Microcapsule granular essence and preparation method thereof

Abstract

The invention discloses a preparation method of microcapsule essence particles, and relates to the technical field of microcapsule essence preparation, in particular to microcapsule granular essence and a preparation method thereof.The preparation method comprises the following steps that an oily essence base is embedded in a first wall material through a spray drying method, and microcapsule essence powder is prepared; carrying out melt extrusion granulation on the microcapsule essence powder obtained in the previous step and a second wall material; through the synergistic combination of two processes, the powdery essence which is easy to absorb moisture and raise dust is converted into a particle product which is high in physical stability and good in controlled release performance, the inherent defects of the traditional spray drying essence are effectively overcome, and the application range of the essence in the fields of foods, tobaccos and the like is widened.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of microcapsule fragrance preparation, and particularly relates to a microcapsule granular fragrance and a preparation method thereof. BACKGROUND

[0002] In the food, tobacco and other consumer product industries, the stabilization and controllable release of fragrances are the key to improving product quality. Microcapsule technology, as an effective embedding means, is widely used to protect fragrances from the influence of the external environment (such as light, oxygen and heat), reduce volatile loss, and achieve the slow release and controlled release of flavors.

[0003] Among the many microencapsulation methods, spray drying has become the most important technology in the industrial embedding of fragrances due to its mature process, popular equipment, ease of continuous and large-scale production. This technology forms a powder-like microcapsule product by atomizing and quickly drying the fragrance emulsion. Such powder fragrances have good storage stability, good dispersibility and long shelf life.

[0004] However, the inherent defects of the powder microcapsules prepared by spray drying are increasingly prominent, which seriously limits their application in a wider range of scenarios, mainly in the following aspects: Poor physical stability: the product has strong hygroscopicity and is easy to clog, affecting the flowability and use accuracy; at the same time, fine powder is easy to produce dust during production and use, causing pollution of the working environment and loss of fragrance.

[0005] Inadequate embedding effect: single spray drying embedding often has an upper limit of embedding rate, and the product is prone to "surface residual oil" phenomenon, that is, part of the fragrance is not effectively embedded and adheres to the surface of the particles, which not only leads to the loss of aroma during the storage period, but also makes it release rapidly when it encounters moisture or oil, with poor controlled release performance.

[0006] Thermal sensitive components are easily damaged: the high temperature in the spray drying process may cause irreversible damage to some thermal sensitive fragrance ingredients, affecting the top notes and overall flavor profile.

[0007] In order to overcome the above defects, the industry has made some explorations. For example, some studies use complex coacervation, interfacial polymerization and other methods to prepare microcapsules with more compact structure, or use cyclodextrin, chitosan and other special wall materials to improve the embedding rate. However, these methods or processes are complex, harsh conditions, difficult to be applied on a large scale; or introduce chemical crosslinking agents, which have safety and environmental concerns; or fail to effectively solve the physical defects such as hygroscopicity and dust of the powder form. Another technical solution attempts to build a double-layer microcapsule, but its core focuses on the secondary encapsulation at the molecular level, and does not change the powder form of the product, which has limited effect on solving the macro physical performance problem.

[0008] Therefore, there is an urgent need in the art for a new technical solution that can retain the high efficiency and maturity of the spray drying method, fundamentally improve the physical defects of the powder flavor, and provide a new flavor product form with low moisture absorption, no dust, less surface oil, and excellent controlled-release performance, as well as a preparation process suitable for industrial production. SUMMARY

[0009] The purpose of the present application is to provide a new flavor with low moisture absorption, no dust, less surface oil, and excellent controlled-release performance, which overcomes the shortcomings of the prior art.

[0010] The purpose of the present application is achieved by the following technical solutions: A preparation method of microcapsule flavor particles, comprising the following steps: S1: embedding an oily fragrance base in a first wall material by a spray drying method to prepare a microcapsule flavor powder; S2: melt-extruding and granulating the microcapsule flavor powder obtained in step S1 with a second wall material, wherein S2 specifically comprises the following steps S21 to S23: S21: pre-mixing the microcapsule flavor powder with the second wall material, the second wall material being one or more of sugar alcohol, modified starch, edible wax, and hydrogenated vegetable oil; S22: melt-extruding the pre-mixed material in step S21Z under a determined temperature condition; S23: cooling and granulating the extrudate to obtain microcapsule flavor particles.

[0011] Specifically, step S1 further comprises the following steps S11 to S13: S11: dissolving the first wall material in water to form a solution, the first wall material being one or more of gum arabic, modified starch, malt dextrin, gelatin, and cellulose derivatives; S12: adding the oily fragrance base to the first wall material solution to form an emulsion after homogenization; S13: spray drying the emulsion to obtain a microcapsule flavor powder.

[0012] More specifically, in step S12, the homogenization is carried out under a pressure of 20-25 MPa; and / or, In step S13, the inlet air temperature of the spray drying is 160-200 DEG C, and the outlet air temperature is 70-95 DEG C.

[0013] The above, before step S21, further comprises step S20: preheating and crushing the selected second wall material, and then passing through a 60-100 mesh screen.

[0014] More specifically, in step S21, the volume ratio of the microcapsule fragrance powder to the second wall material is 1:3 to 1:5.

[0015] More specifically, in step S22, the temperature of the melt extrusion is controlled to be higher than the melting point of the second wall material and lower than the decomposition temperature of the heat-sensitive component in the oily fragrance base.

[0016] More specifically, the temperature of the melt extrusion is 60-90°C.

[0017] More specifically, in step S22, the melt extrusion is performed in a twin-screw extruder, and the screw combination and shearing action are adjusted to enable the molten second wall material to fully infiltrate and coat the microcapsule powder fragrance.

[0018] More specifically, in step S23, the particle size of the granular fragrance is 0.5-2.0 mm.

[0019] According to another aspect of the present application, there is provided a microcapsule fragrance granule prepared by the above-mentioned method for preparing a microcapsule fragrance granule.

[0020] The present application has the following beneficial effects: A method for preparing a microcapsule fragrance granule, comprising the following steps: S1: embedding an oily fragrance base in a first wall material by a spray drying method to prepare a microcapsule fragrance powder; S2: melt extruding and granulating the microcapsule fragrance powder obtained in step S1 with a second wall material, wherein S2 specifically comprises the following steps S21 to S23: S21: pre-mixing the microcapsule fragrance powder with the second wall material, the second wall material being one or more of a sugar alcohol, a modified starch, an edible wax, and a hydrogenated vegetable oil; S22: melt extruding the pre-mixed material under a determined temperature condition; and S23: cooling and granulating the extrudate to obtain a microcapsule fragrance granule. Through the synergistic combination of the two processes, the powder fragrance which is prone to moisture absorption and dusting is converted into a granular product with high physical stability and good controlled release performance, effectively solving the inherent defects of traditional spray-dried fragrances and broadening their application in the fields of food, tobacco, and the like. BRIEF DESCRIPTION OF DRAWINGS

[0021] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed in the embodiment description will be briefly introduced as follows. Obviously, the drawings in the following description are some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without any creative effort.

[0022] Figure 1 is a first schematic flow chart of a method for preparing a microcapsule fragrance granule according to an embodiment of the present application; Figure 2is a second schematic flow chart of a method for preparing a microcapsule fragrance particle according to an embodiment of the present application.

[0023] Figure 3 is a third schematic flow chart of a method for preparing a microcapsule fragrance particle according to an embodiment of the present application. DETAILED DESCRIPTION

[0024] For the purposes of the present application, the technical solutions and advantages thereof will be more apparent from the following detailed description of the embodiments of the present application, with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments of the present application, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the scope of the present application.

[0025] Embodiment 1 One of the embodiments of the method for preparing a microcapsule fragrance particle according to the present application, as shown in Figure 1 , comprises the following steps S1 and S2.

[0026] S1: preparing a microcapsule fragrance powder by embedding an oily fragrance base in a first wall material through a spray drying method.

[0027] S2: melt-extruding granulation of the microcapsule fragrance powder obtained in step S1 with a second wall material.

[0028] Specifically, as shown in Figure 2 , step S1 further comprises the following steps S11 to S13: S11: dissolving the first wall material in water to form a solution, the first wall material being one or more of gum arabic, modified starch, malt dextrin, gelatin and cellulose derivatives.

[0029] S12: adding the oily fragrance base to the first wall material solution to form an emulsion after homogenization.

[0030] Specifically, the oily fragrance base is added to the above wall material solution, and after preliminary shearing, high-pressure homogenization treatment is performed under a pressure of 20-25 MPa to form an oil-in-water (O / W) emulsion with uniform and stable particle size distribution; the homogenization treatment can be performed multiple times until the emulsion stability meets the requirements of spray drying.

[0031] The oily fragrance base is mainly composed of a plurality of natural plant essential oils and fragrance ingredients, as well as oil antioxidants.

[0032] In the configuration of the fragrance base, part of the fragrance base uses natural plant essential oils as the main ingredient, and other fragrance ingredients are also added to supplement the fragrance characteristics. At the same time, there are also cases of using fragrance ingredients to configure the fragrance base.

[0033] In the present embodiment, the oily fragrance base comprises one or more of the following components: 1: Natural plant essential oil configured fragrance base ingredients, (such as citrus essential oil) such as: sweet orange, lemon, grapefruit, etc. 2: Take the spice ingredients as the characteristic aroma ingredients in the oily fragrance base, such as: ethyl acetoacetate, ethyl hexanoate, etc. for apple aroma; leaf alcohol, strawberry acid, etc. for strawberry aroma; propyl-undecanolide, propyl-decanolide, etc. for juicy peach.

[0034] 3: In order to slow down the speed of oil oxidation, appropriate amount of oil antioxidant is added according to the regulations as required, such as: 2, 6-di-tert-butyl-p-cresol (BHT), butylated hydroxyanisole (BHA), vitamin E, ascorbic acid palmitate (AP), etc.

[0035] S13: Spray drying the emulsion to obtain microcapsule fragrance powder.

[0036] Specifically, the obtained emulsion is conveyed to the spray drying tower by peristaltic pump for drying treatment, the inlet air temperature is set to 160-200 °C, and the outlet air temperature is set to 70-95 °C. The emulsion is atomized into fine droplets by centrifugal or pressure atomizer, and solid powder is formed after hot air drying. After collection, the microcapsule powder fragrance is obtained.

[0037] More specifically, as shown in Figure 3 S2 specifically includes the following steps S20 to S23: S20: Preheat and crush the selected second wall material, then pass through a 60-100 mesh sieve.

[0038] Specifically, a hydrophobic polymer is selected as the secondary embedding wall material, and the wall material is selected from one or more of sugar alcohol (maltitol, sorbitol), modified starch, edible wax, hydrogenated vegetable oil, and colloid; the selected wall material is preheated at 40-60 °C and crushed, and then passed through a 60-100 mesh sieve for standby.

[0039] S21: Pre-mix the microcapsule fragrance powder in step S20 with the second wall material.

[0040] Specifically, the microcapsule powder fragrance prepared by the spray drying method in step S13 is placed in a high-speed mixer with the wall material selected in step S20 at a volume ratio of 1:3 to 1:5, and mixed at a speed of 500-800 rpm for 5-10 minutes until a uniform pre-mixed material is formed.

[0041] S22: Melt extrude the pre-mixed material in step S21 under a determined temperature condition.

[0042] Specifically, the premix is fed into a twin-screw extruder, and the temperature of each section of the extruder is set to rise in a gradient within the range of 60-90°C (which can be adjusted according to the melting point of the wall material). The temperature is ensured to be higher than the melting point of the wall material to make it melt, while being far lower than the decomposition temperature of the heat-sensitive components in the essence (usually only a safety window of 10-20°C). If the temperature is too low, the coating will be uneven and the torque will increase sharply; if the temperature is too high, the essence will be directly damaged, losing the top notes.

[0043] The screw rotation speed is controlled at 80-200 rpm, and the material is extruded in a molten state through kneading and compression. The screw combination and shearing action are adjusted to enable the molten second wall material to fully infiltrate and coat the microcapsule powder essence, forming a dense barrier layer.

[0044] If necessary, an appropriate amount of interfacial compatibility agent can be added to enhance the affinity of the two-phase interface. To further ensure the coating quality, the secondary wall material and the powder essence should be uniformly premixed before feeding to avoid holes or defects in the coating layer due to uneven dispersion.

[0045] S23: cooling and granulating the extrudate to obtain microcapsule essence particles. Specifically, it includes: 1) molding and cooling The extruded continuous strip-shaped product is conveyed to a cooling tank through a cooling conveyor belt; it is forcibly cooled at 5-15°C using cold air or cooling water to solidify and shape.

[0046] 2) granulation and screening The cooled strip-shaped material is broken and granulated using a rotary granulator or a crushing and granulating machine, and the obtained particles are classified by a vibrating screening device to collect target particles with a particle size of 0.5-2.0 mm (about 20 mesh).

[0047] 3) packaging and storage The screened granular essence is placed in an aluminum foil composite bag, sealed and packaged, and stored in a cool and dry place.

[0048] Innovations and advantages of a microcapsule essence particle preparation method of the present application 1. Synergistic combination process, complementary advantages The "spray drying" and "hot melt extrusion" mature processes are creatively combined. The former efficiently realizes high-embedding-rate primary microencapsulation, and the latter excellently solves the physical defects of the primary product and endows it with new controlled-release functions. The two processes complement each other, producing a synergistic effect of "1+1>2".

[0049] 2. Simple process flow, suitable for industrialization The whole process is a pure physical process, without complex pH adjustment, chemical reaction or solvent recovery, with mild production conditions, simple operation and relatively low energy consumption, which is very suitable for large-scale industrial continuous production.

[0050] 3. High environmental protection and safety The hot melt extrusion process does not require any organic solvent, avoiding the pollution of solvent residues to the product and the harm to the environment, and the product is safer and more environmentally friendly.

[0051] 4. Good flavor fidelity By accurately controlling the temperature window (60-90℃) of hot melt extrusion, while realizing the melting of the second wall material, the primary flavor microcapsule embedded inside, especially the heat-sensitive top note ingredients, is maximally protected, ensuring the purity and fullness of the flavor of the final product.

[0052] According to another aspect of the present application, a microcapsule flavor particle is provided, which is prepared by the above-mentioned method for preparing a microcapsule flavor particle.

[0053] The microcapsule flavor particle prepared by the method has significantly improved product performance: 1. Greatly enhanced physical stability Low hygroscopicity: Through the melting coating of the second wall material (sugar alcohol, edible wax and other hydrophobic substances), a dense physical barrier is formed, effectively blocking the intrusion of environmental moisture, solving the industry problem of easy moisture absorption and caking of traditional spray-dried powder flavor, and prolonging the shelf life of the product.

[0054] No dust: The product is regular granular, with large particle size (0.5-2.0 mm), which fundamentally eliminates the dust problem of fine powder flavor in the production and application process, improves the working environment, and reduces flavor loss and cross contamination.

[0055] 2. Optimized embedding effect and controlled release performance Reduced surface residual oil: The secondary coating layer completely encapsulates the primary powder flavor, avoiding direct exposure of the core material to the outside environment, significantly reducing the surface residual oil rate of the product, and making the aroma more stable during storage.

[0056] Achieve controlled release: By selecting second wall materials with different melting points (such as different types of edible wax or hydrogenated vegetable oil), the release temperature of the flavor can be adjusted. When applied to heated food or tobacco products, the particles can melt and break at a specific temperature, achieving timed and targeted release of flavor, improving the accuracy and effectiveness of application.

[0057] 3. Wide application scenarios The microcapsule fragrance particle has good flowability, is easy to be uniformly mixed with other granular raw materials (such as granulated sugar, milk powder, tobacco sheet, etc.), and is particularly suitable for solid and semi-solid foods (such as candies, cakes, powdered beverages) and tobacco products (especially heat-not-burn cigarettes), greatly expanding the application range of spray-dried fragrances.

[0058] It should be noted that the above only describes the preferred embodiments of the present application and the principles of the technology applied. Those skilled in the art will understand that the present application is not limited to the specific embodiments described herein, and that various obvious changes, re-adjustments and substitutions can be made by those skilled in the art without departing from the scope of the present application. Therefore, although the present application has been described in more detail through the above embodiments, the present application is not limited to the above embodiments, and can include more other equivalent embodiments without departing from the concept of the present application, and the scope of the present application is determined by the scope of the appended claims.

Claims

1. A process for the preparation of microencapsulated perfume particles, characterized in that, The method comprises the following steps: S1: preparing a microcapsule fragrance powder by embedding an oily fragrance base in a first wall material through a spray drying method; S2: melt-extruding granulation of the microcapsule fragrance powder obtained in step S1 with a second wall material, wherein S2 specifically comprises the following steps S21 to S23: S21: pre-mixing the microcapsule fragrance powder with the second wall material, the second wall material being one or more of a sugar alcohol, a modified starch, an edible wax, and a hydrogenated vegetable oil; S22: melt-extruding the pre-mixed material in step S21Z under a determined temperature condition; S23: cooling and granulating the extrudate to obtain the microcapsule fragrance granules.

2. A process for the preparation of microencapsulated perfume particles according to claim 1, characterized in that, The step S1 further comprises the following steps S11 to S13: S11: dissolving the first wall material in water to form a solution, the first wall material being one or more of gum arabic, a modified starch, malt dextrin, gelatin, and a cellulose derivative; S12: adding the oily fragrance base to the first wall material solution to form an emulsion through emulsification and homogenization; S13: spray drying the emulsion to obtain the microcapsule fragrance powder.

3. The method according to claim 2, wherein: in the step S12, the emulsification and homogenization are performed under a pressure of 20-25 MPa; and / or in the step S13, the inlet air temperature of the spray drying is 160-200°C, and the outlet air temperature is 70-95°C.

4. A process for the preparation of microencapsulated flavour particles according to any one of claims 1 to 3, characterised in that, Before the step S21, the method further comprises a step S20 of preheating and crushing the selected second wall material, and then passing it through a 60-100 mesh sieve.

5. The method according to claim 4, wherein: in the step S21, the volume ratio of the microcapsule fragrance powder to the second wall material is 1:3 to 1:

5.

6. The method according to claim 1, wherein: in the step S22, the temperature of the melt-extrusion is controlled to be higher than the melting point of the second wall material and lower than the decomposition temperature of the heat-sensitive components in the oily fragrance base.

7. The method according to claim 6, wherein: the temperature of the melt-extrusion is 60-90°C.

8. The method according to claim 1, wherein: in the step S22, the melt-extrusion is performed in a twin-screw extruder, and the screw combination and shearing action are adjusted to enable the melt-extruded second wall material to fully infiltrate and coat the microcapsule fragrance powder.

9. The method according to claim 1, wherein: in the step S23, the particle size of the granular fragrance is 0.5-2.0 mm.

10. A microencapsulated flavour particle characterised in that, The microcapsule fragrance granules are prepared by the method of any one of claims 1-9.

Images