Temperature-sensitive phase-change reversible perfume capsule and application thereof

Abstract

The invention discloses a temperature-sensitive phase-change reversible perfume capsule and application thereof. The perfume capsule comprises a synergistic system consisting of a phase-change medium and an essence liquid mixture, the phase change medium comprises polycaprolactone; the essence liquid mixture comprises caprylic capric triglyceride and an essence material; the essence material comprises one or more of ethyl acetate, ethyl butyrate, ethyl hexanoate, allyl hexanoate, allyl heptanoate, benzyl alcohol, limonene, furanone and maltol; the synergetic system is in a gel state at room temperature, and when the synergetic system is heated to 45 DEG C or above, the synergetic system is converted from the gel state to a liquid state within 1-3 minutes. According to the invention, the purposes of solid storage at normal temperature and liquid release at suction temperature are achieved.

Description

Technical Field

[0001] This patent belongs to the field of cigarette flavoring technology, specifically relating to a temperature-sensitive phase change reversible flavoring capsule and its application. Background Technology

[0002] Flavorings and fragrances in cigarettes can mask tobacco defects, improve aroma and taste, enhance the physical properties of tobacco, and give cigarettes a unique flavor and style, thus differentiating their quality. Maintaining a stable aroma quality in cigarettes has a significant impact on the formation of cigarette style and quality. Currently, flavor enhancement is mainly achieved by directly adding flavor capsules to cigarette filters.

[0003] Traditional flavor capsules have the following problems: liquid flavorings are prone to volatilization and migration during storage, resulting in a weaker aroma in cigarettes and large batch-to-batch differences; solid flavorings (such as powders and granules) have a slow release rate and poor aroma layering when smoking; existing phase change materials in the flavoring field mostly focus on slow release and have not achieved a reversible design of "solid aroma locking during storage and liquid aroma release during use".

[0004] During long-term storage and transportation, even with encapsulation materials, small-molecule flavoring substances can still slowly permeate, migrate, or diffuse through the gaps in the polymer chains, leading to weakened aroma, cross-contamination, or packaging contamination. Therefore, there is a need for a cigarette flavoring that can be stored in a solid state at room temperature and released in a liquid state at smoking temperatures. Summary of the Invention

[0005] The purpose of this patent is to provide a temperature-sensitive phase-change reversible flavor capsule and its application, so as to achieve solid storage at room temperature and liquid release at suction temperature.

[0006] To solve the above-mentioned technical problems, this patent adopts the following technical solution:

[0007] A temperature-sensitive, phase-change reversible fragrance capsule, the fragrance capsule comprising a synergistic system composed of a phase-change medium and a liquid mixture of fragrance;

[0008] Phase change media include polycaprolactone;

[0009] The liquid flavoring mixture includes caprylic / capric triglyceride and flavoring materials;

[0010] The flavoring materials include one or more of ethyl acetate, ethyl butyrate, ethyl hexanoate, allyl hexanoate, allyl heptaate, benzyl alcohol, limonene, furanone, and maltol;

[0011] The synergistic system is in a gel state at room temperature. When the synergistic system is heated to above 45°C, it transforms from a gel state to a liquid state within 1-3 minutes.

[0012] Furthermore, the yield stress of the gel state is 30-50 Pa;

[0013] The flavoring ingredients also include linalool, menthol, and vanillin.

[0014] Furthermore, the content of each component in the fragrance material, by mass percentage, is as follows:

[0015] Ethyl acetate is 1-2%, 2-3%, or 3-4%;

[0016] Ethyl butyrate is present at concentrations of 0.4-0.5%, 0.5-0.6%, 0.6-0.7%, or 0.7-0.9%.

[0017] Ethyl hexanoate is present at concentrations of 0.4-0.5%, 0.5-0.6%, 0.6-0.7%, or 0.7-0.9%.

[0018] Allyl hexanoate is present at 2-3%, 3-4%, or 4-5%;

[0019] Allyl heptaate is present at concentrations of 1.0-1.2%, 1.2-1.4%, 1.4-1.6%, 1.6-1.8%, or 1.8-2.0%.

[0020] Benzyl alcohol is 2-3%, 3-4%, or 4-5%;

[0021] Limonene content was 1.0-1.2%, 1.2-1.4%, 1.4-1.6%, 1.6-1.8%, or 1.8-2.0%.

[0022] Linalool is present at concentrations of 1.0-1.2%, 1.2-1.4%, 1.4-1.6%, 1.6-1.8%, or 1.8-2.0%.

[0023] The furanone content is 0.2-0.3%, 0.3-0.4%, 0.4-0.5%, or 0.5-0.6%;

[0024] Menthol content is 7-9%, 9-10%, 10-11%, or 11-12%;

[0025] Vanillin content is 2.0-2.2%, 2.2-2.4%, 2.4-2.6%, 2.6-2.8%, or 2.8-3.0%;

[0026] Maltol content is 2.0-2.2%, 2.2-2.4%, 2.4-2.6%, 2.6-2.8%, or 2.8-3.0%;

[0027] Caprylic / capric triglycerides are 60-65%, 65-70%, 70-75%, or 75-80%.

[0028] Furthermore, the flavor capsule also includes a support layer.

[0029] The support layer material is polylactic acid;

[0030] The phase change medium is bonded to the forming paper to form an encapsulation layer;

[0031] The fragrance material is contained in the support layer and can contact the phase change medium of the encapsulation layer;

[0032] The thickness of the support layer is 50-60 micrometers, 60-70 micrometers, 70-80 micrometers, or 80-100 micrometers;

[0033] The thickness of the phase change medium is 30-40 micrometers, 40-50 micrometers, or 50-60 micrometers;

[0034] Polycaprolactone has a molecular weight of 50,000-80,000.

[0035] Furthermore, the preparation method of the thermosensitive phase change reversible flavor capsule includes the following steps:

[0036] Step A: Prepare a support layer for the cavity structure, inject the liquid fragrance mixture into the cavity structure, the phase change medium in the encapsulation layer comes into contact with the liquid fragrance mixture, and the support layer and the encapsulation layer are sealed together to obtain a liquid fragrance capsule;

[0037] Step B: Incubate the liquid flavor capsules at 40-50℃ for more than 1 hour to activate them, thereby obtaining flavor capsules with a synergistic system.

[0038] Furthermore, step A includes the following steps:

[0039] Step A1: Place polylactic acid material into a mold and hot press to prepare a cavity structure. The hot pressing temperature is 80-110℃ and the hot pressing time is 1-3 seconds. Leave a liquid injection port.

[0040] Step A2: The phase change medium and the forming paper are bonded together by hot pressing at 60-90℃ to form a wrapping layer;

[0041] Step A3: Inject the liquid fragrance mixture into the cavity structure through the injection port, and heat-press the side of the encapsulation layer with the phase change medium close to the injection port to the support layer to obtain a liquid fragrance capsule.

[0042] Furthermore, in step A1, the volume of the cavity structure is 15-25 microliters.

[0043] In step A3, the temperature for hot pressing and sealing is 80-90℃.

[0044] The hot-press sealing time is 1-3 seconds.

[0045] Furthermore, step B includes the following steps:

[0046] Step B1: Incubate the liquid flavor capsules in an oven at 40-50℃ for at least 1 hour to activate them;

[0047] Step B2: Cool the activated sample to room temperature and store the synergistic system in a gel state in the cavity structure.

[0048] Furthermore, in step B2, the room temperature is below 30°C.

[0049] This patent also provides an aerosol-generating article, which includes any of the above-mentioned temperature-sensitive phase-change reversible flavor capsules.

[0050] Aerosol-generating articles are smoking articles, including aerosol-forming matrix, which generates aerosols through heating that can be directly inhaled into the lungs of a user through their mouth.

[0051] Preferably, the aerosol forming matrix is ​​a solid aerosol forming matrix.

[0052] The solid aerosol forming matrix may include one or more of the following: powder, granules, pellets, fragments, strips, bars or sheets, and may contain one or more of the following: herbaceous plant leaves, tobacco leaves, tobacco ribs, flat tobacco and homogenized tobacco.

[0053] Alternatively, the solid aerosol forming matrix may contain tobacco volatile aromatic compounds or non-tobacco volatile aromatic compounds released when the solid aerosol forming matrix is ​​heated. The solid aerosol forming matrix may also contain one or more flavor capsules of this patent, and the flavor capsules may melt and release flavoring materials during heating of the solid aerosol forming matrix.

[0054] In this patent, homogeneous tobacco material refers to a material formed by aggregating particulate tobacco.

[0055] In this patent, sheet refers to a layered element having a width and length substantially greater than its thickness.

[0056] Aerosol-generated products can have the shape of traditional cigarettes. Cigarette-like cigarette products and their specifications are usually named according to the length of the cigarette, as described below. "Standard" typically refers to cigarettes in the range of 68mm to 75mm, for example, approximately 68mm to 72mm in length; "short" or "mini" refers to cigarettes shorter than 68mm; "extra-standard" typically refers to cigarettes in the range of 75mm to 91mm, for example, approximately 79mm to 88mm in length; "long" or "extra-long" typically refers to cigarettes in the range of 91mm to 105mm, for example, approximately 94mm to 101mm in length; and "extra-long" typically refers to cigarettes in the range of approximately 110mm to 121mm in length. Additionally, cigarette products are named according to the outer circumference of the cigarette, as described below. The terms "standard" and "extra-fine" refer to cigarettes with a circumference of approximately 23mm to 25mm; "coarse" refers to cigarettes with a circumference of more than 25mm; "fine" refers to cigarettes with a circumference of approximately 22mm to 23mm; "long and thin" refers to cigarettes with a circumference of approximately 19mm to 22mm; "extra-fine" refers to cigarettes with a circumference of approximately 16mm to 19mm; and "micro-fine" refers to cigarettes with a circumference of less than 16mm. Therefore, extra-standard and extra-fine cigarettes have, for example, a length of approximately 83mm and a circumference of approximately 17mm. Standard and extra-standard cigarettes, with a length of 75mm to 91mm and a circumference of 23mm to 25mm, are popular with many customers. Cigarette products of various sizes can also be manufactured with filters (i.e., filter segments) of different lengths. Generally, short filters are used for cigarette products with both short length and short circumference. Typically, filter tip lengths range from 15mm, used with "short" and "standard" cigarettes, to 30mm, used with "extra long" and "extra thin" cigarettes. The tipping paper in the longitudinal direction of the cigarette with a filter tip is, for example, 3mm to 10mm longer than the filter tip.

[0057] Preferably, the aerosol forming article includes an aerosol forming matrix, a support element, an aerosol cooling element, and a filter nozzle.

[0058] Preferably, the aerosol forming matrix, support element, aerosol cooling element, and filter nozzle are generally cylindrical and have substantially similar outer diameters. For example, they have an outer diameter of at least 5 mm. Preferably, they have an outer diameter between about 5 mm and about 12 mm, for example, between about 5 mm and about 10 mm, or between about 6 mm and about 8 mm.

[0059] The support element can be located directly downstream of the aerosol forming matrix and can be close to the aerosol forming matrix.

[0060] The support element can be formed from any suitable material or combination of materials. For example, the support element can be formed from one or more materials selected from the group consisting of: cellulose acetate; paperboard; crimped paper, such as crimped heat-resistant paper or crimped parchment; and polymeric materials, such as low-density polyethylene (LDPE). In a preferred embodiment, the support element is formed from cellulose acetate.

[0061] The support element may include a hollow tubular element. In a preferred embodiment, the support element includes a cellulose acetate tube.

[0062] The support element can have a length between approximately 5 mm and approximately 15 mm. In a preferred embodiment, the support element has a length of approximately 8 mm.

[0063] The aerosol cooling element can be located downstream of the aerosol forming matrix. For example, the aerosol cooling element can be located directly downstream of and adjacent to the support element. Alternatively, the aerosol cooling element can be located between the support element and a filter nozzle, which is located at the downstream end of the aerosol-generating article.

[0064] Preferably, the aerosol cooling element has low suction resistance. That is, preferably, the aerosol cooling element provides low resistance to air passing through the aerosol-generated article. Preferably, the aerosol cooling element has virtually no impact on the suction resistance of the aerosol-generated article.

[0065] The aerosol cooling element may include multiple longitudinally extending channels. These multiple longitudinally extending channels may be defined by a sheet material that has undergone one or more of curling, pleating, gathering, and folding to form the channels. Alternatively, the multiple longitudinally extending channels may be defined by a single sheet that has undergone one or more of curling, pleating, gathering, and folding to form multiple channels.

[0066] In some embodiments, the aerosol cooling element may include an aggregate sheet of material selected from the group consisting of: metal foil, polymeric materials, and substantially non-porous paper or paperboard. In some embodiments, the aerosol cooling element may include an aggregate sheet of material selected from the group consisting of: polyethylene (PE), polypropylene (PP), polyvinyl chloride (PVC), polyethylene terephthalate (PET), polylactic acid (PLA), cellulose acetate (CA), and aluminum foil. In a preferred embodiment, the aerosol cooling element includes an aggregate sheet of biodegradable material. For example, an aggregate sheet of non-porous paper or an aggregate sheet of biodegradable polymeric material (such as polylactic acid).

[0067] The filter tip can be located directly downstream of and close to the aerosol cooling element. The filter tip can be formed from one or more suitable filter materials. Many such filter materials are known in the art. In one embodiment, the filter tip can be formed from cellulose acetate tow.

[0068] The filter tip can have a length between approximately 5 mm and approximately 20 mm. In a preferred embodiment, the filter tip has a length of approximately 14 mm. The filter tip can also have a length between approximately 5 mm and approximately 14 mm. In a preferred embodiment, the filter tip has a length of approximately 7 mm.

[0069] The components of the aerosol-generating article (e.g., the aerosol-forming matrix and any other components of the aerosol-generating article, such as support elements, aerosol cooling elements, and filters) are surrounded by an outer packaging. The outer packaging is formed of any suitable material or combination of materials. Preferably, the outer packaging paper is cigarette paper.

[0070] This patent provides a temperature-sensitive phase change reversible fragrance capsule and its application. It creatively discovers that after the PCL material coating layer is swollen and activated by a specific fragrance (i.e., a liquid mixture of fragrance) at a specific temperature for a period of time, it can act as a highly efficient nucleating agent for the crystallization of the contents, inducing it to form a gel or semi-solid state when cooled, thereby achieving low loss of fragrance during storage and liquid recovery during use, taking into account both storage stability and ease of use.

[0071] Meanwhile, PCL is selected as the core phase change medium for the encapsulation layer. Utilizing its reversible crystallization-melting properties at around 45℃, it crystallizes at room temperature to form a solid matrix, locking in fragrance molecules; at high temperatures (≥45℃), it melts back to a liquid state, releasing fragrance activity. The phase change temperature of PCL is adjusted by adding plasticizers to ensure crystallization and solidification within 3 hours at 45℃, followed by rapid melting upon heating, thus improving conversion sensitivity. The PLA film serves as a support layer, providing structural strength and not participating in the phase change process, preventing encapsulation collapse during the process. PCL, as an integrated encapsulation and phase change medium, achieves both thermo-sealing and liquid-solid conversion, with the dual-layer structure working together to ensure storage and usage stability.

[0072] In addition, the fragrance capsules of this patent undergo a key activation process, namely, being kept at 40-50°C for at least 1 hour to achieve stable and reversible gelation. Attached Figure Description

[0073] The above content of this patent and the following detailed embodiments will be better understood when read in conjunction with the accompanying drawings. It should be noted that the drawings are merely examples of the claimed technical solution.

[0074] Figure 1This is a schematic diagram of the thermosensitive phase change reversible flavor capsule in this patent;

[0075] Figure 2 The graph shows a comparison of the loss of flavor capsules in Example 1 and Comparative Example 1 (the numerical curve after treatment is the loss curve of the gel flavor capsules in Example 1, and the numerical curve before treatment is the loss curve of the liquid flavor capsules in Comparative Example 1).

[0076] The reference numerals in the attached figures are explained as follows:

[0077] Support layer: 10

[0078] Encapsulation layer: 20 Detailed Implementation

[0079] The detailed features and advantages of this patent are described below in the specific embodiments. The content is sufficient to enable any person skilled in the art to understand the technical content of this patent and implement it accordingly. Based on the specification, claims and drawings disclosed in this specification, a person skilled in the art can easily understand the related objectives and advantages of this patent.

[0080] This specification also uses several compound terms to describe devices, components, equipment, etc. that include more than one function, or to assign additional functions to a corresponding device, component, equipment, etc. Those skilled in the art will understand that such compound terms can be implemented by a single or multiple devices, components, equipment, etc., as long as they are reasonable under the interpretation rules of this patent terminology.

[0081] It should be noted that in this specification, similar reference numerals and letters in the following figures denote similar items; therefore, once an item is defined in one figure, it does not need to be further defined and interpreted in subsequent figures. In this specification and claims, several terms will be used, and unless otherwise indicated, these terms will be defined as having the following meanings:

[0082] The terms “comprising” or “having” have the same meaning as “containing”, and also include other forms of the term, such as the gerund and singular forms in English, meaning including but not limited to, and not intended to exclude, for example, other elements, components, integers or steps.

[0083] All other terms used herein for special definition are intended to have the general meaning understood by one of ordinary skill in the art, in particular meaning that one of ordinary skill in the art, upon reading the claims, specification and drawings of this patent, can directly and without doubt determine how the technical solution of this patent can be implemented.

[0084] Even if there are incomplete descriptions, omissions, or ambiguities in the grammar, words, punctuation, graphics, symbols, etc. of the claims, specification, and drawings of this patent, a person skilled in the art can still arrive at the only correct understanding by reading the claims, specification, and drawings as a whole without extensive reasoning or experimentation, and effectively exclude various incorrect interpretations that are not aimed at achieving the purpose of this patent.

[0085] Those skilled in the art would first choose to read the claims, specification, and drawings of this patent to reasonably interpret the terms; secondly, they would choose to refer to the relevant definitions in other documents published by the applicant before the filing date to reasonably interpret the terms; thirdly, they would choose the references cited in this patent to reasonably interpret the terms; and finally, they would choose to combine the technical dictionaries, technical manuals, reference books, textbooks, national or industry technical standards, etc., commonly used by those skilled in the art to reasonably interpret the terms.

[0086] All references cited in this application are incorporated herein by way of quotation, to the extent that they do not contradict the disclosure herein. It will be apparent to those skilled in the art that products (apparatus, components, devices, compounds, compositions, materials, etc.) and methods (processes, steps, conditions, parameters, equipment, and test methods, equipment, etc.) not specifically described herein can be applied to the implementation of the inventions fully disclosed herein without the need for excessive experimentation. This patent is intended to cover all functional equivalents known in the art of the methods, apparatus, apparatus components, materials, processes, and techniques specifically described herein. All cited references include:

[0087] The following publications are included: Marks' Standard Handbook for Mechanical Engineers (11th edition and other editions prior to this patent application date), published by McGraw-Hill, Inc.; DeGarmo's Materials and Processes in Manufacturing (13th edition and other editions prior to this patent application date), published by Wiley; Machinery's Handbook (32nd edition and other editions prior to this patent application date), published by IndustrialPress Inc.; Mechanical Design Handbook (6th edition and other editions prior to this patent application date), edited by Cheng Daxian, published by Chemical Industry Press; and Modern Mechanical Design Handbook (6th edition and other editions prior to this patent application date), edited by Wen Bangchun, published by Machinery Industry Press.

[0088] This patent will now be described with reference to the accompanying drawings, in which similar reference numerals denote similar elements. While specific structures and arrangements are discussed, it should be understood that this is done merely for illustrative purposes. Those skilled in the art will recognize that other structures and arrangements can be used without departing from the spirit and scope of this patent. It will be clear to those skilled in the art that this patent can also be used in a variety of other applications.

[0089] This patent provides a temperature-sensitive, phase-change reversible flavor capsule, the preparation method of which includes the following steps:

[0090] 1. Material preparation: PLA film with a thickness of 50-100 micrometers, PCL film with a thickness of 30-60 micrometers, PCL film with a molecular weight of 50,000-80,000, forming paper, and liquid fragrance mixture.

[0091] 2. Support layer forming: Place the PLA film into the mold, hot press at 80-110℃ for 1-3 seconds to form a rectangular closed cavity with a volume of 15-25 microliters, with a liquid injection port reserved.

[0092] 3. Coating Layer Forming: The PCL film and the forming paper are hot-pressed together at 60-90℃ to form a coating layer. The coating layer has a two-layer structure. The PCL film is placed on the upper layer near the injection port so that it can directly contact the liquid fragrance mixture. The forming paper is placed on the lower layer to cover the outside of the cavity, which can play a role in heat insulation and subsequent adsorption and slow release of fragrance.

[0093] 4. Filling and encapsulation: The liquid fragrance mixture is injected into the PLA cavity through the injection port. Then, the coating layer is heat-sealed onto the injection port and the outside of the cavity. The heat-sealing temperature is 80-90℃ and the heat-sealing time is 1-3 seconds to obtain a sealed liquid fragrance capsule.

[0094] The formulation of the fragrance liquid mixture consists of the components listed in Table 1, and each component is mixed evenly at room temperature.

[0095] Table 1: Formulation Table of Flavor Liquid Mixtures

[0096]

[0097] 5. Activation treatment: Place the sealed liquid fragrance capsules in an environment of 40-50℃ for more than 1 hour, and then place them at room temperature (below 30℃) to obtain gel-state fragrance capsules. At this time, the liquid fragrance mixture in the fragrance capsules and the phase change medium form a semi-solid or gel-state synergistic system.

[0098] This patent features a closed cavity formed by hot-pressing a polylactic acid (PLA) support layer. The cavity is filled with a liquid fragrance mixture, which is in direct contact with a phase change medium. The support layer is sealed by hot-pressing through a PCL encapsulation layer containing the phase change medium. The phase change medium is polycaprolactone (PCL) or a PCL-modified composition, with crystallization triggering conditions of at least 1 hour at 40°C-50°C and a melting temperature ≥45°C. This encapsulation structure (i.e., the synergistic system) is solid at room temperature (PCL crystallizes in the mixture), reducing volatilization and loss of fragrance during storage. When heated to above 45°C, the synergistic system gradually returns to a liquid state within 1-3 minutes, enabling the gradual release and use of the fragrance. This liquid-solid conversion process can be repeated.

[0099] The synergistic system of this patent is specifically composed of a PCL coating layer wall material and a liquid fragrance mixture after activation treatment. The fragrance contains solvents and high-melting-point crystalline components that can interact with PCL. The core mechanism of the synergistic system is the surface reconstruction and crystallization template effect of the coating layer induced by the contents. That is, after the PCL coating layer swells and is activated by the fragrance solution at a specific temperature for a period of time, it can act as a highly efficient nucleating agent for the crystallization of the contents, inducing it to form a gel or semi-solid state upon cooling. This achieves low loss of fragrance during storage and liquid recovery during use, balancing storage stability and ease of use.

[0100] Example 1

[0101] like Figure 1 As shown, this embodiment provides a temperature-sensitive phase change reversible flavor capsule, the preparation method of which includes the following steps:

[0102] 1. Material preparation: PLA film with a thickness of 100 micrometers, PCL film with a thickness of 50 micrometers, forming paper with a molecular weight of about 60,000 and a mesh count of about 8,000 for PCL film, and a liquid mixture of fragrance.

[0103] 2. Support layer forming: Place the PLA film into the mold, hot press at 100℃ for 2 seconds to form a rectangular closed cavity with a volume of 20 microliters, with a liquid injection port reserved.

[0104] 3. Coating layer forming: The PCL film and the forming paper are hot-pressed together at 80°C to form the coating layer 20. The forming paper serves to insulate heat and slow-release fragrance.

[0105] 4. Filling and encapsulation: The liquid fragrance mixture is injected into the PLA cavity through the injection port. Then, the coating layer is heat-sealed onto the injection port and the outside of the cavity. The heat-sealing temperature is 80℃ and the heat-sealing time is 3 seconds to obtain a sealed liquid fragrance capsule.

[0106] The formulation of the flavor liquid mixture consists of the components listed in Table 2.

[0107] Table 2: Formulation table of the flavor liquid mixture of Example 1

[0108]

[0109] 5. Activation Treatment: After the liquid fragrance capsules are kept in an oven at 45°C for 3 hours, they are cooled to room temperature to obtain gel-state fragrance capsules, which are sealed and protected by the support layer 10. When the gel-state fragrance capsules are reheated to 45°C, the gel formed by the synergistic system begins to melt into a liquid state, which is then adsorbed and released by the forming paper.

[0110] The synergistic system in the fragrance capsule of this embodiment was placed at room temperature (25°C) for 30 days, and the fragrance volatilization was ≤5% (the volatilization of traditional liquid encapsulation is ≥30%). After being kept at 45°C for 3 hours, the finished product after cooling to room temperature was semi-solid or gel-like. After being heated to 45°C again, it returned to liquid state within 1 minute. After repeating this process 30 times, there was no significant change in the phase change rate and fragrance retention rate.

[0111] Comparative Example 1

[0112] The difference between this comparative example and Example 1 is that the activation treatment step was not performed. The specific steps are as follows:

[0113] 1. Material preparation: PLA film with a thickness of 100 micrometers, PCL film with a thickness of 50 micrometers, forming paper with a molecular weight of about 60,000 and a mesh count of about 8,000 for PCL film, and a liquid mixture of fragrance.

[0114] 2. Support layer forming: Place the PLA film into the mold, hot press at 100℃ for 2 seconds to form a rectangular closed cavity with a volume of 20 microliters, with a liquid injection port reserved.

[0115] 3. Coating layer forming: The PCL film and the forming paper are hot-pressed together at 80°C to form a coating layer. The forming paper serves to insulate heat and slow-release fragrance.

[0116] 4. Filling and Encapsulation: The liquid fragrance mixture is injected into the PLA cavity through the injection port. The encapsulation layer is then heat-sealed onto the injection port and the outside of the cavity at 80°C for 3 seconds, resulting in a sealed liquid fragrance capsule. The liquid fragrance mixture is formulated with the components listed in Table 2.

[0117] Comparative Example 2

[0118] The difference between this comparative example and Example 1 is that the coating layer uses a PLA film. The specific steps are as follows:

[0119] 1. Material preparation: PLA film with thicknesses of 100 micrometers and 50 micrometers respectively, forming paper with a mesh count of approximately 8000, and a liquid mixture of fragrance.

[0120] 2. Support layer molding: Place a 100-micron PLA film into the mold, hot press at 100℃ for 2 seconds to form a rectangular closed cavity with a volume of 20 microliters, with a pre-reserved liquid injection port.

[0121] 3. Coating layer forming: A 50-micron PLA film and a forming paper are hot-pressed together at 80°C to form a coating layer. The forming paper serves to insulate heat and slow-release fragrance.

[0122] 4. Filling and Encapsulation: The liquid fragrance mixture is injected into the PLA cavity through the injection port. The encapsulation layer is then heat-sealed onto the injection port and the outside of the cavity at 80°C for 3 seconds, resulting in a sealed liquid fragrance capsule. The liquid fragrance mixture is formulated with the components listed in Table 2.

[0123] 5. Activation treatment: After the liquid flavor capsules are kept at 45°C in an oven for 3 hours, they are cooled to room temperature to obtain liquid flavor capsules.

[0124] Comparative Example 3

[0125] The difference between this comparative example and Example 1 lies in the formulation of the flavor liquid mixture. The specific steps are as follows:

[0126] 1. Material preparation: PLA film with a thickness of 100 micrometers, PCL film with a thickness of 50 micrometers, forming paper with a molecular weight of about 60,000 and a mesh count of about 8,000 for PCL film, and a liquid mixture of fragrance.

[0127] 2. Support layer forming: Place the PLA film into the mold, hot press at 100℃ for 2 seconds to form a rectangular closed cavity with a volume of 20 microliters, with a liquid injection port reserved.

[0128] 3. Coating layer forming: The PCL film and the forming paper are hot-pressed together at 80°C to form a coating layer. The forming paper serves to insulate heat and slow-release fragrance.

[0129] 4. Filling and encapsulation: The liquid fragrance mixture is injected into the PLA cavity through the injection port. Then, the coating layer is heat-sealed onto the injection port and the outside of the cavity. The heat-sealing temperature is 80℃ and the heat-sealing time is 3 seconds to obtain a sealed liquid fragrance capsule.

[0130] The formulation of the flavor liquid mixture in this comparative example consists of the components listed in Table 3.

[0131] Table 3: Formulation table of the flavor liquid mixture of Comparative Example 3

[0132]

[0133] 5. Activation treatment: After the liquid flavor capsules are kept at 45°C in an oven for 3 hours, they are cooled to room temperature to obtain liquid flavor capsules.

[0134] Comparative Example 4

[0135] The difference between this comparative example and Example 1 lies in the holding temperature during the activation treatment. The specific steps are as follows:

[0136] 1. Material preparation: PLA film with a thickness of 100 micrometers, PCL film with a thickness of 50 micrometers, forming paper with a molecular weight of about 60,000 and a mesh count of about 8,000 for PCL film, and a liquid mixture of fragrance.

[0137] 2. Support layer forming: Place the PLA film into the mold, hot press at 100℃ for 2 seconds to form a rectangular closed cavity with a volume of 20 microliters, with a liquid injection port reserved.

[0138] 3. Coating layer forming: The PCL film and the forming paper are hot-pressed together at 80°C to form a coating layer. The forming paper serves to insulate heat and slow-release fragrance.

[0139] 4. Filling and Encapsulation: The liquid fragrance mixture is injected into the PLA cavity through the injection port. The encapsulation layer is then heat-sealed onto the injection port and the outside of the cavity at 80°C for 3 seconds, resulting in a sealed liquid fragrance capsule. The liquid fragrance mixture is formulated with the components listed in Table 2.

[0140] 5. Activation treatment: After the liquid flavor capsules were kept at 80°C in an oven for 1 hour and then cooled to room temperature, it was found that the PCL membrane melted, the capsule structure was destroyed, and the flavor liquid mixture flowed out. The flavor capsules of this comparative example could not be used.

[0141] To further illustrate the advantages of this patent, the following tests and analyses were conducted on the spice capsules obtained in Example 1 and the spice capsules obtained in each comparative example.

[0142] 1. Physical property testing

[0143] The yield stress of the fragrance capsules of Example 1 and Comparative Examples 2-3 was tested at room temperature, and the morphology of the liquid fragrance mixture was observed. The results are shown in Table 4.

[0144] Table 4: Physical Properties Test Table of Flavor Capsules in Example 1 and Comparative Examples 2-3

[0145]

[0146] As shown in Table 4, the fragrance capsules of Example 1, under the synergistic effect of the specific formulation of the fragrance liquid mixture and the PCL material, formed a gel-like state and exhibited good yield stress. In contrast, the specific formulation of the fragrance liquid mixture in Comparative Example 2 could not synergize with the PLA material, and even after activation treatment, it could not form a gel-like state; therefore, its fragrance liquid mixture remained liquid, and its yield stress was not significantly observed. Similarly, the fragrance liquid mixture formulation of Comparative Example 3 could not synergize with the PCL material, and therefore its yield stress was also not significantly observed.

[0147] 2. Spice loss test

[0148] The gel-like fragrance capsules obtained in Example 1 and the liquid fragrance capsules obtained in Comparative Example 1 were stored at 25°C and 40-70% humidity for one month. The weight changes of the fragrance capsules were measured using a balance with an accuracy of 1 / 100,000 on days 1, 2, 3, 7, 14, and 28. The loss (mg) results are as follows: Figure 2 As shown in Table 5.

[0149] Table 5: Results of Flavor Capsule Loss in Example 1 and Comparative Example 1

[0150]

[0151] As can be seen from Table 5, the sealing performance of the unactivated fragrance capsules in Comparison 1 is significantly reduced. This is because the gel-state fragrance capsules of Example 1 have a much greater fragrance-locking ability than liquid fragrances during daily storage. Moreover, the gel-state fragrance capsules of Example 1 can revert to a liquid state within 1 minute when heated to above 45°C. The volatile effect of liquid fragrances is stronger than that of gel materials, fully leveraging the advantages of both liquid and gel materials.

[0152] The flavor capsule of Example 1 is then embedded in the filter section or the front section of the tobacco (i.e., the aerosol forming matrix) to obtain a cigarette product (i.e., an aerosol-generating product). The flavor evaporation rate is ≤5% after 30 days of storage at room temperature, and the flavor release rate is ≥80% when smoking.

[0153] The terms and expressions used in this specification are for illustrative purposes and not for limitation. Their use is not intended to exclude any equivalents of the features or portions thereof shown, but rather to facilitate the understanding that various modifications may be possible within the scope of this patent claim. Therefore, it should be understood that while this patent has been specifically disclosed through preferred embodiments, exemplary embodiments, and optional features, variations or modifications of the concepts disclosed herein may be adopted by those skilled in the art, and such variations and modifications are therefore considered to be within the scope of this patent as defined by the appended claims. The specific embodiments given in this specification are examples of useful embodiments of this patent, and it will be apparent to those skilled in the art that this patent can be implemented using many variations of the devices, device components, and method steps disclosed herein.

[0154] The foregoing description of specific embodiments fully discloses the general features of this patent, enabling others to easily modify and / or adapt such embodiments for various applications by applying knowledge within the scope of the art, without excessive experimentation or deviation from the general concept of this patent. Therefore, based on the teachings and guidance provided herein, it is intended that such modifications and alterations be included within the meaning and scope of equivalents of the disclosed embodiments. It should be understood that the wording or terminology used herein is for descriptive purposes and not intended to be limiting; thus, the wording or terminology in this specification will be interpreted by those skilled in the art based on the foregoing teachings and guidance.

[0155] Furthermore, the scope of this patent should not be limited to any of the exemplary embodiments described above, but only to the appended claims and their equivalents.

Claims

1. A temperature-sensitive phase change reversible flavor capsule, characterized in that, The fragrance capsule comprises a synergistic system consisting of a phase change medium and a liquid mixture of fragrance; The phase change medium includes polycaprolactone; The flavor liquid mixture includes caprylic / capric triglyceride and flavoring materials; The fragrance material includes one or more of ethyl acetate, ethyl butyrate, ethyl hexanoate, allyl hexanoate, allyl heptaate, benzyl alcohol, limonene, furanone, and maltol. The synergistic system is in a gel state at room temperature. When the synergistic system is heated to above 45°C, the synergistic system transforms from the gel state to the liquid state within 1-3 minutes.

2. The temperature-sensitive phase change reversible flavor capsule according to claim 1, characterized in that, The yield stress of the gel state is 30-50 Pa; The flavoring materials also include linalool, menthol, and vanillin.

3. The temperature-sensitive phase change reversible flavor capsule according to claim 2, characterized in that, The content of each component in the fragrance material, by mass percentage, is as follows: The ethyl acetate is 1-2%, 2-3%, or 3-4%; The ethyl butyrate content is 0.4-0.5%, 0.5-0.6%, 0.6-0.7%, or 0.7-0.9%. The ethyl hexanoate content is 0.4-0.5%, 0.5-0.6%, 0.6-0.7%, or 0.7-0.9%. The allyl hexanoate content is 2-3%, 3-4%, or 4-5%. The allyl heptaate is present in concentrations of 1.0-1.2%, 1.2-1.4%, 1.4-1.6%, 1.6-1.8%, or 1.8-2.0%. The benzyl alcohol content is 2-3%, 3-4%, or 4-5%. The limonene content is 1.0-1.2%, 1.2-1.4%, 1.4-1.6%, 1.6-1.8%, or 1.8-2.0%. The linalool is 1.0-1.2%, 1.2-1.4%, 1.4-1.6%, 1.6-1.8%, or 1.8-2.0%; The furanone is present at 0.2-0.3%, 0.3-0.4%, 0.4-0.5%, or 0.5-0.6%; The menthol content is 7-9%, 9-10%, 10-11%, or 11-12%; The vanillin content is 2.0-2.2%, 2.2-2.4%, 2.4-2.6%, 2.6-2.8%, or 2.8-3.0%. The maltol content is 2.0-2.2%, 2.2-2.4%, 2.4-2.6%, 2.6-2.8%, or 2.8-3.0%. The caprylic / capric glyceride is 60-65%, 65-70%, 70-75%, or 75-80%.

4. The temperature-sensitive phase change reversible flavor capsule according to claim 1, characterized in that, The spice capsule also includes a support layer. The support layer material is polylactic acid. The phase change medium is connected to the forming paper to form a wrapping layer; The fragrance material is contained in the support layer and can contact the phase change medium of the encapsulation layer; The thickness of the support layer is 50-60 micrometers, 60-70 micrometers, 70-80 micrometers, or 80-100 micrometers; The thickness of the phase change medium is 30-40 micrometers, 40-50 micrometers, or 50-60 micrometers; The molecular weight of the polycaprolactone is 50,000-80,000.

5. The temperature-sensitive phase change reversible flavor capsule according to claim 1, characterized in that, The preparation method of the thermosensitive phase change reversible flavor capsule includes the following steps: Step A: Prepare a support layer for the cavity structure, inject the liquid fragrance mixture into the cavity structure, the phase change medium in the encapsulation layer comes into contact with the liquid fragrance mixture, and the support layer and the encapsulation layer are sealed together to obtain a liquid fragrance capsule; Step B: The liquid flavor capsules are kept at 40-50°C for more than 1 hour to activate them, thereby obtaining the flavor capsules with the synergistic system.

6. The temperature-sensitive phase change reversible flavor capsule according to claim 5, characterized in that, Step A includes the following steps: Step A1: Place polylactic acid material into a mold and hot-press to prepare the cavity structure. The hot-pressing temperature is 80-110℃ and the hot-pressing time is 1-3 seconds. Leave a liquid injection port. Step A2: The phase change medium and the forming paper are hot-pressed together at 60-90°C to form an encapsulation layer; Step A3: Inject the liquid fragrance mixture into the cavity structure through the injection port, and heat-press the side of the phase change medium in the encapsulation layer close to the injection port to the support layer to obtain a liquid fragrance capsule.

7. The temperature-sensitive phase change reversible flavor capsule according to claim 6, characterized in that, In step A1, the volume of the cavity structure is 15-25 microliters. In step A3, the temperature of the hot-press sealing is 80-90℃. The hot-press sealing time is 1-3 seconds.

8. The temperature-sensitive phase change reversible flavor capsule according to claim 5, characterized in that, Step B includes the following steps: Step B1: Incubate the liquid flavor capsules in an oven at 40-50°C for at least 1 hour to perform the activation treatment; Step B2: Cool the activated sample to room temperature, and store the synergistic system in a gel state in the cavity structure.

9. The temperature-sensitive phase change reversible flavor capsule according to claim 8, characterized in that, In step B2, the room temperature is below 30°C.

10. An aerosol-generating product, characterized in that, The aerosol-generating product includes the thermosensitive phase change reversible flavor capsule as described in any one of claims 1-9.

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