Preparation method and application of long-lasting fragrance microcapsules

Abstract

A preparation method and application of a long-lasting flavor microcapsule, belonging to the field of chemical flavor technology, the inner layer of the flavor microcapsule is a core material, which is a coated flavor nanoliposome, and the surface of the core material is coated with an interlayer agent, a coating agent I, an interlayer agent and a coating agent II in sequence, wherein the coating agent I and the coating agent II contain flavor components with different smells. The method of the present invention is designed to use peach fat to load the inner layer flavor to prepare nanoliposomes, and then the polyvinyl pyrrolidone is mixed and coated to obtain a core material with good stability and good sustained release effect. The core material is then subjected to an interlayer agent and a coating agent containing flavors with different smells, and a multi-layer coating is performed by sulfurization spray to obtain a microcapsule with good packaging quality, distinct smells released by each layer, no mixed taste, different smells of each layer, which can improve the diversity of smells, and will not cause fragrance olfactory fatigue when used for a long time. It has good safety and is suitable for all kinds of people. The flavor microcapsule is used for washing clothes, and the wardrobe is stored for 150 days and still retains fragrance.

Description

Technical Field

[0001] The invention belongs to the technical field of chemical fragrances, and in particular relates to a preparation method and application of long-acting fragrance microcapsules. Background Art

[0002] In people's daily life, we cannot do without fragrance substances. Food, cosmetics, toiletries, clothing, bedding, humidifiers, perfumes, sachets, air fresheners, indoor aromatherapy, load-bearing aromatherapy and other products are all added with fragrance substances, which can cover up bad odors, emit fragrance, refresh the mind, cheer up the mood and improve the quality of life. At present, the development of various spices has basically met people's demand for fragrance categories. However, fragrance substances evaporate over time, and the persistence of the fragrance is poor. Therefore, microcapsule technology is used in this field to improve the persistence. Microcapsule technology mainly attaches sustained-release materials to the surface of the core material. The core material contains fragrance ingredients, which can improve photosensitivity or heat sensitivity to improve the stability and sustained-release performance of the fragrance.

[0003] However, the current flavor microcapsules still have deficiencies in terms of encapsulation rate, fragrance retention time and controlled release degree, resulting in uneven fragrance distribution and a short fragrance retention time. The preparation technology of flavor microcapsules needs to be improved. In addition, the current flavor microcapsules have a single fragrance and no diversity. Long-term use of one fragrance can easily cause people to have olfactory fatigue. Summary of the invention

[0004] The existing flavor microcapsules have poor packaging quality, the fragrance emission time and uniformity still need to be improved, and the fragrance is single, and long-term use can easily cause people to have fragrance and olfactory fatigue. The present invention provides a preparation method and application of long-lasting flavor microcapsules, which uses peach fat to load the inner layer of flavor to prepare nanoliposomes, and then uses polyvinyl pyrrolidone mixed film to obtain a core substance with good stability and good sustained release effect. The core substance is then subjected to interlayer agents and coating agents containing flavors of different odors, and subjected to vulcanization spray multi-layer coating to obtain microcapsules with good packaging quality, distinct odors released by each layer, and no mixed tastes. The odors of each layer are different, which can improve the diversity of odors, and long-term use will not cause fragrance and olfactory fatigue. It has good safety and is suitable for all kinds of people. The specific technical scheme is as follows:

[0005] A method for preparing long-lasting fragrance microcapsules comprises the following steps:

[0006] S1, Preparation of core material:

[0007] S1.1: Dissolve peach fat in ethanol solution according to the mass ratio of ethanol water solution: flavor I: peach fat = (80-90): (0.5-8): (0.5-3), then add flavor I, mix and dissolve evenly to obtain a fragrance liquid;

[0008] S1.2: according to the mass ratio of anhydrous ethanol:soybean lecithin:cholesterol = (40-60):(4-8):(1-2), the soybean lecithin, cholesterol and anhydrous ethanol are uniformly mixed, and then the anhydrous ethanol is removed by negative pressure evaporation to obtain a wall-hanging film;

[0009] S1.3: The fragrance liquid and the film are ultrasonically mixed to form an emulsion in a mass ratio of fragrance liquid: film = 100: (3-6), and then the emulsion is repeatedly inserted and pushed out using a 0.5μm-0.8μm filter membrane syringe to prepare a nanoemulsion; then the nanoemulsion and polyvinyl pyrrolidone are uniformly mixed in a mass ratio of nanoemulsion: polyvinyl pyrrolidone = 100: (0.5-1), and spray-dried to obtain a core mass;

[0010] S2, preparation of flavor microcapsules:

[0011] S2.1, according to the mass ratio of core material: interlayer agent = 100: (3-10), the core material and the interlayer agent are sprayed on the surface of the core material by fluidized spraying, and then freeze-dried to form microparticles A;

[0012] S2.2, according to the mass ratio of microparticle A: coating agent I = 100: (5-15), microparticle A and coating agent I are sprayed on the surface of microparticle A by fluidized spraying method, and then freeze-dried to form microparticle B;

[0013] S2.3, according to the mass ratio of microparticles B: interlayer agent = 100: (3-10), the microparticles B and the interlayer agent are sprayed on the surface of the microparticles B by fluidized spraying, and then freeze-dried to form microparticles C;

[0014] S2.4, according to the mass ratio of microparticles C: coating agent II = 100: (5-15), the microparticles C and coating agent II are fluidized sprayed, the coating agent II is sprayed on the surface of the microparticles C, and after freeze-drying, the flavor microcapsules are formed.

[0015] In S1.1 of the above preparation method, the volume concentration of the ethanol aqueous solution is 40% to 50%.

[0016] In S1.2 of the above preparation method, the evaporation temperature is 60°C to 65°C.

[0017] In S1.3 of the above preparation method, the frequency of the ultrasound is 40KHz to 45KHz.

[0018] In S2.1 of the above preparation method, the interlayer agent is a methyl cellulose aqueous solution with a mass concentration of 5% to 10%.

[0019] In S2.3 of the above preparation method, the interlayer agent is a methyl cellulose aqueous solution with a mass concentration of 5% to 10%.

[0020] In S2.2 of the above preparation method, the components of the coating agent I are composed of 80 to 90 parts of ethanol aqueous solution, 2 to 5 parts of pregelatinized starch, 0.5 to 1 part of methyl cellulose and 1 to 5 parts of flavor II in mass fractions; the volume concentration of the ethanol aqueous solution is 40% to 50%.

[0021] In S2.4 of the above preparation method, the components of the coating agent II are composed of 80 to 90 parts of ethanol aqueous solution, 2 to 5 parts of pregelatinized starch, 0.5 to 1 part of methyl cellulose and 1 to 5 parts of flavor III in mass fraction; the volume concentration of the ethanol aqueous solution is 40% to 50%.

[0022] In S2 of the above preparation method, the parameters of the fluidized spray are: interlayer agent inlet temperature 10°C to 20°C, spray speed 0.2L / min to 0.5L / min, atomization pressure 0.2MPa to 0.4MPa, and spray drying temperature 50°C to 60°C.

[0023] In the above preparation method, the flavor I, flavor II and flavor III are all water-soluble flavors, and the flavor I, flavor II and flavor III are flavors with different smells.

[0024] The above-mentioned application of the long-lasting fragrance microcapsule is that the fragrance microcapsule is used by a wet method, and the fragrance microcapsule and an emulsifier are configured into a water-soluble suspension for fragrance application.

[0025] Compared with the prior art, the preparation method and application of the long-lasting fragrance microcapsule of the present invention have the following beneficial effects:

[0026] 1. The method of the present invention designs three flavors to prepare composite flavor microcapsules, and various scents can be well released in layers, which can improve the diversity of the fragrance, change the scent, and not easily cause people to have fragrance olfactory fatigue. Among them, the interlayer agent coating is designed to have a certain fragrance component barrier effect, so that adjacent fragrance components are not easy to penetrate each other in the microcapsule, so that two adjacent fragrance components are not easy to mix when released, and the clarity of different fragrance switching is improved.

[0027] Second, due to the barrier effect of the interlayer, the degree of overall fragrance release at one time is reduced, that is, the initial fragrance concentration becomes lighter, but the overall fragrance release concentration is more balanced, and the fragrance lasting time is extended. It is a light and lasting release that will not be too strong to irritate the sense of smell.

[0028] 3. The method of the present invention is designed to load the inner layer flavor (flavor I) with peach fat to prepare nanoliposomes, and then coat the mixture with polyvinyl pyrrolidone to make the matrix nanoliposomes more stable, improve the storage stability, and prolong the sustained release time of the matrix.

[0029] Fourth, the present invention adopts a fluidized spray method for encapsulation, and pregelatinized starch and methyl cellulose are added to the encapsulant (coating agent). On the one hand, it can achieve good encapsulation of the inner layer and play a sustained release role. On the other hand, flavors are added to the encapsulant to release the flavor, making the flavor release continuous.

[0030] 5. According to the composition and properties of the interlayer agent and the coating agent, the invention designs the encapsulation ratio and fluidized spray parameters: inlet temperature 10℃~20℃, spray speed 0.2L / min~0.5L / min, atomization pressure 0.2MPa~0.4MPa, spray drying temperature 50℃~60℃; it can well achieve uniform and dense encapsulation effect, long sustained release time, and the odors of each layer are not easy to mix and confuse.

[0031] 6. During the washing process of clothes in the washing machine, the clothes are filled with fragrance microcapsules. The washed clothes are stored in a closed wardrobe for 150 days. When you take out the clothes and smell them, the clothes still retain the fragrance and have a particularly long-lasting fragrance retention performance.

[0032] 7. The essence microcapsule ingredients of the present invention are highly safe, without adding any harmful substances, and are suitable for use by infants and pregnant women. DETAILED DESCRIPTION

[0033] The present invention is further described below in conjunction with specific implementation cases, but the present invention is not limited to these embodiments.

[0034] Example 1

[0035] A method for preparing long-lasting fragrance microcapsules comprises the following steps:

[0036] S1, Preparation of core material:

[0037] S1.1: Dissolve peach fat in 40% ethanol solution by mass ratio of ethanol water solution: flavor I: peach fat = 85:5:2, then add flavor I, mix and dissolve evenly to obtain a fragrance liquid;

[0038] S1.2: Soybean lecithin, cholesterol and anhydrous ethanol are uniformly mixed in a mass ratio of anhydrous ethanol:soybean lecithin:cholesterol=50:6:1.5, and then the anhydrous ethanol is evaporated at 60°C under negative pressure to obtain a wall-hanging film;

[0039] S1.3: The fragrance liquid and the film are mixed by 40KHz ultrasound at a mass ratio of 100:5 to form an emulsion, and then the emulsion is repeatedly inserted and pushed out using a 0.6μm filter syringe to prepare a nanoemulsion; then the nanoemulsion and polyvinyl pyrrolidone are mixed evenly at a mass ratio of 100:0.8, and spray-dried to obtain a core mass;

[0040] S2, preparation of flavor microcapsules:

[0041] S2.1, according to the mass ratio of core material: interlayer agent = 100:5, the core material and the interlayer agent are fluidized sprayed, the interlayer agent is sprayed on the surface of the core material, and then freeze-dried to form microparticles A;

[0042] The interlayer agent is a methylcellulose aqueous solution with a mass concentration of 8%. The parameters of the fluidized spray are: the interlayer agent inlet temperature is 15°C, the spray speed is 0.3L / min, the atomization pressure is 0.3MPa, and the spray drying temperature is 55°C.

[0043] S2.2, according to the mass ratio of microparticle A: coating agent I = 100:10, microparticle A and coating agent I are sprayed on the surface of microparticle A by fluidized spraying method, and then freeze-dried to form microparticle B;

[0044] The mass fraction of the coating agent I is 85 parts of ethanol aqueous solution, 3 parts of pregelatinized starch, 0.8 parts of methyl cellulose and 3 parts of flavor II; the volume concentration of ethanol aqueous solution is 40%; the parameters of fluidized spray are: interlayer agent inlet temperature 15°C, spray speed 0.3L / min, atomization pressure 0.3MPa, spray drying temperature 55°C;

[0045] S2.3, according to the mass ratio of microparticles B: interlayer agent = 100:6, the microparticles B and the interlayer agent are sprayed on the surface of the microparticles B by fluidized spraying, and then freeze-dried to form microparticles C;

[0046] The interlayer agent is a methylcellulose aqueous solution with a mass concentration of 8%. The parameters of the fluidized spray are: the interlayer agent inlet temperature is 15°C, the spray speed is 0.3L / min, the atomization pressure is 0.3MPa, and the spray drying temperature is 55°C.

[0047] S2.4, according to the mass ratio of microparticle C: coating agent II = 100:10, the microparticle C and the coating agent II are sprayed on the surface of the microparticle C by fluidized spraying, and the coating agent II is freeze-dried to form flavor microcapsules;

[0048] Among them, the mass fractions of the components of coating agent II are 85 parts of ethanol aqueous solution, 3 parts of pregelatinized starch, 0.8 parts of methyl cellulose and 3 parts of flavor III; the volume concentration of ethanol aqueous solution is 40%; the parameters of fluidized spray are: interlayer agent inlet temperature 15°C, spray speed 0.3L / min, atomization pressure 0.3MPa, and spray drying temperature 55°C.

[0049] The flavors I, II and III used in the method of this embodiment are all water-soluble flavors, and the flavors I, II and III are flavors with different smells. The flavor I of this embodiment uses vanilla flavor, the flavor II uses pineapple flavor, and the flavor III uses tea flavor. The flavor microcapsules are used by the wet method, and the flavor microcapsules and emulsifiers are configured into a water-soluble suspension to emit fragrance for application.

[0050] Example 2

[0051] A method for preparing long-lasting fragrance microcapsules comprises the following steps:

[0052] S1, Preparation of core material:

[0053] S1.1: Dissolve peach fat in 45% ethanol solution by mass ratio of ethanol water solution: flavor I: peach fat = 80:8:0.5, then add flavor I, mix and dissolve evenly to obtain a fragrance liquid;

[0054] S1.2: Soybean lecithin, cholesterol and anhydrous ethanol are uniformly mixed in a mass ratio of anhydrous ethanol:soybean lecithin:cholesterol=40:8:1, and then the anhydrous ethanol is evaporated at 65°C under negative pressure to obtain a wall-hanging film;

[0055] S1.3: The fragrance liquid and the film are mixed by 45KHz ultrasound at a mass ratio of 100:3 to form an emulsion, and then the emulsion is repeatedly inserted and pushed out using a 0.5μm filter syringe to prepare a nanoemulsion; then the nanoemulsion and polyvinyl pyrrolidone are mixed evenly at a mass ratio of nanoemulsion: polyvinyl pyrrolidone = 100:1, and spray-dried to obtain a core mass;

[0056] S2, preparation of flavor microcapsules:

[0057] S2.1, according to the mass ratio of core material to interlayer agent = 100:3, the core material and the interlayer agent are fluidized sprayed, the interlayer agent is sprayed on the surface of the core material, and then freeze-dried to form microparticles A;

[0058] The interlayer agent is a methylcellulose aqueous solution with a mass concentration of 10%; the parameters of fluidized spray are: interlayer agent inlet temperature 10°C, spray speed 0.5L / min, atomization pressure 0.2MPa, spray drying temperature 60°C;

[0059] S2.2, particle A and coating agent I are fluidized sprayed in a mass ratio of 100:5, coating agent I is sprayed on the surface of particle A, and then freeze-dried to form particle B;

[0060] The mass fraction of the coating agent I is 90 parts of ethanol aqueous solution, 2 parts of pregelatinized starch, 1 part of methyl cellulose and 1 part of flavor II; the volume concentration of ethanol aqueous solution is 45%; the parameters of fluidized spray are: interlayer agent inlet temperature 10°C, spray speed 0.5L / min, atomization pressure 0.2MPa, spray drying temperature 60°C;

[0061] S2.3, according to the mass ratio of microparticles B: interlayer agent = 100:3, the microparticles B and the interlayer agent are sprayed on the surface of the microparticles B by fluidized spraying, and then freeze-dried to form microparticles C;

[0062] The interlayer agent is a methylcellulose aqueous solution with a mass concentration of 10%; the parameters of fluidized spray are: interlayer agent inlet temperature 10°C, spray speed 0.5L / min, atomization pressure 0.2MPa, spray drying temperature 60°C;

[0063] S2.4, according to the mass ratio of microparticle C: coating agent II = 100:5, the microparticle C and the coating agent II are sprayed on the surface of the microparticle C by the fluidized spray method, and the coating agent II is freeze-dried to form the flavor microcapsules;

[0064] Among them, the mass fractions of the components of coating agent II are 90 parts of ethanol aqueous solution, 2 parts of pregelatinized starch, 1 part of methyl cellulose and 1 part of flavor III; the volume concentration of ethanol aqueous solution is 45%; the parameters of fluidized spray are: interlayer agent inlet temperature is 10°C, spray speed is 0.5L / min, atomization pressure is 0.2MPa, and spray drying temperature is 60°C.

[0065] The flavors I, II and III used in the method of this embodiment are all water-soluble flavors, and the flavors I, II and III are flavors with different smells. The flavor I of this embodiment uses vanilla flavor, the flavor II uses pineapple flavor, and the flavor III uses tea flavor. The flavor microcapsules are used by the wet method, and the flavor microcapsules and emulsifiers are configured into a water-soluble suspension to emit fragrance for application.

[0066] Example 3

[0067] A method for preparing long-lasting fragrance microcapsules comprises the following steps:

[0068] S1, Preparation of core material:

[0069] S1.1: Dissolve peach fat in 50% ethanol solution by mass ratio of ethanol water solution: flavor I: peach fat = 80:0.5:0.5, then add flavor I, mix and dissolve evenly to obtain a fragrance liquid;

[0070] S1.2: Soybean lecithin, cholesterol and anhydrous ethanol are uniformly mixed in a mass ratio of anhydrous ethanol:soybean lecithin:cholesterol=40:4:1, and then the anhydrous ethanol is evaporated at 60°C under negative pressure to obtain a wall-hanging film;

[0071] S1.3: The fragrance liquid and the film are mixed by 40KHz ultrasound at a mass ratio of 100:3 to form an emulsion, and then the emulsion is repeatedly inserted and pushed out using a 0.5μm filter syringe to prepare a nanoemulsion; then the nanoemulsion and polyvinyl pyrrolidone are mixed evenly at a mass ratio of 100:0.5, and spray-dried to obtain a core mass;

[0072] S2, preparation of flavor microcapsules:

[0073] S2.1, according to the mass ratio of core material to interlayer agent = 100:3, the core material and the interlayer agent are fluidized sprayed, the interlayer agent is sprayed on the surface of the core material, and then freeze-dried to form microparticles A;

[0074] The interlayer agent is a methylcellulose aqueous solution with a mass concentration of 5%. The parameters of fluidized spray are: interlayer agent inlet temperature of 10°C, spray speed of 0.2L / min, atomization pressure of 0.2MPa, and spray drying temperature of 50°C.

[0075] S2.2, particle A and coating agent I are fluidized sprayed in a mass ratio of 100:5, coating agent I is sprayed on the surface of particle A, and then freeze-dried to form particle B;

[0076] The mass fraction of the coating agent I is 80 parts of ethanol aqueous solution, 2 parts of pregelatinized starch, 0.5 parts of methyl cellulose and 1 part of flavor II; the volume concentration of ethanol aqueous solution is 50%; the parameters of fluidized spray are: interlayer agent inlet temperature 10°C, spray speed 0.2L / min, atomization pressure 0.2MPa, spray drying temperature 50°C;

[0077] S2.3, according to the mass ratio of microparticles B: interlayer agent = 100:3, the microparticles B and the interlayer agent are sprayed on the surface of the microparticles B by fluidized spraying, and then freeze-dried to form microparticles C;

[0078] The interlayer agent is a methylcellulose aqueous solution with a mass concentration of 5%. The parameters of fluidized spray are: interlayer agent inlet temperature of 10°C, spray speed of 0.2L / min, atomization pressure of 0.2MPa, and spray drying temperature of 50°C.

[0079] S2.4, according to the mass ratio of microparticle C: coating agent II = 100:5, the microparticle C and the coating agent II are sprayed on the surface of the microparticle C by the fluidized spray method, and the coating agent II is freeze-dried to form the flavor microcapsules;

[0080] Among them, the mass fractions of the components of coating agent II are 80 parts of ethanol aqueous solution, 2 parts of pregelatinized starch, 0.5 parts of methyl cellulose and 1 part of flavor III; the volume concentration of ethanol aqueous solution is 50%; the parameters of fluidized spray are: interlayer agent inlet temperature 10°C, spray speed 0.2L / min, atomization pressure 0.2MPa, and spray drying temperature 50°C.

[0081] The flavors I, II and III used in the method of this embodiment are all water-soluble flavors, and the flavors I, II and III are flavors with different smells. The flavor I of this embodiment uses vanilla flavor, the flavor II uses pineapple flavor, and the flavor III uses tea flavor. The flavor microcapsules are used by the wet method, and the flavor microcapsules and emulsifiers are configured into a water-soluble suspension to emit fragrance for application.

[0082] Example 4

[0083] A method for preparing long-lasting fragrance microcapsules comprises the following steps:

[0084] S1, Preparation of core material:

[0085] S1.1: Dissolve peach fat in 45% ethanol solution in a mass ratio of ethanol water solution: flavor I: peach fat = 90:0.5:3, then add flavor I, mix and dissolve evenly to obtain a fragrance liquid;

[0086] S1.2: Soybean lecithin, cholesterol and anhydrous ethanol are uniformly mixed in a mass ratio of anhydrous ethanol:soybean lecithin:cholesterol=60:4:2, and then the anhydrous ethanol is evaporated at 60°C under negative pressure to obtain a wall-hanging film;

[0087] S1.3: The fragrance liquid and the film are mixed by 40KHz ultrasound at a mass ratio of 100:6 to form an emulsion, and then the emulsion is repeatedly inserted and pushed out using a 0.8μm filter syringe to prepare a nanoemulsion; then the nanoemulsion and polyvinyl pyrrolidone are mixed evenly at a mass ratio of nanoemulsion: polyvinyl pyrrolidone = 100:0.5, and spray-dried to obtain a core mass;

[0088] S2, preparation of flavor microcapsules:

[0089] S2.1, according to the mass ratio of core material to interlayer agent = 100:10, the core material and the interlayer agent are sprayed on the surface of the core material by fluidized spraying, and then freeze-dried to form microparticles A;

[0090] The interlayer agent is a methylcellulose aqueous solution with a mass concentration of 5%. The parameters of fluidized spray are: interlayer agent inlet temperature 20°C, spray speed 0.2L / min, atomization pressure 0.4MPa, spray drying temperature 50°C.

[0091] S2.2, according to the mass ratio of microparticle A: coating agent I = 100:15, microparticle A and coating agent I are sprayed on the surface of microparticle A by fluidized spraying method, and then freeze-dried to form microparticle B;

[0092] The mass fraction of the coating agent I is 80 parts of ethanol aqueous solution, 5 parts of pregelatinized starch, 0.5 parts of methyl cellulose and 5 parts of flavor II; the volume concentration of ethanol aqueous solution is 50%; the parameters of fluidized spray are: interlayer agent inlet temperature 20°C, spray speed 0.2L / min, atomization pressure 0.4MPa, spray drying temperature 50°C;

[0093] S2.3, according to the mass ratio of microparticles B: interlayer agent = 100:10, the microparticles B and the interlayer agent are sprayed on the surface of the microparticles B by fluidized spraying, and then freeze-dried to form microparticles C;

[0094] The interlayer agent is a methylcellulose aqueous solution with a mass concentration of 5%. The parameters of fluidized spray are: interlayer agent inlet temperature 20°C, spray speed 0.2L / min, atomization pressure 0.4MPa, spray drying temperature 50°C.

[0095] S2.4, according to the mass ratio of microparticle C: coating agent II = 100:15, the microparticle C and the coating agent II are sprayed on the surface of the microparticle C by fluidized spraying, and after freeze drying, the flavor microcapsules are formed;

[0096] Among them, the mass fractions of the components of coating agent II are 80 parts of ethanol aqueous solution, 5 parts of pregelatinized starch, 0.5 parts of methyl cellulose and 5 parts of flavor III; the volume concentration of ethanol aqueous solution is 50%; the parameters of fluidized spray are: interlayer agent inlet temperature 20°C, spray speed 0.2L / min, atomization pressure 0.4MPa, and spray drying temperature 50°C.

[0097] The flavors I, II and III used in the method of this embodiment are all water-soluble flavors, and the flavors I, II and III are flavors with different smells. The flavor I of this embodiment uses vanilla flavor, the flavor II uses pineapple flavor, and the flavor III uses tea flavor. The flavor microcapsules are used by the wet method, and the flavor microcapsules and emulsifiers are configured into a water-soluble suspension to emit fragrance for application.

[0098] Example 5

[0099] A method for preparing long-lasting fragrance microcapsules comprises the following steps:

[0100] S1, Preparation of core material:

[0101] S1.1: Dissolve peach fat in 42% ethanol solution by mass ratio of ethanol water solution: flavor I: peach fat = 90:8:3, then add flavor I, mix and dissolve evenly to obtain a fragrance liquid;

[0102] S1.2: Soybean lecithin, cholesterol and anhydrous ethanol are uniformly mixed in a mass ratio of anhydrous ethanol:soybean lecithin:cholesterol=60:8:2, and then the anhydrous ethanol is evaporated at 65°C under negative pressure to obtain a wall-hanging film;

[0103] S1.3: The fragrance liquid and the film are mixed by 45KHz ultrasound at a mass ratio of 100:6 to form an emulsion, and then the emulsion is repeatedly inserted and pushed out using a 0.8μm filter syringe to prepare a nanoemulsion; then the nanoemulsion and polyvinyl pyrrolidone are mixed evenly at a mass ratio of nanoemulsion: polyvinyl pyrrolidone = 100:1, and spray-dried to obtain a core mass;

[0104] S2, preparation of flavor microcapsules:

[0105] S2.1, according to the mass ratio of core material to interlayer agent = 100:10, the core material and the interlayer agent are sprayed on the surface of the core material by fluidized spraying, and then freeze-dried to form microparticles A;

[0106] The interlayer agent is a methylcellulose aqueous solution with a mass concentration of 10%; the parameters of fluidized spray are: interlayer agent inlet temperature 20°C, spray speed 0.5L / min, atomization pressure 0.4MPa, spray drying temperature 60°C;

[0107] S2.2, according to the mass ratio of microparticle A: coating agent I = 100:15, microparticle A and coating agent I are sprayed on the surface of microparticle A by fluidized spraying method, and then freeze-dried to form microparticle B;

[0108] The mass fraction of the coating agent I is 90 parts of ethanol aqueous solution, 5 parts of pregelatinized starch, 1 part of methyl cellulose and 5 parts of flavor II; the volume concentration of ethanol aqueous solution is 42%; the parameters of fluidized spray are: interlayer agent inlet temperature 20°C, spray speed 0.5L / min, atomization pressure 0.4MPa, spray drying temperature 60°C;

[0109] S2.3, according to the mass ratio of microparticles B: interlayer agent = 100:10, the microparticles B and the interlayer agent are sprayed on the surface of the microparticles B by fluidized spraying, and then freeze-dried to form microparticles C;

[0110] The interlayer agent is a methylcellulose aqueous solution with a mass concentration of 10%; the parameters of fluidized spray are: interlayer agent inlet temperature 20°C, spray speed 0.5L / min, atomization pressure 0.4MPa, spray drying temperature 60°C;

[0111] S2.4, according to the mass ratio of microparticle C: coating agent II = 100:15, the microparticle C and the coating agent II are sprayed on the surface of the microparticle C by fluidized spraying, and after freeze drying, the flavor microcapsules are formed;

[0112] Among them, the mass fractions of the components of coating agent II are 90 parts of ethanol aqueous solution, 5 parts of pregelatinized starch, 1 part of methyl cellulose and 5 parts of flavor III; the volume concentration of ethanol aqueous solution is 42%; the parameters of fluidized spray are: interlayer agent inlet temperature 20°C, spray speed 0.5L / min, atomization pressure 0.4MPa, and spray drying temperature 60°C.

[0113] The flavors I, II and III used in the method of this embodiment are all water-soluble flavors, and the flavors I, II and III are flavors with different smells. The flavor I of this embodiment uses vanilla flavor, the flavor II uses pineapple flavor, and the flavor III uses tea flavor. The flavor microcapsules are used by the wet method, and the flavor microcapsules and emulsifiers are configured into a water-soluble suspension to emit fragrance for application.

[0114] Example 6

[0115] A method for preparing long-lasting fragrance microcapsules comprises the following steps:

[0116] S1, Preparation of core material:

[0117] S1.1: Dissolve peach fat in 46% ethanol solution by mass ratio of ethanol water solution: flavor I: peach fat = 90:4:2.5, then add flavor I, mix and dissolve evenly to obtain a fragrance liquid;

[0118] S1.2: Soybean lecithin, cholesterol and anhydrous ethanol are uniformly mixed in a mass ratio of anhydrous ethanol:soybean lecithin:cholesterol=55:5:1.8, and then the anhydrous ethanol is evaporated at a negative pressure of 62°C to obtain a wall-hanging film;

[0119] S1.3: The fragrance liquid and the film are mixed by 42KHz ultrasound at a mass ratio of 100:4 to form an emulsion, and then the emulsion is repeatedly inserted and pushed out using a 0.6μm filter syringe to prepare a nanoemulsion; then the nanoemulsion and polyvinyl pyrrolidone are mixed evenly at a mass ratio of nanoemulsion: polyvinyl pyrrolidone = 100:0.6, and spray-dried to obtain a core mass;

[0120] S2, preparation of flavor microcapsules:

[0121] S2.1, according to the mass ratio of core material to interlayer agent = 100:5, the core material and the interlayer agent are sprayed on the surface of the core material by fluidized spraying, and then freeze-dried to form microparticles A;

[0122] The interlayer agent is a methylcellulose aqueous solution with a mass concentration of 6%. The parameters of fluidized spray are: interlayer agent inlet temperature 16°C, spray speed 0.4L / min, atomization pressure 0.3MPa, spray drying temperature 56°C.

[0123] S2.2, according to the mass ratio of microparticle A: coating agent I = 100:12, microparticle A and coating agent I are sprayed on the surface of microparticle A by fluidized spraying method, and then freeze-dried to form microparticle B;

[0124] The mass fraction of the coating agent I is 82 parts of ethanol aqueous solution, 4 parts of pregelatinized starch, 0.6 parts of methyl cellulose and 4 parts of flavor II; the volume concentration of ethanol aqueous solution is 48%; the parameters of fluidized spray are: interlayer agent inlet temperature 18°C, spray speed 0.4L / min, atomization pressure 0.3MPa, spray drying temperature 56°C;

[0125] S2.3, according to the mass ratio of microparticles B: interlayer agent = 100:5, the microparticles B and the interlayer agent are sprayed on the surface of the microparticles B by fluidized spraying, and then freeze-dried to form microparticles C;

[0126] The interlayer agent is a methylcellulose aqueous solution with a mass concentration of 6%. The parameters of fluidized spray are: interlayer agent inlet temperature 16°C, spray speed 0.4L / min, atomization pressure 0.3MPa, spray drying temperature 56°C.

[0127] S2.4, according to the mass ratio of microparticle C: coating agent II = 100:12, the microparticle C and the coating agent II are sprayed on the surface of the microparticle C by the fluidized spray method, and the coating agent II is freeze-dried to form the flavor microcapsules;

[0128] Among them, the mass fractions of the components of coating agent II are 84 parts of ethanol aqueous solution, 4 parts of pregelatinized starch, 0.6 parts of methyl cellulose and 2 parts of flavor III; the volume concentration of ethanol aqueous solution is 48%; the parameters of fluidized spray are: interlayer agent inlet temperature 18°C, spray speed 0.4L / min, atomization pressure 0.3MPa, and spray drying temperature 56°C.

[0129] The flavors I, II and III used in the method of this embodiment are all water-soluble flavors, and the flavors I, II and III are flavors with different smells. The flavor I of this embodiment uses vanilla flavor, the flavor II uses pineapple flavor, and the flavor III uses tea flavor. The flavor microcapsules are used by the wet method, and the flavor microcapsules and emulsifiers are configured into a water-soluble suspension to emit fragrance for application.

[0130] Preparation Comparative Example 1

[0131] The fragrance microcapsules were prepared by conventional methods, referring to the prior art patent CN108125799A, a composite sustained-release fragrance microcapsule and its preparation method.

[0132] According to the mass proportions, 6 parts of flavor, 1.4 parts of ethyl cellulose, 1.6 parts of glyceryl monostearate, 0.09 parts of SDS emulsifier, 0.7 parts of RS3 modified corn starch, 74 parts of deionized water, 0.74 parts of polyvinyl alcohol and 18.5 parts of ethanol were prepared;

[0133] Disperse ethyl cellulose in ethanol, then add glyceryl monostearate, mix evenly, then add RS3 modified corn starch, disperse evenly, then add SDS emulsifier, disperse evenly, finally add flavor, disperse evenly, and obtain mixed solution XⅠ;

[0134] Dispersing polyvinyl alcohol uniformly in deionized water to obtain a mixed solution XII;

[0135] The mixed solution XⅠ and the mixed solution XⅡ are uniformly mixed to obtain a mixed solution XⅢ, which is placed in ice water at 4°C and rapidly cooled under homogenization conditions at a homogenization speed of 10000 r / min to obtain a microcapsule suspension, which is separated and the upper microcapsule suspension is taken and spray-dried to obtain flavor microcapsules.

[0136] The flavor of this comparative example is 4 parts of vanilla, 2 parts of pineapple, and 2 parts of tea.

[0137] Preparation Comparative Example 2

[0138] During the preparation of the S1 core material, no polyvinyl pyrrolidone was added; other parameters were the same as in Example 1.

[0139] Preparation Comparative Example 3

[0140] During the preparation of S2 flavor microcapsules, no interlayer coating is performed, that is, S2.1 and S2.3 are omitted; other parameters are the same as in Example 1.

[0141] The fragrance microcapsules of Examples 1 to 6 and the fragrance microcapsules of Comparative Examples 1 to 3 were respectively prepared into sprays, and the fragrance retention time was tested by spraying:

[0142] The components of the spray are composed of 3 parts of flavor microcapsules, 0.03 parts of gellan gum, 0.04 parts of xanthan gum, 2 parts of Tween 40 and 100 parts of deionized water in parts by weight.

[0143] 1 mL of each spray was placed in a culture dish and stored separately in an open environment at 30°C and 60% humidity. 20 people were selected to smell the odor of each culture dish at different time periods to evaluate the fragrance retention. The highest and lowest scores were removed and the average score of the 18 people was rounded off to an integer. The results are shown in Table 1 below:

[0144] Table 1 Test results

[0145]

[0146]

[0147] Among them, according to the test subjects, the initial smell of Examples 1 to 6 was tea fragrance, pineapple smell on the 6th day, stronger pineapple smell on the 9th day, vanilla smell on the 36th day, and the mixed smells at each stage were not obvious. According to the test subjects, the fragrance of Comparative Example 1 was mixed, and the smell perception was poor. According to the test subjects, the smell of Comparative Example 3 was mixed to varying degrees from 6th day to 36th day, and the smell perception was poor.

[0148] From the above results, it can be seen that the fragrance retention of Examples 1 to 6 is relatively uniform, the fragrance retention lasts for a long time, and different stages have different fragrances. The three fragrances can be released in layers, and the mixed smell is not obvious. The smell of Comparative Example 1 is mixed and unpleasant, the smell change trend is large, and the fragrance retention time is short. The fragrance retention of Comparative Example 2 drops significantly after 72 days, and the overall fragrance retention time is shortened. Comparative Example 3 has different degrees of mixed smells from 6 days to 36 days, and the smell perception is poor.

[0149] During the washing process of clothes in a washing machine, 0.5 g of the fragrance microcapsules of Examples 1 to 6 were added to the clothes for rinsing; after the clothes were dried, they were placed in a sealed wardrobe for storage for 150 days, and the clothes were taken out and smelled, and the clothes still retained the fragrance.

Claims

1. A method for preparing long-lasting fragrance microcapsules, characterized in that: The steps include: S1, Preparation of core material: S1.1: According to the mass ratio, ethanol water solution: flavor I: peach fat = (80-90): (0.5-8): (0.5-3), dissolve peach fat in ethanol solution, then add flavor I, mix and dissolve evenly to obtain a fragrance liquid; S1.2: According to the mass ratio of anhydrous ethanol: soybean lecithin: cholesterol = (40-60): (4-8): (1-2), soybean lecithin, cholesterol and anhydrous ethanol are uniformly mixed, and then the anhydrous ethanol is removed by negative pressure evaporation to obtain a wall-hanging film; S1.3: According to the mass ratio of fragrance liquid: film = 100: (3-6), the fragrance liquid and the film are ultrasonically mixed to form an emulsion, and then the emulsion is repeatedly inserted and pushed out using a 0.5μm-0.8μm filter membrane syringe to prepare a nanoemulsion; then, according to the mass ratio of nanoemulsion: polyvinyl pyrrolidone = 100: (0.5-1), the nanoemulsion and polyvinyl pyrrolidone are evenly mixed, spray-dried, and a core mass is obtained; S2, preparation of flavor microcapsules: S2.1, according to the mass ratio of core material: interlayer agent = 100: (3-10), the core material and interlayer agent are sprayed on the surface of the core material by fluidized spraying, and then freeze-dried to form microparticles A; S2.2, according to the mass ratio of microparticle A: coating agent I = 100: (5-15), microparticle A and coating agent I are fluidized sprayed, coating agent I is sprayed on the surface of microparticle A, and after freeze drying, microparticle B is formed; S2.3, according to the mass ratio of microparticle B: interlayer agent = 100: (3-10), the microparticle B and the interlayer agent are sprayed on the surface of the microparticle B by fluidized spraying, and then freeze-dried to form microparticle C; S2.4, according to the mass ratio of microparticle C: coating agent II = 100: (5-15), the microparticle C and the coating agent II are sprayed on the surface of the microparticle C by the fluidized spray method, and the coating agent II is freeze-dried to form the flavor microcapsule; In S2.1 and S2.3, the interlayer agent is a methyl cellulose aqueous solution with a mass concentration of 5% to 10%; In S2.2, the composition of the coating agent I is composed of 80 to 90 parts of ethanol aqueous solution with a volume concentration of 40% to 50%, 2 to 5 parts of pregelatinized starch, 0.5 to 1 part of methyl cellulose and 1 to 5 parts of flavor II in mass fractions; In S2.4, the components of the coating agent II are composed by mass fraction of 80 to 90 parts of ethanol aqueous solution with a volume concentration of 40% to 50%, 2 to 5 parts of pregelatinized starch, 0.5 to 1 part of methyl cellulose and 1 to 5 parts of flavor III.

2. The method for preparing a long-lasting fragrance microcapsule according to claim 1, characterized in that: In S1.1, the volume concentration of the ethanol aqueous solution is 40% to 50%.

3. The method for preparing a long-lasting fragrance microcapsule according to claim 1, characterized in that: In S1.2, the evaporation temperature is 60°C to 65°C.

4. The method for preparing a long-lasting fragrance microcapsule according to claim 1, characterized in that: In S1.3, the frequency of the ultrasound is 40KHz to 45KHz.

5. The method for preparing a long-lasting fragrance microcapsule according to claim 1, characterized in that: In S2, the parameters of the fluidized spray are: interlayer agent inlet temperature 10°C to 20°C, spray speed 0.2L / min to 0.5L / min, atomization pressure 0.2MPa to 0.4MPa, and spray drying temperature 50°C to 60°C.

6. The method for preparing a long-lasting fragrance microcapsule according to claim 1, characterized in that: The flavor I, flavor II and flavor III are all water-soluble flavors, and the flavor I, flavor II and flavor III are flavors with different smells.

7. Application of a long-acting flavor microcapsule, the flavor microcapsule prepared by the method for preparing a long-acting flavor microcapsule according to any one of claims 1 to 6, characterized in that: The flavor microcapsules are used by the wet method, in which the flavor microcapsules and emulsifiers are formulated into a water-soluble suspension for fragrance application.

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