阅读说明：本技术 一种精油微胶囊的制备方法 (Preparation method of essential oil microcapsule ) 是由 郑遂 盛文文 郭华 王良 李海涛 戴俊 于 2021-10-25 设计创作，主要内容包括：本发明公开了一种精油微胶囊的制备方法,包括制备初级精油,精油改性,制备油相,制备水相,制备初级精油微胶囊,后处理；其中,制备初级精油为将鲜橙皮和鲜牛志混合混匀后进行真空烘干,然后粉碎至80-90目,再装入萃取釜中进行超临界CO2萃取,然后将萃取液进行减压浓缩,待减压浓缩结束后加入香芹酚和纳米氮化硼,再进行机械振荡,机械振荡结束后得到初级精油；本发明的制备方法能够在降低微胶囊孔隙,防止精油微胶囊中精油挥发过快的同时,提高在使用中有效成分的释放,并降低精油微胶囊中精油对皮肤的刺激。(The invention discloses a preparation method of an essential oil microcapsule, which comprises the steps of preparing primary essential oil, modifying the essential oil, preparing an oil phase, preparing a water phase, preparing the primary essential oil microcapsule and carrying out aftertreatment; the preparation method comprises the steps of mixing and uniformly mixing fresh orange peels and fresh fructus phyllanthi, drying in vacuum, crushing to 80-90 meshes, then placing the obtained product into an extraction kettle for supercritical CO2 extraction, then carrying out reduced pressure concentration on the extract liquor, adding carvacrol and nano boron nitride after the reduced pressure concentration is finished, carrying out mechanical oscillation, and obtaining primary essential oil after the mechanical oscillation is finished; the preparation method of the invention can reduce the pores of the microcapsules, prevent the essential oil in the essential oil microcapsules from volatilizing too fast, improve the release of effective components in use and reduce the irritation of the essential oil in the essential oil microcapsules to skin.)

1. A preparation method of essential oil microcapsules is characterized by comprising the steps of preparing primary essential oil, modifying the essential oil, preparing an oil phase, preparing a water phase, preparing the primary essential oil microcapsules and carrying out aftertreatment;

the preparation of the primary essential oil comprises the steps of mixing and uniformly mixing fresh orange peel and fresh oregano according to the mass ratio of 1:2-3, then carrying out vacuum drying, controlling the vacuum degree to be 0.07-0.08MPa, the drying temperature to be 50-60 ℃, crushing after drying for 1-1.5h, crushing to 80-90 meshes to obtain crushed orange peel powder and oregano powder, then loading the crushed orange peel powder and oregano powder into an extraction kettle, adding 3-4 times of anhydrous ethanol, then carrying out supercritical CO2 extraction, controlling the extraction pressure to be 25-30MPa, the extraction temperature to be 40-45 ℃, the extraction time to be 2-2.5h, and the flow of CO2 to be 120-130kg/h, and obtaining an extraction liquid after the extraction is finished; then carrying out reduced pressure concentration on the extract liquor, controlling the temperature during reduced pressure distillation to be 35-40 ℃ and the pressure during reduced pressure distillation to be 0.07-0.075MPa, and carrying out reduced pressure distillation for 0.5-1h to obtain a concentrated solution; adding carvacrol and nano boron nitride into the concentrated solution, controlling the mass ratio of carvacrol to nano boron nitride to be 50-60:6-8:1-2, then carrying out mechanical oscillation, controlling the rotation speed of the mechanical oscillation to be 200-210rpm, controlling the time of the mechanical oscillation to be 45-50min, and obtaining primary essential oil after the mechanical oscillation is finished.

2. The preparation method of essential oil microcapsules as claimed in claim 1, wherein the essential oil modification comprises the steps of uniformly mixing primary essential oil and nano zeolite powder, adding the mixture into a high shear reaction kettle, setting the shear speed of the high shear reaction kettle to 2500rpm, adding diallyl dimethyl ammonium chloride, polyvinyl amine and tea polyphenol after shearing for 30-40min, controlling the shear speed to 3000rpm, and continuously shearing for 40-50min to obtain the modified essential oil.

3. The preparation method of essential oil microcapsules of claim 2, wherein the mass ratio of the primary essential oil, the nano zeolite powder, the diallyldimethylammonium chloride, the polyvinylamine and the tea polyphenol in the essential oil modification step is 30-40:20-23:1-2:1-1.2: 3-5.

4. The method for preparing essential oil microcapsules according to claim 1, wherein the oil phase is prepared by mixing the modified essential oil and xanthan gum, adding the mixture into n-hexadecane, then performing radiation modification by using intermediate energy electron beams while stirring at the speed of 100-120rpm, controlling the energy of the intermediate energy electron beams to be 3-4MeV and the radiation dose to be 200-250kGy, and stopping stirring and radiation after 30-40min to obtain the oil phase.

5. The method for preparing essential oil microcapsules of claim 4, wherein the mass ratio of the modified essential oil, xanthan gum and n-hexadecane in the oil phase preparation step is 10-12:1-2: 50-60.

6. The method for preparing essential oil microcapsules of claim 1, wherein the aqueous phase is prepared by uniformly mixing sodium dodecyl sulfate and zwitterionic polyacrylamide and dissolving the mixture in deionized water.

7. The method for preparing essential oil microcapsules of claim 6, wherein the mass ratio of the sodium dodecyl sulfate, the zwitterionic polyacrylamide and the deionized water in the step of preparing the aqueous phase is 5-8:2-4: 25-30.

8. The preparation method of essential oil microcapsules as claimed in claim 1, wherein the primary essential oil microcapsules are prepared by mixing an oil phase and a water phase, adding the mixture into a high-shear reaction kettle, setting the temperature of the high-shear reaction kettle to 30-35 ℃, setting the shear speed to 2000-2500rpm, shearing for 30-40min, adding polyethylene glycol 6000 and diethylenetriamine into the high-shear reaction kettle, setting the temperature of the high-shear reaction kettle to 35-40 ℃, setting the shear speed to 2500-3000rpm, cutting for 25-30min, stopping high-shear, setting the temperature of the high-shear reaction kettle to 50-55 ℃, standing for 45-60min to obtain a reactant, performing suction filtration on the reactant, and washing for 2-3 times by using deionized water to obtain the primary essential oil microcapsules.

9. The method for preparing essential oil microcapsules of claim 8, wherein the mass ratio of the oil phase, the water phase, the polyethylene glycol 6000 and the diethylenetriamine in the step of preparing the primary essential oil microcapsules is 20-22:60-70:2-5: 1-3.

10. The preparation method of essential oil microcapsules according to claim 1, wherein in the post-treatment, the primary essential oil microcapsules are placed in a nitrogen atmosphere, the pressure of nitrogen is controlled to be 0.15-0.18MPa, the temperature is raised to 40-45 ℃, then the post-treatment liquid is sprayed on the surfaces of the primary essential oil microcapsules, the mass ratio of the primary essential oil microcapsules to the post-treatment liquid is controlled to be 1:1.4-1.6, the spraying speed is 30-35kg/h, the micro-current treatment is carried out while spraying, the current is controlled to be 4-6uA, after the spraying is finished, the micro-current is stopped, the sprayed primary essential oil microcapsules are obtained, the sprayed primary essential oil microcapsules are placed in an oven to be dried, the drying temperature is controlled to be 40-45 ℃, the drying time is 2-2.5h, and the essential oil microcapsules are obtained after the drying is finished.

Technical Field

The invention relates to a preparation method of an essential oil microcapsule, belonging to the technical field of plant essential oil.

Background

The essential oil is a general term of volatile aromatic substances obtained by processing and extracting from aromatic plants or secreted animals. Generally, the essential oil is volatile aromatic substance extracted from flower, leaf, root, seed, fruit, bark, resin, and core of plant by steam distillation, cold pressing, fat absorption or solvent extraction; the essential oil has strong volatility, and can be volatilized quickly once contacting air, the essential oil is easy to deteriorate after being unsealed, afraid of high temperature and low temperature, and is difficult to store, in addition, the concentration of the essential oil is too large, the irritation is too large when the essential oil is used, and if the essential oil is directly smeared on a body, the body can be burnt, and the popularization and the use of the essential oil are limited.

In order to improve the stability of essential oil and prevent the volatilization of the essential oil, the essential oil is usually prepared into essential oil microcapsules so as to improve the stability of the essential oil, but after the essential oil is subjected to microencapsulation, the release of active ingredients in the essential oil is unstable, so that the use effect of the essential oil can be greatly reduced, and the surface of the microcapsules is a sunken and porous unsealed structure when the essential oil microcapsules are prepared, so that the protection effect on a core material is influenced, the shelf life of a product is easily shortened, although the preparation method can be improved so as to reduce the pores on the surfaces of the microcapsules, the release of the active ingredients is easily reduced while the release of the active ingredients is improved, so that the pores on the surfaces of the microcapsules are reduced, and the protection on the core material is improved, which is a technical problem which is urgently needed to be solved at present; in addition, for essential oils that are irritating to the skin, such as oregano essential oil, it is still difficult to solve the problem of irritating to the skin by means of microcapsules.

Patent CN110743472A discloses an essential oil microcapsule composition, which comprises a core material, a wall material, an emulsifier and water, wherein the weight of the core material accounts for 30-80% of the total dry weight of the essential oil microcapsule composition, the weight of the wall material accounts for 10-45% of the total dry weight of the essential oil microcapsule composition, the weight of the emulsifier accounts for 2-35% of the total dry weight of the essential oil microcapsule composition, the core material is an essential oil, based on the total weight of the wall material, the wall material comprises 70-100% by weight of a hyaluronic acid-based component, and the hyaluronic acid-based component comprises: hydrolyzed hyaluronic acid and/or a salt thereof having a molecular weight of not more than 10kDa, hyaluronic acid and/or a salt thereof having a molecular weight of 100kDa to 800kDa, and a crosslinked polymer of hyaluronic acid or a salt thereof; the patent has the following defects: the drying process causes great loss of essential oil, and the essential oil microcapsules have more pores on the surface, so that the shelf life of the essential oil microcapsules is short.

Patent CN106509893A discloses an essential oil microcapsule and a preparation method thereof, the essential oil microcapsule comprises a wall material, a first emulsifier, a stabilizer, and a buffer salt, wherein the core of the essential oil microcapsule comprises a core material and a second emulsifier; the wall material consists of a component A and a component B, wherein the component A is maltodextrin and/or maltose syrup, and the component B is whey protein isolate and/or soybean protein isolate; the patent has the following defects: the prepared essential oil microcapsule has unstable release of effective components, reduces the use effect of essential oil, and causes great loss of essential oil in the drying process during preparation of the essential oil microcapsule.

Disclosure of Invention

Aiming at the defects in the prior art, the invention provides the preparation method of the essential oil microcapsule, which can improve the release of effective components in use and reduce the stimulation of the essential oil in the essential oil microcapsule to the skin while reducing the pore space of the microcapsule and preventing the essential oil in the essential oil microcapsule from volatilizing too fast.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows:

a method for preparing essential oil microcapsule comprises preparing primary essential oil, modifying essential oil, preparing oil phase, preparing water phase, preparing primary essential oil microcapsule, and post-treating.

The preparation of the primary essential oil comprises the steps of mixing and uniformly mixing fresh orange peel and fresh oregano according to the mass ratio of 1:2-3, then carrying out vacuum drying, controlling the vacuum degree to be 0.07-0.08MPa, the drying temperature to be 50-60 ℃, crushing after drying for 1-1.5h, crushing to 80-90 meshes to obtain crushed orange peel powder and oregano powder, then loading the crushed orange peel powder and oregano powder into an extraction kettle, adding 3-4 times of anhydrous ethanol, then carrying out supercritical CO2 extraction, controlling the extraction pressure to be 25-30MPa, the extraction temperature to be 40-45 ℃, the extraction time to be 2-2.5h, and the flow of CO2 to be 120-130kg/h, and obtaining an extraction liquid after the extraction is finished; then carrying out reduced pressure concentration on the extract liquor, controlling the temperature during reduced pressure distillation to be 35-40 ℃ and the pressure during reduced pressure distillation to be 0.07-0.075MPa, and carrying out reduced pressure distillation for 0.5-1h to obtain a concentrated solution; adding carvacrol and nano boron nitride into the concentrated solution, controlling the mass ratio of carvacrol to nano boron nitride to be 50-60:6-8:1-2, then carrying out mechanical oscillation, controlling the rotation speed of the mechanical oscillation to be 200-210rpm, controlling the time of the mechanical oscillation to be 45-50min, and obtaining primary essential oil after the mechanical oscillation is finished.

And the essential oil modification step comprises the steps of uniformly mixing the primary essential oil and the nano zeolite powder, adding the mixture into a high-shear reaction kettle, setting the shearing speed of the high-shear reaction kettle to 2500 plus materials at 2500rpm, shearing for 30-40min, adding diallyl dimethyl ammonium chloride, polyvinylamine and tea polyphenol, controlling the shearing speed to 2500 plus materials at 3000rpm, and continuously shearing for 40-50min to obtain the modified essential oil.

In the step of modifying the essential oil, the primary essential oil, the nano zeolite powder, the diallyl dimethyl ammonium chloride, the polyvinylamine and the tea polyphenol are mixed according to the mass ratio of 30-40:20-23:1-2:1-1.2: 3-5.

The effective content of the diallyl dimethyl ammonium chloride is 65%.

The particle size of the nano zeolite powder is 200-300 nm.

The oil phase is prepared, the modified essential oil and xanthan gum are mixed and then added into n-hexadecane, and then the mixture is stirred at the speed of 100-120rpm while radiation modification is carried out by adopting intermediate energy electron beams, the energy of the intermediate energy electron beams is controlled to be 3-4MeV, the radiation dose is controlled to be 200-250kGy, and stirring and radiation are stopped after 30-40min, so that the oil phase is obtained.

The mass ratio of the modified essential oil, the xanthan gum and the n-hexadecane in the oil phase preparation step is 10-12:1-2: 50-60.

The preparation method comprises the steps of uniformly mixing sodium dodecyl sulfate and zwitterionic polyacrylamide, and dissolving the mixture in deionized water to obtain the water phase.

In the step of preparing the water phase, the mass ratio of the sodium dodecyl sulfate to the zwitterionic polyacrylamide to the deionized water is 5-8:2-4: 25-30.

The preparation method comprises the steps of mixing an oil phase and a water phase, adding the mixture into a high-shear reaction kettle, setting the temperature of the high-shear reaction kettle to be 30-35 ℃, setting the shearing speed to be 2500rpm, adding polyethylene glycol 6000 and diethylenetriamine into the high-shear reaction kettle after shearing for 30-40min, setting the temperature of the high-shear reaction kettle to be 35-40 ℃, setting the shearing speed to be 2500rpm, stopping high shearing after shearing for 25-30min, setting the temperature of the high-shear reaction kettle to be 50-55 ℃, standing for 45-60min to obtain a reactant, performing suction filtration on the reactant, and then cleaning for 2-3 times by using deionized water to obtain the primary essential oil microcapsule.

In the step of preparing the primary essential oil microcapsule, the mass ratio of the oil phase, the water phase, the polyethylene glycol 6000 and the diethylenetriamine is 20-22:60-70:2-5: 1-3.

And the post-treatment, namely placing the primary essential oil microcapsules in a nitrogen atmosphere, controlling the pressure of nitrogen to be 0.15-0.18MPa, raising the temperature to 40-45 ℃, then spraying the post-treatment liquid on the surfaces of the primary essential oil microcapsules, controlling the mass ratio of the primary essential oil microcapsules to the post-treatment liquid to be 1:1.4-1.6, controlling the spraying speed to be 30-35kg/h, carrying out micro-current treatment while spraying, controlling the current to be 4-6uA, stopping micro-current after spraying to obtain the sprayed primary essential oil microcapsules, placing the sprayed primary essential oil microcapsules in a drying oven for drying, controlling the drying temperature to be 40-45 ℃, the drying time to be 2-2.5h, and obtaining the essential oil microcapsules after drying.

The post-treatment liquid comprises the following components in parts by weight: 2-5 parts of polyvinyl alcohol 1788, 1-3 parts of glyoxal, 0.2-0.4 part of acetic acid, 0.5-1 part of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, 1-3 parts of glycerol and 18-20 parts of deionized water.

Compared with the prior art, the invention has the beneficial effects that:

(1) according to the preparation method of the essential oil microcapsule, the pores of the essential oil microcapsule can be reduced by modifying the essential oil and post-treating the essential oil microcapsule, so that the essential oil in the essential oil microcapsule is prevented from volatilizing too fast, and the weight reduction rate of the essential oil microcapsule is 2.4-3.6% after the essential oil microcapsule is placed in an open environment at the temperature of 35 ℃ and the humidity of 70% for 10 days;

(2) according to the preparation method of the essential oil microcapsule, the stimulation of the oregano essential oil to the whole skin can be reduced by modifying the essential oil and performing post-treatment on the essential oil microcapsule, and through carrying out a plurality of times of complete skin irritation tests, the essential oil microcapsule has the stimulation index of 0 to the multiple times of the complete skin and has no irritation in the stimulation intensity level;

(3) according to the preparation method of the essential oil microcapsule, the stimulation of the oregano essential oil to damaged skin can be reduced by modifying the essential oil and performing post-treatment on the essential oil microcapsule, and through performing a damaged skin irritation test for one time, the essential oil microcapsule has the stimulation index of 0 to the damaged skin for one time and has no stimulation in the stimulation intensity level;

(4) according to the preparation method of the essential oil microcapsule, the release speed of active ingredients can be improved by modifying the essential oil and performing radiation modification on the oil phase in the preparation of the essential oil microcapsule, and a suspension quantitative bacteriostasis test is performed according to the evaluation method of the antibacterial and bacteriostasis effects of WS/T650-2019 of the national standards of health and State of the people's republic of China, so that the bacteriostasis rate of the prepared essential oil microcapsule to staphylococcus aureus can reach 99.98-100%, the bacteriostasis rate to escherichia coli can reach 99.92-100%, and the bacteriostasis rate to candida albicans can reach 99.95-100% within 1 min; the bacteriostasis rate to staphylococcus aureus can reach 99.92-100 percent in 3min, the bacteriostasis rate to escherichia coli can reach 99.86-99.92 percent, and the bacteriostasis rate to candida albicans can reach 99.92-100 percent; the bacteriostasis rate to staphylococcus aureus can reach 99.91-100 percent, the bacteriostasis rate to escherichia coli can reach 99.84-99.91 percent and the bacteriostasis rate to candida albicans can reach 99.91-100 percent in 6 min; the bacteriostatic rate of the antibacterial agent for staphylococcus aureus can reach 99.91-99.98 percent in 10min, the bacteriostatic rate for escherichia coli can reach 99.82-99.88 percent, and the bacteriostatic rate for candida albicans can reach 99.91-100 percent.

Detailed Description

In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.

Example 1

A preparation method of an essential oil microcapsule comprises the following steps:

1. preparing primary essential oil: mixing and uniformly mixing fresh orange peel and fresh fructus Origani according to the mass ratio of 1:2, then drying in vacuum, controlling the vacuum degree to be 0.07MPa, the drying temperature to be 50 ℃, crushing after drying for 1h, and crushing to 80 meshes to obtain crushed orange peel powder and origanum powder, then loading the crushed orange peel powder and origanum powder into an extraction kettle, adding 3 times of absolute ethyl alcohol by mass, then carrying out supercritical CO2 extraction, controlling the extraction pressure to be 25MPa, the extraction temperature to be 40 ℃, the extraction time to be 2h, and the flow of CO2 to be 120kg/h, and obtaining an extraction liquid after the extraction is finished; then concentrating the extract under reduced pressure, controlling the temperature at 35 deg.C and the pressure at 0.07MPa, and distilling under reduced pressure for 0.5 hr to obtain concentrated solution; and then adding carvacrol and nano boron nitride into the concentrated solution, controlling the mass ratio of carvacrol to nano boron nitride to be 50:6:1, then carrying out mechanical oscillation, controlling the rotation speed of the mechanical oscillation to be 200rpm, controlling the time of the mechanical oscillation to be 45min, and obtaining primary essential oil after the mechanical oscillation is finished.

2. Modifying the essential oil: uniformly mixing primary essential oil and nano zeolite powder, adding the mixture into a high-shear reaction kettle, setting the shearing speed of the high-shear reaction kettle to 2000rpm, adding diallyl dimethyl ammonium chloride, polyvinylamine and tea polyphenol after shearing for 30min, controlling the shearing speed to 2500rpm, and continuously shearing for 40min to obtain modified essential oil;

wherein the mass ratio of the primary essential oil, the nano zeolite powder, the diallyl dimethyl ammonium chloride, the polyvinyl amine and the tea polyphenol is 30:20:1:1: 3;

the effective content of the diallyl dimethyl ammonium chloride is 65%;

the particle size of the nano zeolite powder is 200 nm.

3. Preparing an oil phase: mixing the modified essential oil and xanthan gum, adding the mixture into n-hexadecane, stirring at the speed of 100rpm, performing radiation modification by adopting intermediate-energy electron beams while controlling the energy of the intermediate-energy electron beams to be 3MeV and the radiation dose to be 200kGy, and stopping stirring and radiation after 30min to obtain an oil phase;

wherein the mass ratio of the modified essential oil, the xanthan gum and the n-hexadecane is 10:1: 50.

4. Preparing an aqueous phase: uniformly mixing sodium dodecyl sulfate and zwitterionic polyacrylamide, and dissolving the mixture in deionized water to obtain a water phase;

wherein the mass ratio of the sodium dodecyl sulfate to the zwitterionic polyacrylamide to the deionized water is 5-8:2-4: 25-30.

5. Preparing primary essential oil microcapsules: mixing an oil phase and a water phase, adding the mixture into a high-shear reaction kettle, setting the temperature of the high-shear reaction kettle to 30 ℃, setting the shearing speed to 2000rpm, adding polyethylene glycol 6000 and diethylenetriamine into the high-shear reaction kettle after shearing for 30min, setting the temperature of the high-shear reaction kettle to 35 ℃, setting the shearing speed to 2500rpm, stopping high shearing after shearing for 25min, setting the temperature of the high-shear reaction kettle to 50 ℃, standing for 45min to obtain a reactant, performing suction filtration on the reactant, and then washing for 2 times by using deionized water to obtain a primary essential oil microcapsule;

wherein the mass ratio of the oil phase to the water phase to the polyethylene glycol 6000 to the diethylenetriamine is 20:60:2: 1.

6. And (3) post-treatment: placing the primary essential oil microcapsule in a nitrogen atmosphere, controlling the pressure of nitrogen to be 0.15MPa, raising the temperature to 40 ℃, then spraying a post-treatment liquid on the surface of the primary essential oil microcapsule, controlling the mass ratio of the primary essential oil microcapsule to the post-treatment liquid to be 1:1.4, controlling the spraying speed to be 30kg/h, carrying out micro-current treatment while spraying, controlling the current to be 4uA, stopping micro-current after spraying is finished, obtaining the sprayed primary essential oil microcapsule, placing the sprayed primary essential oil microcapsule in an oven for drying, controlling the drying temperature to be 40 ℃, controlling the drying time to be 2h, and obtaining the essential oil microcapsule after drying is finished;

the post-treatment liquid comprises the following components in parts by weight: 2 parts of polyvinyl alcohol 1788, 1 part of glyoxal, 0.2 part of acetic acid, 0.5 part of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, 1 part of glycerol and 18 parts of deionized water.

Example 2

A preparation method of an essential oil microcapsule comprises the following steps:

1. preparing primary essential oil: mixing and uniformly mixing fresh orange peel and fresh oregano according to the mass ratio of 1:2.5, then drying in vacuum, controlling the vacuum degree to be 0.07MPa, the drying temperature to be 55 ℃, crushing after drying for 1.2h, and crushing to 85 meshes to obtain crushed orange peel powder and oregano powder, then loading the crushed orange peel powder and oregano powder into an extraction kettle, adding 3.5 times of absolute ethyl alcohol by mass, then performing supercritical CO2 extraction, controlling the extraction pressure to be 28MPa, the extraction temperature to be 42 ℃, the extraction time to be 2.2h, controlling the flow of CO2 to be 125kg/h, and obtaining an extraction solution after the extraction is finished; then concentrating the extract under reduced pressure, controlling the temperature at 38 deg.C and the pressure at 0.072MPa, and distilling under reduced pressure for 0.8 hr to obtain concentrated solution; and then adding carvacrol and nano boron nitride into the concentrated solution, controlling the mass ratio of carvacrol to nano boron nitride to be 55:7:1.5, then carrying out mechanical oscillation, controlling the rotating speed of the mechanical oscillation to be 205rpm, controlling the time of the mechanical oscillation to be 48min, and obtaining primary essential oil after the mechanical oscillation is finished.

2. Modifying the essential oil: uniformly mixing primary essential oil and nano zeolite powder, adding the mixture into a high-shear reaction kettle, setting the shearing speed of the high-shear reaction kettle to 2200rpm, adding diallyl dimethyl ammonium chloride, polyvinylamine and tea polyphenol after shearing for 35min, controlling the shearing speed to 2800rpm, and continuously shearing for 45min to obtain modified essential oil;

wherein the mass ratio of the primary essential oil, the nano zeolite powder, the diallyl dimethyl ammonium chloride, the polyvinyl amine and the tea polyphenol is 35:22:1.5:1.1: 4;

the effective content of the diallyl dimethyl ammonium chloride is 65%;

the particle size of the nano zeolite powder is 250 nm.

3. Preparing an oil phase: mixing the modified essential oil and xanthan gum, adding the mixture into n-hexadecane, stirring at the speed of 110rpm, performing radiation modification by adopting intermediate-energy electron beams while controlling the energy of the intermediate-energy electron beams to be 3MeV and the radiation dose to be 220kGy, and stopping stirring and radiation after 35min to obtain an oil phase;

wherein the mass ratio of the modified essential oil, the xanthan gum and the n-hexadecane is 11:1.5: 55.

4. Preparing an aqueous phase: uniformly mixing sodium dodecyl sulfate and zwitterionic polyacrylamide, and dissolving the mixture in deionized water to obtain a water phase;

wherein the mass ratio of the sodium dodecyl sulfate to the zwitterionic polyacrylamide to the deionized water is 6:3: 28.

5. Preparing primary essential oil microcapsules: mixing an oil phase and a water phase, adding the mixture into a high-shear reaction kettle, setting the temperature of the high-shear reaction kettle to 32 ℃, setting the shearing speed to 2200rpm, adding polyethylene glycol 6000 and diethylenetriamine into the high-shear reaction kettle after shearing for 35min, then setting the temperature of the high-shear reaction kettle to 38 ℃, setting the shearing speed to 2800rpm, stopping high shearing after shearing for 28min, setting the temperature of the high-shear reaction kettle to 52 ℃, standing for 50min to obtain a reactant, performing suction filtration on the reactant, and then washing for 2 times by using deionized water to obtain a primary essential oil microcapsule;

wherein the mass ratio of the oil phase to the water phase to the polyethylene glycol 6000 to the diethylenetriamine is 21:65:3: 2.

6. And (3) post-treatment: placing the primary essential oil microcapsule in a nitrogen atmosphere, controlling the pressure of nitrogen to be 0.17MPa, raising the temperature to 42 ℃, then spraying a post-treatment liquid on the surface of the primary essential oil microcapsule, controlling the mass ratio of the primary essential oil microcapsule to the post-treatment liquid to be 1:1.5, controlling the spraying speed to be 32kg/h, carrying out micro-current treatment while spraying, controlling the current to be 5uA, stopping micro-current after spraying is finished, obtaining a sprayed primary essential oil microcapsule, placing the sprayed primary essential oil microcapsule in an oven for drying, controlling the drying temperature to be 42 ℃, and drying for 2.2h, thus obtaining the essential oil microcapsule after drying is finished;

the post-treatment liquid comprises the following components in parts by weight: 3 parts of polyvinyl alcohol 1788, 2 parts of glyoxal, 0.3 part of acetic acid, 0.8 part of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, 2 parts of glycerol and 19 parts of deionized water.

Example 3

A preparation method of an essential oil microcapsule comprises the following steps:

1. preparing primary essential oil: mixing and uniformly mixing fresh orange peel and fresh oregano according to a mass ratio of 1:3, then drying in vacuum, controlling a vacuum degree to be 0.08MPa, drying at 60 ℃, drying for 1.5h, then crushing, crushing to 90 meshes to obtain crushed orange peel powder and crushed oregano powder, then loading the crushed orange peel powder and crushed oregano powder into an extraction kettle, adding 3-4 times of absolute ethyl alcohol by mass, then performing supercritical CO2 extraction, controlling an extraction pressure to be 30MPa, an extraction temperature to be 45 ℃, extracting for 2.5h, controlling a flow rate of CO2 to be 130kg/h, and obtaining an extraction liquid after extraction is finished; then carrying out reduced pressure concentration on the extract liquor, controlling the temperature during reduced pressure distillation to be 40 ℃ and the pressure during reduced pressure distillation to be 0.075MPa, and carrying out reduced pressure distillation for 1h to obtain a concentrated solution; and then adding carvacrol and nano boron nitride into the concentrated solution, controlling the mass ratio of carvacrol to nano boron nitride to be 60:8:2, then carrying out mechanical oscillation, controlling the rotating speed of the mechanical oscillation to be 210rpm, controlling the time of the mechanical oscillation to be 50min, and obtaining primary essential oil after the mechanical oscillation is finished.

2. Modifying the essential oil: uniformly mixing primary essential oil and nano zeolite powder, adding the mixture into a high-shear reaction kettle, setting the shearing speed of the high-shear reaction kettle to 2500rpm, adding diallyl dimethyl ammonium chloride, polyvinylamine and tea polyphenol after shearing for 40min, controlling the shearing speed to 3000rpm, and continuously shearing for 50min to obtain modified essential oil;

wherein the mass ratio of the primary essential oil, the nano zeolite powder, the diallyl dimethyl ammonium chloride, the polyvinyl amine and the tea polyphenol is 40:23:2:1.2: 5;

the effective content of the diallyl dimethyl ammonium chloride is 65%;

the particle size of the nano zeolite powder is 300 nm.

3. Preparing an oil phase: mixing the modified essential oil and xanthan gum, adding the mixture into n-hexadecane, stirring at the speed of 120rpm, performing radiation modification by adopting intermediate-energy electron beams while controlling the energy of the intermediate-energy electron beams to be 4MeV and the radiation dose to be 250kGy, and stopping stirring and radiation after 40min to obtain an oil phase;

wherein the mass ratio of the modified essential oil, the xanthan gum and the n-hexadecane is 12:2: 60.

4. Preparing an aqueous phase: uniformly mixing sodium dodecyl sulfate and zwitterionic polyacrylamide, and dissolving the mixture in deionized water to obtain a water phase;

wherein the mass ratio of the sodium dodecyl sulfate to the zwitterionic polyacrylamide to the deionized water is 8:4: 30.

5. Preparing primary essential oil microcapsules: mixing an oil phase and a water phase, adding the mixture into a high-shear reaction kettle, setting the temperature of the high-shear reaction kettle to 35 ℃, setting the shearing speed to 2500rpm, adding polyethylene glycol 6000 and diethylenetriamine into the high-shear reaction kettle after shearing for 40min, setting the temperature of the high-shear reaction kettle to 40 ℃, setting the shearing speed to 3000rpm, stopping high shearing after shearing for 30min, setting the temperature of the high-shear reaction kettle to 55 ℃, standing for 60min to obtain a reactant, performing suction filtration on the reactant, and cleaning for 3 times by using deionized water to obtain a primary essential oil microcapsule;

wherein the mass ratio of the oil phase to the water phase to the polyethylene glycol 6000 to the diethylenetriamine is 22:70:5: 3.

6. And (3) post-treatment: placing the primary essential oil microcapsule in a nitrogen atmosphere, controlling the pressure of nitrogen to be 0.18MPa, raising the temperature to 45 ℃, then spraying a post-treatment liquid on the surface of the primary essential oil microcapsule, controlling the mass ratio of the primary essential oil microcapsule to the post-treatment liquid to be 1:1.6, controlling the spraying speed to be 35kg/h, carrying out micro-current treatment while spraying, controlling the current to be 6uA, stopping micro-current after spraying is finished, obtaining the sprayed primary essential oil microcapsule, placing the sprayed primary essential oil microcapsule in an oven for drying, controlling the drying temperature to be 45 ℃, and the drying time to be 2.5h, thus obtaining the essential oil microcapsule after drying is finished;

the post-treatment liquid comprises the following components in parts by weight: 5 parts of polyvinyl alcohol 1788, 3 parts of glyoxal, 0.4 part of acetic acid, 1 part of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, 3 parts of glycerol and 20 parts of deionized water.

Comparative example 1

The essential oil microcapsule preparation method described in example 1 was used, except that: and (3) omitting the modification of the essential oil in the step (2), namely directly using the primary essential oil obtained in the preparation of the primary essential oil in the step (1) for preparing primary essential oil microcapsules.

Comparative example 2

The essential oil microcapsule preparation method described in example 1 was used, except that: the radiation modification was omitted in step 3 preparation of the oil phase.

Comparative example 3

The essential oil microcapsule preparation method described in example 1 was used, except that: step 6, i.e. the post-processing step, is omitted.

The volatility tests of examples 1 to 3 and comparative examples 1 to 3 were carried out by weighing 50g of the essential oil microcapsules of examples 1 to 3 and comparative examples 1 to 3, respectively, and placing the weighed essential oil microcapsules in 250ml beakers, respectively, and then placing the beakers in an environment with an open mouth at a temperature of 35 ℃ and a humidity of 70%, and after 10 days, weighing the remaining essential oil microcapsules, respectively, and the test results are as follows:

the essential oil microcapsules of examples 1 to 3 and comparative examples 1 to 3 were subjected to a skin irritation test, the test method and the results were as follows:

respectively dissolving the essential oil microcapsules of examples 1-3 and comparative examples 1-3 in deionized water, controlling the mass ratio of the essential oil microcapsules to the deionized water to be 1:3 to obtain an essential oil microcapsule aqueous solution, then selecting 60 Chinese white rabbits with the age of 10-12 months, averagely dividing the Chinese white rabbits into 6 groups, carrying out a skin irritation test, shearing off hairs on two sides of a spinal column of the back of the Chinese white rabbits 24 hours before the test, wherein the hair removal ranges are respectively 3cm multiplied by 3cm, respectively, in the test, respectively taking 0.5mL of the essential oil microcapsule aqueous solution prepared in the examples 1-3 and the comparative examples 1-3, coating the essential oil microcapsule aqueous solution on one side, with the area of 2.5cm multiplied by 2.5cm, of intact skin on the other side as a blank control, cleaning the essential oil microcapsules with water for 4 hours after coating, removing residues, coating the essential oil microcapsules once every day, continuously coating the essential oil microcapsules for 14 days, observing results 24 hours after each coating, and scoring according to disinfection technical specifications of 2019 edition, the scoring results were as follows:

the essential oil microcapsules of examples 1 to 3 and comparative examples 1 to 3 were subjected to a one-time damage skin irritation test, the test method and results were as follows:

respectively dissolving the essential oil microcapsules of examples 1-3 and comparative examples 1-3 in deionized water, controlling the mass ratio of the essential oil microcapsules to the deionized water to be 1:3 to obtain an essential oil microcapsule aqueous solution, then selecting 60 Chinese white rabbits with the age of 10-12 months, averagely dividing the Chinese white rabbits into 6 groups, carrying out a damaged skin irritation test, shearing off hairs on two sides of a back spine of the Chinese white rabbits 24 hours before the test, wherein the hair removal ranges are respectively 3cm multiplied by 3cm, cleaning and disinfecting exposed skin by using 75% alcohol on the hair removal skin with the size of 2.5cm multiplied by 2.5cm on one side during the test, and after the alcohol is volatilized, scratching a 'well' -shaped damaged wound in a skin area by using a sterilizing blade, wherein the damaged skin only reaches epidermis without damaging dermis. Then 0.5mL of the essential oil microcapsule aqueous solution prepared in each of examples 1 to 3 and comparative examples 1 to 3 was applied to the damaged skin on one side having an area of 2.5cm × 2.5cm, covered with a non-irritating plastic film and then fixed with a non-irritating adhesive tape, and the depilated skin on the other side was used as a blank control. The application time is 4h, and after the test is finished, the residual essential oil microcapsule water solution is removed by warm water. And observing local skin reactions for 1h, 24h and 48h after the essential oil microcapsule aqueous solution is removed, and scoring according to the 2019 edition of disinfection technical Specification, wherein the scoring results are as follows:

the essential oil microcapsules of examples 1 to 3 and comparative examples 1 to 3 were subjected to a release rate test of the effective ingredient, and the test method and results were as follows:

the samples of examples 1-3 and comparative examples 1-3 were subjected to a suspension quantitative bacteriostatic test according to the evaluation method of the antibacterial and bacteriostatic effects of WS/T650-2019, Standard of the health of the people's republic of China.

The test temperature was controlled to 20 ℃, then the essential oil microcapsules of examples 1-3 and comparative examples 1-3 were respectively applied to staphylococcus aureus, escherichia coli, candida albicans for 1min, 3min, 6min and 10min, and the corresponding test results were recorded as follows:

all percentages used in the present invention are mass percentages unless otherwise indicated.

Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.