Preparation method and application of sustained-release flavor material

Abstract

The present invention relates to the technical field of cigarette processing, and in particular to a method for preparing a sustained-release flavor material, comprising the following steps: S1 adsorption: placing mesoporous hollow nano-silicon spheres in a flavor and fragrance solution, allowing the solution to stand for 2-5 hours, and obtaining mesoporous hollow nano-silicon spheres to which flavors and fragrances are added for standby use; S2 preparation of a composite flavor material: wrapping the mesoporous hollow nano-silicon spheres processed by the S1 step with a coating layer, and drying them under low temperature conditions after the coating is completed to obtain a composite flavor material. The purpose of the present invention is to enable flavors and fragrances to be prepared into a sheet or granular form, on the one hand, to reduce the volatilization of the flavor during storage, and on the other hand, to be easily added to a filter rod or a cigarette cartridge, so that the cigarette or cigarette cartridge can continuously release the flavor of the flavor when inhaled, thereby improving the consumer experience.

Description

Technical Field

[0001] The present invention relates to the technical field of cigarette processing, and in particular to a preparation method and application of a slow-release flavor material. Background Art

[0002] Flavoring is a handcrafted mixture containing two or more, or even dozens, of flavoring agents (sometimes also containing a suitable solvent or carrier), resulting in a specific aroma. With the development of the cigarette industry, flavorings are added at different steps during the cigarette production process, tailored to the specific cigarette type. This creates cigarettes with varying aromas to meet the needs of diverse consumers. However, because flavorings are highly reactive substances, they can easily evaporate during storage or use, resulting in low flavor utilization.

[0003] To enhance the consumer experience, flavors and fragrances are currently added to different steps of the production process, depending on the type of cigarette being produced. Ordinary cigarettes typically have flavors and fragrances added during the shredding process to ensure they are thoroughly mixed with the tobacco. Some cigarettes are prepared by adding flavors and fragrances to filter rods after they have been prepared into tows. Electric-heated smoking devices typically mix flavors and fragrances with tobacco to create heatable cartridges. However, when flavors and fragrances are prepared into tows or cartridges, the aroma evaporates easily during storage. When consumers smoke the cigarettes, the aroma they perceive is either unclear or overly strong, resulting in a poor user experience. Summary of the Invention

[0004] In view of this, the purpose of the present invention is to provide a preparation method and application of a sustained-release flavor material, so that flavors and fragrances can be prepared into flakes or granules. On the one hand, the volatilization of the flavor can be reduced during storage. On the other hand, it can be easily added to filter rods or cigarette cartridges, so that the flavor of the flavor can be continuously released when the cigarette or cigarette cartridge is inhaled, thereby improving the consumer experience.

[0005] The present invention solves the above technical problems through the following technical means:

[0006] A method for preparing a sustained-release flavor material comprises the following steps:

[0007] S1 adsorption: placing the mesoporous hollow nano-silicon spheres in the flavor and fragrance solution and letting it stand for 2-5 hours. After the standing is completed, the mesoporous hollow nano-silicon spheres with added flavor and fragrance are obtained and set aside;

[0008] S2 Preparation of composite flavor material: The mesoporous hollow nano-silicon spheres treated in step S1 are wrapped with a coating layer. After the coating is completed, they are dried under low temperature conditions to obtain a composite flavor material.

[0009] By using nanomaterial mesoporous hollow nano-silicon balls to adsorb flavors and fragrances, and then coating the nano-mesoporous material that adsorbs the flavors and fragrances with a coating layer, a composite flavor material is obtained. On the one hand, the flavor material can reduce the volatilization of the flavor when stored; on the other hand, the flavor material can slowly release the flavor when added to cigarettes or cigarette cartridges, thereby improving the consumer experience.

[0010] Furthermore, in the S1 step, before placing the mesoporous hollow nano-silicon spheres in the flavor and fragrance solution, the following steps are also included: placing the mesoporous hollow nano-silicon spheres in a sealed heating container, placing ferrocene under the mesoporous hollow nano-silicon spheres, heating at 105-120°C for 1-3 hours, cooling after heating, transferring to a closed reactor, and introducing inert protective gas under a certain pressure to react for 4-8 hours to obtain pretreated mesoporous hollow nano-silicon spheres.

[0011] Since ferrocene will sublime at temperatures above 100°C, ferrocene and mesoporous hollow nano-silicon spheres are placed in a sealed heating container, with ferrocene located below the mesoporous hollow nano-silicon spheres, so that ferrocene is heated and sublimated, and the mesoporous hollow nano-silicon spheres adsorb ferrocene. After cooling, the container is transferred to a closed reactor, where, under the conditions of inert protective gas, a certain pressure and high temperature, ferrocene is converted into iron carbide, and the iron carbide is cross-linked in the mesopores of the mesoporous hollow nano-silicon spheres, thereby enhancing the thermal conductivity and sustained-release performance of the mesoporous hollow nano-silicon spheres.

[0012] Furthermore, the step S1 further includes the following steps: placing the flavors and fragrances in a mixed solution of lauric acid and stearic acid, stirring evenly, transferring the mixture to a water bath shaker, and reacting for 12-24 hours to obtain esterified flavors and fragrances.

[0013] By mixing flavors and fragrances with lauric acid and stearic acid to create esterified flavors and fragrances, the esterified flavors and fragrances can be easily added to the mesoporous hollow nano-silicon spheres, further extending the shelf life of the flavors and fragrances. Furthermore, due to the low melting points of lauric acid and stearic acid, the flavoring material can cooperate with the mesoporous hollow nano-silicon spheres to release fragrance during use.

[0014] Furthermore, the step S1 further includes the following steps: the lipidated flavors and fragrances are poured into the mesoporous hollow nano-silicon spheres by heating and vacuum infusion.

[0015] Through heated vacuum infusion, it is easier to fill the lipidated flavors and spices into the mesoporous hollow nano-silicon balls, and the amount added can be controlled, thereby controlling the fragrance concentration.

[0016] Furthermore, in step S1, the flavor and fragrance is one of citric acid, vanillin, theobroma cacao, butyrylberry ketone and pyroacetic acid lactone.

[0017] Furthermore, in the step S1, the coating layer is a thermosensitive liposome, and the thermosensitive liposome is one of lecithin compounds or plant wax.

[0018] Both lecithin compounds and plant waxes have low melting points. On the one hand, by coating the mesoporous hollow nano-silicon spheres, the escape of fragrance of flavors and fragrances when they are not in use can be further slowed down. On the other hand, when they are in use, the lecithin membrane layer heats and shrinks or the plant wax melts, gradually exposing the mesoporous hollow nano-silicon spheres and further slowly releasing the fragrance.

[0019] Furthermore, during the reaction in the closed reactor, the inert protective gas is nitrogen, the reaction pressure is 1-2 MPa, and the reaction temperature is 400-550°C.

[0020] By introducing inert protective gas under certain reaction temperature and pressure conditions, the content of iron carbide is increased. On the one hand, the generation of iron oxide is reduced, thereby reducing the rust smell of iron oxide and reducing the impact on fragrance. On the other hand, the thermal conductivity of the mesoporous hollow nano-silicon spheres is enhanced.

[0021] The present invention also discloses an application of a sustained-release flavor material, including the flavor material described above, wherein the flavor material is applied to a cigarette cartridge or a filter rod of an electrically heated or electromagnetically heated smoking device.

[0022] When iron carbide exists in the flavor material through electric heating or electromagnetic heating, the iron carbide can be inductively heated to increase the sustained-release speed of the flavor material.

[0023] Furthermore, the process of applying the flavor material to the cigarette cartridge or filter rod of the electrically heated smoking device also includes the following steps: evenly dispersing the flavor material particles, pouring the dispersed flavor material into the expanded tobacco stem particles through vacuum filling, transferring the filled expanded tobacco stem particles into a container, adding carboxymethyl cellulose solution, and continuing to stir for 40-60 minutes. After the stirring is completed, preparing them into flakes or particles, freeze-drying, and obtaining composite flakes or composite particles.

[0024] Since the expanded tobacco stem particles themselves have pores, the flavor material can be adsorbed by the expanded tobacco stem particles, which facilitates subsequent processing. By adding carboxymethyl cellulose, they are prepared into composite sheets or particles, which enhances the toughness of the sheets or particles and avoids damage during storage or adding to cigarette cartridges or filter rods.

[0025] Furthermore, the thickness of the composite sheet is 1-3 mm, and the particle size of the composite particles is 0.5-2 mm.

[0026] Beneficial effects of the present invention:

[0027] 1. By using mesoporous hollow nano-silicon spheres to adsorb flavors and fragrances or preparing the flavors and fragrances into a gel state, and then filling them into the mesoporous hollow nano-silicon spheres, the amount of flavors and fragrances in the mesoporous hollow nano-silicon spheres is increased, and then the mesoporous hollow nano-silicon spheres are coated with a coating layer to obtain a flavor material. This allows the flavor material to slow down the volatilization of the fragrance during storage, and to slowly release the fragrance of the flavor and fragrance during use, thereby improving the consumer experience;

[0028] 2. By adsorbing sublimated ferrocene onto mesoporous hollow nano-silicon spheres, and then introducing inert gas under closed conditions at a certain pressure and high temperature to decompose the ferrocene to obtain iron carbide, the iron carbide is cross-linked within the mesoporous hollow nano-silicon spheres, and then the flavors and fragrances are adsorbed onto the treated mesoporous hollow nano-silicon spheres or gel-like flavors and fragrances are filled into the treated mesoporous hollow nano-silicon spheres to obtain flavor materials. The flavor materials are more easily heated in the cigarette cartridge or filter rod, making it easier for consumers to feel the fragrance when smoking the cigarette, thereby improving the consumer experience;

[0029] 3. The prepared flavor material is mixed with expanded tobacco stem particles and carboxymethyl cellulose to prepare composite sheets or composite particles, so that the composite sheets or composite particles are easier to add to cigarette cartridges or filter rods without affecting the sustained release of flavor by the flavor material. DETAILED DESCRIPTION

[0030] The present invention will be described in detail below with reference to specific embodiments:

[0031] Example 1, Preparation of composite particles

[0032] Treatment of mesoporous hollow nano-silicon spheres: 5 parts by mass of ferrocene are placed on the bottom tray of a sealed heating container, and 4.5 parts by mass of mesoporous hollow nano-silicon spheres are placed in the sealed heating container above the ferrocene, and heated at 105°C for 3 hours. After the heating is completed, the container is first sealed and cooled for 1 hour, then opened and cooled for 0.5 hours. After the cooling is completed, the container is transferred to a closed reactor, nitrogen protective gas is introduced, and the reaction is carried out at a pressure of 1 MPa and a reaction temperature of 400°C for 8 hours to generate iron carbide from ferrocene, and the iron carbide is cross-linked in the mesoporous hollow nano-silicon spheres to obtain pretreated mesoporous hollow nano-silicon spheres;

[0033] Adsorption: 3 parts by mass of pretreated mesoporous hollow nano-silica spheres were placed in 10 parts by mass of a mixed flavor of citric acid and vanillin, and allowed to stand for 2 hours. After the standing time was complete, the mesoporous hollow nano-silica spheres with added flavors and fragrances were obtained;

[0034] Preparation of the composite flavor material: 3 parts by mass of mesoporous hollow nano-silica spheres containing flavors and fragrances were spread flatly in a container. A soybean lecithin solution was then sprayed onto the mesoporous hollow nano-silica spheres. During the spraying process, the container was rotated at a speed of 10 r / min to allow the soybean lecithin to fully coat the mesoporous hollow nano-silica spheres. After coating, the container was placed in a vacuum freeze dryer and dried at -5°C for 30 minutes. After drying, the composite flavor material was obtained. The AAS test showed a flavor loading of 72.3%.

[0035] Preparation of composite particles: Place 3 parts by mass of composite flavor material in a sealed container, rotate the sealed container at a speed of 60r / min to fully disperse the composite flavor material, place 5 parts by mass of expanded tobacco stem particles on the filling position of a vacuum filler, and then fill the dispersed composite flavor material into the expanded tobacco stem particles through a vacuum filler, add the filled expanded tobacco stem particles into 10 parts by mass of carboxymethyl cellulose solution, stir for 40 minutes, and after stirring, remove from the solution, place in a freeze dryer, and dry at -5°C for 30 minutes to obtain composite particles. The particle size of the composite particles measured by a measuring instrument is 0.5 mm.

[0036] Example 2, Preparation of Composite Sheet

[0037] Treatment of mesoporous hollow nano-silicon spheres: 5 parts by mass of ferrocene are placed on a tray at the bottom of a sealed heating container, and 6 parts by mass of mesoporous hollow nano-silicon spheres are placed in the sealed heating container above the ferrocene, and heated at 105°C for 3 hours. After the heating is completed, the container is first cooled in a sealed manner for 1 hour, then cooled with the door open for 0.5 hours. After the cooling is completed, the container is transferred to a closed reactor, nitrogen protective gas is introduced, and the reaction is carried out at a pressure of 1 MPa and a reaction temperature of 400°C for 8 hours to generate iron carbide from ferrocene, and the iron carbide is cross-linked in the mesoporous hollow nano-silicon spheres to obtain pretreated mesoporous hollow nano-silicon spheres;

[0038] Adsorption: 5 parts by weight of pretreated mesoporous hollow nano-silica spheres were placed in 15 parts by weight of a mixed flavor of citric acid and vanillin, and allowed to stand for 3.5 hours. After the standing time was complete, the mesoporous hollow nano-silica spheres with added flavors and fragrances were obtained;

[0039] Preparation of the composite flavor material: 5 parts by weight of mesoporous hollow nano-silica spheres containing flavors and fragrances were spread flatly in a container. A soybean lecithin solution was then sprayed onto the mesoporous hollow nano-silica spheres. During the spraying process, the container was rotated at 15 rpm to allow the soybean lecithin to fully coat the mesoporous hollow nano-silica spheres. After coating, the container was placed in a vacuum freeze dryer and dried at -5°C for 40 minutes. After drying, the composite flavor material was obtained. The AAS test showed a flavor loading of 75.3%.

[0040] Preparation of composite particles: Place 5 parts by mass of composite flavor material in a sealed container, rotate the sealed container at a speed of 60r / min to fully disperse the composite flavor material, place 7.5 parts by mass of expanded tobacco stem particles on the filling position of a vacuum filler, and then fill the dispersed composite flavor material into the expanded tobacco stem particles through a vacuum filler, add the filled expanded tobacco stem particles to 16 parts by mass of carboxymethyl cellulose solution, stir for 50 minutes, and after stirring, pour into a bar mold, and then place in a freeze dryer, dry at -5°C for 40 minutes to obtain a composite sheet. The thickness of the composite sheet is 1 mm when measured by a measuring instrument.

[0041] Example 3, Preparation of composite particles

[0042] Treatment of mesoporous hollow nano-silicon spheres: 9 parts by mass of ferrocene are placed on the bottom tray of a sealed heating container, and 7.5 parts by mass of mesoporous hollow nano-silicon spheres are placed in the sealed heating container above the ferrocene. The mixture is heated at 120° C. for 1 hour. After heating, the mixture is cooled in a sealed container for 0.5 hour, then cooled with the door open for 0.5 hour. After cooling, the mixture is transferred to a closed reactor, nitrogen protective gas is introduced, and the reaction is carried out at a pressure of 2 MPa and a reaction temperature of 490° C. for 4 hours to generate iron carbide from ferrocene, and the iron carbide is cross-linked in the mesoporous hollow nano-silicon spheres to obtain pretreated mesoporous hollow nano-silicon spheres.

[0043] Flavor and fragrance treatment: 10 parts by mass of citric acid and vanillin were mixed evenly, and then 13.5 parts by mass of a mixed solution of lauric acid and stearic acid was added. The mixture was stirred at a speed of 30 r / min for 40 minutes, and then transferred to a water bath shaker. The mixture was reacted at 30°C for 24 hours to obtain esterified flavor and fragrance. The esterified flavor and fragrance was then filled into the pretreated mesoporous hollow nano-silicon spheres by a vacuum filling machine while being heated.

[0044] Preparation of a composite flavor material: 5 parts by weight of mesoporous hollow nano-silica spheres containing flavors and fragrances were spread flat in a container. A soybean lecithin solution was then sprayed onto the mesoporous hollow nano-silica spheres. During the spraying process, the container was rotated at 20 r / min to allow the soybean lecithin to fully coat the mesoporous hollow nano-silica spheres. After coating, the container was placed in a vacuum freeze dryer and dried at -5°C for 40 minutes. After drying, a composite flavor material was obtained. AAS testing showed a flavor loading of 73.1%.

[0045] Preparation of composite particles: Place 5 parts by mass of composite flavor material in a sealed container, rotate the sealed container at a speed of 80r / min to fully disperse the composite flavor material, place 8 parts by mass of expanded tobacco stem particles on the filling position of a vacuum filler, and then fill the dispersed composite flavor material into the expanded tobacco stem particles through a vacuum filler, add the filled expanded tobacco stem particles into 15 parts by mass of carboxymethyl cellulose solution, stir for 50 minutes, and after stirring is completed, remove and place in a freeze dryer, dry at -5°C for 40 minutes to obtain composite particles. The particle size of the composite particles measured by a measuring instrument is 1.2 mm.

[0046] Example 4, Preparation of Composite Sheet II

[0047] Treatment of mesoporous hollow nano-silicon spheres: 10 parts by mass of ferrocene are placed on a tray at the bottom of a sealed heating container, and then 12 parts by mass of mesoporous hollow nano-silicon spheres are placed in a sealed heating container and located above the ferrocene. The mixture is heated at 120°C for 1 hour. After the heating is completed, the mixture is first cooled in a sealed container for 0.5 hours, then cooled with the door open for 0.5 hours, and then transferred to a closed reactor. Nitrogen protective gas is introduced, and the reaction is carried out at a pressure of 2 MPa and a reaction temperature of 490°C for 4 hours to generate iron carbide from ferrocene, and the iron carbide is cross-linked in the mesoporous hollow nano-silicon spheres to obtain pretreated mesoporous hollow nano-silicon spheres.

[0048] Flavor and fragrance treatment: 15 parts by mass of citric acid and vanillin were mixed evenly, and then 24 parts by mass of a mixed solution of lauric acid and stearic acid were added. The mixture was stirred at a speed of 30 r / min for 50 minutes, and then transferred to a water bath shaker. The mixture was reacted at 30°C for 24 hours to obtain esterified flavor and fragrance. The esterified flavor and fragrance was then filled into the pretreated mesoporous hollow nano-silicon spheres by a vacuum filling machine while being heated.

[0049] Preparation of a composite flavor material: 10 parts by weight of mesoporous hollow nano-silica spheres containing flavors and fragrances were spread flat in a container. A soybean lecithin solution was then sprayed onto the mesoporous hollow nano-silica spheres. During the spraying process, the container was rotated at 30 r / min to allow the soybean lecithin to fully coat the mesoporous hollow nano-silica spheres. After coating, the container was placed in a vacuum freeze dryer and dried at -5°C for 50 minutes. After drying, a composite flavor material was obtained. The AAS test showed a flavor loading of 76.8%.

[0050] Preparation of composite particles: Place 10 parts by mass of composite flavor material in a sealed container, rotate the sealed container at a speed of 85r / min to fully disperse the composite flavor material, place 14 parts by mass of expanded tobacco stem particles on the filling position of a vacuum filler, and then fill the dispersed composite flavor material into the expanded tobacco stem particles through a vacuum filler, add the filled expanded tobacco stem particles into 22 parts by mass of carboxymethyl cellulose solution, stir for 65 minutes, and after stirring, pour into a bar mold, and then place in a freeze dryer, dry at -5°C for 55 minutes to obtain a composite sheet. The thickness of the composite sheet is 2 mm as measured by a measuring instrument.

[0051] Example 5, Preparation of composite particles

[0052] Adsorption: 10 parts by mass of mesoporous hollow nano-silica spheres are placed in a mixed solution of 20 parts by mass of citric acid and vanillin, and allowed to stand for 5 hours. After the standing is completed, the mesoporous hollow nano-silica spheres with added flavors and fragrances are obtained and set aside;

[0053] Preparation of a composite flavor material: 10 parts by weight of flavor-added mesoporous hollow nano-silicon spheres were spread flatly in a container. A soybean lecithin solution was sprayed on the container. During the spraying process, the container was rotated at 20 r / min to evenly coat the mesoporous hollow nano-silicon spheres with the soybean lecithin. The container was then placed in a freeze dryer and dried at -5°C for 45 minutes to obtain a composite flavor material. AAS testing showed a flavor loading of 68.8%.

[0054] Preparation of composite particles: Place 10 parts by mass of composite flavor material in a sealed container, rotate the sealed container at a speed of 85r / min to fully disperse the composite flavor material, place 16 parts by mass of expanded tobacco stem particles on the filling position of a vacuum filler, and then fill the dispersed composite flavor material into the expanded tobacco stem particles through a vacuum filler, add the filled expanded tobacco stem particles into 25 parts by mass of carboxymethyl cellulose solution, stir for 70 minutes, and after stirring, remove them and place them in a freeze dryer, dry them at -5°C for 60 minutes to obtain composite particles. The particle size of the composite particles is 2 mm as measured by a measuring instrument.

[0055] Example 6, Preparation of Composite Sheet III

[0056] Adsorption: 12 parts by mass of mesoporous hollow nano-silica spheres are placed in a mixed solution of 25 parts by mass of citric acid and vanillin, and allowed to stand for 5 hours. After the standing is completed, the mesoporous hollow nano-silica spheres with added flavors and fragrances are obtained and set aside;

[0057] Preparation of the composite flavor material: 10 parts by weight of flavor-added mesoporous hollow nano-silica spheres were spread flatly in a container. A soybean lecithin solution was sprayed on the container. During the spraying process, the container was rotated at 20 r / min to evenly coat the mesoporous hollow nano-silica spheres with the soybean lecithin. The container was then placed in a freeze dryer and dried at -5°C for 50 minutes to obtain a composite flavor material. AAS testing showed a flavor loading of 70.5%.

[0058] Preparation of composite particles: Place 10 parts by mass of composite flavor material in a sealed container, rotate the sealed container at a speed of 85r / min to fully disperse the composite flavor material, place 16 parts by mass of expanded tobacco stem particles on the filling position of a vacuum filler, and then fill the dispersed composite flavor material into the expanded tobacco stem particles through a vacuum filler, add the filled expanded tobacco stem particles into 25 parts by mass of carboxymethyl cellulose solution, stir for 70 minutes, and after stirring, pour into a bar mold, and then place in a freeze dryer, dry at -5°C for 60 minutes to obtain a composite sheet. The thickness of the composite sheet is 3 mm as measured by a measuring instrument.

[0059] Example 7, Preparation of composite particles

[0060] Processing of flavors and fragrances: 5 parts by mass of citric acid and vanillin were uniformly mixed, and then 8 parts by mass of a mixed solution of lauric acid and stearic acid were added. The mixture was stirred at a speed of 20 r / min for 45 minutes, and then transferred to a water bath shaker. The mixture was reacted at 50°C for 12 hours to obtain esterified flavors and fragrances. The esterified flavors and fragrances were then filled into 5 parts by mass of mesoporous hollow nano-silicon spheres by a vacuum filling machine under heating.

[0061] Preparation of composite flavors and fragrances: 5 parts by mass of mesoporous hollow nano-silica spheres containing flavors and fragrances were spread flatly in a container. Soy lecithin solution was then sprayed onto the mesoporous hollow nano-silica spheres. During the spraying process, the container was rotated at 20 r / min to allow the soybean lecithin to fully coat the mesoporous hollow nano-silica spheres. After coating, the container was placed in a vacuum freeze dryer and dried at -5°C for 40 minutes. After drying, a composite flavor material was obtained. AAS testing showed a flavor loading of 73.4%.

[0062] Preparation of composite particles: Place 5 parts by mass of composite flavor material in a sealed container, rotate the sealed container at a speed of 80r / min to fully disperse the composite flavor material, place 8 parts by mass of expanded tobacco stem particles on the filling position of a vacuum filler, and then fill the dispersed composite flavor material into the expanded tobacco stem particles through a vacuum filler, add the filled expanded tobacco stem particles into 11 parts by mass of carboxymethyl cellulose solution, stir for 45 minutes, and after stirring is completed, remove and place in a freeze dryer, dry at -5°C for 40 minutes to obtain composite particles. The particle size of the composite particles measured by a measuring instrument is 1.5 mm.

[0063] Example 8, Preparation of Composite Sheet IV

[0064] Processing of flavors and fragrances: 5 parts by mass of citric acid and vanillin were uniformly mixed, and then 8 parts by mass of a mixed solution of lauric acid and stearic acid were added. The mixture was stirred at a speed of 20 r / min for 45 minutes, and then transferred to a water bath shaker. The mixture was reacted at 50°C for 12 hours to obtain esterified flavors and fragrances. The esterified flavors and fragrances were then filled into 5 parts by mass of mesoporous hollow nano-silicon spheres by a vacuum filling machine under heating.

[0065] Preparation of composite flavors and fragrances: 5 parts by weight of mesoporous hollow nano-silica spheres containing flavors and fragrances were spread flatly in a container. Soy lecithin solution was then sprayed onto the mesoporous hollow nano-silica spheres. During the spraying process, the container was rotated at 20 r / min to allow the soybean lecithin to fully coat the mesoporous hollow nano-silica spheres. After coating, the container was placed in a vacuum freeze dryer and dried at -5°C for 40 minutes. After drying, a composite flavor material was obtained. AAS testing showed a flavor loading of 76.1%.

[0066] Preparation of composite particles: Place 5 parts by mass of composite flavor material in a sealed container, rotate the sealed container at a speed of 80r / min to fully disperse the composite flavor material, place 8 parts by mass of expanded tobacco stem particles on the filling position of a vacuum filler, and then fill the dispersed composite flavor material into the expanded tobacco stem particles through a vacuum filler, add the filled expanded tobacco stem particles into 11 parts by mass of carboxymethyl cellulose solution, stir for 45 minutes, and after stirring, pour into a bar mold, and then place in a freeze dryer, dry at -5°C for 35 minutes to obtain a composite sheet. The thickness of the composite sheet is measured by a measuring instrument to be 2.4 mm.

[0067] The composite particles prepared in Example 1, Example 3, Example 5 and Example 7 were tested for encapsulation efficiency:

[0068] The loss rate of the flavor was tested by thermal gravimetric analysis at room temperature. The results are shown in Table 1 below:

[0069] Example 1 Example 3 Example 5 Example 7 7d 0.98% 0.97% 0.97% 0.98% 30d 1.44% 1.36% 1.50% 1.42% 60d 2.91% 2.72% 2.75% 2.98% 90d 5.78% 5.99% 6.25% 6.11% 180d 9.45% 9.36% 9.47% 9.52%

[0070] It can be seen from the data in Table 1 that the composite particles prepared in Example 1, Example 3, Example 5 and Example 7 can be more completely coated by controlling the rotation speed during the preparation process, so that the composite particles can be stored for a longer time at room temperature, the volatilization rate of the flavor material is reduced, and the storage life of the composite particles is extended.

[0071] The composite particles prepared in Examples 1, 3, 5, and 7 were added to cigarette filter rods or cigarette cartridges used in electrically heated smoking devices for sensory testing. Flavors and fragrances were added directly to cut tobacco or cigarette cartridges for comparison. The test results are shown in Table 2 below:

[0072]

[0073] The sensory data in Table 2 show that the composite particles prepared in Examples 1, 3, 5, and 7 have a richer aroma when smoked, and the aroma is delicate, soft, and non-irritating, and has a better taste. This indicates that the composite particles prepared in this solution can, on the one hand, slowly release the aroma when heated, and on the other hand, when slowly releasing the aroma, the aroma is released faster and has a better taste than existing cigarettes, which can effectively improve the consumer experience.

[0074] The composite sheets prepared in Example 2, Example 4, Example 6 and Example 8 were subjected to a thermal gravimetric test. The loss rate of the flavor was measured under normal temperature. The results are shown in Table 3 below:

[0075]

[0076] It can be seen from the data in Table 3 that the composite sheets prepared in Examples 2, 4, 6 and 8 can be stored for a longer period of time at room temperature, thereby reducing the volatilization rate of the flavor material and extending the storage life of the composite sheets.

[0077] The composite sheets prepared in Examples 2, 4, 6, and 8 were added to cigarette filter rods or tobacco cartridges used in electrically heated smoking devices, and flavors and fragrances were added directly to tobacco shreds or tobacco cartridges for comparison. The test results are shown in Table 4 below:

[0078]

[0079] It can be seen from the sensory data in Table 4 that the composite sheets prepared in Examples 2, 4, 6 and 8 have a richer aroma, a delicate and soft aroma without irritation, and a better taste when smoked, compared with ordinary tobacco or tobacco cartridges with added flavors and fragrances. Compared with the composite particles, the aroma and taste are similar, indicating that the composite sheets prepared in this scheme can, on the one hand, slowly release the aroma when heated, and on the other hand, when slowly releasing the aroma, the aroma release speed is faster and the taste is better than that of existing cigarettes, which can effectively improve the consumer experience.

[0080] The above embodiments are intended only to illustrate the technical solutions of the present invention and are not intended to limit the scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art will appreciate that the technical solutions of the present invention may be modified or replaced with equivalents without departing from the spirit and scope of the technical solutions of the present invention, and such modifications or equivalents shall be encompassed by the claims of the present invention. Any techniques, shapes, and structures not described in detail herein are well known.

Claims

1. A method for preparing a sustained-release flavor material, characterized in that: The following steps are involved: S1 adsorption: placing the mesoporous hollow nano-silicon spheres in the flavor and fragrance solution and letting it stand for 2-5 hours. After the standing is completed, the mesoporous hollow nano-silicon spheres with added flavor and fragrance are obtained and set aside; In the step S1, before placing the mesoporous hollow nano-silicon spheres in the flavor and fragrance solution, the following steps are also included: placing the mesoporous hollow nano-silicon spheres in a sealed heating container, placing ferrocene below the mesoporous hollow nano-silicon spheres, heating at 105-120° C. for 1-3 hours, cooling after heating, transferring the container to a sealed reactor, and introducing an inert protective gas under a certain pressure for a reaction of 4-8 hours to obtain pretreated mesoporous hollow nano-silicon spheres; During the reaction in the closed reactor, the inert protective gas is nitrogen, the nitrogen introduction pressure is 1-2 MPa, and the reaction temperature is 400-550°C; S2 Preparation of composite flavor material: The mesoporous hollow nano-silicon spheres treated in step S1 are wrapped with a coating layer. After the coating is completed, they are dried under low temperature conditions to obtain a composite flavor material.

2. The method for preparing a sustained-release flavor material according to claim 1, characterized in that: The step S1 further includes placing flavors and fragrances in a mixed solution of lauric acid and stearic acid, stirring evenly, transferring the mixture to a water bath shaker, and reacting for 12-24 hours to obtain esterified flavors and fragrances.

3. The method for preparing a sustained-release flavor material according to claim 2, characterized in that: The step S1 further includes the following steps: injecting the lipidated flavors and fragrances into the mesoporous hollow nano-silicon spheres by heating and vacuum infusion.

4. The method for preparing a sustained-release flavor material according to claim 1, characterized in that: In the step S1, the flavor is one of citric acid, vanillin, theobroma cacao, butyrylberry ketone and pyroacetic acid lactone.

5. The method for preparing a sustained-release flavor material according to claim 1, characterized in that: In the step S1, the coating layer is a thermosensitive liposome, and the thermosensitive liposome is one of lecithin compounds or plant wax.

6. An application of a sustained-release flavor material, characterized in that: The invention relates to a sustained-release flavor material prepared by the method for preparing a sustained-release flavor material according to any one of claims 1 to 5, wherein the sustained-release flavor material is applied to a cigarette cartridge or a filter rod of an electrically heated or electromagnetically heated smoking device.

7. The use of a sustained-release flavor material according to claim 6, characterized in that: The process of applying the sustained-release flavor material to the cigarette cartridge or filter rod of the electrically heated smoking device also includes the following steps: uniformly dispersing the sustained-release flavor material particles, pouring the dispersed sustained-release flavor material into expanded tobacco stem particles through vacuum filling, transferring the filled expanded tobacco stem particles into a container, adding a carboxymethyl cellulose solution, and continuing to stir for 40-60 minutes. After the stirring is completed, preparing them into thin sheets or particles, and freeze-drying them to obtain composite thin sheets or composite particles.

8. The use of a sustained-release flavor material according to claim 7, characterized in that: The thickness of the composite sheet is 1-3 mm, and the particle size of the composite particles is 0.5-2 mm.

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