Composite fiber membrane and preparation method thereof

Abstract

The present invention discloses a composite fiber membrane and a preparation method thereof. The spinning solution of the composite fiber membrane includes: a shell layer spinning solution and a core layer spinning solution, the shell layer spinning solution includes: a hydrophilic high molecular polymer and a first essential oil smart microcapsule; the core layer spinning solution includes: an essential oil emulsion, a first essential oil inclusion compound and a second essential oil smart microcapsule; the essential oil emulsion includes: a first plant essential oil and an emulsifier; the first essential oil inclusion compound includes: a second plant essential oil and an inclusion body; the second essential oil smart microcapsule includes: a second essential oil inclusion compound, a liposome and a thermosensitive protein, and the second essential oil inclusion compound includes: a second plant essential oil and an inclusion body. The second plant essential oil is secondary-encapsulated using the inclusion body and the liposome, and the prepared composite fiber membrane has a shell-core structure by utilizing the sensitive characteristics of the thermosensitive protein and coaxial electrospinning. The shell-core structure can release the active ingredients in the composite fiber membrane layer by layer, achieving a sustained-release effect, so that the second plant essential oil has a more lasting effect on the human body.

Description

Technical Field

[0001] The present invention relates to the field of composite materials, and in particular to a composite fiber membrane and a preparation method thereof. Background Art

[0002] Essential oils are extracted from herbs, known for their unique aromatic properties, either distilled or pressed. They have been shown to refresh the mind, soothe the nerves and promote sleep, have antibacterial and anti-inflammatory properties, and stimulate metabolism. To use, a suitable amount of essential oil mixed with a base oil is applied to the skin. The oil easily penetrates the skin's capillaries, enters the bloodstream, and is ultimately delivered to various organs in the body, accelerating metabolism and providing nutrients to organ cells. The entire process takes just over ten minutes. Essential oils are colorless, odorous liquids composed of a mixture of saturated and unsaturated hydrocarbons, ethers, ketones, oxides, phenols, and terpenes. These aromas can be inhaled through the nose, where they are transmitted through nerves to soothe the mind and reduce stress. However, due to their high volatility, the effects of essential oils on the body are often less long-lasting. Summary of the Invention

[0003] In order to solve the problems of the prior art, the present invention provides a composite fiber membrane and a method for preparing the same. The technical solution is as follows:

[0004] In one aspect, an embodiment of the present invention provides a composite fiber membrane, wherein the spinning solution of the composite fiber membrane comprises: a shell layer spinning solution and a core layer spinning solution.

[0005] The shell spinning solution comprises: a hydrophilic high molecular polymer and a first essential oil smart microcapsule;

[0006] The core layer spinning solution includes: an essential oil emulsion, a first essential oil inclusion compound and a second essential oil smart microcapsule; the essential oil emulsion includes a first plant essential oil and an emulsifier; the first essential oil inclusion compound includes a second plant essential oil and an inclusion body; the second essential oil smart microcapsule includes: a second essential oil inclusion compound, a liposome and a thermosensitive protein; the second essential oil inclusion compound includes: the second plant essential oil and the inclusion body; the first essential oil smart microcapsule includes: the second essential oil inclusion compound, the liposome and the thermosensitive protein.

[0007] Specifically, the hydrophilic polymer is at least one of gelatin, hyaluronic acid, polyglutamic acid, polyvinyl alcohol, chitosan and bacterial cellulose.

[0008] Specifically, the inclusion body is cyclodextrin or cucurbituril.

[0009] Specifically, the liposome is at least one of cholesterol and phosphatidylcholine.

[0010] Specifically, the first plant essential oil is at least one of lavender essential oil, chamomile essential oil, tea tree essential oil, rose essential oil, ylang-ylang essential oil, frankincense essential oil, sandalwood essential oil and Atlantic cedar essential oil.

[0011] Specifically, the second plant essential oil is at least one of lavender essential oil, chamomile essential oil, tea tree essential oil, rose essential oil, ylang-ylang essential oil, frankincense essential oil, sandalwood essential oil and Atlantic cedar essential oil.

[0012] In another aspect, the present invention provides a method for preparing the composite fiber membrane as described above, the method comprising:

[0013] Mixing the first plant essential oil and the emulsifier in deionized water and homogenizing to obtain the essential oil emulsion;

[0014] mixing the inclusion body and the second plant essential oil to obtain the first essential oil inclusion compound and the second essential oil inclusion compound;

[0015] mixing the liposome, the second essential oil inclusion compound and the phosphate buffer and refrigerating the mixture to obtain a mixed solution;

[0016] Chimerizing the mixed solution with the temperature-sensitive protein through a freeze-thaw method to obtain the first essential oil smart microcapsules and the second essential oil smart microcapsules;

[0017] mixing the hydrophilic high molecular polymer and the first essential oil smart microcapsule to obtain the shell spinning solution;

[0018] mixing the essential oil emulsion, the first essential oil inclusion compound, and the second essential oil smart microcapsules to obtain the core layer spinning solution;

[0019] The shell layer spinning solution and the core layer spinning solution are coaxially electrospun to obtain the composite fiber membrane.

[0020] Specifically, silicone oil paper is used as a receiving substrate during spinning, and the composite fiber membrane on the silicone oil paper is collected by a rotating drum.

[0021] Specifically, in the essential oil emulsion, the mass ratio of the first plant essential oil to water is 1:(3-8); and the mass ratio of the emulsifier to the first plant essential oil is 1:(4-5).

[0022] Specifically, the mass ratio of the second plant essential oil to the inclusion is 4:(5-16).

[0023] Specifically, the mass ratio of the second essential oil inclusion compound to the liposome is 4:(5-20).

[0024] Specifically, the mass ratio of the temperature-sensitive protein to the liposome is 1:(18-22).

[0025] Specifically, in the shell spinning solution, the mass ratio of the hydrophilic polymer to the first essential oil smart microcapsule is 100:(2-15).

[0026] Specifically, the solvent in the shell spinning solution is deionized water, and the mass fraction of the hydrophilic polymer is 2-20%.

[0027] Specifically, in the core layer spinning solution, the solvent is an ethanol solution, and the mass ratio of ethanol to deionized water in the ethanol solution is 70:100; the mass ratio of the essential oil emulsion to the ethanol solution is 2:(9-10); the mass ratio of the first essential oil inclusion complex to the ethanol solution is (5-15):100; the mass ratio of the second essential oil smart microcapsule to the ethanol solution is (2-10):100.

[0028] The technical solution provided by the embodiment of the present invention has the following beneficial effects:

[0029] The spinning solution of the composite fiber membrane provided by the embodiments of the present invention includes a shell layer spinning solution and a core layer spinning solution. The first essential oil inclusion complex in the core layer spinning solution includes: a second plant essential oil and an inclusion body. The inclusion body encapsulates the second plant essential oil, thereby extending the time the plant essential oil acts on the human body and making the second plant essential oil's effect on the human body more lasting. Under the action of an emulsifier, the interfacial tension between the oil phase and the aqueous phase of the first plant essential oil is reduced, forming a low-viscosity, transparent or translucent dispersion system. The tiny emulsion particles overcome gravity through Brownian motion, reducing the occurrence of instabilities such as sedimentation and flocculation of the first plant essential oil during storage and preparation, and effectively encapsulating the transport system. The essential oil emulsion can ensure that the first plant essential oil maintains its properties while continuously emitting a pleasant aroma. The inclusion body and liposomes are used to secondary encapsulate the second plant essential oil. At the same time, the composite fiber membrane prepared by electrospinning has a shell-core structure. The shell-core structure enables the active ingredients to be released layer by layer, achieving a sustained-release effect, making the effect of the second plant essential oil on the human body more lasting. Both the first essential oil smart microcapsule and the second essential oil smart microcapsule can be degraded under specific conditions (for example, when the temperature of the composite fiber membrane reaches the user's body temperature). After degradation, holes are formed at the position of the temperature-sensitive protein on the liposome. When the eye mask is in contact with the skin, the first essential oil smart microcapsule degrades the temperature-sensitive protein embedded in the liposome. After degradation, holes are formed at the position of the temperature-sensitive protein on the liposome, which is conducive to the sustained release and diffusion of the active ingredients of the second plant essential oil through the holes, thereby realizing the intelligent controlled release of the second plant essential oil. This is conducive to the sustained release and diffusion of the active ingredients in the plant essential oil through the holes, thereby prolonging the time for the plant essential oil to act on the human body, and thereby improving the durability of the plant essential oil's effect on the human body. DETAILED DESCRIPTION

[0030] To make the objectives, technical solutions and advantages of the present invention more clear, the embodiments of the present invention will be described in further detail below.

[0031] Example 1

[0032] An embodiment of the present invention provides a composite fiber membrane. The spinning solution of the composite fiber membrane includes a shell layer spinning solution and a core layer spinning solution. The shell layer spinning solution includes a hydrophilic polymer and a first essential oil smart microcapsule. The core layer spinning solution includes an essential oil emulsion, a first essential oil inclusion compound, and a second essential oil smart microcapsule. The essential oil emulsion includes a first plant essential oil and an emulsifier. The first essential oil inclusion compound includes a second plant essential oil and an inclusion compound. The second essential oil smart microcapsules include a second essential oil inclusion compound, liposomes, and a thermosensitive protein. The first essential oil smart microcapsules include a second essential oil inclusion compound, liposomes, and a thermosensitive protein. The composite fiber membrane can be used as various dressings, such as eye patches.

[0033] Specifically, the inclusion body can be cyclodextrin or cucurbituril. In this embodiment, the inclusion body is cyclodextrin. The inner cavity of cyclodextrin and cucurbituril is lipophilic, and the outer wall of cyclodextrin and cucurbituril is hydrophilic, which can encapsulate plant essential oil in its cavity.

[0034] Specifically, the liposome can be at least one of cholesterol and lecithin, and the lecithin can be at least one of soybean lecithin, egg yolk lecithin, hydrogenated lecithin, corn lecithin and rapeseed lecithin. In this embodiment, the lecithin is soybean lecithin, and the mass ratio of soybean lecithin to cholesterol is 1:1.

[0035] In the present embodiment, the first plant essential oil and the second plant essential oil can be at least one of the more weak lavender quintessence oil, chamomile quintessence oil, tea tree quintessence oil, Flos Rosae Rugosae quintessence oil, Ylang Ylang quintessence oil, frankincense quintessence oil, sandalwood quintessence oil and the Atlantic cedar quintessence oil.In the present embodiment, used lavender quintessence oil, chamomile quintessence oil, tea tree quintessence oil, Flos Rosae Rugosae quintessence oil, Ylang Ylang quintessence oil, frankincense quintessence oil, sandalwood quintessence oil and Atlantic cedar quintessence oil are all purchased from Yiwu Lantian Import and Export Co., Ltd., and its purity is 99%.In the present embodiment, the first plant essential oil and the second plant essential oil are that Flos Rosae Rugosae quintessence oil, lavender quintessence oil, chamomile quintessence oil and tea tree quintessence oil mix and make mixed plant essential oil, wherein, the mass ratio of Flos Rosae Rugosae quintessence oil, lavender quintessence oil, chamomile quintessence oil and tea tree quintessence oil is 1:1:1:1, and this composite fiber membrane with the addition of Flos Rosae Rugosae quintessence oil has good beauty and skin care effect.When actual production is used, the mass ratio of Flos Rosae Rugosae quintessence oil, lavender quintessence oil, chamomile quintessence oil and tea tree quintessence oil can be adjusted according to effect. The mixed plant essential oil contains linalool and acetate, which have strong antibacterial effects. This makes the plant essential oil have a certain antibacterial effect on Escherichia coli, Staphylococcus aureus and Candida albicans, which can effectively prevent the proliferation of microorganisms, thereby effectively reducing the chance of infection, reducing the consumption of skin tissue and lipids, and thus reducing the production of harmful substances and alleviating the metabolic burden on the skin. In addition, the mixed plant essential oil has the effect of promoting the synthesis of nitric oxide in tissue cells. The synthesis of a small amount of nitric oxide can act as a vasodilator factor, increase blood flow, promote blood circulation, relieve eye fatigue and have antibacterial properties. At the same time, it accelerates the metabolism of tissues, thereby alleviating fatigue and melanin deposition at the site of action, and accelerates the repair process and improves local water retention. The mixed plant essential oil has a light fragrance and a better experience.

[0036] Specifically, the hydrophilic polymer is at least one of gelatin, hyaluronic acid, polyglutamic acid, polyvinyl alcohol, chitosan and bacterial cellulose. In the present embodiment, the hydrophilic polymer is hyaluronic acid. Hyaluronic acid, also known as hyaluronic acid, is a viscous polysaccharide and is one of the components of human skin. It is produced by microbial fermentation and has the characteristics of low cost, simple process and high output. Hyaluronic acid can generally be divided into cosmetic, edible and pharmaceutical grades. Cosmetic grade hyaluronic acid has the effects of moisturizing, preventing and repairing skin damage, and nourishing the skin. Its theoretical water retention value is as high as 500mL / g or more, making it the best moisturizing factor in nature. In addition, hyaluronic acid is also a good delivery carrier and can be used with various plant extracts and water-soluble ingredients. Therefore, the addition of hyaluronic acid, a safe and natural raw material, can not only greatly enhance the moisturizing effect of the composite fiber membrane, but also play a certain repair and nutritional role on human skin.

[0037] Specifically, the volume ratio of the shell layer spinning solution to the core layer spinning solution is 1:1.

[0038] Specifically, silicone oil paper is used as a receiving substrate during spinning, and the composite fiber membrane on the silicone oil paper is collected by a rotating drum.

[0039] Specifically, the mass ratio of the first plant essential oil to water in the essential oil emulsion is 1:3; the mass ratio of the emulsifier to the first plant essential oil is 1:4. The emulsifier reduces the interfacial tension between the oil phase and the aqueous phase of the first plant essential oil, forming a low-viscosity, transparent or translucent dispersion. The tiny emulsion particles overcome gravity through Brownian motion, reducing instabilities such as sedimentation and flocculation during storage and preparation of the first plant essential oil, effectively encapsulating the transport system. The essential oil emulsion allows the first plant essential oil to maintain stable properties while continuing to emit a pleasant aroma.

[0040] Specifically, the mass ratio of the second plant essential oil to the inclusion complex is 4:5. The inclusion complex secures the second plant essential oil within its inner cavity through host-guest complexation, enhancing its solubility while also improving its stability against oxidative degradation and its control over visible or ultraviolet light, heat, volatility, and sublimation. The addition of the first essential oil inclusion complex stabilizes the second plant essential oil and provides a controlled release of the second plant essential oil after complete volatilization of the first essential oil. The second essential oil inclusion complex is then secondary encapsulated by liposomes to produce first and second essential oil smart microcapsules.

[0041] Specifically, the mass ratio of the second essential oil inclusion complex to the liposome is 4:5.

[0042] Specifically, the mass ratio of the thermosensitive protein to the liposome is 1: 18. In this embodiment, the thermosensitive protein was purchased from Macklin, with the product number: C823250.

[0043] Specifically, in the shell spinning solution, the mass ratio of the hydrophilic polymer to the first essential oil smart microcapsule is 100:2.

[0044] Specifically, when the eye mask contacts the skin, the temperature-sensitive protein embedded in the liposome degrades when the first essential oil smart microcapsule is in contact with the skin. After degradation, holes are formed at the position of the temperature-sensitive protein on the liposome, which facilitates the slow release and diffusion of the active ingredients of the second plant essential oil through the holes, thereby realizing the intelligent controlled release of the second plant essential oil.

[0045] Specifically, the solvent in the shell spinning solution is deionized water, and the mass fraction of the hydrophilic polymer is 2-20%. In this embodiment, the mass fraction of the hydrophilic polymer is 2%.

[0046] Specifically, in the core layer spinning solution, the solvent is an ethanol solution, the mass ratio of ethanol to deionized water in the ethanol solution is 70:100; the mass ratio of the essential oil emulsion to the ethanol solution is 2:9; the mass ratio of the first essential oil inclusion complex to the ethanol solution is 5:100; and the mass ratio of the second essential oil smart microcapsule to the ethanol solution is 1:100.

[0047] Specifically, the shell-core electrospinning method prevents the destruction and loss of bioactive ingredients during the preparation process while also enabling layer-by-layer release of the active ingredients, achieving a sustained-release effect. The second smart microcapsules in the core structure continue to release the second plant essential oil after the first smart microcapsules have gradually released it, ensuring the continuous and effective release of the essential oil components during use of the composite fiber membrane.

[0048] The following briefly introduces the preparation method of the composite fiber membrane provided by the embodiment of the present invention, which is as follows:

[0049] 10 mL of rose essential oil, 10 mL of lavender essential oil, 10 mL of chamomile essential oil and 10 mL of tea tree essential oil were stirred at 300 rpm at 25° C. for 20 min to obtain a first plant essential oil and a second plant essential oil.

[0050] 30 mL of the first plant essential oil was mixed with 90 mL of deionized water, 7.5 mL of Tween 20 emulsifier was added, and the mixture was stirred at 300 rpm for 0.5 h at 25° C. for thorough mixing, and then homogenized at 700 rpm for 10 min to obtain a uniformly mixed essential oil emulsion.

[0051] 5 g of cyclodextrin inclusions and 50 mL of deionized water were mixed and stirred at 300 rpm at 60° C. for 2 h to obtain a cyclodextrin solution; 4 g of the second plant essential oil and 4 g of ethanol were stirred and mixed uniformly at 200 rpm, and then added dropwise into the cyclodextrin solution at a rate of 2 mL / min, and then stirred at 300 rpm at 25° C. for 6 h; after stirring, the mixture was refrigerated at 4° C. for 1 h, and then filtered at a pore size of 0.22 μm. After filtration, the mixture was dried at 40° C. for 3 h to obtain powdered first essential oil inclusion complex and second essential oil inclusion complex.

[0052] 500 mg of soybean lecithin and 500 mg of cholesterol were respectively mixed with 50 mL of chloroform, and ultrasonicated at 80° C. at a frequency of 30 kHz for 15 min. The chloroform was completely removed by rotary drying at control parameters of 30° C. and a rotation speed of 300 rpm for 9 h to obtain treated soybean lecithin and cholesterol. 250 mg of the treated soybean lecithin, 250 mg of cholesterol, 400 mg of the second essential oil inclusion compound and 100 mL of phosphate buffer with a concentration of 0.03 mol / L were mixed, and the mixture was centrifuged at a rotation speed of 5000 rpm for 15 min. After the centrifugation, the mixture was refrigerated at 4° C. for 24 h to obtain a mixed solution.

[0053] 540 mg of mixed liposomes and 30 mg of thermosensitive protein were ultrasonically treated at a frequency of 30 kHz for 10 min at 0°C to obtain a mixed solution. The mixed solution was cooled to -15°C and maintained for 2 h, and then thawed at 25°C for 2 h to complete one freeze-thaw cycle. A total of 5 freeze-thaw cycles were performed to obtain the first essential oil smart microcapsules and the second essential oil smart microcapsules.

[0054] 600 mg of hyaluronic acid, 12 mg of the first essential oil smart microcapsules and 30 g of deionized water were mixed and stirred at 500 rpm for 4 h to obtain a shell spinning solution.

[0055] 1 g of the first essential oil inclusion complex, 0.4 g of the second essential oil smart microcapsules and 20 g of a 70% ethanol solution were mixed so that the mass fraction of the first essential oil inclusion complex was 5% and the mass fraction of the second essential oil smart microcapsules was 10%. After the first essential oil inclusion complex was dissolved, 4.4 g of the essential oil emulsion was added so that the mass ratio of the essential oil emulsion to the ethanol solution was 2:9. The mixture was homogenized at 800 rpm for 10 minutes to obtain a core layer spinning solution.

[0056] 10mL of shell and core spinning solution were fed into standard syringes connected to the outer and inner orifices, respectively. The inner and outer diameters of the nozzles were 0.5 and 1mm, respectively. Spinning was performed at a voltage of 20kV, a receiving distance of 15cm, and a propulsion rate of 1mL / h. Silicone oil paper was used as the receiving substrate, and the composite fiber membrane on the paper was collected by a rotating drum.

[0057] Example 2

[0058] This embodiment differs from the first embodiment in that the first and second plant essential oils provided in this embodiment include rose essential oil, lavender essential oil, chamomile essential oil, and tea tree essential oil, wherein the mass ratio of rose essential oil, lavender essential oil, chamomile essential oil, and tea tree essential oil is 99:1:1:1. The composite fiber membrane containing rose essential oil has excellent skin care effects.

[0059] At the same time, in the present embodiment, the hydrophilic polymer can be hyaluronic acid, polyvinyl alcohol and chitosan, and the mass ratio of hyaluronic acid, polyvinyl alcohol and chitosan is 1:2:1. Hyaluronic acid, polyvinyl alcohol and chitosan are hydrophilic polymers for configuring the wall material solution. After spinning into a film, when this composite fiber membrane comes into contact with water, polyvinyl alcohol and chitosan are insoluble in water, play a skeleton role, and maintain the morphological structure of the membrane; hyaluronic acid will dissolve in water and be locked in the skeleton structure formed by polyvinyl alcohol and chitosan, play a moisturizing effect, and slowly release the essential oil under the action of external conditions. From the perspective of overall morphology, the composite fiber membrane does not dissolve after absorbing water, but forms a gel-like structure, which can better fit the skin while locking in moisture and essential oils.

[0060] Specifically, the volume ratio of the shell layer spinning solution to the core layer spinning solution is 1:2.

[0061] Specifically, the mass ratio of the first plant essential oil to water in the essential oil emulsion is 1:8; the mass ratio of the emulsifier to the first plant essential oil is 1:5.

[0062] Specifically, the mass ratio of the second plant essential oil to the inclusion is 1:4.

[0063] Specifically, the mass ratio of the second essential oil inclusion compound to the liposome is 1:5.

[0064] Specifically, the mass ratio of the thermosensitive protein to the liposome is 1:22.

[0065] Specifically, in the shell spinning solution, the mass ratio of the hydrophilic polymer to the first essential oil smart microcapsule is 100:15.

[0066] Specifically, the solvent in the shell spinning solution is deionized water, and the mass fraction of the hydrophilic polymer is 20%.

[0067] Specifically, in the core layer spinning solution, the solvent is an ethanol solution, in which the mass ratio of ethanol to deionized water is 70:100; the mass ratio of the essential oil emulsion to the ethanol solution is 1:5; the mass ratio of the first essential oil inclusion complex to the B solution is 15:100; and the mass ratio of the second essential oil smart microcapsule to the ethanol solution is 10:100.

[0068] The following briefly introduces the preparation method of the composite fiber membrane provided by the embodiment of the present invention, which is as follows:

[0069] 19.8 mL of rose essential oil, 0.1 mL of lavender essential oil, 0.1 mL of chamomile essential oil and 0.1 mL of tea tree essential oil were stirred at 300 rpm at 25° C. for 20 min to obtain a first plant essential oil and a second plant essential oil.

[0070] 30 mL of the first mixed plant essential oil was mixed with 240 mL of deionized water, 6 mL of Tween 20 emulsifier was added, and the mixture was stirred at 300 rpm for 0.5 h at 25° C. to be fully mixed. The resulting emulsion was homogenized at 700 rpm for 10 min to obtain a uniformly mixed essential oil solution emulsion.

[0071] 5 g of cyclodextrin and 50 mL of deionized water were mixed and stirred at 300 rpm at 60° C. for 2 h to obtain a cyclodextrin solution; 1.25 g of the second plant essential oil and 1.25 g of ethanol were stirred at 200 rpm until uniformly mixed, and then added dropwise into the ethanol aqueous solution of cyclodextrin at a rate of 2 mL / min, and then stirred at 300 rpm at 25° C. for 6 h; after stirring, refrigerated at 4° C. for 1 h, and then filtered at a pore size of 0.22 μm. After filtration, the mixture was dried at 40° C. for 3 h to obtain a powdered first essential oil inclusion complex and a second essential oil inclusion complex.

[0072] 6 g of soybean lecithin and 300 mL of chloroform were mixed, and the mixture was ultrasonically treated at a frequency of 30 kHz for 15 min at 80° C., and the chloroform was completely removed by rotary drying at control parameters of 30° C. and a rotation speed of 300 rpm for 9 h to obtain treated soybean lecithin; 5 g of the treated soybean lecithin, 1 g of the second essential oil inclusion compound, and 500 mL of 0.03 mol / L phosphate buffer were mixed, and the mixture was centrifuged at a rotation speed of 5000 rpm for 15 min. After the centrifugation, the mixture was refrigerated at 4° C. for 24 h to obtain a mixed solution.

[0073] 4.4 g of mixed liposomes and 0.2 g of thermosensitive protein were ultrasonically treated at a frequency of 30 kHz for 10 min at 0°C to obtain a mixed solution. The mixed solution was cooled to -15°C and maintained for 2 h, and then thawed at 25°C for 2 h to complete one freeze-thaw cycle. A total of 5 freeze-thaw cycles were performed to obtain the first essential oil smart microcapsules and the second essential oil smart microcapsules.

[0074] 1 g of hyaluronic acid, 2 g of polyvinyl alcohol, 1 g of chitosan, 0.6 g of the first essential oil smart microcapsule and 20 g of deionized water were mixed and stirred at 500 rpm for 2 h to obtain a shell spinning solution.

[0075] 3 g of the first essential oil inclusion compound, 2 g of the second essential oil smart microcapsules and 20 g of a 70% ethanol solution were mixed so that the mass fraction of the first essential oil inclusion compound was 15% and the mass fraction of the second essential oil smart microcapsules was 10%. After the first essential oil inclusion compound was dissolved, 4 g of the essential oil emulsion was added after dissolution so that the mass ratio of the essential oil emulsion to the ethanol solution was 2:10. The mixture was homogenized at 800 rpm for 10 min to obtain a core layer spinning solution b.

[0076] 7 mL of shell spinning solution a and 14 mL of core spinning solution b were fed into standard syringes connected to the outer and inner orifices, respectively. The inner and outer diameters of the nozzles were 0.5 mm and 1 mm, respectively. The spinning voltage was 20 kV, the receiving distance was 15 cm, and the propulsion rate was 1 mL / h. Silicone oil paper was used as the receiving substrate, and the composite fiber membrane on the paper was collected by a rotating drum.

[0077] Example 3

[0078] The difference between this embodiment and the first embodiment is that the first plant essential oil and the second plant essential oil provided in this embodiment both include rose essential oil, lavender essential oil, chamomile essential oil and tea tree essential oil, wherein the mass ratio of rose essential oil, lavender essential oil, chamomile essential oil and tea tree essential oil is 44:1:1:1, and the hydrophilic polymer can be polyvinyl alcohol, chitosan and gelatin: the mass ratio of polyvinyl alcohol, chitosan and gelatin is 1:1:2, wherein the water solubility of polyvinyl alcohol decreases with the increase of alcoholysis degree, and polyvinyl alcohol with a high alcoholysis degree (88%) is almost insoluble in cold water. At the same time, polyvinyl alcohol has excellent mechanical properties, transparency and other characteristics, which are conducive to the fixation of the morphology of the composite fiber membrane after water absorption; chitosan has good water absorption and air permeability, and the film made by spinning has excellent air permeability; at the same time, the spinning solution is weakly acidic, and chitosan is positively charged in a weakly acidic environment, which makes chitosan have better adsorption properties, so that the composite fiber membrane is more in contact with the skin. Gelatin forms a hydrogel at room temperature, absorbing water and providing a supporting skeleton. It dissolves in water at 35°C and is locked within the skeleton structure of polyvinyl alcohol and chitosan, providing a moisturizing effect. The composite fiber membrane, infused with rose essential oil, has excellent skincare and beauty benefits.

[0079] The following briefly introduces the preparation method of the composite fiber membrane provided by the embodiment of the present invention, which is as follows:

[0080] Specifically, the volume ratio of the shell layer spinning solution to the core layer spinning solution is 2:3.

[0081] Specifically, the mass ratio of the first plant essential oil to water in the essential oil emulsion is 1:5; the mass ratio of the emulsifier to the first plant essential oil is 1:4.5.

[0082] Specifically, the mass ratio of the second plant essential oil to the inclusion is 1:4.

[0083] Specifically, the mass ratio of the second essential oil inclusion compound to the liposome is 1:2.5.

[0084] Specifically, the mass ratio of the thermosensitive protein to the liposome is 1:20.

[0085] Specifically, in the shell spinning solution, the mass ratio of the hydrophilic polymer to the first essential oil smart microcapsule is 100:10.

[0086] Specifically, the solvent in the shell spinning solution is deionized water, and the mass fraction of the hydrophilic polymer is 10%.

[0087] Specifically, in the core layer spinning solution, the solvent is an ethanol solution, in which the mass ratio of ethanol to deionized water is 70:100; the mass ratio of the essential oil emulsion to the ethanol solution is 1:3; the mass ratio of the first essential oil inclusion complex to the B solution is 10:100; and the mass ratio of the second essential oil smart microcapsule to the ethanol solution is 5:100.

[0088] The following briefly introduces the preparation method of the composite fiber membrane provided by the embodiment of the present invention, which is as follows:

[0089] 17.6 mL of rose essential oil, 0.4 mL of lavender essential oil, 0.4 mL of chamomile essential oil and 0.4 mL of tea tree essential oil were stirred at 300 rpm at 25° C. for 20 min to obtain a first plant essential oil and a second plant essential oil.

[0090] 50 mL of the first mixed plant essential oil was mixed with 250 mL of deionized water, 11 mL of Tween 20 emulsifier was added, and the mixture was stirred at 300 rpm for 0.5 h at 25° C. to fully mix. The resulting emulsion was homogenized at 700 rpm for 10 min to obtain a uniformly mixed essential oil solution emulsion.

[0091] 4 g of cyclodextrin and 40 mL of deionized water were mixed and stirred at 300 rpm at 60°C for 2 h to obtain a cyclodextrin solution; 1 g of the second plant essential oil and 1 g of ethanol were stirred and mixed uniformly at 200 rpm, and then added dropwise into the ethanol aqueous solution of cyclodextrin at a rate of 2 mL / min, and then stirred at 300 rpm at 25°C for 6 h; after stirring, refrigerated at 4°C for 1 h, and then filtered at a pore size of 0.22 μm. After filtration, the mixture was dried at 40°C for 3 h to obtain powdered first essential oil inclusion complex and second essential oil inclusion complex.

[0092] 5 g of cholesterol and 250 mL of chloroform were mixed, ultrasonicated at 80° C. at a frequency of 30 kHz for 15 min, and rotary dried at a control parameter of 30° C. and a rotation speed of 300 rpm for 9 h to completely remove the chloroform to obtain treated soybean lecithin; 5 g of the treated cholesterol, 2 g of the second essential oil inclusion complex, and 500 mL of 0.03 mol / L phosphate buffer were mixed, and the mixture was centrifuged at a rotation speed of 5000 rpm for 15 min. After the centrifugation, the mixture was refrigerated at 4° C. for 24 h to obtain a mixed solution.

[0093] 4 g of mixed liposomes and 0.2 g of thermosensitive protein were ultrasonically treated at a frequency of 30 kHz for 10 min at 0°C to obtain a mixed solution. The mixed solution was cooled to -15°C and maintained for 2 h, and then thawed at 25°C for 2 h to complete one freeze-thaw cycle. A total of 5 freeze-thaw cycles were performed to obtain the first essential oil smart microcapsules and the second essential oil smart microcapsules.

[0094] 0.5 g of polyvinyl alcohol, 0.5 g of chitosan, 2 g of gelatin, 0.3 g of the first essential oil smart microcapsule and 30 g of deionized water were mixed and stirred at 500 rpm for 2 h to obtain a shell spinning solution.

[0095] 2 g of the first essential oil inclusion compound, 5 g of the second essential oil smart microcapsules and 20 g of a 70% ethanol solution were mixed so that the mass fraction of the first essential oil inclusion compound was 15% and the mass fraction of the second essential oil smart microcapsules was 10%. After the first essential oil inclusion compound was dissolved, 6.7 g of the essential oil emulsion was added after dissolution so that the mass ratio of the essential oil emulsion to the ethanol solution was 1:3. The mixture was homogenized at 800 rpm for 10 min to obtain a core layer spinning solution b.

[0096] 8 mL of shell spinning solution a and 12 mL of core spinning solution b were fed into standard syringes connected to the outer and inner orifices, respectively. The inner and outer diameters of the nozzles were 0.5 and 1 mm, respectively. The spinning voltage was 20 kV, the receiving distance was 15 cm, and the propulsion rate was 1 mL / h. Silicone oil paper was used as the receiving substrate, and the composite fiber membrane on the silicone oil paper was collected by a rotating drum.

[0097] Example 4

[0098] The difference between this embodiment and the first embodiment is that the mass ratio of ylang-ylang essential oil, lavender essential oil, chamomile essential oil and tea tree essential oil is 1:1:1:1. The composite fiber membrane with ylang-ylang essential oil added has a good effect of relieving tension.

[0099] Example 5

[0100] The difference between this embodiment and the fourth embodiment is that the mass ratio of ylang-ylang essential oil, lavender essential oil, chamomile essential oil and tea tree essential oil is 99:1:1:1. The composite fiber membrane with ylang-ylang essential oil added has a good effect of relieving tension.

[0101] Example 6

[0102] The difference between this embodiment and embodiment 4 is that the first plant essential oil and the second plant essential oil provided in this embodiment both include: ylang-ylang essential oil, lavender essential oil, chamomile essential oil and tea tree essential oil, wherein the mass ratio of ylang-ylang essential oil, lavender essential oil, chamomile essential oil and tea tree essential oil is 25:1:1:1, and the composite fiber membrane with added ylang-ylang essential oil has a good effect of relieving tension.

[0103] Example 7

[0104] The difference between this embodiment and the first embodiment is that the mass ratio of sandalwood essential oil, lavender essential oil, chamomile essential oil and tea tree essential oil is 1:1:1:1. The composite fiber membrane with added sandalwood essential oil has a good effect of reducing fine lines on the skin.

[0105] Example 8

[0106] The difference between this embodiment and embodiment 7 is that the mass ratio of sandalwood essential oil, lavender essential oil, chamomile essential oil and tea tree essential oil is 99:1:1:1. The composite fiber membrane with added sandalwood essential oil has a good effect of reducing fine lines on the skin.

[0107] Embodiment 9

[0108] This embodiment differs from the seventh embodiment in that the first and second plant essential oils provided in this embodiment both comprise sandalwood essential oil, lavender essential oil, chamomile essential oil, and tea tree essential oil, which are mixed to form a mixed plant essential oil. The mass ratio of sandalwood essential oil, lavender essential oil, chamomile essential oil, and tea tree essential oil is 16:1:1:1. The composite fiber membrane containing sandalwood essential oil exhibits a good effect in reducing fine lines on the skin.

[0109] Example 10

[0110] The difference between this embodiment and the first embodiment is that the mass ratio of Atlantic cedar essential oil, lavender essential oil, chamomile essential oil and tea tree essential oil is 1:1:1:1. The composite fiber membrane with Atlantic cedar essential oil added has good anti-inflammatory and antibacterial effects.

[0111] Example 11

[0112] The difference between this embodiment and the tenth embodiment is that the mass ratio of Atlantic cedar essential oil, lavender essential oil, chamomile essential oil and tea tree essential oil is 99:1:1:1. The composite fiber membrane with Atlantic cedar sandalwood essential oil added has good anti-inflammatory and antibacterial effects.

[0113] Example 12

[0114] This embodiment differs from the tenth embodiment in that the first and second plant essential oils provided in this embodiment both include cedarwood essential oil, lavender essential oil, chamomile essential oil, and tea tree essential oil, wherein the mass ratio of cedarwood essential oil, lavender essential oil, chamomile essential oil, and tea tree essential oil is 35:1:1:1. The composite fiber membrane containing cedarwood essential oil exhibits excellent anti-inflammatory and antibacterial effects.

[0115] The composite fiber membrane prepared in this example was tested to determine the release content of the plant essential oil in the spinning membrane in the ethanol solution at different times. The results are recorded in Table 1.

[0116] Table 1 is the test results of composite fiber membrane

[0117]

[0118] As can be seen from Table 1, the composite fiber membranes provided by Examples 1, 3, and 6 of the present invention can all make the plant essential oil have good durability. Specifically, the essential oil is dispersed in deionized water to obtain an essential oil emulsion, the essential oil is encapsulated by inclusions and liposomes, and embedded in thermosensitive proteins to obtain essential oil smart microcapsules, which are mixed with a hydrophilic polymer solution to prepare a spinning solution, and a composite fiber membrane with a shell-core structure is prepared by coaxial electrospinning. The active ingredients in the essential oil are well preserved during the preparation process, and the holes formed by the degradation of the phospholipid bilayer of the liposome by the thermosensitive protein achieve the effect of layer-by-layer release, thereby extending the time for the plant essential oil to act on the human body, thereby improving the durability of the plant essential oil on the human body and meeting the effect of long-lasting soothing release of the active ingredients of the essential oil in the steam eye mask.

[0119] The spinning solution of the composite fiber membrane provided by the embodiment of the present invention includes a shell layer spinning solution and a core layer spinning solution, and the first essential oil inclusion compound in the core layer spinning solution includes: a second plant essential oil and an inclusion body, and the second plant essential oil is embedded by the inclusion body, thereby prolonging the time for the plant essential oil to act on the human body, making the effect of the second plant essential oil on the human body more lasting. At the same time, the composite fiber membrane prepared by electrospinning has a shell-core structure, so that the composite fiber membrane can release the active ingredients layer by layer to achieve a sustained release effect. In addition, the first essential oil smart microcapsules and the second essential oil smart microcapsules can be degraded under specific conditions, and holes are formed at the position of the temperature-sensitive protein on the liposome after degradation, which is conducive to the sustained release and diffusion of the active ingredients in the plant essential oil through the holes, thereby prolonging the time for the plant essential oil to act on the human body, thereby improving the durability of the plant essential oil on the human body.

[0120] The composite fiber membrane provided by the present invention can also be used to prepare steam eye masks. In addition to its own aromatic effect, plant essential oils also have the effects of refreshing the brain, calming the nerves and promoting sleep, antibacterial and anti-inflammatory, and promoting metabolism. Through the heating of the self-heating patch, the plant essential oils in the steam eye mask can be gradually released. Through contact with the skin, etc., it can relieve fatigue and melanin deposition in the affected area (such as the eyes), accelerate the repair process, and improve local water retention. The essential oils can also be absorbed by human skin and enter the human body, promoting blood circulation in the body, improving fatigue, and soothing the body and mind.

[0121] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A composite fiber membrane, characterized in that: The spinning solution of the composite fiber membrane includes: shell layer spinning solution and core layer spinning solution, The shell spinning solution comprises: a hydrophilic high molecular polymer and a first essential oil smart microcapsule; The core layer spinning solution includes: an essential oil emulsion, a first essential oil inclusion compound and a second essential oil smart microcapsule; the essential oil emulsion includes: a first plant essential oil and an emulsifier; the first essential oil inclusion compound includes: a second plant essential oil and an inclusion body; the second essential oil smart microcapsule includes: a second essential oil inclusion compound, a liposome and a thermosensitive protein; the second essential oil inclusion compound includes: the second plant essential oil and the inclusion body; the first essential oil smart microcapsule includes: the second essential oil inclusion compound, the liposome and the thermosensitive protein.

2. The composite fiber membrane according to claim 1, characterized in that The hydrophilic high molecular polymer is at least one of gelatin, hyaluronic acid, polyglutamic acid, polyvinyl alcohol, chitosan and bacterial cellulose.

3. The composite fiber membrane according to claim 1, characterized in that The inclusions are cyclodextrin or cucurbituril.

4. The composite fiber membrane according to claim 1, characterized in that The liposome is at least one of cholesterol and phosphatidylcholine.

5. The composite fiber membrane according to claim 1, characterized in that The first plant essential oil is at least one of lavender essential oil, chamomile essential oil, tea tree essential oil, rose essential oil, ylang-ylang essential oil, frankincense essential oil, sandalwood essential oil and Atlantic cedar essential oil.

6. The composite fiber membrane according to claim 1, characterized in that The second plant essential oil is at least one of lavender essential oil, chamomile essential oil, tea tree essential oil, rose essential oil, ylang-ylang essential oil, frankincense essential oil, sandalwood essential oil and Atlantic cedar essential oil.

7. A method for preparing a composite fiber membrane according to any one of claims 1 to 6, characterized in that: The preparation method comprises: Mixing the first plant essential oil and the emulsifier in deionized water and homogenizing to obtain the essential oil emulsion; mixing the inclusion body and the second plant essential oil to obtain the first essential oil inclusion compound and the second essential oil inclusion compound; mixing the liposome, the second essential oil inclusion compound and the phosphate buffer and refrigerating the mixture to obtain a mixed solution; Chimerizing the mixed solution with the temperature-sensitive protein through a freeze-thaw method to obtain the first essential oil smart microcapsules and the second essential oil smart microcapsules; mixing the hydrophilic high molecular polymer and the first essential oil smart microcapsule to obtain the shell spinning solution; mixing the essential oil emulsion, the first essential oil inclusion compound, and the second essential oil smart microcapsules to obtain the core layer spinning solution; The shell layer spinning solution and the core layer spinning solution are coaxially electrospun to obtain the composite fiber membrane.

8. The preparation method according to claim 7, characterized in that The volume ratio of the first plant essential oil to water in the essential oil emulsion is 1:(3-8); the mass ratio of the emulsifier to the first plant essential oil is 1:(4-5).

9. The preparation method according to claim 7, characterized in that The mass ratio of the second plant essential oil to the inclusions is 4:(5-16).

10. The preparation method according to claim 7, characterized in that The mass ratio of the temperature-sensitive protein to the liposome is 1:(18-22).

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