CN116948747A - Method for realizing full recycling of lavender based on green extraction technology - Google Patents
Method for realizing full recycling of lavender based on green extraction technology Download PDFInfo
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- CN116948747A CN116948747A CN202310818644.0A CN202310818644A CN116948747A CN 116948747 A CN116948747 A CN 116948747A CN 202310818644 A CN202310818644 A CN 202310818644A CN 116948747 A CN116948747 A CN 116948747A
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- China
- Prior art keywords
- lavender
- essential oil
- extraction technology
- deep eutectic
- eutectic solvent
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Classifications
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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
- C11B9/025—Recovery by solvent extraction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0207—Control systems
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
- B01D11/0296—Condensation of solvent vapours
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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
- B01D61/58—Multistep processes
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Acoustics & Sound (AREA)
- Mechanical Engineering (AREA)
- Automation & Control Theory (AREA)
- Water Supply & Treatment (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a method for realizing full recycling of lavender based on a green extraction technology, which comprises the following steps: step S1: pretreatment of lavender: fresh lavender flower ears are used as raw materials, dried and chopped for standby; step S2: preparing Deep Eutectic Solvent (DES); step S3: biological enzyme-deep eutectic solvent leaching; step S4: microwave-assisted water distillation; step S5: purifying by a nanofiltration membrane; step S6: ultrafiltration-reverse osmosis membrane concentration; step S7: and (5) treating solid residues. The invention can prepare high-quality essential oil and pure dew, shortens the extraction time, reduces the cost, realizes the full resource utilization of the lavender, improves the added value and economic benefit of resources, and reduces the resource waste and environmental pollution.
Description
Technical Field
The invention relates to the technical field of plant extracts, in particular to a method for realizing full recycling of lavender based on a green extraction technology.
Background
Lavender is a perennial vanilla plant native to the Mediterranean coastal region and is now widely cultivated worldwide. Lavender has various biological activities such as antibacterial, anti-inflammatory, antioxidant, sleep improving, etc., and thus has been widely used in the fields of medicine, cosmetics, foods, fragrances, etc. The main active ingredients of lavender are volatile essential oils, which contain abundant monoterpene and sesquiterpene compounds, such as linalool, linalyl acetate, eucalyptol, camphor, etc., which impart unique fragrance and physiological activity to the lavender essential oils. In addition to essential oils, lavender contains other valuable ingredients such as polyphenols, flavonoids, amino acids, etc., which are mainly present in the water-soluble part of lavender, i.e. the hydrosol, also known as floral or floral water. The hydrosol is a byproduct generated in the process of extracting essential oil, and is a liquid composed of water-soluble components in plants carried by water vapor and a small amount of essential oil. The hydrosol has fragrance and activity similar to or complementary to those of essential oils, but is milder and safer than essential oils, and thus can also be used for various purposes such as skin care, aromatherapy, air fresheners, etc. Besides essential oil and pure dew, a large amount of solid residues are generated in the extraction process of the lavender, and the solid residues are generally regarded as waste to be discarded or used inefficiently, so that resource waste and environmental pollution are caused. However, the solid residue still contains a certain amount of organic substances and inorganic salts, and can be used for preparing fertilizer, feed or other functional products, so that the full resource utilization of the lavender is realized.
At present, common methods for extracting lavender essential oil include a water distillation method, a steam distillation method, an organic solvent extraction method and a supercritical fluid extraction method. However, the method has low essential oil yield, long extraction time, large equipment investment and high operation cost.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for realizing full recycling of lavender based on a green extraction technology, which can prepare high-quality essential oil and hydrolat and shorten the extraction time.
The invention is realized by the following technical scheme:
a method for realizing full recycling of lavender based on a green extraction technology comprises the following steps:
step S1: pretreatment of lavender: fresh lavender flower ears are used as raw materials, dried and chopped for standby;
step S2: preparation of Deep Eutectic Solvent (DES): mixing a hydrogen bond donor and a hydrogen bond acceptor, heating to dissolve the hydrogen bond donor and the hydrogen bond acceptor into a uniform liquid solvent, and cooling and filtering the prepared liquid solvent to obtain a pure deep eutectic solvent;
step S3: biological enzyme-deep eutectic solvent leaching: mixing the lavender flower ears pretreated in the step S1 with the deep eutectic solvent obtained in the step S2, sequentially adding biological enzyme and water, adjusting the pH value and leaching to obtain a leached mixture;
step S4: microwave-assisted water distillation: transferring the mixture leached in the step S3 into a microwave reactor, heating under constant microwave power to enable the DES solution to boil and take away volatile components in the lavender, cooling by a condenser and collecting condensate, and layering and separating the condensate to obtain an upper essential oil phase and a lower pure dew phase;
step S5: purifying by using nanofiltration membranes: purifying the upper essential oil phase obtained in the step S4 by using a nanofiltration membrane under constant pressure to obtain high-quality lavender essential oil;
step S6: ultrafiltration-reverse osmosis membrane concentration: and (3) filtering the lower-layer pure dew phase obtained in the step (S4) by adopting an ultrafiltration membrane, and concentrating by combining the lower-layer pure dew phase with a reverse osmosis membrane to obtain high-quality concentrated pure dew.
Further, the biological enzyme in the step S3 is one or two of cellulase, hemicellulase, pectinase and xylanase.
Further, the mass ratio of the lavender flower spike to the deep eutectic solvent in the step S3 is (1-2): 10; and step S3, sequentially adding biological enzyme and water to obtain a biological enzyme solution with the mass concentration of 0.5% -3.0%.
Further, in the step S3, the pH value is 2.0-5.0, and the solid-liquid ratio of the mixture to be immersed in advance is 1/5-1/16 g/mL; the leaching temperature in the step S3 is 25-45 ℃; the leaching time is 1-5 h.
Further, the microwave power in the step S4 is 300-800W, and the heating time is 10-60 min.
Further, in the step S2, the hydrogen bond donor is selected from one of ethylene glycol, glycerol, sorbitol, and lemon, and the hydrogen bond acceptor is selected from one of choline chloride and acetylcholine.
Further, the molar ratio of the hydrogen bond donor to the hydrogen bond acceptor in the step S2 is (1-2): 1, a step of; and step S2, heating at 40-80 ℃ for 20-40 min and cooling at 0-25 ℃.
Further, the molecular weight cut-off of the nanofiltration membrane in the step S5 is 150-500 Da, the nanofiltration membrane is a solvent-resistant composite nanofiltration membrane, and the nanofiltration membrane is one of a polytetrafluoroethylene composite nanofiltration membrane and a polyamide/ceramic composite nanofiltration membrane.
Further, the microwave power in the step S4 is 300-800W, and the heating time is 10-60 min.
Further, the pressure in the step S5 is 0.2MPa to 0.5MPa.
Further, the ultrafiltration membrane adopted in the step S6 has a molecular weight cutoff of 1000Da to 8000Da, and the ultrafiltration membrane is made of one of ceramics, polytetrafluoroethylene, polysulfone and polyvinylidene fluoride.
Further, the pore diameter of the reverse osmosis membrane adopted in the step S6 is 0.3nm to 0.8nm.
Further, the operating pressure of the step S6 is 0.6-1.5 MPa, and the operating temperature is 20-45 ℃.
Further, the method further comprises: step S7: solid residue treatment: and (3) drying and crushing the solid residues remained in the microwave reactor in the step (S4) to obtain lavender solid residues, wherein the lavender solid residues can be used for preparing fertilizers, feeds or other functional products.
Compared with the prior art, the invention has the advantages that:
1. the invention adopts the green and sustainable deep eutectic solvent as the solvent, avoids using organic solvents or a large amount of water and other traditional solvents, reduces the cost and toxicity, and improves the safety and biocompatibility.
2. The invention adopts the microwave-assisted water distillation extraction technology, shortens the extraction time and improves the extraction efficiency and quality; because the DES is applied to lavender extraction, the permeability is poor, the extraction effect is poor, and the DES and the enzyme are combined to enable deep eutectic solvent and the enzyme to permeate into the interior of lavender cells, so that the cell wall structure is degraded, and the release of active ingredients is promoted; adopts nanofiltration membrane purification and ultrafiltration-reverse osmosis membrane concentration technology, realizes effective separation, concentration and purification of essential oil and pure dew, and improves the purity and stability of the product.
3. The residue obtained by the traditional steam distillation method has the characteristics of wetting, color, smell and the like, which indicates that part of essential oil cannot be extracted, and the residual residue is colorless and odorless and is detected by GCMS gas chromatography and a mass spectrometer to be free of essential oil components, so that the DES and enzyme synergistic degradation cell wall structure is further verified, the release of the effective components is promoted, the full resource utilization of lavender is realized, the additional value and the economic benefit of resources are improved, the waste of resources and the environmental pollution are reduced, the operation cost is low, and the equipment is simple.
4. In the process of preparing Deep Eutectic Solvent (DES) in step S2, the molar ratio of Hydrogen Bond Donor (HBD) to Hydrogen Bond Acceptor (HBA) is optimized to be (1-2): 1, the generated deep eutectic solvent can be ensured to have excellent solubility and stability; the uniform and impurity-free deep eutectic solvent can be obtained by adjusting the temperature of heating treatment to 40-80 ℃ and the heating time to 20-40 min, so that the quality of the solvent is improved, and the subsequent extraction efficiency is improved; the cooling temperature is 0-25 ℃, which can further remove the impurities possibly existing and improve the purity of the deep eutectic solvent.
5. In the step S3, the mass ratio of the lavender flower ears to the deep eutectic solvent is (1-2): 10 and leaching conditions (including biological enzyme addition, leaching time, temperature, pH value and the like) can effectively improve the release rate of the lavender active ingredient. Firstly, the solid-liquid ratio is 1/5-1/16 g/mL, so that the deep eutectic solvent can be fully contacted with the lavender flower ears, and the permeability and the solubility are improved; and secondly, the mass concentration of the enzyme is regulated to be 0.5% -3.0%, the enzymolysis time (leaching time) is 1-5 h, the enzymolysis temperature (leaching temperature) is 25-45 ℃ and the pH value is 2.0-5.0, so that the degradation of a cell wall structure can be fully promoted, the permeability and the solubility of DES to a plant matrix are further enhanced, and the release and the transfer of target components are greatly improved.
6. The step S4 of the invention can effectively control the efficiency and quality of the microwave-assisted water distillation extraction process through optimizing the microwave power and the heating time. The microwave power of 300-800W and the heating time of 10-60 min can make the deep eutectic solvent boil and take away volatile components in the lavender, and simultaneously prevent the loss or degradation of active components caused by too fast reaction and save energy.
7. According to the invention, the essential oil phase is purified by using the nanofiltration membrane, so that macromolecules such as macromolecular proteins, sugar, free fatty acid and the like in the essential oil are intercepted, the purity and stability of the essential oil are improved, and the high-quality lavender essential oil is obtained. The pure dew phase is ultrafiltered firstly, impurities in the pure dew are removed, membrane pollution is reduced, and then the pure dew phase is combined with a reverse osmosis membrane for concentration, so that redundant water is removed, the concentration of active ingredients in the pure dew is improved, and the high-quality concentrated pure dew is obtained.
Drawings
FIG. 1 is a process flow diagram of a method for achieving full recycling of lavender based on green extraction technology according to an embodiment of the present invention;
FIG. 2 is a process flow diagram of S3 in FIG. 1;
fig. 3 is a process flow diagram of S4 in fig. 1.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent, so that those skilled in the art can fully understand the technical contents of the present invention. It is to be understood that the following examples are given by way of illustration of the present invention and are not to be construed as limiting the scope of the present invention, since various modifications and alterations of no particular nature will fall within the scope of the invention as defined by the appended claims. The specific manufacturing process parameters and the like described below are also only one example of suitable ranges, i.e., a person skilled in the art can select from the description herein without limiting to the specific values described below.
As shown in fig. 1, a method for realizing full recycling of lavender based on a green extraction technology according to an embodiment of the present invention includes the following steps:
step S1: pretreatment of lavender: fresh lavender flower ears are used as raw materials, the flower ears are the parts of lavender plants containing the most essential oil components, and are generally picked in the flowering period so as to ensure the quality and yield of essential oil; drying fresh lavender flower ears, and cutting up to an average granularity of 1-3 mm for later use;
step S2: preparation of Deep Eutectic Solvent (DES): hydrogen bond donor and hydrogen bond acceptor are mixed according to the following ratio (1-2): 1, heating at 40-80 ℃ for 20-40 min to dissolve the mixture into uniform liquid solvent, and cooling and filtering the prepared liquid solvent at 0-25 ℃ to obtain pure deep eutectic solvent;
step S3: biological enzyme-deep eutectic solvent leaching: and (2) mixing the lavender flower ears pretreated in the step S1 with the deep eutectic solvent obtained in the step S2 according to the following steps: 10, adding a biological enzyme solution with the mass concentration of 0.5-3.0%, regulating the pH value to 2.0-5.0 to obtain an acidic mixture, and leaching for 1-5 hours at the temperature of 25-45 ℃ to enable deep eutectic solvent and biological enzyme to permeate into lavender cells, degrading cell wall structures and promoting the release of active ingredients;
step S4: microwave-assisted water distillation: transferring the mixture leached in the step S3 into a microwave reactor, heating for 10-60 min under the microwave power of 300-800W to enable the DES solution to boil and take away volatile components in the lavender, cooling the volatile components into liquid, namely condensate through a condenser, collecting the liquid, and then placing the condensate into a dropping funnel for standing and layering to obtain an upper essential oil phase and a lower pure dew phase;
step S5: purifying by using nanofiltration membranes: purifying the upper essential oil phase obtained in the step S4 by using a nanofiltration membrane under the operating pressure of 0.2-0.5 MPa, wherein macromolecular proteins, sugar and free fatty acid in the essential oil are mainly intercepted, and high-quality lavender essential oil is obtained;
step S6: ultrafiltration-reverse osmosis membrane concentration: filtering the lower-layer pure dew phase obtained in the step S4 by adopting an ultrafiltration membrane, and concentrating by combining with a reverse osmosis membrane to reduce membrane pollution, remove impurities and redundant water in the pure dew, and improve the concentration of active ingredients in the pure dew to obtain high-quality concentrated pure dew;
step S7: solid residue treatment: and (3) drying and crushing residues remained in the microwave reactor in the step (S4) to obtain lavender solid residues, wherein the lavender solid residues can be used for preparing fertilizers, feeds or other functional products and can also be used as valuable substitute biomass for fuel production.
Further, in the step S3, the biological enzyme solution with the mass concentration of 0.5% -3.0% is obtained after the biological enzyme and the water are sequentially added.
Further, the hydrogen bond donor in step S2 is selected from one of ethylene glycol, glycerol, sorbitol, and citric acid.
Further, the hydrogen bond acceptor in step S2 is selected from one of choline chloride and acetylcholine.
Further, in the step S5, the interception molecular weight of the nanofiltration membrane is 150-500 Da, the nanofiltration membrane is made of a solvent-resistant composite nanofiltration membrane, and the nanofiltration membrane is made of one of a polytetrafluoroethylene composite nanofiltration membrane and a polyamide/ceramic composite nanofiltration membrane.
Further, the ultrafiltration membrane adopted in the step S6 has a molecular weight cutoff of 1000 Da-8000 Da, and is made of one of ceramic, polytetrafluoroethylene, polysulfone and polyvinylidene fluoride.
Further, the pore diameter of the reverse osmosis membrane used in the step S6 is 0.3nm to 0.8nm.
Further, the operating pressure of the step S6 is 0.6-1.5 MPa, and the operating temperature is 20-45 ℃.
After the purification of the nanofiltration membrane in the step S5 is finished, in order to avoid the waste caused by intercepting part of essential oil active ingredients on the residual side of the nanofiltration membrane, the residual side of the nanofiltration membrane is mixed with the pure dew phase at the lower layer of the step S4 to enter an ultrafiltration-reverse osmosis membrane concentration step, and at the moment, the active ingredients intercepted by the nanofiltration membrane are finally reserved in the concentrated pure dew, so that the full resource of green extraction of the lavender is further realized.
In the manufacturing method, the residue sample in the step S7 is dissolved by proper ethyl acetate, solid impurities are removed by filtration or centrifugation, a sample solution is obtained, the sample solution is detected by GCMS gas chromatography and a mass spectrometer, no essential oil component exists, the cell wall structure is further verified to be degraded by the cooperation of DES and enzyme, the release of effective components is promoted, the full resource utilization of lavender is realized, the added value and the economic benefit of resources are improved, and the resource waste and the environmental pollution are reduced.
DES has been mixed with water to reduce its viscosity in the past because of its high viscosity, but DES aqueous solutions have been found to have poor permeability to plant substrates, affecting extraction. By utilizing an enzyme-assisted pretreatment technology, the DES and the enzyme are cooperatively treated, so that deep eutectic solvent and the enzyme can permeate into lavender cells, and the permeability and the solubility of the deep eutectic solvent to a plant matrix are enhanced by degrading the lavender cell wall structure, thereby promoting the release and the transfer of target components, improving the extraction efficiency and improving the oil yield of essential oil.
In the process of preparing Deep Eutectic Solvent (DES) in step S2, the molar ratio of Hydrogen Bond Donor (HBD) to Hydrogen Bond Acceptor (HBA) is optimized to be (1-2): 1, the generated deep eutectic solvent can be ensured to have excellent solubility and stability; the uniform and impurity-free deep eutectic solvent can be obtained by adjusting the temperature of heating treatment to 40-80 ℃ and the heating time to 20-40 min, so that the quality of the solvent is improved, and the subsequent extraction efficiency is improved; the cooling temperature is 0-25 ℃, which can further remove the impurities possibly existing and improve the purity of the deep eutectic solvent.
In the step S3, the mass ratio of the lavender flower ears to the deep eutectic solvent is (1-2): 10 and leaching conditions (including biological enzyme addition, leaching time, temperature, pH value and the like) can effectively improve the release rate of the lavender active ingredient. Firstly, the solid-liquid ratio is 1/5-1/16 g/mL, so that the deep eutectic solvent can be fully contacted with the lavender flower ears, and the permeability and the solubility are improved; and secondly, the mass concentration of the enzyme is regulated to be 0.5% -3.0%, the enzymolysis time (leaching time) is 1-5 h, the enzymolysis temperature (leaching temperature) is 25-45 ℃ and the pH value is 2.0-5.0, so that the degradation of a cell wall structure can be fully promoted, the permeability and the solubility of DES to a plant matrix are further enhanced, and the release and the transfer of target components are greatly improved.
The step S4 of the invention can effectively control the efficiency and quality of the microwave-assisted water distillation extraction process through optimizing the microwave power and the heating time. The microwave power of 300-800W and the heating time of 10-60 min can make the deep eutectic solvent boil and take away volatile components in the lavender, and simultaneously prevent the loss or degradation of active components caused by too fast reaction and save energy.
The molecular weight cut-off of the nanofiltration membrane is optimized to be 150-500 Da in the step S5, so that macromolecular proteins, sugar and free fatty acid in the essential oil can be intercepted, impurities in the essential oil can be effectively removed, and the purity of the essential oil is improved.
In the step S6, the interception molecular weight of the ultrafiltration membrane is optimized to be 1000 Da-8000 Da, the aperture of the reverse osmosis membrane is 0.3 nm-0.8 nm, so that the effective components in the pure dew phase penetrate the ultrafiltration membrane and do not penetrate the reverse osmosis membrane, macromolecular proteins, colloids, suspended matters and insoluble substances in the pure dew phase are intercepted by the ultrafiltration membrane, and the redundant moisture in the pure dew phase is removed by the reverse osmosis membrane, thereby improving the quality of the pure dew.
The invention adopts nanofiltration membrane purification and ultrafiltration-reverse osmosis membrane concentration technical reasons are as follows: the condensate in the step S3 contains macromolecular proteins, wherein the macromolecular proteins refer to water-soluble proteins in the lavender, such as enzymes, antibodies, hormones and the like, and the macromolecular proteins enter an upper essential oil phase along with water vapor in a microwave-assisted water distillation process, so that the essential oil in the upper essential oil phase is purified by using a nanofiltration membrane firstly because of no moisture, so that active components of the essential oil permeate to intercept macromolecules in the essential oil, such as macromolecular proteins, sugar, free fatty acids and the like, so that the purity and stability of the essential oil are improved, and interception substances enter a permeate side, and the high-quality lavender essential oil is obtained on the permeate side. The substances on the residual side of the nanofiltration membrane can be added into the lower layer pure dew phase to perform ultrafiltration treatment at first, so that the essential oil active ingredients on the residual side permeate the ultrafiltration membrane but not permeate the reverse osmosis membrane, and at the moment, the essential oil active ingredients on the residual side are all reserved in the pure dew, thereby further realizing full resource extraction of lavender, having no environmental pollution, improving the purity and stability of the essential oil and avoiding discoloration or deterioration of the essential oil.
The lavender essential oil treated by the traditional steam is yellow, and the essential oil purified by the nanofiltration membrane is colorless, which indicates that the nanofiltration membrane adopted by the invention can intercept pigments, and further improves the quality of the essential oil.
The pure dew component contains more than 3 to 6 percent of essential oil compounds, and the rest 94 to 97 percent of the pure dew component is water-soluble nutrient substances, wherein the water-soluble nutrient substances are organic acid, flavonoid, polysaccharide, amino acid, vitamin, tannic acid, triterpene, diterpene and the like. The organic acid in the hydrosol is mainly weak acid extracted from plants, is water-soluble, does not damage skin, is a good anti-inflammatory substance, and has the effects of brightening, shrinking pores, resisting aging and the like; common organic molecules in the alcohol essential oil have the effects of resisting bacteria, enhancing immunity and the like, which is one of the reasons that the pure dew can be preserved for a long time without adding a preservative, and the effects are often used for acne removal, dermatitis treatment and the like; aldehyde substances with the main effects of pacifying, resisting bacteria and diminishing inflammation; the main smell of the ester substance is reflected by the ester substance, is an aromatic molecule, has mild property and has the effects of soothing, calming and relieving red swelling and allergy; the flavonoid can improve the oxidation resistance of the organism and the capability of scavenging free radicals, thereby reducing the aging speed of the organism, and simultaneously, once entering into blood vessels, the flavonoid can scavenge triglyceride and cholesterol attached to the walls of the blood vessels, and achieves the effects of reducing cholesterol, reducing blood fat and preventing various cardiovascular diseases by dilating the blood vessels and improving the permeability of the blood vessels.
Most essential oils do not act directly on the skin, but rather are blended with vegetable oils in proportions that would otherwise burn the skin. The pure dew well avoids the problem, can be directly used, has good mildness, and has the effects of resisting bacteria, diminishing inflammation, regulating the balance of flora, relieving and calming, regulating skin and the like; the organic acid component can regulate the growth of skin cells and help the synthesis of collagen, promote the regeneration of fibroblasts, and has certain benefit for repairing scars of skin; improving keratinization of skin and softening skin cutin layer; helps skin to remove free radicals, has antioxidant effect, and can promote skin regeneration.
The combination of flavone and tannic acid in the concentrated hydrolat has excellent antioxidation effect, when the skin cells of a human body are damaged or the antioxidation function is attenuated, more various free radicals can be generated in the organism, especially the hydroxyl free radicals in the active oxygen free radicals have extremely strong electron-obtaining capability, the reaction activity is extremely strong, the toxicity and the harm are also extremely high, the flavone and tannic acid can quickly react with any biological molecules, organic matters or inorganic matters in living cells, and further cause degradation of DNA, cell membranes and polysaccharide compounds, serious damage is caused to the organism, the skin is aged and dark, and the hydrolat extracted by the invention has strong scavenging capability to the hydroxyl free radicals, strong antioxidation capability and strong bacteriostasis and is most suitable for being used as a skin care product.
In the step S6, the ultrafiltration membrane filters macromolecular proteins, colloid, suspended matters, insoluble matters and other impurities, the liquid after the membrane filtration is treated by reverse osmosis, the reverse osmosis membrane only permeates water, but not permeates the ultrafiltration membrane, and the concentration multiple is about 20 times, and at the moment, the water is not completely permeated in the reverse osmosis process.
The following is a description of the concepts of the invention in conjunction with specific embodiments, but is not intended to limit the invention to the specific embodiments described below. Any particular value within the scope of the invention as described herein may be practiced.
Example 1
Step S1: pretreatment of lavender: drying and cutting fresh lavender ears picked in the flowering period to obtain a particle size of 1mm;
step S2: preparation of Deep Eutectic Solvent (DES): ethylene glycol (HBD) and choline chloride (HBA) were mixed at 0.5:1, heating at 40 ℃ for 40min to dissolve the mixture into a uniform liquid solvent, cooling the prepared liquid solvent at 25 ℃, and filtering with filter paper to remove impurities and undissolved solid substances possibly existing, thus obtaining a pure deep eutectic solvent;
step S3: biological enzyme-deep eutectic solvent leaching: the lavender flower spike pretreated in the step S1 and the deep eutectic solvent obtained in the step S2 are mixed according to the mass ratio of 1:10, and sequentially adding the components with the mass ratio of 1:1, mixing biological enzyme and water, wherein the mass concentration of the enzyme is 0.5%, the pH value is regulated to 2, an acidic mixture with the solid-to-liquid ratio of 1/16g/mL is obtained, and leaching is carried out for 5 hours at 25 ℃, so that deep eutectic solvent and enzyme penetrate into lavender cells, the cell wall structure is degraded, and the release of active ingredients is promoted;
step S4: microwave-assisted water distillation: transferring the mixture leached in the step S3 into a microwave reactor, heating for 60min under the microwave power of 300W, boiling the deep eutectic solvent and taking away volatile components in the lavender, cooling the volatile components into liquid, namely condensate through a condenser, collecting, and then placing the condensate into a dropping funnel for standing and layering to obtain an upper essential oil phase and a lower pure dew phase;
step S5: purifying by using nanofiltration membranes: purifying the essential oil phase at the upper layer in the step S4 by using a nanofiltration membrane, wherein macromolecular proteins, sugar and free fatty acid in the essential oil are mainly intercepted, the interception molecular weight of the nanofiltration membrane is 500Da, the operating pressure is 0.5MPa, and the high-quality lavender essential oil is obtained at the permeation side;
step S6: ultrafiltration-reverse osmosis membrane concentration: and (3) filtering the pure dew phase at the lower layer of the step (S4) by adopting an ultrafiltration membrane with the molecular weight cut-off of 1000Da and made of polytetrafluoroethylene, and then concentrating by combining with a reverse osmosis membrane to reduce membrane pollution, remove macromolecular proteins, insoluble substances and other impurities and redundant moisture in the pure dew phase, and improve the concentration of active ingredients in the pure dew to obtain high-quality concentrated pure dew. The aperture of the reverse osmosis membrane is 0.3nm, the operating pressure is 1.5MPa, and the operating temperature is 45 ℃;
step S7: solid residue treatment: and (3) drying and crushing residues remained in the microwave reactor in the step (S4) to obtain lavender solid residues, wherein the lavender solid residues can be used for preparing fertilizers, feeds or other functional products and can also be used as valuable substitute biomass for fuel production.
The quality and mass fractions of lavender essential oil, hydrolat and solid residue prepared by the method of example 1 of the present invention are shown in table 1.
TABLE 1
The yield of lavender essential oil is calculated to be 2.53%, the pure dew contains 5% of essential oil compounds and 95% of water-soluble nutrient substances, the remaining solid residue is colorless and odorless, a residue sample is dissolved by proper ethyl acetate, and solid impurities are removed by filtration or centrifugation, so that a sample solution is obtained. The sample solution was checked by GCMS gas chromatography and mass spectrometry, and the peak area in the residue, which was kept at the same or similar time as the lavender essential oil, was close to zero, indicating that there was no essential oil component. The solid residue becomes a valuable alternative biomass for fuel production.
Example 2
Step S1: pretreatment of lavender: drying and cutting fresh lavender ears picked in the flowering period to obtain a 2mm average particle size;
step S2: preparation of Deep Eutectic Solvent (DES): ethylene glycol (HBD) and choline chloride (HBA) were mixed according to a ratio of 4:1, heating the mixture at 80 ℃ for 20min to dissolve the mixture into a uniform liquid solvent, cooling the prepared liquid solvent at 10 ℃, and filtering with filter paper to remove impurities and undissolved solid substances possibly existing, thereby obtaining a pure deep eutectic solvent;
step S3: biological enzyme-deep eutectic solvent leaching: the lavender flower spike pretreated in the step S1 and the deep eutectic solvent obtained in the step S2 are mixed according to the mass ratio of 1.2:10, and sequentially adding the components with the mass ratio of 2:1, mixing biological enzyme and water, wherein the biological enzyme and the water are composed of cellulase and pectase, so that the mass concentration of the enzyme is 2%, regulating the pH value to be 4, obtaining an acidic mixture with the solid-to-liquid ratio of 1/8g/mL, leaching the acidic mixture for 2 hours at 35 ℃, enabling deep eutectic solvent and enzyme to permeate into lavender cells, degrading cell wall structures and promoting the release of active ingredients;
step S4: microwave-assisted water distillation: transferring the mixture leached in the step S3 into a microwave reactor, heating for 40min under the microwave power of 500W, boiling the deep eutectic solvent and taking away volatile components in the lavender, cooling the volatile components into liquid, namely condensate through a condenser, collecting, and then placing the condensate into a dropping funnel for standing and layering to obtain an upper essential oil phase and a lower pure dew phase;
step S5: purifying by using nanofiltration membranes: purifying the upper essential oil phase obtained in the step S4 by using a nanofiltration membrane, wherein macromolecular proteins, sugar and free fatty acid in the essential oil are mainly intercepted, the interception molecular weight of the nanofiltration membrane is 500Da, and the operation pressure is 0.5MPa, so that the high-quality lavender essential oil is obtained on the permeation side;
step S6: ultrafiltration-reverse osmosis membrane concentration: and (3) filtering the pure dew phase at the lower layer of the step (S4) by adopting an ultrafiltration membrane with the molecular weight cut-off of 1000Da and made of polytetrafluoroethylene, and then concentrating by combining with a reverse osmosis membrane to reduce membrane pollution, remove macromolecular proteins, insoluble substances and other impurities and redundant moisture in the pure dew phase, and improve the concentration of active ingredients in the pure dew to obtain high-quality concentrated pure dew. The aperture of the reverse osmosis membrane is 0.3nm, the operating pressure is 1.5MPa, and the operating temperature is 45 ℃;
step S7: solid residue treatment: and (3) drying and crushing residues remained in the microwave reactor in the step (S4) to obtain lavender solid residues, wherein the lavender solid residues can be used for preparing fertilizers, feeds or other functional products.
The quality and mass fractions of lavender essential oil, hydrolat and solid residue prepared by the method of example 2 of the present invention are shown in table 2.
TABLE 2
| Product(s) | Quality of | Mass fraction of main ingredient |
| Essential oil | 0.5kg | Linalool: 39.3% linalyl acetate: 30.1% of Lavender acetate: 11.2% |
| Pure dew | 16.4kg | Linalool: 1.6% linalyl acetate: 1.2% of lavender acetate: 0.4% |
| Solid residue | 33.2kg | Cellulose: 39%, hemicellulose: 21%, lignin: 18% |
The yield of lavender essential oil was calculated to be 2.35%, and the hydrosol contained 4% of essential oil compound.
Example 3
Step S1: pretreatment of lavender: drying and cutting fresh lavender ears picked in the flowering period to obtain a lavender ears average particle size of 3mm;
step S2: preparation of Deep Eutectic Solvent (DES): ethylene glycol (HBD) and choline chloride (HBA) were mixed at 1:1, heating the mixture at 60 ℃ for 30min to dissolve the mixture into a uniform liquid solvent, cooling the prepared liquid solvent at 20 ℃, and filtering with filter paper to remove impurities and undissolved solid substances possibly existing, thereby obtaining a pure deep eutectic solvent;
step S3: biological enzyme-deep eutectic solvent leaching: the pretreated lavender flower ears and deep eutectic solvent are mixed according to the mass ratio of 2:10, and sequentially adding the components with the mass ratio of 1:1, the concentration of enzyme solution is 0.5% by weight of mixed biological enzyme and water consisting of cellulase and pectase, and the mass ratio of the mixed biological enzyme to the water is 1:50, regulating the pH value to be 2, regulating the solid-to-liquid ratio of the mixture to be 1/5g/mL, leaching the mixture for 1h at 45 ℃ with the mass concentration of enzyme to ensure that deep eutectic solvent and enzyme permeate into lavender cells to degrade cell wall structures and promote the release of active ingredients;
step S4: microwave-assisted water distillation: transferring the mixture leached in the step S3 into a microwave reactor, heating for 30min under the microwave power of 700W, boiling the deep eutectic solvent and taking away volatile components in the lavender, cooling the volatile components into liquid, namely condensate through a condenser, collecting, and then placing the condensate into a dropping funnel for standing and layering to obtain an upper essential oil phase and a lower pure dew phase;
step S5: purifying by using nanofiltration membranes: purifying the essential oil phase at the upper layer in the step S4 by using a nanofiltration membrane, wherein macromolecular proteins, sugar and free fatty acid in the essential oil are mainly intercepted, the interception molecular weight of the nanofiltration membrane is 500Da, the operating pressure is 0.5MPa, and the high-quality lavender essential oil is obtained at the permeation side;
step S6: ultrafiltration-reverse osmosis membrane concentration: and (3) filtering the pure dew phase at the lower layer of the step (S4) by adopting an ultrafiltration membrane with the molecular weight cut-off of 1000Da and made of polytetrafluoroethylene, and then concentrating by combining with a reverse osmosis membrane to reduce membrane pollution, remove macromolecular proteins, insoluble substances and other impurities and redundant moisture in the pure dew phase, and improve the concentration of active ingredients in the pure dew to obtain high-quality concentrated pure dew. The aperture of the reverse osmosis membrane is 0.3nm, the operating pressure is 1.5MPa, and the operating temperature is 45 ℃;
step S7: solid residue treatment: and (3) drying and crushing residues remained in the microwave reactor in the step (S4) to obtain lavender solid residues, wherein the lavender solid residues can be used for preparing fertilizers, feeds or other functional products.
The quality and mass fractions of lavender essential oil, hydrolat and solid residue prepared by using the method of the present invention in example 3 are shown in table 3.
TABLE 3 Table 3
| Product(s) | Quality of | Mass fraction of main ingredient |
| Essential oil | 0.6kg | Linalool: 37.5 percent, linalyl acetate: 34.5% Lavender acetate: 9.6% |
| Pure dew | 15.5kg | Linalool: 2.1%, linalyl acetate: 1.8%, lavender acetate: 0.6% |
| Solid residue | 33.0kg | Cellulose: 39.5%, hemicellulose 21%, lignin 18.3% |
The yield of lavender essential oil was calculated to be 2.26%, and the hydrosol contained 6% of essential oil compound.
Example 4
Step S1: pretreatment of lavender: drying and cutting fresh lavender ears picked in the flowering period to obtain a particle size of 1mm;
step S2: preparation of Deep Eutectic Solvent (DES): ethylene glycol (HBD) and choline chloride (HBA) were mixed at 0.5:1, heating at 40 ℃ for 40min to dissolve the mixture into a uniform liquid solvent, cooling the prepared liquid solvent at 25 ℃, and filtering with filter paper to remove impurities and undissolved solid substances possibly existing, thus obtaining a pure deep eutectic solvent;
step S3: biological enzyme-deep eutectic solvent leaching: the lavender flower spike pretreated in the step S1 and the deep eutectic solvent obtained in the step S2 are mixed according to the mass ratio of 1:10, and sequentially adding the components with the mass ratio of 1:200, wherein the mass concentration of the cellulase and water is 0.5%, the pH value is regulated to 2, an acidic mixture with the solid-to-liquid ratio of 1/16g/mL is obtained, and leaching is carried out for 5 hours at 25 ℃, so that deep eutectic solvent and the enzyme penetrate into lavender cells, the cell wall structure is degraded, and the release of active ingredients is promoted;
step S4: microwave-assisted water distillation: transferring the mixture leached in the step S3 into a microwave reactor, heating for 60min under the microwave power of 300W, boiling the deep eutectic solvent and taking away volatile components in the lavender, cooling the volatile components into liquid, namely condensate through a condenser, collecting, and then placing the condensate into a dropping funnel for standing and layering to obtain an upper essential oil phase and a lower pure dew phase;
step S5: purifying by using nanofiltration membranes: purifying the essential oil phase at the upper layer in the step S4 by using a nanofiltration membrane, wherein macromolecular proteins, sugar and free fatty acid in the essential oil are mainly intercepted, the interception molecular weight of the nanofiltration membrane is 500Da, the operating pressure is 0.5MPa, and the high-quality lavender essential oil is obtained at the permeation side;
step S6: ultrafiltration-reverse osmosis membrane concentration: and (3) filtering the pure dew phase at the lower layer of the step (S4) by adopting an ultrafiltration membrane with the molecular weight cut-off of 1000Da and made of polytetrafluoroethylene, and then concentrating by combining with a reverse osmosis membrane to reduce membrane pollution, remove macromolecular proteins, insoluble substances and other impurities and redundant moisture in the pure dew phase, and improve the concentration of active ingredients in the pure dew to obtain high-quality concentrated pure dew. The aperture of the reverse osmosis membrane is 0.3nm, the operating pressure is 1.5MPa, and the operating temperature is 45 ℃;
step S7: solid residue treatment: and (3) drying and crushing residues remained in the microwave reactor in the step (S4) to obtain lavender solid residues, wherein the lavender solid residues can be used for preparing fertilizers, feeds or other functional products and can also be used as valuable substitute biomass for fuel production.
The yields and mass fractions of lavender essential oil, hydrolat and solid residue prepared by using the method of the present invention in example 4 are shown in table 4.
TABLE 4 Table 4
| Product(s) | Quality of | Mass fraction of main ingredient |
| Essential oil | 0.35kg | Linalool: 37.6%, linalyl acetate: 36.4% of Lavender acetate: 9.7% |
| Pure dew | 12.9kg | Linalool: 0.9% linalyl acetate: 0.8% of lavender acetate: 0.5% |
| Solid residue | 33.2kg | Cellulose: 39.5%, hemicellulose: 24%, lignin: 15% |
The yield of the lavender essential oil is calculated to be 1.5%, the pure dew contains 3% of essential oil compounds, and the yield of the essential oil is higher than that of single enzyme (cellulase) after the mixed enzyme (cellulase and pectase) is selected by combining the biological enzymes shown in the table 1 and the table 4, because the mixed enzyme is added into the DES solution, the cell wall structure is thoroughly destroyed due to the synergistic effect of the mixed enzyme, the mass transfer resistance is reduced, the sufficient release of the essential oil in the lavender is further promoted, the release rate of the essential oil is improved, the extraction time is shortened, the damage effect of the single enzyme to the cell wall is weaker, the essential oil can not be sufficiently released within the same time, and the essential oil yield is relatively low.
Comparative example 5
Step S1: pretreatment of lavender: drying and cutting fresh lavender ears picked in the flowering period to obtain a lavender ears average particle size of 3mm;
step S2: steam distillation: extracting volatile components in the lavender by adopting traditional steam distillation from the pretreated lavender flower ears, cooling and collecting condensate through a condenser, layering and separating the condensate to obtain an upper essential oil phase and a lower pure dew phase, extracting and rectifying the upper essential oil phase to obtain the lavender essential oil, and concentrating the lower pure dew phase to obtain the lavender pure dew. The extraction rate of the essential oil is 0.82%, and the hydrosol extracted by steam distillation only contains 0.17% of essential oil compounds.
As can be seen from the combination of the examples 1 to 4, compared with the conventional steam distillation method, the yield of the lavender essential oil prepared by adopting the mixed biological enzyme is improved by more than 186%, and the yield of the essential oil compound in the concentrated hydrosol is improved by more than 22.5 times; the yield of the lavender essential oil prepared by adopting a single biological enzyme is improved by 82.9%, and the yield of the essential oil compound in the concentrated pure dew is improved by 16.64 times.
It should be noted that the foregoing description of the preferred embodiments is merely illustrative of the technical concept and features of the present invention, and is not intended to limit the scope of the invention, as long as the scope of the invention is defined by the claims and their equivalents. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (10)
1. The method for realizing full recycling of lavender based on the green extraction technology is characterized by comprising the following steps of:
step S1: pretreatment of lavender: fresh lavender flower ears are used as raw materials, dried and chopped for standby;
step S2: preparation of Deep Eutectic Solvent (DES): mixing a hydrogen bond donor and a hydrogen bond acceptor, heating to dissolve the hydrogen bond donor and the hydrogen bond acceptor into a uniform liquid solvent, and cooling and filtering the prepared liquid solvent to obtain a pure deep eutectic solvent;
step S3: biological enzyme-deep eutectic solvent leaching: mixing the lavender flower ears pretreated in the step S1 with the deep eutectic solvent obtained in the step S2, sequentially adding biological enzyme and water, adjusting the pH value and leaching to obtain a leached mixture;
step S4: microwave-assisted water distillation: transferring the mixture leached in the step S3 into a microwave reactor, heating under constant microwave power to enable the DES solution to boil and take away volatile components in the lavender, cooling by a condenser and collecting condensate, and layering and separating the condensate to obtain an upper essential oil phase and a lower pure dew phase;
step S5: purifying by using nanofiltration membranes: purifying the upper essential oil phase obtained in the step S4 by using a nanofiltration membrane under constant pressure to obtain high-quality lavender essential oil;
step S6: ultrafiltration-reverse osmosis membrane concentration: and (3) filtering the lower-layer pure dew phase obtained in the step (S4) by adopting an ultrafiltration membrane, and concentrating by combining the lower-layer pure dew phase with a reverse osmosis membrane to obtain high-quality concentrated pure dew.
2. The method for realizing full recycling of lavender based on green extraction technology according to claim 1, wherein the biological enzyme in the step S3 is one or two of cellulase, hemicellulase, pectase and xylanase.
3. The method for realizing full recycling of lavender based on the green extraction technology according to claim 1, wherein the mass ratio of the lavender flower ears to the deep eutectic solvent in the step S3 is (1-2): 10; and step S3, sequentially adding biological enzyme and water to obtain the biological enzyme solution with the mass concentration of 0.5-3.0%.
4. The method for realizing full recycling of lavender based on the green extraction technology according to claim 1, wherein the pH value in the step S3 is 2.0-5.0, and the solid-liquid ratio of the mixture in advance of leaching is 1/5-1/16 g/mL; the leaching temperature in the step S3 is 25-45 ℃; the leaching time is 1-5 h.
5. The method for realizing full recycling of lavender based on green extraction technology according to claim 1, wherein the microwave power in the step S4 is 300-800W, and the heating time is 10-60 min.
6. The method for realizing full recycling of lavender based on green extraction technology according to claim 1, wherein the hydrogen bond donor in the step S2 is selected from one of ethylene glycol, glycerin, sorbitol and lemon, and the hydrogen bond acceptor is selected from one of choline chloride and acetylcholine.
7. The method for realizing full recycling of lavender based on green extraction technology according to claim 1, wherein the molar ratio of hydrogen bond donor to hydrogen bond acceptor in step S2 is (1-2): 1, a step of; and step S2, heating at 40-80 ℃ for 20-40 min and cooling at 0-25 ℃.
8. The method for realizing full recycling of lavender based on the green extraction technology according to claim 1, wherein the molecular weight cut-off of the nanofiltration membrane in the step S5 is 150-500 Da, and the nanofiltration membrane is made of one of polytetrafluoroethylene composite nanofiltration membrane and polyamide/ceramic composite nanofiltration membrane; the pressure in the step S5 is 0.2MPa to 0.5MPa.
9. The method for realizing full recycling of lavender based on the green extraction technology according to claim 1, wherein the ultrafiltration membrane adopted in the step S6 has a molecular weight cut-off of 1000 Da-8000 Da, and the ultrafiltration membrane is made of one of ceramics, polytetrafluoroethylene, polysulfone and polyvinylidene fluoride;
the pore diameter of the reverse osmosis membrane adopted in the step S6 is 0.3 nm-0.8 nm.
10. The method for realizing full recycling of lavender based on green extraction technology according to claim 1, which is characterized in that the method further comprises step S7: solid residue treatment: the solid residue remained in the microwave reactor is dried and crushed to obtain lavender solid residue, which can be used for preparing fertilizer, feed or other functional products, and can also be used as valuable substitute biomass for fuel production.
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