Temperature-stimulated material, its preparation method and application in cigarette products

Abstract

The application relates to a temperature stimulus responsive material, a preparation method thereof and application thereof in a cigarette product. The temperature stimulus responsive material comprises a core and a shell material wrapping the core; the core comprises an oil-soluble aroma substance, the shell material comprises a polymer and a phase transition oil phase, the polymer comprises one or more of lacquer and polycaprolactone, and the mass-volume ratio of the polymer and the phase transition oil phase is 1 g:(0.05-3) mL. The material can realize stable loading, long-term preservation of the aroma substance in the cigarette product, and quick and controllable release in response to the heat of the smoke during smoking, so that the sensory quality and smoking experience of the cigarette are significantly improved.

Description

Technical Field

[0001] This application relates to the field of cigarette flavoring technology, and in particular to temperature-responsive materials, their preparation methods, and their application in cigarette products. Background Technology

[0002] The aroma of cigarettes is a core element determining the smoking quality of cigarettes, and a stable, uniform, and controllable aroma release effect is a key direction in cigarette product development. Currently, the main method of flavoring cigarettes relies on directly adding flavorings to the tobacco. This process is simple to operate and highly adaptable, and has been widely used in industrial production. However, it has many inherent technical defects in practical applications. In the high-temperature baking environment at the beginning of cigarette combustion and the high-temperature pyrolysis environment during combustion, tobacco flavorings are prone to complex chemical reactions such as oxidation, pyrolysis, and polymerization. This causes the effective aroma components to deteriorate and degrade, easily leading to problems such as aroma distortion, weak aroma accompanied by off-flavors, and increased irritation. At the same time, the flavoring components loaded in the tobacco are highly volatile, and a large amount is lost during cigarette storage and the initial smoking period, making it impossible to release stably throughout the entire smoking process. This results in significant differences in aroma concentration before and after smoking, obvious aroma decay with each puff, poor aroma consistency and smoking smoothness, seriously affecting the consumer's sensory experience.

[0003] To overcome the drawbacks of directly adding flavoring to tobacco, such as poor aroma stability and uncontrollable release, the industry has gradually developed flavoring technologies based on cigarette auxiliary materials. These mainly include flavoring filter rods and tipping paper, aiming to avoid the damage of flavorings caused by high combustion temperatures and achieve stable aroma release. Traditional flavoring technologies primarily involve directly spraying liquid flavorings onto the surface of tipping paper. This method is simple, inexpensive, and requires no complex modification processes. However, this method relies solely on physical adsorption to attach the flavoring, resulting in weak binding force and poor stability. The flavoring is prone to volatilization, migration, and loss during long-term storage and transportation of cigarettes, leading to poor shelf-life aroma retention and a lack of responsive aroma release performance.

[0004] Therefore, traditional technologies still need improvement. Summary of the Invention

[0005] Based on this, this application provides a temperature-responsive material, its preparation method, and its application in cigarette products. This material can achieve stable loading and long-term preservation of aroma substances in cigarettes, and can release them rapidly and controllably in response to the heat of the smoke during smoking, thereby significantly improving the sensory quality and smoking experience of cigarettes.

[0006] The specific technical solution is as follows:

[0007] One aspect of this application provides a temperature-responsive material comprising a core and a shell enclosing the core; the core comprises an oil-soluble aroma substance, and the shell comprises a polymer and a phase-inversion oil phase, wherein the polymer comprises one or more of shellac and polycaprolactone, and the mass-to-volume ratio of the polymer to the phase-inversion oil phase is 1 g: (0.05~3) mL.

[0008] In some embodiments, the mass-to-volume ratio of the polymer to the phase-transformation oil phase is 1 g: (0.2~2) mL;

[0009] And / or, the mass ratio of the oil-soluble aroma substance to the polymer is 1:0.1~40;

[0010] And / or, the melting point of the phase transformation oil phase is 40℃~60℃.

[0011] In some embodiments, the phase transformation oil phase includes one or more of paraffin wax, beeswax, and coconut oil;

[0012] And / or, the oil-soluble aroma substances include one or more of menthol, sophora japonica essential oil, rose essential oil, peppermint essential oil, jasmine essential oil, sandalwood essential oil, wintersweet essential oil, lavender essential oil, ginger essential oil, and camellia essential oil.

[0013] In some embodiments, the particle size of the temperature-responsive material is 150 nm to 1500 nm.

[0014] This application also provides a method for preparing a temperature-responsive material, comprising the following steps:

[0015] The polymer, phase-transformation oil phase, oil-soluble aroma substance, and solvent are mixed to obtain an oil phase solution;

[0016] At 65℃~85℃, the oil phase solution and the aqueous phase are mixed using microfluidic technology, and then cooled to 20℃~25℃ to induce the phase-transformation oil phase and the polymer to form a shell to encapsulate the oil-soluble aroma substance, thereby preparing a temperature-responsive material. The mass-volume ratio of the polymer and the phase-transformation oil phase is 1 g: (0.05~3) mL.

[0017] In some embodiments, the solvent includes one or more of ethanol, acetone, and tetrahydrofuran;

[0018] And / or, the concentration of the polymer in the oil phase solution is 10 mg / mL to 200 mg / mL;

[0019] And / or, the concentration of the phase-transformed oil phase in the oil phase solution is 10 μL / mL to 100 μL / mL;

[0020] And / or, the concentration of oil-soluble aroma substances in the oil phase solution is 5 mg / mL to 100 mg / mL.

[0021] In some embodiments, the mixing method includes mixing using a microfluidic mixer;

[0022] The microfluidic mixer includes an oil phase inlet channel, an aqueous phase inlet channel, a mixing chamber, and a material outlet channel. During the mixing process of the oil phase solution and the aqueous phase, the oil phase solution and the aqueous phase enter the mixing chamber tangentially through the oil phase inlet channel and the aqueous phase inlet channel, respectively. After vortex mixing in the mixing chamber, the mixture flows out through the material outlet channel.

[0023] In some embodiments, the diameter of the oil phase inlet channel is 200μm~1000μm, the diameter of the water phase inlet channel is 700μm~1300μm, and the diameter of the material outlet channel is 800μm~2000μm.

[0024] And / or, the volumetric flow rate of the oil phase solution is 20 μL / min to 900 μL / min, and the volumetric flow rate of the aqueous phase is 100 μL / min to 36000 μL / min;

[0025] And / or, the volumetric flow rate ratio of the oil phase solution to the water phase is 1:5 to 1:40.

[0026] This application also provides the application of the aforementioned temperature-responsive materials in the preparation of cigarette products.

[0027] Another aspect of this application provides a cigarette, including tobacco segments and filter segments, wherein the tobacco segments and filter segments are wrapped by tipping paper to form a cigarette; the tipping paper and / or the filter segments comprise the temperature-responsive material described above or the temperature-responsive material prepared by the method described above.

[0028] The aforementioned temperature-responsive material utilizes a core-shell structure formed by a specific polymer and a phase-transition oil phase during the phase transition process to firmly encapsulate oil-soluble aroma substances. At room temperature, the shell remains solid, effectively preventing aroma evaporation and loss. When a cigarette is smoked, the heat transfer from the smoke causes the phase-transition oil phase in the shell to melt, disrupting the shell's integrity. This allows for the rapid and targeted release of oil-soluble aroma substances when needed, significantly improving the consistency of aroma before and after smoking. Attached Figure Description

[0029] Figure 1 This is a thermogravimetric comparison diagram of the materials of Example 1 and Comparative Example 8 at 25°C.

[0030] Figure 2 This is a thermogravimetric comparison diagram of the materials of Example 1 and Comparative Example 8 at 70°C;

[0031] Figure 3 This is a differential scanning calorimetry (DSC) curve of the temperature-responsive material system of Embodiment 1 of this application. Detailed Implementation

[0032] To facilitate understanding of this application, a more complete description is provided below, along with preferred embodiments. However, this application can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a thorough and complete understanding of the disclosure of this application.

[0033] The implementation of this application will be described in detail below with reference to some implementation methods and embodiments. This embodiment is implemented based on the technical solution of this application, and provides detailed implementation methods and specific operation processes, but the protection scope of this application is not limited to the following embodiments.

[0034] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.

[0035] Unless otherwise stated or in case of contradiction, the terms or phrases used herein shall have the following meanings:

[0036] In this application, the terms "multiple" or "various" are used unless otherwise specified, referring to a quantity greater than or equal to 2. For example, "one or more" means one or more types.

[0037] In this application, terms such as "further" and "especially" are used to describe purposes and indicate differences in content, but should not be construed as limiting the scope of protection of this application.

[0038] In this application, the technical features described in an open-ended manner include both closed technical solutions consisting of the listed features and open technical solutions that include the listed features.

[0039] In this application, when numerical intervals (i.e., numerical ranges) are mentioned, unless otherwise specified, the distribution of selectable numerical values ​​within the numerical interval is considered continuous, and includes the two endpoints of the numerical interval (i.e., the minimum and maximum values), as well as every numerical value between these two endpoints. Unless otherwise specified, when a numerical interval refers only to integers within that numerical interval, including the two endpoint integers of the numerical range, as well as every integer between the two endpoints, is equivalent to directly listing every integer. When multiple numerical ranges are provided to describe features or characteristics, these numerical ranges can be merged. In other words, unless otherwise specified, the numerical ranges disclosed herein should be understood to include any and all subranges included therein. The "numerical value" in the numerical interval can be any quantitative value, such as a number, percentage, ratio, etc. The term "numerical interval" can be broadly included to include numerical interval types such as percentage intervals, ratio intervals, and proportion intervals.

[0040] In this application, unless otherwise specified, the temperature parameters are permitted to be either constant temperature treatment or variations within a certain temperature range. It should be understood that the constant temperature treatment allows temperature fluctuations within the precision range controlled by the instrument. Fluctuations are permitted within ranges such as ±5℃, ±4℃, ±3℃, ±2℃, and ±1℃.

[0041] In this application, if the unit for a data range is only followed by the right endpoint, it indicates that the units for the left and right endpoints are the same. For example, 2~5 h means that the units for the left endpoint "2" and the right endpoint "5" are both h (hours). ‰: thousands sign, indicating one-thousandth.

[0042] Traditional tipped fragrance systems lack temperature-responsive characteristics. The filter and tipped paper are located in a non-combustion zone, where fragrances tend to slowly evaporate and dissipate at room temperature. However, the hot vapor (60℃~85℃) flowing through the filter during inhalation provides a stable heat source. Traditional fragrance systems cannot utilize this temperature field to trigger fragrance release on demand, failing to achieve the effects of locking in fragrance at room temperature and releasing it during inhalation. This results in poor fragrance enhancement and an inability to effectively improve the sensory experience during inhalation.

[0043] Based on this, one embodiment of this application provides a temperature-responsive material, which includes a core and a shell enclosing the core. The core includes an oil-soluble aroma substance, and the shell includes a polymer and a phase-inversion oil phase. The polymer includes one or more of shellac and polycaprolactone. The mass-to-volume ratio of the polymer to the phase-inversion oil phase is 1 g: (0.05~3) mL. As an example, the mass ratio can be 1 g: 0.05 mL, 1 g: 0.55 mL, 1 g: 1.05 mL, 1 g: 1.55 mL, 1 g: 2.05 mL, 1 g: 2.55 mL, or 1 g: 3 mL. In some examples, it can be any two of these point values ​​forming a range, and the same applies below.

[0044] The aforementioned temperature-responsive material utilizes a core-shell structure formed by a specific polymer and a phase-transition oil phase during the phase transition process to firmly encapsulate oil-soluble aroma substances. At room temperature, the shell remains solid, effectively preventing aroma evaporation and loss. When a cigarette is smoked, the heat transfer from the smoke causes the phase-transition oil phase in the shell to melt, disrupting the shell's integrity. This allows for the rapid and targeted release of oil-soluble aroma substances when needed, significantly improving the consistency of aroma before and after smoking.

[0045] Furthermore, the temperature-responsive shell material prevents direct contact between the core oil-soluble aroma components and the tipping paper fibers, thus largely avoiding the "oil stain" problem and maintaining the original appearance of the cigarette product.

[0046] In some embodiments, the mass-to-volume ratio of the polymer to the phase-transformation oil phase is 1 g: (0.2~2) mL.

[0047] In some embodiments, the mass ratio of the oil-soluble aroma substance to the polymer is 1:0.1 to 40. For example, the mass ratio can be 1:0.1, 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, 1:16, 1:17, 1:18, 1:19, 1:20, 1:21, 1:22, 1:23, 1:24, 1:25, 1:26, 1:27, 1:28, 1:29, 1:30, 1:31, 1:32, 1:33, 1:34, 1:35, 1:36, 1:37, 1:38, 1:39, or 1:40.

[0048] In some embodiments, the melting point of the phase transformation oil phase is 40°C to 60°C.

[0049] In some embodiments, the phase transition oil phase includes one or more of paraffin wax, beeswax, and coconut oil.

[0050] In some embodiments, the oil-soluble aroma substances mentioned above include one or more of menthol, sophora japonica essential oil, rose essential oil, peppermint essential oil, jasmine essential oil, sandalwood essential oil, wintersweet essential oil, lavender essential oil, ginger essential oil, and camellia essential oil.

[0051] In some embodiments, the particle size of the temperature-responsive material is 150nm to 1500nm, for example, 150nm, 250nm, 350nm, 450nm, 550nm, 650nm, 750nm, 850nm, 950nm, 1050nm, 1150nm, 1250nm, 1350nm, 1450nm or 1500nm.

[0052] One embodiment of this application provides a method for preparing a temperature-responsive material, including the following steps S100 to S200.

[0053] Step S100: Mix the polymer, phase-transformation oil phase, oil-soluble aroma substance and solvent to obtain an oil phase solution.

[0054] In some embodiments, the above-mentioned polymer, the above-mentioned phase-transformation oil phase, the above-mentioned oil-soluble aroma substance and solvent raw material are mixed.

[0055] Step S200: At 65℃~85℃, using microfluidic technology, the above oil phase solution and aqueous phase are mixed and then cooled to 20℃~25℃ to induce the above phase-transformation oil phase and the above polymer to form a shell material to encapsulate the above oil-soluble aroma substance, thus preparing a temperature-responsive material. The mass-volume ratio of polymer to phase-transformation oil phase is 1 g: (0.05~3) mL.

[0056] In some embodiments, the above-mentioned temperature-responsive material can be prepared by this preparation method.

[0057] Understandably, this application utilizes the principle of cooling-induced phase transition to co-solidify the polymer and the phase-transformation oil phase into a dense solid shell, completely encapsulating the internal oil-soluble aroma substances. Under normal storage conditions, the solid shell can form a stable physical barrier, effectively preventing the aroma components from volatilizing and migrating outward, avoiding the loss of fragrance during long-term storage, and significantly extending the product's aroma shelf life. During cigarette smoking, the 60℃~85℃ warm smoke flowing through the filter area can trigger the melting of the phase-transformation oil phase inside the shell, destroying the integrity of the core-shell structure, achieving rapid, targeted, and explosive release of aroma substances, effectively compensating for the aroma decay defect in the later stages of smoking, solving the problem of aroma decay with each puff and large sensory differences between the beginning and end of traditional flavoring technologies, and improving the smoking stability and sensory quality of cigarettes.

[0058] In some of these embodiments, the solvents include one or more of ethanol, acetone, and tetrahydrofuran.

[0059] In some embodiments, the concentration of the polymer in the oil phase solution is 10 mg / mL to 200 mg / mL. For example, the concentration can be 10 mg / mL, 20 mg / mL, 30 mg / mL, 40 mg / mL, 50 mg / mL, 60 mg / mL, 70 mg / mL, 80 mg / mL, 90 mg / mL, 100 mg / mL, 110 mg / mL, 120 mg / mL, 130 mg / mL, 140 mg / mL, 150 mg / mL, 160 mg / mL, 170 mg / mL, 180 mg / mL, 190 mg / mL, or 200 mg / mL.

[0060] In some embodiments, the concentration of the phase-transformed oil phase in the above-mentioned oil phase solution is 10 μL / mL to 100 μL / mL. For example, the concentration can be 10 μL / mL, 20 μL / mL, 30 μL / mL, 40 μL / mL, 50 μL / mL, 60 μL / mL, 70 μL / mL, 80 μL / mL, 90 μL / mL, or 100 μL / mL.

[0061] In some embodiments, the concentration of oil-soluble aroma substances in the oil phase solution is 5 mg / mL to 100 mg / mL. For example, the concentration can be 5 mg / mL, 10 mg / mL, 15 mg / mL, 20 mg / mL, 25 mg / mL, 30 mg / mL, 35 mg / mL, 40 mg / mL, 45 mg / mL, 50 mg / mL, 55 mg / mL, 60 mg / mL, 65 mg / mL, 70 mg / mL, 75 mg / mL, 80 mg / mL, 85 mg / mL, 90 mg / mL, 95 mg / mL, or 100 mg / mL.

[0062] It is understandable that by controlling the concentrations of polymers, phase-transformation oil phases, and oil-soluble aroma substances within the above-mentioned ranges, a stable core-shell structure can be formed, which firmly encapsulates the oil-soluble aroma substances. When cigarettes are smoked, the heat transfer from the smoke causes the phase-transformation oil phase in the shell to melt, thereby achieving rapid and targeted release of the oil-soluble aroma substances when needed.

[0063] In some embodiments, the mixing method includes mixing using a microfluidic mixer.

[0064] In some embodiments, the microfluidic mixer includes a vortex micromixer or a flow-focusing micromixer.

[0065] In some embodiments, the microfluidic mixer includes an oil phase inlet channel, an aqueous phase inlet channel, a mixing chamber, and a material outlet channel. During the mixing process of the oil phase solution and the aqueous phase, the oil phase solution and the aqueous phase enter the mixing chamber tangentially through the oil phase inlet channel and the aqueous phase inlet channel, respectively. After vortex mixing in the mixing chamber, the mixture flows out through the material outlet channel.

[0066] In some embodiments, the diameter of the oil phase inlet channel is 200μm to 1000μm, the diameter of the water phase inlet channel is 700μm to 1300μm, and the diameter of the material outlet channel is 800μm to 2000μm.

[0067] In some embodiments, the volumetric flow rate of the oil phase solution is 20 μL / min to 900 μL / min, and the volumetric flow rate of the aqueous phase is 100 μL / min to 36000 μL / min. For example, the volumetric flow rate of the oil phase solution can be 20 μL / min, 70 μL / min, 120 μL / min, 170 μL / min, 220 μL / min, 270 μL / min, 320 μL / min, 370 μL / min, 420 μL / min, 470 μL / min, etc. 0μL / min, 520μL / min, 570μL / min, 620μL / min, 670μL / min, 720μL / min, 770μL / min, 820μL / min, 870μL / min or 9 00μL / min, the volume flow rate of the aqueous phase can be 100μL / min, 1000μL / min, 2000μL / min, 3000μL / min, 4000μL / min, 5000μL / min, 6000μL / min, 7000μL / min, 8000μL / min, 9000μL / min, 10000μL / min, 11000μL / min, 12000μL / min, 13000μL / min, 14000 μL / min, 15000μL / min, 16000μL / min, 17000μL / min, 18000μL / min, 19000μL / min, 20000μL / min, 21000μL / min, 22000μL / min, 23000μL / min, 24000μL / min, 25000μL / min, 26000μL / min, 27000μL / min, 28000μL / min, 29000μ L / min, 30000μL / min, 31000μL / min, 32000μL / min, 33000μL / min, 34000μL / min, 35000μL / min or 36000μL / min.

[0068] In some embodiments, the volumetric flow rate ratio of the oil phase solution to the aqueous phase is 1:5 to 1:40. For example, the volumetric flow rate ratio can be 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, 1:16, 1:17, 1:18, 1:19, 1:20, 1:21, 1:22, 1:23, 1:24, 1:25, 1:26, 1:27, 1:28, 1:29, 1:30, 1:31, 1:32, 1:33, 1:34, 1:35, 1:36, 1:37, 1:38, 1:39, or 1:40.

[0069] Understandably, the microfluidic technology described above, used to prepare temperature-responsive materials, results in high product uniformity and excellent system stability, making them suitable for stable industrial production. This application utilizes a microfluidic mixer to achieve high-temperature oil-water two-phase mixing, and relies on controllable flow channels and specific flow ratios to prepare core-shell materials with uniform particle size, good monodispersity, and stable structure. Compared to traditional emulsification processes, the microfluidic preparation process offers strong controllability and minimal batch-to-batch variation, effectively avoiding the defects of traditional encapsulated products such as uneven structure, unstable aroma release, and inconsistent quality. This provides a high-quality carrier foundation for stable, uniform, and controllable intelligent aroma enhancement in cigarettes.

[0070] Another embodiment of this application also provides the application of the above-mentioned temperature-stimulation-responsive material in the preparation of cigarette products.

[0071] Another embodiment of this application provides a splicing paper comprising the above-described temperature-responsive material.

[0072] This application completely encapsulates oil-soluble aroma substances through a core-shell solid shell, effectively isolating the core fragrance from direct contact with the cellulose paper base of the tipping paper. This avoids the problems of oil-soluble fragrance penetrating, spreading, and migrating on the paper base surface, and solves the problems of oil stains and mottled defects that are prone to occur in traditional liquid fragrance spraying processes. It fully preserves the original appearance, texture, and quality of cigarette tipping paper, and improves the market quality and visual appeal of the product.

[0073] Another embodiment of this application provides a method for preparing splicing paper, wherein the above-mentioned temperature-stimulation-responsive material is applied to the surface of a paper base to prepare splicing paper.

[0074] In some embodiments, the application method includes spraying.

[0075] In some embodiments, the amount of the temperature-responsive material added is 0.1‰ to 5‰ of the paper base weight. For example, the amount added can be 0.1‰, 0.3‰, 0.5‰, 0.7‰, 0.9‰, 1.1‰, 1.3‰, 1.5‰, 1.7‰, 1.9‰, 2.1‰, 2.3‰, 2.5‰, 2.7‰, 2.9‰, 3.1‰, 3.3‰, 3.5‰, 3.7‰, 3.9‰, 4.1‰, 4.3‰, 4.5‰, 4.7‰, or 4.9‰.

[0076] The temperature-responsive material of this application adheres to the surface of the paper base or the inside of the filter rod in the form of tiny, uniform droplets. It does not block the natural air-permeable pores of the tipping paper, and can completely preserve the original physical properties of the substrate, such as air permeability and flexibility. At the same time, it does not change the original combustion characteristics and basic smoke style of the cigarette. While achieving intelligent temperature control and aroma enhancement, it ensures the stability of the basic quality of the cigarette product and is suitable for the modification and upgrading of various specifications of cigarette products.

[0077] One embodiment of this application also provides a cigarette filter rod internally loaded with a temperature-responsive material prepared as described above; optionally, the temperature-responsive material is added to the cigarette tow.

[0078] Understandably, this application uses temperature-responsive materials as post-treatment additives, applying them directly to the surface of the tipping paper base or filter rod filament bundles. Unlike the traditional microcapsule paper base blending process, this method does not require the use of pulping, high-pressure pressing, high-temperature drying, or other harsh mechanical shearing and high-temperature-pressure processes. This avoids problems such as damage to the coating structure and premature leakage of fragrance, reduces fragrance loss during processing, effectively improves the fragrance retention rate and product qualification rate of the finished product, has strong batch production stability, and is suitable for large-scale industrial production.

[0079] Another embodiment of this application provides a cigarette, including tobacco segments and filter segments, wherein the tobacco segments and filter segments are wrapped with tipping paper to form a cigarette, and the tipping paper and / or filter segments include the temperature-responsive material described above or a temperature-responsive material prepared by the method for preparing the temperature-responsive material described above.

[0080] This application utilizes specific temperature-responsive materials to achieve temperature-responsive aroma release in cigarette tipping paper and filter rod substrates. It effectively balances the core technical contradictions of flavor processing stability, storage stability, room temperature aroma retention, and precise aroma release during smoking, overcoming many bottlenecks of traditional cigarette flavoring technology. It has significant application value for the research and industrialization of high-quality flavored cigarettes.

[0081] To make the objectives, technical solutions, and advantages of this application clearer and more concise, the following specific embodiments are used for illustration, but this application is by no means limited to these embodiments. The embodiments described below are merely preferred embodiments of this application and can be used to describe this application, but should not be construed as limiting the scope of this application. It should be noted that any modifications, equivalent substitutions, and improvements made within the spirit and principles of this application should be included within the protection scope of this application.

[0082] To better illustrate this application, the following description, in conjunction with embodiments, further explains the content of this application.

[0083] Example 1

[0084] I. Preparation of Temperature-Responsive Materials

[0085] (1) Measure 100 mL of anhydrous ethanol into a sealed container, heat it in a water bath to 65°C and keep it at a constant temperature. While stirring continuously, add 5.0 g of shellac to the above anhydrous ethanol and stir until completely dissolved. Then, add 5.0 mL of beeswax (phase transformation oil phase) and 1.0 g of menthol (oil-soluble aroma substance) to the solution and continue stirring at 65°C for 30 minutes until the system is clear and homogeneous, and obtain an oil phase solution.

[0086] (2) The above oil phase solution and ultrapure water are delivered by two independent high-precision injection pumps. Before entering the microfluidic mixer, the two phase fluids are maintained at (65±2)℃ by a preheating module. The microfluidic mixer used is a vortex structure with an oil phase inlet diameter of 300μm, a water phase inlet diameter of 1100μm, a cylindrical mixing chamber diameter of 6mm, and an outlet diameter of 1600μm. The total injection flow rate of the oil phase solution is set to 800μL / min, and the total injection flow rate of the water phase is set to 25mL / min (the oil-water volume flow rate ratio is about 1:31). The two phases are rapidly and fully mixed in the microfluidic mixer at 65℃ to form a primary emulsion.

[0087] (3) Collect the outflowing primary emulsion and cool it to below 25°C. The shellac and paraffin precipitate together and form a solid shell, finally obtaining a milky white temperature-responsive material with a core-shell structure containing menthol, with a particle size of 155 nm.

[0088] II. Application of Temperature-Responsive Materials in Cigarette Products

[0089] The collected temperature-responsive material was evenly coated onto the surface of the tipping paper base at a dosage of 1‰, ensuring a uniform and liquid-free coating. The coated tipping paper was then placed in a 30°C forced-air oven for 30 minutes to remove residual moisture and ethanol, yielding the peppermint-scented tipping paper.

[0090] Example 2

[0091] The preparation methods of temperature-responsive materials in Example 2 and Example 1 are basically the same, except that the oil-soluble aroma substance used in step (1) is a compound of Sophora japonica essential oil and jasmine essential oil (mass ratio of 1:1), and its total addition amount is consistent with the mass-volume ratio of menthol in Example 1.

[0092] All other steps and parameters are the same as in Example 1.

[0093] Example 3

[0094] The preparation method of the temperature-responsive material in Example 3 is basically the same as that in Example 1, except that the concentration of shellac in the oil phase solution is adjusted to 100 mg / mL in step (1).

[0095] All other steps and parameters are the same as in Example 1.

[0096] Example 4

[0097] The preparation method of the temperature-responsive material in Example 4 is basically the same as that in Example 1, except that the concentration of menthol in the oil phase solution is adjusted to 20 mg / mL in step (1).

[0098] All other steps and parameters are the same as in Example 1.

[0099] Example 5

[0100] The preparation method of the temperature-stimulated responsive material in Example 5 is basically the same as that in Example 1. The difference is that the total flow rate of the oil phase solution and the water phase in step (2) is different. The total flow rate of the oil phase solution is set to 800 μL / min and the total flow rate of the water phase is 4 mL / min (the oil-water volume flow rate ratio is about 1:5).

[0101] All other steps and parameters are the same as in Example 1.

[0102] Example 6

[0103] The preparation method of the temperature-stimulated responsive material in Example 6 is basically the same as that in Example 1. The difference is that the total flow rate of the oil phase solution and the water phase in step (2) is different. The total flow rate of the oil phase solution is set to 800 μL / min and the total flow rate of the water phase is 32 mL / min (the oil-water volume flow rate ratio is about 1:40).

[0104] All other steps and parameters are the same as in Example 1.

[0105] Example 7

[0106] The preparation method of the temperature-responsive material in Example 7 is basically the same as that in Example 1, except that the amount of shellac added in step (1) is different. Under continuous stirring, 2.5 grams of shellac are added to ethanol and stirred until completely dissolved.

[0107] All other steps and parameters are the same as in Example 1.

[0108] Example 8

[0109] The preparation method of the temperature-stimulated responsive material in Example 8 is basically the same as that in Example 1, except that the amount of beeswax added in step (1) is different. 1.0 mL of beeswax (phase transformation oil phase) and 1.0 g of menthol (oil-soluble aroma substance) are added to the solution and stirred at 65°C for 30 minutes until the system is clear and uniform, and an oil phase mixed solution is obtained.

[0110] All other steps and parameters are the same as in Example 1.

[0111] Example 9

[0112] The preparation method of the temperature-stimulated responsive material in Example 9 is basically the same as that in Example 1, except that the amount of beeswax added in step (1) is different. 10.0 mL of beeswax (phase transformation oil phase) and 1.0 g of menthol (oil-soluble aroma substance) are added to the solution and stirred at 65°C for 30 minutes until the system is clear and uniform, and an oil phase mixed solution is obtained.

[0113] All other steps and parameters are the same as in Example 1.

[0114] Example 10

[0115] The preparation method of the temperature-stimulated responsive material in Example 10 is basically the same as that in Example 1, except that the amount of menthol added in step (1) is different. 5.0 mL of beeswax (phase transformation oil phase) and 0.5 g of menthol (oil-soluble aroma substance) are added to the solution, and the mixture is stirred at 65°C for 30 minutes until the system is clear and uniform, and an oil phase mixed solution is obtained.

[0116] All other steps and parameters are the same as in Example 1.

[0117] Example 11

[0118] The preparation method of the temperature-stimulated responsive material in Example 11 is basically the same as that in Example 1, except that the amount of menthol added in step (1) is different. 5.0 mL of beeswax (phase transformation oil phase) and 10 g of menthol (oil-soluble aroma substance) are added to the solution and stirred at 65°C for 30 minutes until the system is clear and uniform, and an oil phase mixed solution is obtained.

[0119] All other steps and parameters are the same as in Example 1.

[0120] Comparative Example 1

[0121] The difference between Comparative Example 1 and Example 1 is that the microfluidic mixing step in step (2) is omitted.

[0122] Specifically, the 65°C oil phase mixed solution prepared in step (1) was quickly poured into 25 mL of pure water at the same temperature under high-speed magnetic stirring (1000 rpm), and then cooled and dried in the same manner as in Example 1.

[0123] Comparative Example 2

[0124] The difference between Comparative Example 2 and Example 1 is that in step (1), the phase-transformation oil phase paraffin is replaced with corn oil which does not have phase-transformation properties.

[0125] All other steps and parameters are the same as in Example 1.

[0126] Comparative Example 3

[0127] Comparative Example 3 is a control of the conventional method. The same amount of menthol as in Example 1 was directly dissolved in a small amount of ethanol and sprayed directly onto the same type of tipping paper, with the total amount sprayed being the same as in Example 1.

[0128] Comparative Example 4

[0129] The difference between Comparative Example 4 and Example 1 is that the total flow rates of the oil phase solution and the water phase are different in step (2). The total flow rate of the oil phase solution is set to 800 μL / min, and the total flow rate of the water phase is set to 1.6 mL / min (the oil-water volume flow rate ratio is about 1:2).

[0130] All other steps and parameters are the same as in Example 1.

[0131] Comparative Example 5

[0132] The difference between Comparative Example 5 and Example 1 is that the amount of beeswax added in step (1) is different. 16.0 mL of beeswax and 1.0 g of menthol (an oil-soluble aroma substance) are added to the solution and stirred at 65°C for 40 minutes (the stirring time needs to be extended if there is too much beeswax). A small amount of undissolved beeswax particles still exist in the system, and an oil phase solution is barely obtained.

[0133] All other steps and parameters are the same as in Example 1.

[0134] Comparative Example 6

[0135] The difference between Comparative Example 6 and Example 1 is that the type of polymer in step (1) is different. 5.0 g of polylactic acid (PLA) was added to ethanol under continuous stirring and stirred until completely dissolved.

[0136] All other steps and parameters are the same as in Example 1.

[0137] Comparative Example 7

[0138] The specific preparation steps for Comparative Example 7 are as follows:

[0139] (1) Add 5.0 g of gelatin to 15 mL of pure water (mass-volume ratio of 1:3) and dissolve it completely under ultrasonic conditions (power 150 W, frequency 40 kHz) to obtain a gelatin solution;

[0140] (2) Heat 15.0 g of paraffin (melting point about 50°C) to melt, then add 2.0 g of menthol and 0.08 g of Tween-80 (emulsifier), mix evenly to form an oil phase (at this time, the mass ratio of gelatin to paraffin is 1:3).

[0141] (3) The oil phase and gelatin solution are mixed at a high speed of 1000 rpm by magnetic stirring until the solid and liquid phases are completely fused; then the mixture is cooled and cured in water at 25°C for 10 minutes.

[0142] Subsequently, the collected materials were applied to the surface of the tipping paper in the same amount and coating method as in Example 1 to obtain mint-scented tipping paper.

[0143] All other steps and parameters are the same as in Example 1.

[0144] Comparative Example 8

[0145] The difference between Comparative Example 8 and Example 1 is that in step (1), the phase transformation oil phase paraffin is replaced with non-phase transformation oil (safflower seed oil).

[0146] All other steps and parameters are the same as in Example 1.

[0147] test:

[0148] 1. To verify the temperature-responsive release characteristics of phase-change oil relative to temperature-stimulated materials in cigarettes, thermogravimetric analysis (TGA) was performed on materials prepared from the phase-change oil phase (beeswax) of Example 1 and the non-phase-change oil (safflower seed oil) of Comparative Example 8. Specifically, the materials prepared in Example 1 and Comparative Example 8 were freeze-dried, and then the ambient temperature of cigarettes under different conditions was simulated using a thermogravimetric analyzer.

[0149] Storage at room temperature (25℃): To examine the stability of the packaging.

[0150] Filter rod / tip paper heating state (70℃): Simulates the temperature rise environment of flue gas passing through the filter and tip paper during suction (non-combustion zone).

[0151] To further verify the phase transition behavior of the temperature-responsive material system of this application within the cigarette smoking temperature range, differential scanning calorimetry (DSC) was used to perform thermal analysis on the temperature-responsive material prepared in Example 1.

[0152] 2. Sensory evaluation was conducted on the temperature-responsive materials prepared in the above embodiments and comparative examples. The sensory quality evaluation standard referred to the national standard GB 5606.4-2005. The specific method was as follows: the tipping paper with the above temperature-responsive material was applied to the cigarette product, and then sealed and stored for 30 days before being evaluated. The results are shown in Table 1 below.

[0153] Table 1

[0154]

[0155] Note: The scores in parentheses are the maximum scores for each indicator.

[0156] Test results are as follows Figure 1 , Figure 2 As shown: Figure 1 (25℃): At room temperature, the mass loss rates of Example 1 and Comparative Example 8 were both extremely low and showed no significant difference. This indicates that before reaching the phase transition temperature, both the solid shell composed of shellac / beeswax and the ordinary oil phase can physically block aroma substances. Figure 2 (70℃): When the temperature rises to 70℃ (slightly above the melting point of beeswax), the mass loss rate of Example 1 (beeswax) is higher than that of Comparative Example 8. This is because beeswax undergoes a phase transition from solid to liquid, disrupting the density of its shell structure and triggering the rapid release of aroma substances. Experimental results demonstrate that this temperature-responsive material effectively encapsulates aroma substances at room temperature while rapidly releasing them at high temperatures. This characteristic is suitable for application in cigarette filters and tipping paper, effectively encapsulating aroma substances at room temperature, and triggering aroma release under the influence of the hot smoke generated during cigarette smoking, thus enhancing the user's smoking experience.

[0157] To further verify the phase transition behavior of the temperature-responsive material system of this application within the cigarette smoking temperature range, differential scanning calorimetry (DSC) was used to perform thermal analysis on the temperature-responsive material prepared in Example 1, such as... Figure 3As shown in the DSC curve, a distinct endothermic peak appears during the heating process from 30℃ to 200℃, with a peak temperature of approximately 58.3℃. This endothermic peak corresponds to the solid-liquid phase transition process of the oil phase (beeswax) in the shell of the temperature-responsive material. This result directly proves that during cigarette smoking, under the temperature rise environment (approximately 60℃~80℃) as the smoke passes through the filter rod or tipping paper, the solid shell of the temperature-responsive material does indeed undergo a melting transformation, thereby triggering the rapid release of aroma substances. Combined with the above TGA results, it can be confirmed that the temperature-responsive material of this application has good encapsulation stability at room temperature, and can achieve on-demand release when heated during smoking, providing direct thermodynamic evidence for temperature-responsive controlled release.

[0158] As shown in Table 1, the total scores of Examples 1-11 were significantly higher than those of all comparative examples. Comparative Example 3 (directly sprayed fragrance) and Comparative Example 6 (PLA polymer system) had the lowest scores, with total scores as low as 75 and 78 points respectively, showing a particularly significant difference. This fully demonstrates that the core-shell structure formed by the synergistic effect of specific polymers (shellac / polycaprolactone) and phase-transformation oil phases (beeswax, etc.) in this application can achieve efficient encapsulation and stable protection of aroma substances. Furthermore, during cigarette smoking, the shell layer can undergo phase-transformation melting in response to the smoke temperature, allowing for rapid aroma release and avoiding the problems of poor aroma stability and uncontrollable release in traditional processes.

[0159] The aroma and aftertaste scores of Examples 1-11 are significantly higher than those of the comparative examples, directly verifying the reliability of the temperature-responsive controlled-release system of this application. Specifically, Example 3, by increasing the polymer concentration, can prepare a temperature-responsive material with a thicker shell and longer-lasting sustained-release performance. Example 4 achieves high-load encapsulation of aroma substances. The solid core-shell structure can firmly seal the aroma at room temperature, preventing premature escape, while the heat of the smoke during inhalation can precisely trigger shell rupture, allowing for continuous and uniform release of aroma throughout the entire inhalation process, ensuring a consistent and lasting vaping experience. In contrast, Comparative Example 3 (directly sprayed fragrance) lacked an encapsulation structure, resulting in significant aroma loss during the storage stage and the initial inhalation phase; Comparative Example 2 (replacing the phase-inversion oil phase with corn oil without phase-inversion properties) lacked a temperature response mechanism, leading to a noticeable difference in aroma before and after inhalation; Comparative Example 1 (omitting the microfluidic mixing step) suffered from uneven emulsion particle size and incomplete shell, resulting in impaired aroma transfer and release efficiency, and all scores were at a relatively low level among the comparative examples; Comparative Example 6 (PLA polymer system) exhibited poor compatibility between the polymer and the phase-inversion oil phase, a loose core-shell structure, low aroma encapsulation rate, and a significantly deteriorated inhalation experience.

[0160] Furthermore, Examples 1-11 demonstrated stable performance in terms of gloss, off-odors, and harmony, outperforming the comparative examples. This indicates that the fragrance-enhancing technology of this application does not introduce unintended off-odors, achieving the effect of "enhancing fragrance without disturbing the original aroma." Regardless of adjustments to polymer concentration, phase transition oil concentration, oil-water volumetric flow rate ratio, or changes in the types of fragrance substances, the examples maintained excellent overall performance. This fully demonstrates that the parameter range, material selection, and preparation process defined in this application have good adaptability and stability, providing reliable support for the large-scale production of high-quality fragranced tipping paper.

[0161] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0162] The embodiments described above are merely illustrative of several implementation methods of this application, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent application. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this application, and these all fall within the protection scope of this application. Therefore, the protection scope of this patent application should be determined by the appended claims.

Claims

1. A temperature-responsive material, characterized in that, It includes a core and a shell material enclosing the core; the core includes an oil-soluble aroma substance, and the shell material includes a polymer and a phase transition oil phase, wherein the polymer includes one or more of shellac and polycaprolactone, and the mass-to-volume ratio of the polymer to the phase transition oil phase is 1 g: (0.05~3) mL.

2. The temperature-responsive material as described in claim 1, characterized in that, The mass-to-volume ratio of the polymer to the phase-transformation oil phase is 1 g: (0.2~2) mL; And / or, the mass ratio of the oil-soluble aroma substance to the polymer is 1:0.1~40; And / or, the melting point of the phase transformation oil phase is 40℃~60℃.

3. The temperature-responsive material as described in claim 1, characterized in that, The phase transformation oil phase includes one or more of paraffin wax, beeswax, and coconut oil; And / or, the oil-soluble aroma substances include one or more of menthol, sophora japonica essential oil, rose essential oil, peppermint essential oil, jasmine essential oil, sandalwood essential oil, wintersweet essential oil, lavender essential oil, ginger essential oil, and camellia essential oil.

4. The temperature-responsive material according to any one of claims 1 to 3, characterized in that, The temperature-responsive material has a particle size of 150 nm to 1500 nm.

5. A method for preparing a temperature-responsive material, characterized in that, Includes the following steps: The polymer, phase-transformation oil phase, oil-soluble aroma substance, and solvent are mixed to obtain an oil phase solution; At 65℃~85℃, the oil phase solution and the aqueous phase are mixed using microfluidic technology, and then cooled to 20℃~25℃ to induce the phase-transformation oil phase and the polymer to form a shell to encapsulate the oil-soluble aroma substance, thereby preparing a temperature-responsive material. The mass-volume ratio of the polymer and the phase-transformation oil phase is 1 g: (0.05~3) mL.

6. The method for preparing the temperature-responsive material as described in claim 5, characterized in that, The solvent includes one or more of ethanol, acetone, and tetrahydrofuran; And / or, the concentration of the polymer in the oil phase solution is 10 mg / mL to 200 mg / mL; And / or, the concentration of the phase-transformed oil phase in the oil phase solution is 10 μL / mL to 100 μL / mL; And / or, the concentration of oil-soluble aroma substances in the oil phase solution is 5 mg / mL to 100 mg / mL.

7. The method for preparing the temperature-responsive material according to any one of claims 5 to 6, characterized in that, Mixing methods include using microfluidic mixers; The microfluidic mixer includes an oil phase inlet channel, an aqueous phase inlet channel, a mixing chamber, and a material outlet channel. During the mixing process of the oil phase solution and the aqueous phase, the oil phase solution and the aqueous phase enter the mixing chamber tangentially through the oil phase inlet channel and the aqueous phase inlet channel, respectively. After vortex mixing in the mixing chamber, the mixture flows out through the material outlet channel.

8. The method for preparing the temperature-responsive material as described in claim 7, characterized in that, The diameter of the oil phase inlet channel is 200μm~1000μm, the diameter of the water phase inlet channel is 700μm~1300μm, and the diameter of the material outlet channel is 800μm~2000μm. And / or, the volumetric flow rate of the oil phase solution is 20 μL / min to 900 μL / min, and the volumetric flow rate of the aqueous phase is 100 μL / min to 36000 μL / min; And / or, the volumetric flow rate ratio of the oil phase solution to the water phase is 1:5 to 1:

40.

9. The use of the temperature-responsive material according to any one of claims 1 to 4 in the preparation of cigarette products.

10. A cigarette, characterized in that, The cigarette comprises tobacco shreds and filter rod segments, which are wrapped together by tipping paper to form a cigarette; the tipping paper and / or the filter rod segments comprise temperature-responsive materials as described in any one of claims 1 to 4 or temperature-responsive materials prepared by the method described in any one of claims 5 to 8.

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