Perfume sustained-release material as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of heating non-combustion cigarettes, and provides a perfume sustained-release material and a preparation method and application thereof, the perfume sustained-release material comprises the following raw materials: inorganic mineral particles, polysaccharide or modified polysaccharide, perfume and polyol; in the perfume sustained-release material, the polysaccharide or the modified polysaccharide forms a fiber net structure, the inorganic mineral particles and the perfume are adsorbed and directionally distributed in the fiber net structure under the dispersion effect of the polyhydric alcohol, and the perfume is adsorbed through the porous structure of the inorganic mineral particles, so that the perfume is released. And supermolecular forces with polysaccharides or modified polysaccharides are synergistically fixed in the porous structure. The perfume is good in adsorption controllability and high in perfume carrying amount, and has a proper slow release rate, long perfume retention time and good puff-by-puff consistency when being used for heating non-combustible cigarette products.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of heat-not-burn cigarettes, in particular to a flavor release material, a preparation method and application thereof. BACKGROUND

[0002] In the existing tobacco flavor release material technology, the mainstream methods include the following:

[0003] 1. Microcapsule technology, for example, the patent with publication number CN119549075B discloses a flavor microcapsule for heat-not-burn cigarettes, a preparation method and application thereof, including the following steps: dissolving zein in an ethanol aqueous solution to obtain a zein solution; dissolving chitosan in an acetic acid aqueous solution to obtain a chitosan solution, then adding a heterocyclic flavor, polyvinyl alcohol and an antioxidant to the chitosan solution, mixing uniformly to obtain a perfuming solution; mixing and stirring the zein solution and the perfuming solution uniformly; then cold emulsifying, freeze-drying, and obtaining the flavor microcapsule for heat-not-burn cigarettes. The preparation method can obtain a heterocyclic flavor microcapsule with good morphology, high heterocyclic flavor embedding rate and high flavor loading, which has a suitable release rate, long flavor retention time and good puff-by-puff consistency when used in heat-not-burn cigarettes; and the preparation method is simple, safe and environmentally friendly.

[0004] 2. Adsorbent technology, for example, the patent with publication number CN115364782B discloses a preparation method of a slow-release flavor material, including the following steps: S1 adsorption: placing mesoporous hollow nanometer silicon balls in a flavoring solution, standing for 2-5 hours, and obtaining mesoporous hollow nanometer silicon balls with added flavoring after standing, for standby; S2 preparation of a composite flavor material: wrapping the mesoporous hollow nanometer silicon balls treated in the S1 step with a coating layer, drying at low temperature after coating, and obtaining a composite flavor material. The purpose of the present application is to prepare the flavoring into a sheet or particle shape, which can reduce the volatilization of the flavor during storage, and can be easily added to a filter rod or a cartridge, so that the cigarette or cartridge can continuously release the flavor of the flavoring during smoking, improving the experience of consumers.

[0005] 3. Inclusion complex technology, for example, the article “Microencapsulation of Several Tobacco Flavors and Their Application in Tobacco” proposes to use β-cyclodextrin as the capsule material, to control different embedding conditions to obtain target microcapsules by taking β-phenylethanol, isovaleric acid and geranium oil as embedding objects, to determine the embedding and release by infrared analysis and thermogravimetric analysis, and to give sensory evaluation of the sample cigarettes added with the microcapsules. The results show that β-cyclodextrin has a certain embedding effect on the three kinds of tobacco flavors, and can solidify the liquid flavor and prevent the volatilization of the flavoring substances.

[0006] However, the above mainstream methods generally have the problems of single sustained release mechanism and large application limitation. These technologies rely on single mechanism such as diffusion of perfume molecules through the micropores of the wall material, physical adsorption or temperature triggered release, resulting in many performance defects: first, the perfume adsorption controllability is poor, and the initial burst phenomenon is common, and the adsorption selectivity of the carrier to polar / non-polar perfumes is poor, which easily leads to changes in aroma quality; second, the effective perfume loading capacity is limited, and the porous material is limited by the pore structure, while the microcapsule technology has the problems of low drug loading capacity and easy product pulverization; third, the sustained release rate controllability is poor, the release behavior is too sensitive to temperature, and in the like, the perfume release uniformity is poor, and the stability of each puff cannot be guaranteed; finally, the fragrance retention time is short, the traditional perfume volatility loss is serious, and the product environmental stability is poor, which is easily affected by factors such as temperature, humidity, oxygen and light, causing the aroma to deteriorate. These limitations seriously restrict the application effect of the existing technology. SUMMARY

[0007] In view of the deficiencies in the prior art, the present application provides a perfume sustained release material and its preparation method and application, which has good perfume adsorption controllability and high perfume loading capacity, has a suitable sustained release rate when used in a heat-not-burn cigarette, has a long fragrance retention time, and has good consistency in each puff.

[0008] To achieve the above and related purposes, the present application adopts the following technical means:

[0009] The first aspect of the present application provides a perfume sustained release material, the raw materials of which include inorganic mineral particles, polysaccharide or modified polysaccharide, perfume and polyol; in the perfume sustained release material, the polysaccharide or modified polysaccharide forms a fibrous network structure, the inorganic mineral particles and the perfume are adsorbed and directionally distributed in the fibrous network structure under the dispersion of the polyol, and the perfume is cooperatively fixed in the porous structure through the adsorption of the inorganic mineral particles and the supramolecular interaction between the polysaccharide or modified polysaccharide.

[0010] Further, the inorganic mineral particles are selected from one of hydroxyapatite, beta-tricalcium phosphate, montmorillonite, vermiculite and calcium silicate;

[0011] The polysaccharide or modified polysaccharide is selected from one or more of cellulose, hyaluronic acid, chitosan, sodium alginate, dextran, carrageenan, ethyl cellulose, hydroxyethyl cellulose, phosphorylated sodium alginate, carboxymethyl cellulose, dextran phosphate, carboxymethylated dextran, oxidized dextran and aminated dextran;

[0012] The perfume is selected from one or more of alcohol perfume, ester perfume, aldehyde perfume, acid perfume and terpene perfume;

[0013] The polyol is selected from one or more of propylene glycol, glycerol and butanediol.

[0014] Further, the perfume release material is in a granular structure.

[0015] Further, the perfume release material is in a filamentous structure.

[0016] The second aspect of the present application provides a method for preparing a perfume release material, comprising the following steps:

[0017] (1) preparing a first dispersion liquid with inorganic mineral particles and polyhydric alcohol as raw materials;

[0018] (2) preparing a second dispersion liquid with polysaccharide or modified polysaccharide as raw materials;

[0019] (3) adding the first dispersion liquid and perfume to the second dispersion liquid under stirring to prepare a mixed liquid;

[0020] (4) injecting the mixed liquid into a mold, drying, hot pressing, and cutting to prepare a filamentous structure of the perfume release material; or, spraying, spraying, and drying to prepare a granular structure of the perfume release material.

[0021] Further, the mass ratio of the inorganic mineral particles, polysaccharide or modified polysaccharide, perfume, and polyhydric alcohol is (30-50):(5-15):(1-10):(30-50).

[0022] Further, in step (4), the temperature of hot pressing is 40-95℃, the hot pressing pressure is 0.5-1 MPa, and the hot pressing time is 5-15 min.

[0023] The third aspect of the present application provides an application of the perfume release material, which is applied to a heat-not-burn cigarette product.

[0024] Further, the perfume release material is used by being sprayed onto the surface of tobacco sheet and tobacco shred and then added to the tobacco section of the heat-not-burn cigarette product, or mixed with granular smoking material and then added to the tobacco section of the heat-not-burn cigarette product.

[0025] Further, when the perfume release material is in a filamentous structure, it is mixed with tobacco shred and tobacco sheet filament in a certain proportion and then added to the tobacco section of the heat-not-burn cigarette product.

[0026] The beneficial technical effects of the present application are as follows:

[0027] The present application uses the fiber network structure formed by polysaccharide or modified polysaccharide to provide physical restraint for perfume, uses the porous structure of inorganic mineral particles to produce physical adsorption of perfume, and uses the supramolecular force between polysaccharide or modified polysaccharide and perfume molecules to provide chemical anchoring, thereby achieving the effect of synergistic fixation. Therefore, the perfume release material prepared by the present application has good adsorption control.

[0028] The inorganic mineral particles of this invention have high specific surface area and porous structure, which can provide a large number of adsorption sites. The fibrous network structure formed by polysaccharides or modified polysaccharides can also encapsulate fragrances. Polyols, as dispersants, are conducive to the uniform distribution of fragrances and avoid local oversaturation. Based on this, the fragrance sustained-release material prepared by this invention has a high fragrance loading capacity.

[0029] When the flavoring slow-release material of this invention is used in heated non-combustible cigarettes, the flavoring needs to overcome the adsorption force with inorganic mineral particles, the encapsulation of polysaccharide networks and supramolecular forces in sequence before it can be released. The diffusion path is complex and controlled. Therefore, it has a suitable slow-release rate and a long aroma retention time when used in heated non-combustible cigarettes.

[0030] This invention, through a stable fibrous network structure and the synergy of multiple forces, ensures that the flavoring is not rapidly depleted in the initial heating stage (the first few puffs); the dispersing effect of polyols makes the flavoring evenly distributed, which helps to ensure that each puff of smoke carries a relatively stable amount of flavoring. Therefore, it has good consistency in each puff when used for heated non-combustible cigarettes.

[0031] Furthermore, by changing the process, such as mold drying, hot pressing and slicing, and spray granulation, this invention can flexibly prepare filamentous or granular products to meet the needs of different application scenarios.

[0032] It should be understood that the above general description and the following detailed description are exemplary and explanatory only, and do not limit this application. Detailed Implementation

[0033] Unless otherwise defined, all technical and / or scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. It should be understood that certain features of the invention (described in the context of separate embodiments for clarity) may also be provided in a single embodiment. Conversely, multiple features of the invention (described in the context of a single embodiment for brevity) may also be provided separately or in any suitable combination or, where appropriate, in any other described embodiment of the invention. Certain features described in the context of various embodiments will not be considered essential features of those embodiments unless the embodiment is inoperable without those elements. The invention is further illustrated below by specific examples; however, it should be noted that the specific process conditions and results described in the embodiments of the invention are merely illustrative and should not be construed as limiting the scope of protection of the invention. All equivalent changes or modifications made in accordance with the spirit and essence of the invention should be covered within the scope of protection of the invention.

[0034] This invention provides a fragrance sustained-release material, the raw materials of which include inorganic mineral particles, polysaccharides or modified polysaccharides, fragrances, and polyols. In the fragrance sustained-release material, the polysaccharides or modified polysaccharides form a fibrous network structure. The inorganic mineral particles and fragrances are adsorbed and directionally distributed in the fibrous network structure under the dispersion effect of the polyols. The fragrances are adsorbed through the porous structure of the inorganic mineral particles and are synergistically fixed in the porous structure by the supramolecular forces between the fragrances and the polysaccharides or modified polysaccharides.

[0035] Furthermore, the inorganic mineral particles are selected from one of hydroxyapatite, β-tricalcium phosphate, montmorillonite, vermiculite, and calcium silicate;

[0036] The polysaccharide or modified polysaccharide is selected from one or more of the following: cellulose, hyaluronic acid, chitosan, sodium alginate, dextran, carrageenan, ethyl cellulose, hydroxyethyl cellulose, phosphorylated sodium alginate, carboxymethyl cellulose, dextran phosphate, carboxymethylated dextran, oxidized dextran, and aminoated dextran.

[0037] The fragrance is selected from one or more of alcohol fragrances, ester fragrances, aldehyde fragrances, acid fragrances, and terpene fragrances;

[0038] The polyol is selected from one or more of propylene glycol, glycerol, and butanediol.

[0039] Furthermore, the flavor-releasing material has a particulate structure.

[0040] Furthermore, the flavor-releasing material has a filamentous structure.

[0041] This invention also provides a method for preparing a sustained-release fragrance material, comprising the following steps:

[0042] (1) A first dispersion was prepared using inorganic mineral particles and polyols as raw materials;

[0043] (2) Prepare a second dispersion using polysaccharide or modified polysaccharide as raw material;

[0044] (3) Under stirring conditions, the first dispersion and fragrance are added to the second dispersion to obtain a mixture;

[0045] (4) Inject the mixture into a mold, dry it for 10 min to 60 min, then hot press and cut it into shreds to prepare a filamentous fragrance sustained-release material; or, spray the mixture into granules, spray it, and dry it to prepare a granular fragrance sustained-release material.

[0046] Furthermore, the mass ratio of inorganic mineral particles, polysaccharides or modified polysaccharides, fragrances, and polyols is (30~50):(5~15):(1~10):(30~50).

[0047] Furthermore, in step (4), the hot pressing temperature is 40℃~95℃, the hot pressing pressure is 0.5MPa~1MPa, and the hot pressing time is 5min~15min.

[0048] Further, in step (2), the polysaccharide or modified polysaccharide is added to an ethanol aqueous solution, wherein the volume fraction of ethanol in the ethanol aqueous solution is 65%~95%, and the mixture is stirred to obtain a second dispersion.

[0049] The present invention also provides an application of a flavoring sustained-release material, which is applied to heated non-combustible cigarette products.

[0050] Furthermore, the flavoring slow-release material is sprayed onto the surface of tobacco sheets or shredded tobacco and then added to the tobacco segment of heated tobacco products, or it is mixed with granular smoke-generating materials and then added to the tobacco segment of heated tobacco products.

[0051] Furthermore, when the flavoring slow-release material has a filamentous structure, it is mixed with tobacco shreds and tobacco sheet shreds in a certain proportion and then added to the tobacco segments of heated non-combustible cigarette products.

[0052] The present invention will be described in detail below through specific examples and embodiments. It should also be understood that the following embodiments are only for specific illustration of the present invention and should not be construed as limiting the scope of protection of the present invention. Any non-essential improvements and adjustments made by those skilled in the art based on the above description of the present invention are within the scope of protection of the present invention. The specific process parameters, etc., in the following examples are merely examples within a suitable range; that is, those skilled in the art can make appropriate selections within the appropriate range based on the description herein, and are not intended to be limited to the specific values ​​in the examples below.

[0053] Example 1

[0054] (1) At room temperature, 30g of hydroxyapatite particles and 50g of glycerol were placed in a container and stirred to obtain the first dispersion;

[0055] (2) At room temperature, 5g of ethyl cellulose was added to a 75% (v / v) aqueous ethanol solution and stirred to obtain a second dispersion;

[0056] (3) Under stirring conditions at room temperature, add the first dispersion and 2g of fragrance to the second dispersion to obtain a mixture;

[0057] (4) The mixture is injected into the mold, dried for 10 minutes, then hot-pressed and cut into filaments to prepare a filamentous fragrance sustained-release material. The hot-pressing temperature is 50℃, the hot-pressing pressure is 0.5MPa, and the hot-pressing time is 6 minutes.

[0058] Example 2

[0059] The difference between this embodiment and Embodiment 1 is that:

[0060] (4) The mixture is sprayed, granulated, and dried to prepare a granular fragrance sustained-release material.

[0061] Example 3

[0062] (1) At room temperature, 50g of vermiculite particles and 50g of glycerol were placed in a container and stirred to obtain the first dispersion;

[0063] (2) At room temperature, 5g of chitosan and 10g of hydroxyethyl cellulose were mixed and added to an aqueous ethanol solution with a volume fraction of 75%, and stirred to obtain a second dispersion.

[0064] (3) Under stirring conditions at room temperature, add the first dispersion and 5g of fragrance to the second dispersion to obtain a mixture;

[0065] (4) The mixture is injected into the mold, dried for 10 minutes, then hot-pressed and cut into filaments to prepare a filamentous fragrance slow-release material. The hot-pressing temperature is 50℃, the hot-pressing pressure is 0.5MPa, and the hot-pressing time is 10 minutes.

[0066] Example 4

[0067] (1) At room temperature, 40g of calcium silicate particles, 30g of glycerol and 20g of propylene glycol were placed in a container and stirred to obtain the first dispersion;

[0068] (2) At room temperature, 10g of dextran was added to a 75% ethanol aqueous solution and stirred to obtain a second dispersion;

[0069] (3) Under stirring conditions at room temperature, add the first dispersion and 3g of fragrance to the second dispersion to obtain a mixture;

[0070] (4) The mixture is injected into the mold, dried for 10 minutes, then hot-pressed and cut into shreds to prepare a filamentous fragrance slow-release material. The hot-pressing temperature is 50℃, the hot-pressing pressure is 1MPa, and the hot-pressing time is 10 minutes.

[0071] Comparative Example 1

[0072] (1) Mix 30g of hydroxyapatite particles with 50g of glycerol, and at the same time, dissolve 5g of ethyl cellulose in an organic solvent to form a wall material solution;

[0073] (2) 2g of fragrance is used as the core material and added to the wall material solution together with the hydroxyapatite / glycerol mixture. The emulsion is formed by high-speed stirring or homogenization.

[0074] (3) The emulsion formed is added to the coagulation bath, and ethyl cellulose is deposited and solidified on the surface of the droplets by phase separation to form microcapsules. After washing and drying, residual solvent and unreacted substances are removed, and finally dried fragrance sustained-release microcapsules are obtained.

[0075] Comparative Example 2

[0076] The difference between this comparative example and Example 1 is as follows:

[0077] (1) At room temperature, 30g of hydroxyapatite particles and 50g of aqueous solution were placed in a container and stirred to obtain the first dispersion.

[0078] Performance testing

[0079] Characteristic flavoring content in a single cigarette: The flavoring content of each example and comparative example of flavoring sustained-release materials applied to heated tobacco products was determined by puffing. Referencing ISO 20778 deep puff mode, the puff volume was 55 mL, the puff duration was 2 s, the puff interval was 30 s, and a bell flow chart was used. Particulate matter from 2 or 5 heated cigarettes was collected for each Cambridge filter. Two puffed Cambridge filters were placed in a 50 mL stoppered conical flask, and 20 mL of ethanol solution containing the internal standard was added. The mixture was shaken at room temperature for 30 min, and 2 mL of the supernatant was collected for GC / MS analysis. Each sample was measured twice in parallel, and the average value was taken as the experimental result. The results are shown in Table 1.

[0080] Thermogravimetric analysis: The flavoring sustained-release materials of each embodiment and each comparative example were applied to heated non-combustible cigarette products, and the loss rate of flavoring was tested at 40°C. The test results are shown in Table 2.

[0081] Sensory evaluation: The flavoring slow-release materials of each embodiment and each comparative example were applied to heated non-combustible cigarette products, and sensory evaluations were conducted. The evaluation scores are shown in Table 3.

[0082] The experimental data and analysis are as follows:

[0083] Table 1

[0084]

[0085] Table 2

[0086]

[0087] Table 3

[0088]

[0089] Based on the test results in Tables 1, 2, and 3, it can be seen that the method for preparing flavor sustained-release materials provided by this invention has better flavor retention and release capabilities, and when used in heated non-combustible cigarette products, the product's sensory evaluation score is higher.

[0090] The above embodiments are merely illustrative of the principles and effects of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by those skilled in the art without departing from the spirit and technical concept disclosed in the present invention should still be covered by the claims of the present invention.

Claims

1. A flavour release material characterised in that, The raw materials include inorganic mineral particles, polysaccharide or modified polysaccharide, flavor and polyhydric alcohol; in the flavor release material, the polysaccharide or modified polysaccharide forms a fiber network structure, the inorganic mineral particles and the flavor are adsorbed and directionally distributed in the fiber network structure under the dispersion of the polyhydric alcohol, and the flavor is cooperatively fixed in the porous structure of the inorganic mineral particles by adsorption and supramolecular interaction between the inorganic mineral particles and the polysaccharide or modified polysaccharide.

2. The flavor release material of claim 1, wherein, The inorganic mineral particles are selected from one of hydroxyapatite, beta-tricalcium phosphate, montmorillonite, vermiculite and calcium silicate; The polysaccharide or modified polysaccharide is selected from one or more of cellulose, hyaluronic acid, chitosan, sodium alginate, dextran, carrageenan, ethyl cellulose, hydroxyethyl cellulose, phosphorylated sodium alginate, carboxymethyl cellulose, dextran phosphate, carboxymethylated dextran, oxidized dextran and aminated dextran; The flavor is selected from one or more of alcohol flavor, ester flavor, aldehyde flavor, acid flavor and terpene flavor; The polyhydric alcohol is selected from one or more of propylene glycol, glycerol and butylene glycol.

3. The flavor release material of claim 1, wherein, The flavor release material is in a granular structure.

4. The flavor release material of claim 1, wherein, The flavor release material is in a filamentous structure.

5. A process for the preparation of a flavour release material characterised in that, The method comprises the following steps: (1) preparing a first dispersion liquid with inorganic mineral particles and polyhydric alcohol as raw materials; (2) preparing a second dispersion liquid with polysaccharide or modified polysaccharide as raw materials; (3) adding the first dispersion liquid, flavor and polyhydric alcohol to the second dispersion liquid under stirring to obtain a mixed liquid; (4) injecting the mixed liquid into a mold, drying, hot pressing and cutting to obtain a filamentous structure of the flavor release material, or spraying, spraying and drying to obtain a granular structure of the flavor release material.

6. The preparation method according to claim 5, characterized in that, The mass ratio of the inorganic mineral particles, the polysaccharide or modified polysaccharide, the flavor and the polyhydric alcohol is (30-50):(5-15):(1-10):(30-50).

7. The preparation method according to claim 5, characterized in that, In the step (4), the temperature of the hot pressing is 40-95℃, the hot pressing pressure is 0.5-1MPa, and the hot pressing time is 5-15min.

8. Use of a flavour release material, characterized in that The flavor release material is applied to a heat-not-burn cigarette product, wherein the flavor release material is the flavor release material according to any one of claims 1-4, or is prepared by the preparation method according to any one of claims 5-7.

9. Use according to claim 8, characterized in that, The flavor release material is used by being sprayed onto the surface of tobacco sheet and tobacco shred and then added to the tobacco segment of the heat-not-burn cigarette product, or mixed with granular smoking material and then added to the tobacco segment of the heat-not-burn cigarette product.

10. Use according to claim 8, characterized in that, When the flavor release material is in a filamentous structure, the flavor release material is mixed with tobacco shred and tobacco sheet filament in a certain proportion and then added to the tobacco segment of the heat-not-burn cigarette product.

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