of the No. 1 ultrafiltration membrane has the remarkable effect of separating and blocking rose essential oil and rose hydrosol in the oil-water separator to the maximum extent, and simultaneously keeping the pressure balance of the whole essential oil extraction system.
The 2# ultrafiltration membrane damping separator is arranged on a pipeline leading to the rose hydrosol storage tank from the oil-water separator and is close to one side of the oil-water separator, the 2# ultrafiltration membrane is a high molecular polymer ultrafiltration membrane subjected to hydrophilic and oleophobic surface modification, and the 2# ultrafiltration membrane can adopt a laminated, tubular, rolled and hollow fiber membrane. Preferably, the 2# filter membrane adopts a 2-stage series laminated structure, is placed in parallel and adopts a detachable and easy-to-clean structure.
The remarkable effect of the No. 2 ultrafiltration membrane damping separator is to prevent and separate the rose essential oil entrained in the rose hydrosol.
The 3# ultrafiltration membrane damping separator is arranged on a pipeline leading to the rose essential oil (or the essential oil receiver) from the oil-water separator and is close to one side of the oil-water separator, and the 3# ultrafiltration membrane is a high molecular polymer ultrafiltration membrane subjected to oleophylic and hydrophobic surface modification; preferably, a polyethersulfone PES ultrafiltration membrane is used. The 3# ultrafiltration membrane can adopt a laminated, tubular, roll-type and hollow fiber membrane. Preferably, the 3# filter membrane adopts a 2-stage series laminated structure, is placed in parallel and adopts a detachable and easy-to-clean structure.
The 3# ultrafiltration membrane damping separator has the obvious function of filtering out water phase (rose pure dew phase) and other impurities in the crude rose essential oil to obtain the rose essential oil product.
Example 2
As shown in FIG. 2, for the process of extracting rose essential oil by steam distillation including a re-distillation process, 1#, 2# -1, 2# -2 and 3# ultrafiltration membrane damping separators are preferably additionally arranged on the oil-water separator.
1#, 2# -2 and 3# ultrafiltration membrane damped separators were the same as in example 1.
The 2# -1 ultrafiltration membrane damping separator is arranged on a pipeline which is communicated with a pure dew of the oil-water separator and is communicated with a distillation still for a re-distillation process, and is close to one side of the oil-water separator, the 2# -1 ultrafiltration membrane is a high molecular polymer ultrafiltration membrane subjected to hydrophilic and oleophobic surface modification, and the 2# -1 ultrafiltration membrane can adopt a laminated, tubular, rolled and hollow fiber membrane. Preferably, the 2# -1 filter membrane adopts a 2-stage series laminated structure, is placed in parallel and adopts a detachable and easy-to-clean structure.
The remarkable effect of the 2# -1 ultrafiltration membrane damping separator is to prevent and separate the rose essential oil entrained in the rose hydrosol passing through the reciprocating distillation process to the maximum extent.
Example 3
Adopting a Shandong Pingyin Fenghua No. 1 rose sample, picking fresh flowers in the new day, adding no salt, crushing, adding damping separators 1# (CRL 11020200310), 2# -1 (RL 11120190110), 2# -2 (RL 11120190110) and 3# (RL 11320190110), adopting a steam distillation extraction process shown in the figure 2 of an embodiment 2, wherein the material-liquid ratio is 1:3, carrying out co-water distillation, the extraction time is 3h, and the oil yield is 0.540 ‰.
Example 4
Adopting a Shandong Pingyin Fenghua No. 1 rose sample, picking fresh flowers in the day, adding no salt, crushing, adding combined ultrafiltration membrane damping separators 1#, 2# -1, 2# -2 and 3#, wherein the model of the filtration membrane is the same as that in example 3, the method comprises a re-distillation process, adopting the steam distillation extraction process shown in the attached figure 2 of example 2, the material-liquid ratio is 1:3, carrying out co-water distillation, the extraction time is 3h, and the oil yield is 0.473 thousandths.
Example 5
Adopting a Shandong Pingyin Fenghua No. 1 rose sample, picking fresh flowers in the new day, adding no salt, crushing, adding combined ultrafiltration membrane damping separators 1#, 2# -1, 2# -2 and 3#, wherein the model of the filtration membrane is the same as that in example 3, the method comprises a re-distillation process, adopting the steam distillation extraction process shown in the attached figure 2 of example 2, the material-liquid ratio is 1:3, carrying out co-water distillation, the extraction time is 3h, and the oil yield is 0.510 per thousand.
Example 6
Adopting a Shandong Pingyin Fenghua No. 1 rose sample, picking fresh flowers in the new day, adding no salt, crushing, adding combined ultrafiltration membrane damping separators 1#, 2# -1, 2# -2 and 3#, wherein the model of the filtration membrane is the same as that in example 3, the method comprises a re-distillation process, adopting the steam distillation extraction process shown in the attached figure 2 of example 2, the material-liquid ratio is 1:3, carrying out co-water distillation, the extraction time is 3h, and the oil yield is 0.550 per thousand.
Example 7
Adopting a Shandong Pingyin Fenghua No. 1 rose sample, picking fresh flowers in the new day, adding no salt, crushing, adding combined ultrafiltration membrane damping separators 1#, 2# -1, 2# -2 and 3#, wherein the model of the filtration membrane is the same as that in example 3, the method comprises a re-distillation process, adopting the steam distillation extraction process shown in the attached figure 2 of example 2, the material-liquid ratio is 1:3, carrying out co-water distillation, the extraction time is 3h, and the oil yield is 0.560 ‰.
Example 8
Adopting a Shandong Pingyin Fenghua No. 1 rose sample, picking fresh flowers in the new day, adding no salt, crushing, adding combined ultrafiltration membrane damping separators 1#, 2# -1, 2# -2 and 3#, wherein the model of the filtration membrane is the same as that in example 3, the method comprises a re-distillation process, adopting the steam distillation extraction process shown in the attached figure 2 of example 2, the material-liquid ratio is 1:3, carrying out co-water distillation, the extraction time is 3h, and the oil yield is 0.491 per thousand.
Example 9
Adopting a Shandong Pingyin Fenghua No. 1 rose sample, picking fresh flowers in the day, adding no salt, crushing, performing the same filtration membrane type as that in example 3, performing the re-distillation process, adopting the steam distillation extraction process (without an ultrafiltration membrane damping separator) shown in the attached figure 2 of example 2, performing water distillation with the material-liquid ratio of 1:3, extracting for 3 hours, and controlling the oil yield to be 0.366 ‰.
Example 10
Adopting a Shandong Pingyin Fenghua No. 1 rose sample, picking fresh flowers in the new day, adding no salt, crushing, performing the same filtration membrane type as in example 3, performing the re-distillation process, adopting the steam distillation extraction process (without an ultrafiltration membrane damping separator) shown in the attached figure 2 of example 2, performing water distillation with the material-liquid ratio of 1:3, extracting for 3h, and controlling the oil yield to be 0.385 per thousand.
Example 11
Fresh flowers are newly picked by adopting a Shandong Pingyin Fenghua No. 1 rose sample, 10% of salt is added for salting for 3 days, a combined ultrafiltration membrane damping separator 1#, 2# -1, 2# -2 and 3# is additionally arranged, the model of a filter membrane is the same as that in example 3, the method comprises the re-distillation process, the steam distillation extraction process shown in the attached figure 2 of example 2 is adopted, the material-liquid ratio is 1:3, the co-distillation is carried out, the extraction time is 3 hours, and the oil yield is 0.394 per thousand.
Example 12
Fresh flowers are newly picked by adopting a Shandong Pingyin Fenghua No. 1 rose sample, 10% of salt is added for salting for 3 days, a combined ultrafiltration membrane damping separator 1#, 2# -1, 2# -2 and 3# is additionally arranged, the model of a filter membrane is the same as that in example 3, the method comprises a re-distillation process, the steam distillation extraction process shown in the attached figure 2 of example 2 is adopted, the material-liquid ratio is 1:3, the co-distillation is carried out, the extraction time is 3 hours, and the oil yield is 0.388 thousandths.
Example 13
Fresh flowers are newly picked by adopting a Shandong Pingyin Fenghua No. 1 rose sample, and are salted for 3 days by adding 10% of salt, the method comprises the step of redistilling, a steam distillation extraction process (without an ultrafiltration membrane damping separator) shown in the attached figure 2 of an embodiment 2 is adopted, the material-liquid ratio is 1:3, the water distillation is carried out, the extraction time is 3 hours, and the oil yield is 0.292 permillage.
Example 14
Fresh flowers are newly picked by adopting a Shandong Pingyin Fenghua No. 1 rose sample, and are salted for 3 days by adding 10% of salt, the method comprises the step of redistilling, a steam distillation extraction process (without an ultrafiltration membrane damping separator) shown in the attached figure 2 of an example 2 is adopted, the material-liquid ratio is 1:3, the water distillation is carried out, the extraction time is 3 hours, and the oil yield is 0.306 ‰.
Example 15
A Shandong Pingyin Fenghua No. 1 rose sample is salted with 20% of salt, is stored for 60 days in a cold storage mode, is additionally provided with combined ultrafiltration membrane damping separators 1#, 2# -1, 2# -2 and 3#, the model of a filter membrane is the same as that in example 3, the steam distillation extraction process shown in the attached drawing 2 of example 2 is adopted, the material-liquid ratio is 1:3, co-distillation is carried out, the extraction time is 3 hours, and the oil yield is 0.351 permillage.
Example 16
A Shandong Pingyin Fenghua No. 1 rose sample is salted with 20% of salt, is refrigerated and stored for 60 days, is additionally provided with a combined ultrafiltration membrane damping separator 1# (CRL 11020200310), 2# (RL 11120190110) and 3# (RL 11320190110), does not comprise a re-distillation process, adopts the steam distillation extraction process shown in the attached figure 1 of the embodiment 1, has the material-liquid ratio of 1:3, and is subjected to co-hydro-distillation, the extraction time is 3 hours, and the oil yield is 0.296 permillage.
Example 17
A Shandong Pingyin Fenghua No. 1 rose sample is salted with 20% of salt, is refrigerated and stored for 60 days, comprises a re-distillation process, and adopts a water vapor distillation extraction process (without an ultrafiltration membrane damping separator) shown in figure 2 of example 2, wherein the material-liquid ratio is 1:3, the water distillation is carried out, the extraction time is 3 hours, and the oil yield is 0.165 per thousand.
Example 18
A Shandong Pingyin Fenghua No. 1 rose sample is salted with 20% of salt, is stored for 60 days in a cold storage mode, does not include a re-distillation process, adopts a steam distillation extraction process (without an ultrafiltration membrane damping separator) shown in the figure 1 of the example 1, has a material-liquid ratio of 1:3, is subjected to co-water distillation, and is extracted for 3 hours, and the oil yield is 0.151 per thousand.
Example 19
The rose essential oil sample prepared in example 3 was subjected to qualitative analysis of components by GC-MS, and quantitative analysis of each component was performed by combining external standard and area normalization methods. Wherein the chromatographic conditions are as follows: adopting an Rtx-5MS chromatographic column (30 m multiplied by 0.25mm multiplied by 0.25 mu m), the temperature of a column box is 40 ℃, and the temperature of a sample inlet is 250 ℃; high-purity helium is taken as carrier gas, and the flow rate of the carrier gas is 0.5 mL/min; line speed 44.2 cm/sec; the temperature program was set as follows: the initial temperature is 40 ℃, the temperature is kept for 5min, then the temperature is increased to 290 ℃ at the heating rate of 2 ℃/min, and the temperature is kept for 15 min; and (3) sample introduction mode: automatic sample introduction; sample introduction amount: 0.5 μ L. The mass spectrometry conditions were as follows: the temperature of an electron impact ion source (EI) is 230 ℃; the interface temperature is 280 ℃; the vacuum system is a two-stage turbo molecular pump. The obtained rose essential oil comprises the following main aroma components in percentage by weight: citronellol 11.6643%, geraniol 10.2372%, methyl eugenol 1.9965%, linalool 2.0022%, phenethyl alcohol 1.1736%, eugenol 0.8962%, nerol 0.0910%, isomeric eugenol 2.4081%, (R) - (+) -beta-citronellol 1.2157%, and 31.6848% in total.
Example 20
The rose essential oil sample prepared in example 13 was subjected to qualitative analysis of components using a GC-MS spectrometer, and quantitative analysis of each component was performed in combination with external standard and area normalization methods. The chromatographic and mass spectrometric conditions were the same as in example 19. The obtained rose essential oil comprises the following main aroma components in percentage by weight: citronellol 6.1468%, geraniol 2.3709%, methyl eugenol 3.5234%, linalool 0.8370%, phenethyl alcohol 0.6827%, eugenol 0.8355%, nerol 0.1590%, and 14.5553% in total.
Example 21
The rose essential oil products obtained in the embodiments 3 to 8 are respectively expressed as product # 1, product # 2, product # 3, product # 4, product # 5 and product # 6, six parallel extractions of the rose essential oil are performed, the method conditions in the embodiment 19 are adopted to perform GC-MS analysis tests, and the GC-MS total ion flow diagram of each product is shown in the attached figure 4, and the average oil yield is 0.5207 ‰.
Example 22
A newly-harvested lavandula angustifolia sample is adopted and refrigerated for three days, salt is not added, the lavandula angustifolia sample is crushed, a combined ultrafiltration membrane damping separator 1#, 2# -1, 2# -2 and 3# is additionally arranged, the model of a filter membrane is the same as that in example 3, the method comprises a re-distillation process, the steam distillation extraction process shown in the attached drawing 2 of example 2 is adopted, the material-liquid ratio is 1:4, co-water distillation is carried out, the extraction time is 1.5 hours, and the oil yield is 4.96 permillage.
Example 23
A newly-harvested lavandula angustifolia sample is adopted and refrigerated for three days, salt is not added, the lavandula angustifolia sample is crushed, a combined ultrafiltration membrane damping separator 1#, 2# -1, 2# -2 and 3# is additionally arranged, the model of a filter membrane is the same as that in example 3, the method comprises a re-distillation process, the steam distillation extraction process shown in the attached drawing 2 of example 2 is adopted, the material-liquid ratio is 1:4, co-water distillation is carried out, the extraction time is 1.5 hours, and the oil yield is 4.59 permillage.
Example 24
The lavender essential oil products obtained in the examples 22 to 23 are respectively expressed as product # 1 and product # 2, two batches of parallel extraction are performed, GC-MS analysis and test are performed according to the chromatographic and mass spectrum conditions in the example 19, the GC-MS total ion current comparison graph of each product is shown in fig. 5, the average oil yield is 4.78 ‰, and the product consistency and stability are excellent. The main fragrance components and the contents thereof are respectively 33.28 percent of linalool, 15.78 percent of eucalyptol, 8.76 percent of d-camphor, 3.52 percent of alpha-terpineol, 3.22 percent of camphor, 2.66 percent of linalyl acetate and 0.16 percent of lavender alcohol, and the total content of the components is 67.38 percent.
Example 25
The method comprises the steps of drying a newly-collected lemongrass sample, cutting and crushing the sample, extracting the sample without adding salt, adding combined ultrafiltration membrane damping separators 1#, 2# -1, 2# -2 and 3#, wherein the types of filter membranes are the same as those in example 3, the method comprises a re-distillation process, adopting a steam distillation extraction process shown in the attached drawing 2 of example 2, wherein the material-liquid ratio is 1:8, co-distilling is carried out, the extraction time is 3 hours, and the oil yield is 1.69%.
Example 26
The method comprises the steps of drying a newly-collected lemongrass sample, cutting and crushing the sample, extracting the sample without adding salt, adding combined ultrafiltration membrane damping separators 1#, 2# -1, 2# -2 and 3#, wherein the types of filter membranes are the same as those in example 3, the method comprises a re-distillation process, adopting a steam distillation extraction process shown in the attached drawing 2 of example 2, wherein the material-liquid ratio is 1:8, co-distilling is carried out, the extraction time is 3 hours, and the oil yield is 1.52%.
Example 27
The lemongrass essential oil products obtained in examples 25 to 26 are respectively expressed as product # 1 and product # 2, two batches of parallel extraction are performed, the GC-MS analysis test is performed by adopting the method file in example 19, and GC-MS total ion flow diagrams (comparison diagram) of the two batches of products are obtained and are shown in FIG. 6, the average oil yield is 1.60%, and the consistency and stability of the products are excellent. Wherein the average contents of the main body fragrance components citronellal, geraniol, elemenol, citronellol, citronellyl acetate and limonene are respectively 27.50%, 13.81%, 10.27%, 7.10%, 3.71% and 1.91%, and the total content of the components is 64.29%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. An extraction method for improving the oil yield and quality of volatile plant essential oil adopts a steam distillation extraction process, and is characterized in that: a combined ultrafiltration membrane damping separator with remarkably different surface properties and functions is additionally arranged on an oil-water separator of the extraction process.
2. The extraction method for improving the oil yield and quality of volatile plant essential oil according to claim 1, wherein the extraction method comprises the following steps: the pipeline of the oil-water separator communicated with the outside is additionally provided with cold hydrazine, and an ultrafiltration membrane damping separator with double hydrophobic surfaces is additionally arranged at the outlet of the cold hydrazine.
3. The extraction method for improving the oil yield and quality of volatile plant essential oil according to claim 1, wherein the extraction method comprises the following steps: an ultrafiltration membrane damping separator with oleophylic and hydrophobic surface properties is arranged on one side, close to the oil-water separator, of a pipeline from the oil-water separator to the essential oil collector.
4. The extraction method for improving the oil yield and quality of volatile plant essential oil according to claim 1, wherein the extraction method comprises the following steps: an ultrafiltration membrane damping separator with hydrophilic oleophobic surface property is additionally arranged on a pipeline of the oil-water separator leading to the pure dew storage tank.
5. The extraction method for improving the oil yield and quality of volatile plant essential oil according to any one of claims 1 to 4, wherein: the ultrafiltration membrane damping separator adopts an organic ultrafiltration membrane or an inorganic ultrafiltration membrane.
6. The extraction method for improving the oil yield and quality of volatile plant essential oil according to claim 5, wherein the extraction method comprises the following steps: the organic ultrafiltration membrane or the inorganic ultrafiltration membrane is a double-hydrophobic surface modified high molecular polymer ultrafiltration membrane with or after surface modification with hydrophobicity and oleophobicity.
7. The extraction method for improving the oil yield and quality of volatile plant essential oil according to claim 5, wherein the extraction method comprises the following steps: the organic ultrafiltration membrane or the inorganic ultrafiltration membrane is a high molecular polymer ultrafiltration membrane with or after surface modification, hydrophilic and oleophobic surface properties.
8. The extraction method for improving the oil yield and quality of volatile plant essential oil according to claim 5, wherein the extraction method comprises the following steps: the organic ultrafiltration membrane or the inorganic ultrafiltration membrane is a high molecular polymer ultrafiltration membrane with or after surface modification, oleophylic and hydrophobic surface properties.
9. The extraction method for improving the oil yield and quality of volatile plant essential oil according to any one of claims 1 to 4, wherein: the oil-water separator is also provided with a re-distillation pipeline leading to the distillation still, and the re-distillation pipeline is provided with an ultrafiltration membrane damping separator with hydrophilic and oleophobic surface properties.
10. The extraction method for improving the oil yield and quality of volatile plant essential oil according to claim 9, wherein the extraction method comprises the following steps: the ultrafiltration membrane damping separator adopts an organic ultrafiltration membrane or an inorganic ultrafiltration membrane with or after surface modification, hydrophilic and oleophobic surface properties.
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