Rosemary essence as well as preparation method and application thereof

Abstract

The invention provides rosemary essence as well as a preparation method and application thereof, and belongs to the technical field of essence. The preparation method comprises the following steps: preparing rosemary essential oil through supercritical fluid extraction and molecular distillation, adsorbing the rosemary essential oil into high-wrinkle nanoparticles, uniformly mixing the high-wrinkle nanoparticles with molten n-octadecane, cooling, embedding the high-wrinkle nanoparticles into polydopamine, depositing dopamine methacrylamide, 2-hydroxy-4-acryloyloxyethoxy benzophenone and 1-allyl benzotriazole cross-linked substances on the surface, washing, and drying, so as to obtain the high-wrinkle nano-composite material. The rosemary essence is prepared. The rosemary essential oil prepared by the invention is high in purity and strong and pure in fragrance, after the essential oil is adsorbed by the high-fold nano-particles with high specific surface area, the essential oil is sealed by the phase-change material n-octadecane, the release rate of liquid essence is controlled through melting and curing of the sealing agent n-octadecane, and the essential oil is embedded by the polydopamine to isolate oxygen and water vapor, so that the fragrance of the rosemary essential oil is improved. And a light stabilizer is further deposited, so that light degradation is efficiently resisted, and good adhesion is achieved on textiles, so that the washing resistance is improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of essence, in particular to a rosemary essence, a preparation method and application thereof. BACKGROUND

[0002] Rosmarinus officinalis L. is a perennial evergreen shrub of the Labiatae family, and its branches and leaves have a fragrant smell and can be added to food as a spice. It is one of the earliest plants used as medicine and is a kind of aromatic plant with a long history. Studies have shown that the chemical components in rosemary mainly include terpenes, flavonoids, and phenylpropanoid compounds. Among them, terpenes are the most complex and most abundant components in rosemary. So far, the terpenes identified in rosemary volatile oil are mainly monoterpenes, sesquiterpenes and their oxidized derivatives, including alpha-pinene, beta-pinene, camphene, 1,8-cineole, camphor, and verbenone. The content of these components varies with the production location. These components have anti-inflammatory, antibacterial, antiviral, and antioxidant pharmacological effects and are widely used in aromatherapy essential oils, medicine and health, daily chemical products, food preservation, and other fields.

[0003] However, rosemary essential oil has the defects of poor water solubility, easy volatility, easy oxidation and polymerization, instability affected by environmental factors, and short duration, which limits the effective use of spices. In the production, transportation, and use of textiles or personal care products, high temperature, oxygen, light, enzymes, and pH may accelerate the release and even trigger chemical reactions, causing deterioration. Therefore, maintaining stability and prolonging fragrance release have become important aspects to consider. SUMMARY

[0004] The purpose of the present application is to provide a rosemary essence, a preparation method and application thereof. The rosemary essence oil is obtained by a safe and effective method, has high purity, strong and pure fragrance, and is adsorbed by high-crease nano particles with high specific surface area after being sealed by phase change material n-octadecane. The release rate of the liquid essence is controlled by the melting and solidification of the sealing agent n-octadecane, and the oxygen and water vapor are isolated by polydopamine embedding. Further, a light stabilizer is deposited to efficiently resist photodegradation, and the rosemary essence has good adhesion on textiles, thereby improving the water washing resistance.

[0005] The technical solution of the present application is as follows:

[0006] The application provides a preparation method of rosemary essence, which comprises the following steps: supercritical fluid extraction, molecular distillation, adsorption on high-pleated nanoparticles, mixing with melted n-octadecane, cooling, embedding in polydopamine, surface deposition of dopamine methacrylamide, 2-hydroxy-4-acryloyloxyethoxybenzophenone and 1-allyl benzotriazole cross-linking material, washing, drying, and obtaining the rosemary essence.

[0007] As a further improvement of the application, the following steps are included:

[0008] S1. Preparation of rosemary essential oil: washing rosemary petals, supercritical fluid extraction, and obtaining rosemary essential oil through molecular distillation of the product;

[0009] S2. Preparation of high-pleated nanoparticles: uniformly dispersing graphite oxide in water to obtain a graphite oxide solution, and preparing high-pleated nanoparticles through spray drying;

[0010] S3. Preparation of a composite: adding rosemary essential oil to high-pleated nanoparticles, and stirring to mix uniformly to obtain a composite;

[0011] S4. Preparation of a core material: heating and melting n-octadecane, adding the composite, stirring to mix uniformly, cooling to room temperature, crushing, sieving, and obtaining the core material;

[0012] S5. Polydopamine embedding: adding the core material to a Tris-HCl solution, adding dopamine hydrochloride, stirring to react at room temperature, centrifuging, washing, and drying to obtain embedded microspheres;

[0013] S6. Surface second layer embedding: adding the embedded microspheres to N,N-dimethylformamide, adding dopamine methacrylamide, 2-hydroxy-4-acryloyloxyethoxybenzophenone and 1-allyl benzotriazole, stirring to mix uniformly, adding an initiator, stirring to react, centrifuging, washing, and drying to obtain rosemary essence.

[0014] As a further improvement of the application, the supercritical fluid extraction in step S1 is carried out under the following conditions: CO2 flow rate is 25-35 L / h, extraction pressure is 30-35 MPa, extraction temperature is 45-55 DEG C, analysis pressure is 10-11 MPa, analysis temperature is 50-60 DEG C, time is 1-2 h, the entraining agent is ethyl acetate, and the addition amount of the entraining agent is 2-3%. The molecular distillation is carried out by collecting the products at 45-50 DEG C, 70-80 DEG C and 90-100 DEG C respectively, the distillation condensation temperature is 3-7 DEG C, the scraper film rotation speed is 150-250 r / min, the feeding flow rate is 2-4 mL / min, and the system vacuum degree is 50-70 Pa.

[0015] As a further improvement of the present application, the concentration of the graphite oxide solution in step S2 is 10-20 mg / mL, and the conditions of the spray drying are as follows: the inlet air temperature is 80-100 DEG C, the outlet air temperature is 30-80 DEG C, and the evaporated water amount is 1500-2500 mL / h.

[0016] As a further improvement of the present application, the mass ratio of the rosemary essential oil to the high-folded nanoparticles in step S3 is 10:12-15.

[0017] As a further improvement of the present application, the mass ratio of the n-octadecane to the complex in step S4 is 3-5:10, and the temperature of the heating melting is 45-55 DEG C.

[0018] As a further improvement of the present application, the pH value of the Tris-HCl solution in step S5 is 8.5-9.5, the mass ratio of the core material to the dopamine hydrochloride is 10:4-7, and the time of the room temperature stirring reaction is 20-24 h.

[0019] As a further improvement of the present application, the mass ratio of the embedding microspheres, dopamine methacrylamide, 2-hydroxy-4-acryloyloxyethoxybenzophenone, 1-allylbenzotriazole, and the initiator in step S6 is 10:1-2:0.3-0.5:0.1-0.3:0.001-0.0015, and the initiator is selected from at least one of azobisisobutyronitrile, azobisisovaleronitrile, ammonium persulfate, sodium persulfate, and potassium persulfate.

[0020] The present application further protects a rosemary essential oil prepared by the above preparation method.

[0021] The present application further protects an application of the above rosemary essential oil in textile and personal care products.

[0022] The present application has the following beneficial effects:

[0023] The present application extracts rosemary by using a supercritical CO2 extraction method, and performs separation and purification by superimposing molecular distillation, the supercritical CO2 extraction effectively avoids the heat sensitivity of the material, avoids the oxidation, volatilization and browning of important components in the rosemary essential oil, and retains the natural efficacy of the plant essence in the extraction process. The molecular distillation separates and purifies in sections, can efficiently separate terpenes in the rosemary volatile oil, such as alpha-pinene, beta-pinene, camphene, 1,8-eucalyptol, camphor, and verbenone, so that the essential oil has more pure aroma, less odor, reduces the loss of important components, and retains the molecular structure of the original active substance without being decomposed.

[0024] The application adopts the graphite oxide dispersion liquid to be broken into small droplets through a nozzle by the action of air pressure and enter a cyclone separator together with heated nitrogen, and in the process of spray drying, the solvent is rapidly evaporated, resulting in the volume shrinkage of the droplets, effectively reducing the stacking of the graphite oxide, avoiding the agglomeration caused by the ordered structure between the layers, obtaining high-crease nanoparticles with high specific surface area, and through the rich pore structure, a large amount of rosemary essential oil can be adsorbed to prepare a composite.

[0025] The application controls the release rate of the liquid essence by the melt solidification of the sealing agent n-octadecane. When the external temperature is lower than the eutectic point of the mixed core material, the solid phase change material in the mixed core material can cover the liquid essence, realizing self-sealing and reducing the release rate of the essence; when the external temperature is higher than the eutectic point of the mixed core material, the liquid essence is rapidly released through the melted phase change material and the wall material with a microporous structure.

[0026] The surface is embedded with polydopamine, which has the characteristics of high specific surface area, strong adhesion and high chemical activity, and after loading the essence and perfume, the high-loading slow-release effect is achieved. In addition, the excellent hydrophilicity, ultraviolet shielding property, biocompatibility and biodegradability can also improve the water solubility of the essence and perfume, avoid adverse reactions with the human body, and protect the skin from ultraviolet damage.

[0027] Dopamine has ultraviolet light absorption performance, and 99% of the photon energy absorbed by dopamine will be quickly converted into heat energy, ensuring that polydopamine can protect humans and animals from ultraviolet damage. Further deposition of dopamine methacrylamide, 2-hydroxy-4-acryloyloxyethoxybenzophenone and 1-allyl benzotriazole cross-linking material layer on the surface of the polydopamine layer can further improve the protection effect of essential oil, efficiently resist photodegradation, and at the same time, since air and water vapor are isolated, the degradation caused by oxygen and water vapor is also well protected. The polydopamine and the multi-group characteristics of dopamine enable it to have good adhesion on textiles, thereby improving the washing resistance.

[0028] The application adopts a safe and effective method to obtain rosemary essential oil with high purity and strong and pure aroma. After adsorbing the essential oil by high-crease nanoparticles with high specific surface area, the essential oil is sealed by the phase change material n-octadecane, the release rate of the liquid essence is controlled by the melt solidification of the sealing agent n-octadecane, and the oxygen and water vapor are isolated by embedding with polydopamine, and further deposition of light stabilizers efficiently resists photodegradation, and has good adhesion on textiles, thereby improving the washing resistance. DETAILED DESCRIPTION

[0029] The technical solutions in the embodiments of the present application will be clearly and completely described below. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the present application.

[0030] The preparation method of the graphite oxide used in the present application is as follows:

[0031] Step one, 10 g of natural graphite powder, 4 g of potassium persulfate, 10 g of phosphorus pentoxide and 25 mL of sulfuric acid are weighed and mixed, and reacted in a 60℃ constant temperature water bath for 3 h, and then moved to a 25℃ constant temperature water bath for 5 h, filtered, and washed to neutral with ionized water, and dried in air to obtain pre-oxidized graphite;

[0032] Step two, 1 g of pre-oxidized graphite and 25 mL of sulfuric acid are weighed and mixed in an ice water bath, and after the pre-oxidized graphite is completely dissolved, 3 g of potassium permanganate is added, and reacted for 2 h, and then moved to a 35℃ constant temperature water bath for 40 min, and finally deionized water is added, and reacted at 35℃ for 1 h, and finally 30% H2O2 is added dropwise until no gas is generated, and the solution turns bright yellow. Hot centrifugal filtration is carried out, and 5% hydrochloric acid and deionized water are used for washing until neutral. After the final precipitate is ultrasonically vibrated, it is dried at 90℃ for 24 h to obtain graphite oxide.

[0033] Example 1

[0034] The present embodiment provides a preparation method of rosemary essence, comprising the following steps:

[0035] S1. Preparation of rosemary essential oil: rosemary petals are washed and extracted by supercritical fluid extraction, and the product is subjected to molecular distillation to obtain rosemary essential oil;

[0036] The supercritical fluid extraction conditions are as follows: CO2 flow rate is 25 L / h, extraction pressure is 30 MPa, extraction temperature is 45℃, resolution pressure is 10 MPa, resolution temperature is 50℃, time is 1 h, entraining agent is ethyl acetate, and the addition amount of the entraining agent is 2%;

[0037] The products at temperatures of 45-50℃, 70-80℃ and 90-100℃ are collected respectively, mixed uniformly to obtain rosemary essential oil, the distillation condensation temperature is 3℃, the scraping membrane rotation speed is 150 r / min, the feeding flow rate is 2 mL / min, and the system vacuum degree is 50 Pa;

[0038] S2. Preparation of high-crease nanoparticles: graphite oxide is uniformly dispersed in water to obtain a graphite oxide solution with a concentration of 10 mg / mL, and high-crease nanoparticles are prepared by spray drying;

[0039] The spray drying conditions are: the inlet air temperature is 80℃, the outlet air temperature is 30℃, and the evaporation water amount is 1500 mL / h;

[0040] S3. Preparation of the composite: 1 g of rosemary essential oil is added to 1.2 g of high-pleated nanoparticles, and the mixture is stirred until uniform, to obtain the composite;

[0041] S4. Preparation of the core material: 3 g of n-octadecane is heated to 45℃, melted, and 10 g of the composite is added. After stirring until uniform, the mixture is cooled to room temperature, crushed, and sieved through a 200-mesh sieve, to obtain the core material;

[0042] S5. Polydopamine embedding: 10 g of the core material is added to 200 mL of Tris-HCl solution with a pH of 8.5, and 4 g of dopamine hydrochloride is added. The mixture is stirred at room temperature for 20 h, centrifuged, washed, and dried, to obtain the embedded microspheres;

[0043] S6. Surface second layer embedding: 10 g of the embedded microspheres is added to 100 mL of N,N-dimethylformamide, and 1 g of dopamine methacrylamide, 0.3 g of 2-hydroxy-4-acryloyloxyethoxybenzophenone, and 0.1 g of 1-allylbenzotriazole are added. The mixture is stirred until uniform, 0.001 g of azobisisobutyronitrile is added, the mixture is heated to 50℃, and stirred for 5 h. The mixture is centrifuged, washed, and dried, to obtain the rosemary essence.

[0044] Example 2

[0045] The present example provides a method for preparing rosemary essence, comprising the following steps:

[0046] S1. Preparation of rosemary essential oil: rosemary petals are washed, subjected to supercritical fluid extraction, and the product is subjected to molecular distillation to obtain rosemary essential oil;

[0047] The supercritical fluid extraction conditions are: CO2 flow rate is 35 L / h, extraction pressure is 35 MPa, extraction temperature is 55℃, resolution pressure is 11 MPa, resolution temperature is 60℃, time is 2 h, and the entraining agent is ethyl acetate, with an addition amount of 3%;

[0048] The molecular distillation collects the products at temperatures of 45-50℃, 70-80℃, and 90-100℃, respectively, and the products are mixed until uniform, to obtain rosemary essential oil. The distillation condensation temperature is 7℃, the scraper membrane rotation speed is 250 r / min, the feed flow rate is 4 mL / min, and the system vacuum degree is 70 Pa;

[0049] S2. Preparation of high-pleated nanoparticles: graphite oxide is uniformly dispersed in water to obtain a graphite oxide solution with a concentration of 20 mg / mL, and the solution is subjected to spray drying to obtain high-pleated nanoparticles;

[0050] The spray drying conditions are: the inlet air temperature is 100℃, the outlet air temperature is 80℃, and the evaporation water amount is 2500mL / h;

[0051] S3. Preparation of the composite: 1g rosemary essential oil is added to 1.5g high-pleated nanoparticles, and the mixture is stirred until uniform to obtain the composite;

[0052] S4. Preparation of the core material: 5g n-octadecane is heated to 55℃ to melt, 10g of the composite is added, and the mixture is stirred until uniform, and then cooled to room temperature, crushed, and sieved through a 200-mesh sieve to obtain the core material;

[0053] S5. Polydopamine embedding: 10g of the core material is added to 200mL of Tris-HCl solution with a pH of 9.5, 7g of dopamine hydrochloride is added, and the mixture is stirred at room temperature for 24h, centrifuged, washed, and dried to obtain the embedded microspheres;

[0054] S6. Surface second layer embedding: 10g of the embedded microspheres is added to 100mL of N,N-dimethylformamide, 2g of dopamine methacrylamide, 0.5g of 2-hydroxy-4-acryloyloxyethoxybenzophenone, and 0.3g of 1-allylbenzotriazole are added, the mixture is stirred until uniform, 0.0015g of azobisisovaleronitrile is added, the mixture is heated to 50℃, and the mixture is stirred for 7h, centrifuged, washed, and dried to obtain the rosemary essence.

[0055] Example 3

[0056] The present example provides a method for preparing rosemary essence, comprising the following steps:

[0057] S1. Preparation of rosemary essential oil: rosemary petals are washed, subjected to supercritical fluid extraction, and the product is subjected to molecular distillation to obtain rosemary essential oil;

[0058] The supercritical fluid extraction conditions are: CO2 flow rate is 30L / h, extraction pressure is 32MPa, extraction temperature is 50℃, resolution pressure is 10.5MPa, resolution temperature is 55℃, time is 1.5h, entraining agent is ethyl acetate, and the addition amount of the entraining agent is 2.5%;

[0059] The molecular distillation collects the products at temperatures of 45-50℃, 70-80℃, and 90-100℃, respectively, mixes them uniformly to obtain rosemary essential oil, the distillation condensation temperature is 5℃, the scraping membrane rotation speed is 200r / min, the feeding flow rate is 3mL / min, and the system vacuum degree is 60Pa;

[0060] S2. Preparation of high-pleated nanoparticles: graphite oxide is uniformly dispersed in water to obtain a graphite oxide solution with a concentration of 15mg / mL, and the solution is subjected to spray drying to obtain high-pleated nanoparticles;

[0061] The spray drying conditions are as follows: the inlet temperature is 90℃, the outlet temperature is 50℃, and the evaporation water amount is 2000 mL / h;

[0062] S3. Preparation of the composite: 1 g of rosemary essential oil is added to 1.3 g of high-pleated nanoparticles, and the mixture is stirred until uniform, thereby preparing a composite;

[0063] S4. Preparation of the core material: 4 g of n-octadecane is heated to 50℃, melted, and 10 g of the composite is added. After the mixture is stirred until uniform, it is cooled to room temperature, crushed, and sieved through a 200-mesh sieve, thereby preparing a core material;

[0064] S5. Polydopamine embedding: 10 g of the core material is added to 200 mL of a Tris-HCl solution with a pH of 9, and 5 g of dopamine hydrochloride is added. The mixture is stirred at room temperature for 22 h, centrifuged, washed, and dried, thereby preparing embedded microspheres;

[0065] S6. Surface second layer embedding: 10 g of the embedded microspheres is added to 100 mL of N,N-dimethylformamide, and 1.5 g of dopamine methacrylamide, 0.4 g of 2-hydroxy-4-acryloyloxyethoxybenzophenone, and 0.2 g of 1-allylbenzotriazole are added. The mixture is stirred until uniform, 0.0012 g of azobisisobutyronitrile is added, the mixture is heated to 50℃, and stirred for 6 h. The mixture is centrifuged, washed, and dried, thereby preparing rosemary essence.

[0066] Comparative Example 1

[0067] Compared with Example 3, the difference is that no molecular distillation is performed in step S1.

[0068] The following steps are included:

[0069] S1. Preparation of rosemary essential oil: rosemary petals are washed and subjected to supercritical fluid extraction, thereby preparing rosemary essential oil;

[0070] The supercritical fluid extraction conditions are as follows: the CO2 flow rate is 30 L / h, the extraction pressure is 32 MPa, the extraction temperature is 50℃, the resolution pressure is 10.5 MPa, the resolution temperature is 55℃, the time is 1.5 h, the entraining agent is ethyl acetate, and the addition amount of the entraining agent is 2.5%;

[0071] S2. Preparation of high-pleated nanoparticles: graphite oxide is uniformly dispersed in water to obtain a graphite oxide solution with a concentration of 15 mg / mL, and the solution is subjected to spray drying, thereby preparing high-pleated nanoparticles;

[0072] The spray drying conditions are as follows: the inlet temperature is 90℃, the outlet temperature is 50℃, and the evaporation water amount is 2000 mL / h;

[0073] S3. Preparation of the composite: 1 g of rosemary essential oil was added to 1.3 g of high corrugated nanoparticles, and stirred to mix uniformly to obtain a composite;

[0074] S4. Preparation of the core material: 4 g of n-octadecane was heated to 50 °C to melt, 10 g of the composite was added, and stirred to mix uniformly, and then cooled to room temperature, crushed, and sieved through a 200 mesh sieve to obtain a core material;

[0075] S5. Polydopamine embedding: 10 g of the core material was added to 200 mL of Tris-HCl solution with a pH of 9, 5 g of dopamine hydrochloride was added, and stirred to react at room temperature for 22 h, centrifuged, washed, and dried to obtain embedded microspheres;

[0076] S6. Surface second layer embedding: 10 g of the embedded microspheres was added to 100 mL of N,N-dimethylformamide, 1.5 g of dopamine methacrylamide, 0.4 g of 2-hydroxy-4-acryloyloxyethoxybenzophenone, and 0.2 g of 1-allylbenzotriazole were added, stirred to mix uniformly, 0.0012 g of azobisisobutyronitrile was added, heated to 50 °C, and stirred to react for 6 h, centrifuged, washed, and dried to obtain rosemary essence.

[0077] Comparative Example 2

[0078] Compared with Example 3, the difference is that steps S2 and S3 in Example 3 are not performed.

[0079] Comprising the following steps:

[0080] S1. Preparation of rosemary essential oil: rosemary petals were washed, subjected to supercritical fluid extraction, and the product was subjected to molecular distillation to obtain rosemary essential oil;

[0081] The supercritical fluid extraction conditions were a CO2 flow rate of 30 L / h, an extraction pressure of 32 MPa, an extraction temperature of 50 °C, an analysis pressure of 10.5 MPa, an analysis temperature of 55 °C, a time of 1.5 h, and an entrainer of ethyl acetate with an addition amount of 2.5%;

[0082] The molecular distillation collected products at temperatures of 45-50 °C, 70-80 °C, and 90-100 °C, respectively, mixed uniformly to obtain rosemary essential oil, the distillation condensation temperature was 5 °C, the wiped film rotation speed was 200 r / min, the feed flow rate was 3 mL / min, and the system vacuum degree was 60 Pa;

[0083] S2. Preparation of the core material: 4 g of n-octadecane was heated to 50 °C to melt, 10 g of rosemary essential oil was added, and stirred to mix uniformly, and then cooled to room temperature, crushed, and sieved through a 200 mesh sieve to obtain a core material;

[0084] S3. Polydopamine embedding: 10 g of core material was added into 200 mL of Tris-HCl solution with pH value of 9, 5 g of dopamine hydrochloride was added, and the reaction was stirred at room temperature for 22 h, centrifuged, washed, and dried to obtain the embedded microspheres;

[0085] S4. Surface second layer embedding: 10 g of embedded microspheres was added into 100 mL of N,N-dimethylformamide, 1.5 g of dopamine methacrylamide, 0.4 g of 2-hydroxy-4-acryloyloxyethoxybenzophenone, and 0.2 g of 1-allylbenzotriazole were added, and the mixture was stirred and mixed uniformly, 0.0012 g of azobisisobutyronitrile was added, heated to 50 °C, and stirred for 6 h, centrifuged, washed, and dried to obtain rosemary essence.

[0086] Comparative Example 3

[0087] The difference compared with Example 3 is that step S4 in Example 3 is not performed.

[0088] Comprising the following steps:

[0089] S1. Preparation of rosemary essential oil: rosemary petals were washed, subjected to supercritical fluid extraction, and the product was subjected to molecular distillation to obtain rosemary essential oil;

[0090] The supercritical fluid extraction conditions were as follows: CO2 flow rate was 30 L / h, extraction pressure was 32 MPa, extraction temperature was 50 °C, resolution pressure was 10.5 MPa, resolution temperature was 55 °C, time was 1.5 h, entraining agent was ethyl acetate, and the addition amount of the entraining agent was 2.5%;

[0091] The products collected at temperatures of 45-50 °C, 70-80 °C, and 90-100 °C were mixed uniformly to obtain rosemary essential oil, the distillation condensation temperature was 5 °C, the scraped membrane rotation speed was 200 r / min, the feeding flow rate was 3 mL / min, and the system vacuum degree was 60 Pa;

[0092] S2. Preparation of high-fold nanometer particles: graphite oxide was uniformly dispersed in water to obtain a graphite oxide solution with a concentration of 15 mg / mL, and the high-fold nanometer particles were prepared by spray drying;

[0093] The spray drying conditions were as follows: the inlet air temperature was 90 °C, the outlet air temperature was 50 °C, and the evaporation water amount was 2000 mL / h;

[0094] S3. Preparation of the composite: 1 g of rosemary essential oil was added into 1.3 g of high-fold nanometer particles, and the mixture was stirred and mixed uniformly to obtain the composite;

[0095] S4. Polydopamine embedding: 10 g of the composite was added into 200 mL of Tris-HCl solution with pH value of 9, 5 g of dopamine hydrochloride was added, the reaction was stirred at room temperature for 22 h, centrifuged, washed, and dried to obtain the embedded microspheres;

[0096] S5. Surface second layer embedding: 10 g of the embedded microspheres was added into 100 mL of N,N-dimethylformamide, 1.5 g of dopamine methacrylamide, 0.4 g of 2-hydroxy-4-acryloyloxyethoxybenzophenone, and 0.2 g of 1-allylbenzotriazole were added, the mixture was stirred and mixed uniformly, 0.0012 g of azobisisobutyronitrile was added, the reaction was stirred at 50 °C for 6 h, centrifuged, washed, and dried to obtain rosemary essence.

[0097] Comparative Example 4

[0098] Compared with Example 3, the difference is that step S5 in Example 3 is not performed.

[0099] Comprising the following steps:

[0100] S1. Preparation of rosemary essential oil: rosemary petals were washed, subjected to supercritical fluid extraction, and the product was subjected to molecular distillation to obtain rosemary essential oil;

[0101] The supercritical fluid extraction conditions were as follows: CO2 flow rate was 30 L / h, extraction pressure was 32 MPa, extraction temperature was 50 °C, resolution pressure was 10.5 MPa, resolution temperature was 55 °C, time was 1.5 h, and the entraining agent was ethyl acetate, and the addition amount of the entraining agent was 2.5%;

[0102] The products collected at temperatures of 45-50 °C, 70-80 °C, and 90-100 °C were mixed uniformly to obtain rosemary essential oil, the distillation condensation temperature was 5 °C, the scraping membrane rotation speed was 200 r / min, the feeding flow rate was 3 mL / min, and the system vacuum degree was 60 Pa;

[0103] S2. Preparation of high-fold nanometer particles: graphite oxide was uniformly dispersed in water to obtain a graphite oxide solution with a concentration of 15 mg / mL, and the high-fold nanometer particles were prepared by spray drying;

[0104] The spray drying conditions were as follows: the inlet air temperature was 90 °C, the outlet air temperature was 50 °C, and the evaporation water amount was 2000 mL / h;

[0105] S3. Preparation of the composite: 1 g of rosemary essential oil was added into 1.3 g of high-fold nanometer particles, and the mixture was stirred and mixed uniformly to obtain the composite;

[0106] S4. Preparation of the core material: 4 g of n-octadecane was heated to 50 °C, melted, 10 g of the composite was added, stirred and mixed uniformly, cooled to room temperature, pulverized, and sieved through a 200 mesh sieve to obtain the core material;

[0107] S5. Embedding: 10 g of the core material was added to 100 mL of water, 1.5 g of dopamine methacrylamide was added, stirred and mixed uniformly, 100 mL of a N,N-dimethylformamide solution containing 0.4 g of 2-hydroxy-4-acryloyloxyethoxybenzophenone and 0.2 g of 1-allylbenzotriazole was added, stirred and mixed uniformly, 0.0012 g of azobisisobutyronitrile was added, heated to 50 °C, stirred and reacted for 6 h, centrifuged, washed, and dried to obtain rosemary fragrance.

[0108] Comparative Example 5

[0109] The difference compared with Example 3 is that step S6 in Example 3 is not performed.

[0110] Comprising the following steps:

[0111] S1. Preparation of rosemary essential oil: rosemary petals were washed, subjected to supercritical fluid extraction, and the product was subjected to molecular distillation to obtain rosemary essential oil;

[0112] The supercritical fluid extraction conditions were as follows: CO2 flow rate was 30 L / h, extraction pressure was 32 MPa, extraction temperature was 50 °C, resolution pressure was 10.5 MPa, resolution temperature was 55 °C, time was 1.5 h, and the entraining agent was ethyl acetate, and the addition amount of the entraining agent was 2.5%;

[0113] The products collected at temperatures of 45-50 °C, 70-80 °C, and 90-100 °C were mixed uniformly to obtain rosemary essential oil, the distillation condensation temperature was 5 °C, the scraped membrane rotation speed was 200 r / min, the feeding flow rate was 3 mL / min, and the system vacuum degree was 60 Pa;

[0114] S2. Preparation of high-fold nanometer particles: graphite oxide was uniformly dispersed in water to obtain a graphite oxide solution with a concentration of 15 mg / mL, and the high-fold nanometer particles were prepared by spray drying;

[0115] The spray drying conditions were as follows: the inlet air temperature was 90 °C, the outlet air temperature was 50 °C, and the evaporation water amount was 2000 mL / h;

[0116] S3. Preparation of the composite: 1 g of rosemary essential oil was added to 1.3 g of high-fold nanometer particles, stirred and mixed uniformly to obtain the composite;

[0117] S4. Preparation of the core material: 4 g of n-octadecane was heated to 50°C, melted, 10 g of the complex was added, and after stirring and mixing uniformly, it was cooled to room temperature, pulverized, and sieved through a 200-mesh sieve to obtain the core material;

[0118] S5. Polydopamine embedding: 10 g of the core material was added to 200 mL of a Tris-HCl solution with a pH of 9, 5 g of dopamine hydrochloride was added, and the reaction was stirred at room temperature for 22 h, centrifuged, washed, and dried to obtain the embedded microspheres, i.e., rosemary essence.

[0119] Test Example 1: Release performance of the essence under different conditions

[0120] The rosemary essence prepared in Examples 1-3 and Comparative Examples 1-5 was frozen in a -20°C refrigerator for 4 hours, then immediately placed in a freeze dryer for 24 hours, and then taken out to obtain a powder.

[0121] (1) Influence of different humidity environments on the release of the microcapsules

[0122] 0.01 g of the powder was weighed as a sample, and the relative humidity (RH) of the sealed container was adjusted to 32%, 58%, and 85% using saturated magnesium chloride (MgCl2), sodium bromide (NaBr), and potassium chloride (KCl) solutions. After being stored in the dark at 25°C for 5 days, the sample was finally taken out, freeze-dried, and the weight loss rate of the essence was tested.

[0123] (2) Influence of different temperature environments on the release of the microcapsules

[0124] 0.01 g of the powder was weighed as a sample, and the temperature of the incubator was set to 4°C, 25°C, and 50°C (low temperature, room temperature, and high temperature), and the relative humidity (RH) was set to 32%. After being stored in the dark for 5 days, the sample was finally taken out, freeze-dried, and the weight loss rate of the essence was tested.

[0125] The results are shown in Table 1.

[0126] Table 1

[0127]

[0128] As shown in the above table, the rosemary essence prepared by the present application has good moisture resistance, and the release rate is not high under low temperature and room temperature conditions, but there is obvious release under high temperature conditions.

[0129] Test Example 2

[0130] The rosemary essence prepared in Examples 1-3 and Comparative Example 1 was evaluated by 30 professional evaluators, and the color, aroma, aftertaste, odor, and irritation of the essence were evaluated under the same conditions, and the evaluation results are shown in Table 2.

[0131] Table 2

[0132] The evaluation results are shown in Table 3.

[0133] Table 3

[0134]

[0135] Note: Among the color, aroma, aftertaste, the higher the score, the better the effect; among the odor and irritation, the higher the score, the less the irritation and odor.

[0136] From the above table, it can be seen that the rosemary fragrance prepared by the application has good sensory score, among which the aroma and aftertaste are good, and the odor and irritation are small, and it is more mellow and pure.

[0137] Test Example 3

[0138] The cotton fabric was padded (pick-up rate 65%) in the rosemary fragrance emulsion (fragrance concentration 20wt%, sodium dodecyl sulfate 3wt%) prepared in Examples 1-3 and Comparative Examples 1-5, and dried to prepare a fragrant cotton cloth. The weight was weighed as m0. It was washed by a color fastness tester, and the water washing test method referred to AATCC61-2003 "Home and Commercial Washing Fastness - Accelerated Method". After washing for 30 times, it was dried and weighed as m1. The weight loss rate (%) was calculated. The results are shown in Table 4.

[0139] Table 4

[0140]

[0141] From the above table, it can be seen that the rosemary fragrance prepared by the application has good sensory score, among which the aroma and aftertaste are good, and the odor and irritation are small, and it is more mellow and pure.

[0142] The prepared fragrant cotton cloth was naturally placed to test the fragrance retention duration, the environmental temperature was 25℃, the humidity was 32%, and ultraviolet light was irradiated. The evaluation standard is shown in Table 5.

[0143] Table 5

[0144]

[0145] The results are shown in Table 6.

[0146] Table 6

[0147]

[0148] From the above table, it can be seen that the rosemary fragrance prepared by the application has good sensory score, among which the aroma and aftertaste are good, and the odor and irritation are small, and it is more mellow and pure.

[0149] The above merely provides the preferred embodiment of the present application, and is not used to limit the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A method for preparing a rosemary aroma, characterized by, The rosemary essential oil prepared by supercritical fluid extraction and molecular distillation is adsorbed in high-pleated nanoparticles, mixed with molten n-octadecane uniformly, cooled, embedded in polydopamine, and the surface is deposited with dopamine methacrylamide, 2-hydroxy-4-acryloyloxyethoxybenzophenone and 1-allyl benzotriazole cross-linking material, washed, dried, and rosemary essence is prepared.

2. The production method according to claim 1, characterized by, The method comprises the following steps: S1. Preparation of rosemary essential oil: rosemary petals are washed, and then subjected to supercritical fluid extraction, and the product is subjected to molecular distillation to prepare rosemary essential oil; S2. Preparation of high-pleated nanoparticles: graphite oxide is uniformly dispersed in water to obtain a graphite oxide solution, and then subjected to spray drying to prepare high-pleated nanoparticles; S3. Preparation of a composite: rosemary essential oil is added to high-pleated nanoparticles, and then stirred and mixed uniformly to prepare a composite; S4. Preparation of a core material: n-octadecane is heated and melted, and then the composite is added and stirred and mixed uniformly, and then cooled to room temperature, crushed, sieved, and a core material is prepared; S5. Polydopamine embedding: the core material is added to a Tris-HCl solution, and then dopamine hydrochloride is added, and then stirred and reacted at room temperature, centrifuged, washed, and dried to prepare embedded microspheres; S6. Surface second layer embedding: the embedded microspheres are added to N,N-dimethylformamide, and then dopamine methacrylamide, 2-hydroxy-4-acryloyloxyethoxybenzophenone and 1-allyl benzotriazole are added, and then stirred and mixed uniformly, and then an initiator is added, and then stirred and reacted, centrifuged, washed, and dried to prepare rosemary essence.

3. The preparation method according to claim 2, characterized in that, In step S1, the supercritical fluid extraction is performed under the following conditions: CO2 flow rate is 25-35 L / h, extraction pressure is 30-35 MPa, extraction temperature is 45-55 ℃, desorption pressure is 10-11 MPa, desorption temperature is 50-60 ℃, time is 1-2 h, and the entraining agent is ethyl acetate, and the addition amount of the entraining agent is 2-3%. In the molecular distillation, the products collected at 45-50 ℃, 70-80 ℃ and 90-100 ℃, respectively, the distillation condensation temperature is 3-7 ℃, the scraper film rotation speed is 150-250 r / min, the feeding flow rate is 2-4 mL / min, and the system vacuum degree is 50-70 Pa.

4. The production method according to claim 2, characterized by, In step S2, the concentration of the graphite oxide solution is 10-20 mg / mL, and the spray drying is performed under the following conditions: inlet air temperature is 80-100 ℃, outlet air temperature is 30-80 ℃, and evaporation water amount is 1500-2500 mL / h.

5. The preparation method according to claim 2, characterized in that, In step S3, the mass ratio of the rosemary essential oil to the high-pleated nanoparticles is 10: (12-15).

6. The preparation method according to claim 2, characterized in that, In step S4, the mass ratio of the n-octadecane to the composite is (3-5):10, and the heating and melting temperature is 45-55 ℃.

7. The preparation method according to claim 2, characterized in that, In step S5, the pH value of the Tris-HCl solution is 8.5-9.5, the mass ratio of the core material to dopamine hydrochloride is 10: (4-7), and the stirring and reaction time at room temperature is 20-24 h.

8. The preparation method according to claim 2, characterized in that, The mass ratio of the embedding microspheres, dopamine methacrylamide, 2-hydroxy-4-acryloyloxyethoxybenzophenone, 1-allyl benzotriazole, and the initiator selected from at least one of azobisisobutyronitrile, azobisisovaleronitrile, ammonium persulfate, sodium persulfate, and potassium persulfate in step S6 is 10:(1-2):(0.3-0.5):(0.1-0.3):(0.001-0.0015).

9. A rosemary fragrance prepared according to the method of any one of claims 1 to 8.

10. Use of a rosemary fragrance according to claim 9 in textile and personal care products.

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