A filter rod containing a support component, a method for preparing the same, and a cigarette containing the same.
By setting a support component inside the outer tube of the filter rod, the microcapsule wall ruptures due to temperature changes to release the core material and provide support, thus solving the problem of the filter rod softening and collapsing due to heat and moisture during the suction process. This achieves structural stability of the filter rod and slow release of fragrance, improving suction quality.
Patent Information
- Application Number
- CN202311219741.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-21
- Publication Date
- 2025-10-28
- Estimated Expiration
- 2043-09-21
AI Technical Summary
Cigarette filters soften and collapse during smoking due to increased heat and moisture, affecting the smoking experience. Existing technologies struggle to effectively prevent this phenomenon.
A support component is set inside the outer tube of the filter rod. The support component includes a filler and microcapsules dispersed in the filler. The capsule wall of the microcapsule is made of silica and the capsule core is made of poly(N-isopropylacrylamide). The capsule wall is ruptured by temperature change to release the capsule core material to provide support. A photocurable film is prepared on the outer layer of the capsule wall to improve stability.
It effectively prevents the filter rod from softening and collapsing during the suction process, improves the support performance and hydrophobicity of the filter rod, ensures the slow release of fragrance and aroma quality, and enhances the structural stability of the filter rod.
Smart Images

Figure CN117137189B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of heated non-combustible cigarette technology, specifically to a filter rod containing a support component, a method for preparing the same, and cigarettes containing the same. Background Technology
[0002] Cigarette filters are typically made of cellulose acetate or polylactic acid (PLA) tow. During smoking, due to increased heat and moisture, these filters soften and collapse. A large thermal collapse value can affect the filter's stability and smoking quality. The standard YC / T 354-2010, "Determination of Physical Properties of Cigarettes and Filters: Thermal Collapse," specifies the test method for thermal collapse of filter rods.
[0003] Currently, researchers point out that temperature is a major factor affecting thermal collapse value. During combustion, the higher the temperature and the closer the combustion cone is to the pressure application point, the greater the thermal collapse value. Secondly, moisture has a significant impact on thermal collapse; the higher the water content at the pressure application point, the greater the thermal collapse value. To prevent the filter rod from softening and collapsing due to heat during suction, researchers typically reduce the temperature of the smoke reaching the mouthpiece or install a separate support element inside the filter rod. Furthermore, to address the issue of the filter rod softening due to moisture on the contact surface between the filter rod and the lip, a waterproof layer is applied to the filter rod forming paper, or a smooth, waterproof material is used.
[0004] Therefore, improving the support performance and hydrophobicity of the filter rod is an effective means to prevent the filter rod from softening and collapsing during the suction process, and it is also a problem that people hope to solve.
[0005] To address the above problems, this invention is proposed. Summary of the Invention
[0006] The first aspect of the present invention provides a filter rod containing a support component, which includes an outer tube (1) and a support component (4) located inside the outer tube (1), the support component (4) including a filler and microcapsules dispersed in the filler;
[0007] The capsule wall is made of silica, and the capsule core is made of poly(N-isopropylacrylamide) (PNIPAM).
[0008] Preferably, the filter rod containing the support component further includes an inner tube (2) and a groove layer (3) located between the outer tube (1) and the inner tube (2), wherein the groove layer (3) has a support component (4) in the cavity on the side near the inner tube (2);
[0009] Preferably, the outer layer of the microcapsule wall also has a photocurable film.
[0010] Preferably, the inner tube (2) has a filter rod core (5) inside its cavity;
[0011] The inner tube (2) is selected from 8000CU-10000CU high-transparency forming paper, the outer tube (1) is selected from forming paper, and the groove layer (3) is selected from non-woven fabric or fabric with a basis weight of 40-60g / m 2 High-grammage formed paper;
[0012] The cross-sectional shape of the trench layer (3) is "U-shaped", "V-shaped" or "trapezoidal".
[0013] Preferably, the filler is a diacetate cellulose bundle or a polylactic acid cellulose bundle, wherein the amount of microcapsules added to the filler is 0.5mg-0.6mg microcapsules / 1mm cellulose bundle.
[0014] The filter rod containing the supporting component of this invention can be used as a standalone cigarette filter rod, or as a segment of a binary composite filter rod or a ternary composite filter rod. Preferably, the filter rod containing the supporting component is combined with a segment of a filter rod without microcapsule bundles. The filter rod without microcapsule bundles includes an outer tube (1), an inner tube (2), and a grooved layer (3) located between the two. The cavity of the grooved layer (3) near the inner tube (2) does not have a supporting component. The axial length ratio of the filter rod containing the supporting component to the filter rod without microcapsule bundles is 1.39:1-1.46:1. In actual production, the ratio of the axial lengths of the two components can be adjusted according to different specifications and machine models.
[0015] A second aspect of the present invention provides a method for preparing a filter rod containing a support component as described in the first aspect of the present invention, wherein the method for preparing the microcapsules includes the following steps:
[0016] (a) Preparation of hollow silica microspheres,
[0017] (b) Poly-N-isopropylacrylamide was dispersed in hollow silica microspheres using ultrasound to obtain silica microspheres containing poly-N-isopropylacrylamide, namely PNIPAM / SiO2 microcapsules.
[0018] Preferably, the method for preparing microcapsules includes the following steps:
[0019] (a) Preparation of hollow silica microspheres:
[0020] (a1) Measure 22 mL to 24.0 mL of a 10-11 mmol / L aqueous solution of hexadecyltrimethylammonium bromide (CTAB) into a three-necked flask and fix the apparatus;
[0021] (a2) Add 0.4-0.5g of urea and mechanically stir at room temperature to dissolve the urea, forming an aqueous solution A;
[0022] (a3) Add 1.1-1.3 mL (1.0 g) of cyclohexane, 210-220 μL of n-hexadecane (HD), and 3.2-3.5 mL (3.0 g) of tetraethyl orthosilicate (TEOS) sequentially to the aqueous solution A in step (a2);
[0023] (a4) Pre-emulsify by stirring at room temperature, transfer to a colorimetric tube, and further emulsify by ultrasound;
[0024] (a5) After being placed at room temperature and aged, the mixture was placed in a heated oil bath for reaction. After being mixed with anhydrous ethanol at a volume ratio of 1:1 and centrifuged, a white solid was obtained.
[0025] (a6) The white solid obtained in step (a5) is dried to obtain hollow SiO2 microspheres;
[0026] (b) Dispersing poly-N-isopropylacrylamide within hollow silica microspheres using ultrasound:
[0027] (b1) At a temperature of 20℃-25℃, weigh 95-100mg of hollow silica microspheres and place them in a centrifuge tube, then add 0.5-0.6mL of 10-12wt% poly-N-isopropylacrylamide aqueous solution;
[0028] (b2) After ultrasonic dispersion, poly-N-isopropylacrylamide enters the interior of the hollow silica microspheres through the surface pores to form microcapsules, and is then allowed to stand before being evacuated.
[0029] (b3) Then the product from step (b2) is centrifuged, the sample is ultrasonically washed three times with ethanol and then dried to obtain silica microspheres containing poly(N-isopropylacrylamide), namely PNIPAM / SiO2 microcapsules.
[0030] Preferably, in step (a1), the concentration of hexadecyltrimethylammonium bromide is 10-11 mmol / L; in step (a2), the stirring speed is 250 rpm-300 rpm, and the stirring time is 30 min-1 h; in step (a4), the stirring speed is 250 rpm-300 rpm, and the stirring time is 30 min-1 h, with further emulsification using 80 kHz ultrasonic fine emulsification for 30 min-1 h; in step (a5), the aging time is 12 h-36 h, and the oil bath temperature is 60-70 °C. The temperature is ℃, and the reaction time is 24-36h; in step (a6), the drying temperature is 50℃-60℃, and the drying time is 12-24h; in step (b1), the mass fraction of the poly-N-isopropylacrylamide aqueous solution is 10-12wt%; in step (b2), the ultrasonic frequency is 20KHz, the ultrasonic time is 30min-1h, the standing time is 24-36h, and the vacuum time is 10min-30min; in step (b3), the drying conditions are: drying in a vacuum drying oven at 20℃ for 24h-48h.
[0031] Preferably, the outer layer of the microcapsule wall further has a photocurable film, and the method for preparing the filter rod containing the supporting component further includes step (c) forming a photocurable film on the surface of the PNIPAM / SiO2 microcapsule:
[0032] (c1) Take an active diluent, wherein the active diluent comprises one or more of the following: trifunctional trimethylolpropane triacrylate (TMP3EOTA), dual-functional dipropylene glycol diacrylate (TPGDA), and single-functional isoborneol methacrylate (IBOA).
[0033] (c2) Place the main resin, epoxy soybean oil acrylate (AESO), in a disposable flat-bottomed centrifuge tube in the laboratory and add the reactive diluent from step (c1).
[0034] (c3) After stirring evenly, add 0.5-0.6g of Irgacure184 dropwise and dissolve it completely on the stirring table to form a film solution;
[0035] (c4) Place the PNIPAM / SiO2 microspheres in a glass petri dish and pour the membrane solution prepared in step (3) into the petri dish containing the microspheres to ensure that the microspheres are completely immersed in the resin so as to ensure that the microspheres are completely wrapped by the resin.
[0036] (c5) Take the microspheres out one by one from the glass petri dish and place them on a polytetrafluoroethylene plate. Wipe off any excess membrane solution deposited on the plate. Place the membrane solution containing the microspheres in a shaker, turn on the shaker, and roll the microspheres in the polytetrafluoroethylene plate at maximum speed for 30s-1min. Then turn on the LED light in the experimental equipment to irradiate.
[0037] (c6) Repeat steps (c3) and (c4) twice to ensure that the microspheres can be coated with three layers of photocurable film;
[0038] (c7) The final product is dried to obtain PNIPAM / SiO2 microcapsules with a photocurable film.
[0039] Preferably, in step (c1), the active diluent can be any one of the following: trifunctional trimethylolpropane triacrylate (TMP3EOTA), dipropylene glycol diacrylate (TPGDA) with two functional groups, and isoborneol methacrylate (IBOA) with one functional group; more preferably, a combination of the above three is selected; and even more preferably, in step (c1), the trifunctional trimethylolpropane triacrylate (TMP3EOTA) accounts for 0.2%-0.4% of the mass percentage of the main resin, the dipropylene glycol diacrylate (TPGDA) with two functional groups accounts for 0.1% of the mass percentage of the main resin, and the isoborneol methacrylate (IBOA) with one functional group accounts for 0.2%-0.5% of the mass percentage of the main resin.
[0040] Preferably, in step (c5), the LED light irradiation wavelength is 365nm and the continuous irradiation time is 1.5min-2min; in step (c7), the drying conditions are: room temperature drying for 24h-36h.
[0041] The third aspect of the present invention provides a cigarette containing a filter rod with a support component as described in the first aspect of the present invention.
[0042] Compared with the prior art, the present invention has the following beneficial effects:
[0043] 1. This invention first proposes adding a support component inside the outer tube of the filter rod. The support component (4) includes a filler and microcapsules dispersed in the filler. This invention is the first to conceive of adding a material that hardens when heated inside the outer tube. The capsule wall of the microcapsule is silicon dioxide, and the core of the microcapsule is poly(N-isopropylacrylamide). During the filter rod suction process, the filter rod temperature rises, causing the capsule wall of the microcapsule to soften and SiO2 to rupture, thereby releasing the poly(N-isopropylacrylamide) core. The PNIPAM material undergoes a phase change when heated, and the polymer network shrinks into a tight colloidal structure, making the filter rod harden. This provides support for the trench layer (3) and the outer tube (1) and prevents the outer tube (1) from softening and collapsing.
[0044] 2. The present invention further proposes a filter rod structure containing a support component. The filter rod includes an outer tube (1), an inner tube (2), and a groove layer (3) located between the two. The groove layer (3) has a support component (4) in the cavity on the side near the inner tube (2). The support component (4) includes a filler and microcapsules dispersed in the filler. This structure can enable the support component 4 to provide stronger support to the outer tube 1.
[0045] 3. PNIPAM, which hardens after agglomeration due to heat, is hydrophobic and can prevent surface moisture from the filter rod in contact with the lips from entering the filter rod core (5) and causing the filter rod to soften, thus avoiding thermal collapse caused by increased moisture.
[0046] 4. At low temperatures, PNIPAM is in a stretched state in water. As the temperature rises, PNIPAM shrinks, and the loose coil structure agglomerates into a tight colloidal structure, thus hardening and providing support. This invention utilizes this point. At low temperatures, PNIPAM is first placed in a fragrance solution to swell and adsorb fragrance, and then it is encapsulated to form microcapsules. As the temperature rises, the silica capsule wall ruptures, the PNIPAM core is released, and the adsorbed fragrance is slowly released. In other words, PNIPAM can swell and adsorb fragrance when placed in a fragrance solution at low temperatures, and shrinks at high temperatures to release fragrance substances. This not only provides better storage conditions for fragrances, but also enhances the fragrance during aspiration. The microcapsules of this invention can not only achieve the slow release of fragrance after heating, but also support the outer tube (1) after heating.
[0047] 5. The present invention further prepares a photocurable water-retaining resin film on the surface of PNIPAM / SiO2 microcapsules. The photocurable water-retaining resin film can improve the water retention performance of PNIPAM / SiO2 microcapsules, thereby improving the stability of the wall material. This ensures that the PNIPAM core inside the capsule wall is not dried out or flows out of the capsule wall during cigarette transportation or shelf life. It can also prevent the instantaneous release of the PNIPAM core during smoking. Especially for cases where PNIPAM also stores flavorings, the photocurable water-retaining resin film can ensure slow release from the capsule wall, thereby allowing the PNIPAM inside to slowly release the flavorings.
[0048] 6. The filter rod containing the supporting component of this invention can be used as a standalone cigarette filter rod, or as a segment of a binary composite filter rod or a ternary composite filter rod. When the cigarette is smoked to a certain temperature, the outer ring of the filter rod hardens, making the outer layer of the filter rod, which would normally soften after smoking, harder, supporting the cylindrical structure of the filter rod, thereby improving the thermal collapse of the filter rod during smoking. Attached Figure Description
[0049] Figure 1 Electron micrograph of hollow silica;
[0050] Figure 2 This is a cross-sectional view of a filter rod containing supporting components;
[0051] Figure 3 This is a composite diagram of filter rods;
[0052] Figure 4 This is a cross-sectional view of another filter rod containing a support component.
[0053] The names of the reference numerals in the accompanying drawings are as follows: 1-outer tube, 2-inner tube, 3-groove layer, 4-support component, 5-filter rod core, 11-filter rod containing support component, 12-filter rod without support component. Detailed Implementation
[0054] The present invention will now be described in further detail with reference to the embodiments.
[0055] Those skilled in the art will understand that the following embodiments are for illustrative purposes only and should not be construed as limiting the scope of the invention. Where specific techniques or conditions are not specified in the embodiments, they are performed in accordance with the techniques or conditions described in the literature in the field or according to the product instructions. Materials or equipment whose manufacturers are not specified are all conventional products that can be obtained by purchase.
[0056] Those skilled in the art will understand that, unless specifically stated otherwise, the singular forms “a,” “an,” “the,” and “the” used herein may also include the plural forms. It should be further understood that the term “comprising” as used in this specification means the presence of the stated features, integers, steps, operations, elements, and / or components, but does not exclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or groups thereof. It should be understood that when we say an element is “connected” to another element, it can be directly connected to the other element, or there may be an intermediate element. Furthermore, the term “connected” as used herein can include wireless connections.
[0057] In the description of this invention, unless otherwise stated, "a plurality of" means two or more. The terms "inner," "upper," "lower," etc., indicate the orientation or state relationship based on the orientation or state relationship shown in the drawings, and are only for the convenience of describing the invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the invention.
[0058] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installed," "connected," and "equipped with" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium. Those skilled in the art will understand the specific meaning of the above terms in this invention according to the specific circumstances.
[0059] It will be understood by those skilled in the art that, unless otherwise defined, all terms used herein, including technical and scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. It should also be understood that terms such as those defined in general dictionaries should be understood to have the meaning consistent with their meaning in the context of the prior art, and should not be interpreted in an idealized or overly formal sense unless defined as herein.
[0060] Example 1
[0061] I. Preparation of Poly-N-Isopropylacrylamide
[0062] Add 98% concentrated sulfuric acid to a 250ml three-necked flask, stir and add 15ml isopropanol dropwise. Use the heat of dilution reaction to raise the temperature to 50-60℃, add 1% copper chloride dihydrate, and slowly add 13ml (0.2mol) acrylonitrile. Maintain the temperature at 50-60℃ throughout this process.
[0063] After the addition was complete, the reaction was carried out at 60-70℃ for 1 hour. The mixture was then cooled to room temperature, neutralized in filtered water to pH 2, and extracted with 50 ml of diethyl ether until the solution separated into layers. The lower organic layer was dried over anhydrous magnesium sulfate for 12 hours, and the solvent was evaporated at 100℃ to obtain the crude synthesized N-isopropylacrylamide (NIPAM).
[0064] Mix 1 part hexane and 1 part toluene (1:1) in a solvent mixture and heat to 80°C. Stir magnetically at 200 rpm, and add 10 g of crudely synthesized N-isopropylacrylamide (NIPAM) and 0.6 g of photoinitiator Irgacure 184. Irgacure 184 is a photoinitiator with excellent resistance to yellowing and high activity, which helps the polymerization of N-isopropylacrylamide monomers and does not easily change color, thus affecting product quality. Stir manually until completely dissolved, filter the precipitate and insoluble matter with filter paper, and place the remaining solution in an open bottle and seal it. Let it stand in a refrigerator at 4°C for 2 hours to allow crystallization. After crystallization, filter again. After filtering twice, dry under vacuum at 45°C to obtain pure N-isopropylacrylamide.
[0065] Pure N-isopropylacrylamide was mixed with cigarette flavorings. The N-isopropylacrylamide mixture was then placed on a polytetrafluoroethylene (PTFE) plate and placed in a shaker at 100 rpm, continuously irradiated with a 365 nm LED light source for 1 minute. This process allows the N-isopropylacrylamide to be loaded with flavorings during the polymerization of poly(N-isopropylacrylamide). Compared to polymerization using a catalyst, this method produces pure poly(N-isopropylacrylamide) free from other chemical contamination.
[0066] In addition to loading fragrances and flavorings onto N-isopropylacrylamide during its polymerization into polyN-isopropylacrylamide, N-isopropylacrylamide can also be polymerized into polyN-isopropylacrylamide first, and then fragrances and flavorings can be adsorbed onto it. The specific steps are as follows:
[0067] Pure N-isopropylacrylamide was placed on a polytetrafluoroethylene plate and placed in a shaker at 100 rpm, continuously irradiated with a 365 nm LED light source for 1 minute. This allowed the N-isopropylacrylamide to polymerize into polyN-isopropylacrylamide. The prepared polyN-isopropylacrylamide was then immersed in cigarette flavoring and fragrance for 2-3 hours. After removal, polyN-isopropylacrylamide containing the flavoring and fragrance was obtained.
[0068] Compared to polymerizing N-isopropylacrylamide and then adsorbing fragrance, loading fragrance during the polymerization of N-isopropylacrylamide can ensure a larger fragrance loading capacity. Therefore, this embodiment adopts the method of loading fragrance during the polymerization of N-isopropylacrylamide.
[0069] Then it is used as the core material for subsequent steps.
[0070] II. Preparation of PNIPAM / SiO2 microcapsules with photocurable films
[0071] Hollow silica microspheres were first prepared, and then poly(N-isopropylacrylamide) was dispersed in the hollow silica microspheres using ultrasound to obtain silica microspheres PNIPAM / SiO2 containing poly(N-isopropylacrylamide). Then, a photocurable water-retaining resin film was prepared on the surface of the PNIPAM / SiO2 microcapsules.
[0072] (1) Preparation of hollow silica microspheres:
[0073] Step 1: Measure 24.0 mL of a 10 mmol / L hexadecyltrimethylammonium bromide (CTAB) aqueous solution and pour it into a three-necked flask, then fix the apparatus.
[0074] Step 2: Add 0.48g of urea and mechanically stir (250rpm) at room temperature to dissolve the urea and form an aqueous solution A.
[0075] Step 4: Add 1.3 mL (1.0 g) of cyclohexane, 216 L of n-hexadecane (HD), and 3.2 mL (3.0 g) of tetraethyl orthosilicate (TEOS) to the product from Step 3 in sequence.
[0076] Step 3: Pre-emulsify at room temperature (250 rpm) for 30 min, then transfer to a colorimetric tube and sonicate at 80 kHz for 30 min.
[0077] Step 4: After aging at room temperature for 12 hours, place the mixture in an oil bath heated to 70°C and react for 24 hours. After centrifugation with anhydrous ethanol at a 1:1 (v:v) ratio, a white solid is obtained.
[0078] Step 5: The product is dried in a 50℃ forced-air drying oven to obtain hollow SiO2 microspheres.
[0079] from Figure 1 SEM showed that the hollow silica microspheres in Example 1 were not completely sealed. In this example, poly-N-isopropylacrylamide was further injected into the hollow interior by ultrasonic dispersion.
[0080] (2) Preparation by ultrasonic dispersion (PNIPAM / SiO2)
[0081] Step 6: At 20°C, weigh 100 mg of hollow silica microspheres and place them in a centrifuge tube. Add 0.5 mL of 10 wt% poly(N-isopropylacrylamide) aqueous solution.
[0082] Step 7: After ultrasonic dispersion at a frequency of 20 kHz, poly-N-isopropylacrylamide enters the interior of the hollow silica microspheres through the surface pores to form microcapsules. Let stand for 30 minutes and then evacuate for 10 minutes.
[0083] Step 8: Then, the product (PNIPAM / SiO2) from Step 7 is centrifuged, the sample is ultrasonically washed three times with ethanol, and then dried in a vacuum drying oven at 20°C for 24 hours. The ambient temperature is 20°C.
[0084] (3) Preparation of PNIPAM / SiO2 microcapsules with photocurable film
[0085] Step Nine: Take 10g of the main resin AESO and mix it with epoxidized soybean oil acrylate (AESO). Use the following reactive diluents: trifunctional ethoxylated trimethylolpropane triacrylate (TMP3EOTA), dimethylolpropane diacrylate (TPGDA) with two functional groups, and isobornyl methacrylate (IBOA) with one functional group. The trifunctional ethoxylated trimethylolpropane triacrylate (TMP3EOTA) accounts for 0.2%-0.4% of the main resin by mass, the dimethylolpropane diacrylate (TPGDA) with two functional groups accounts for 0.1% of the main resin by mass, and the isobornyl methacrylate (IBOA) with one functional group accounts for 0.2%-0.5% of the main resin by mass.
[0086] Step 10: Place the main resin, epoxy soybean oil acrylate (AESO), into a flat-bottomed disposable centrifuge tube in the laboratory and add 0.04g of IBOA.
[0087] Step 11: After stirring evenly, add 0.6g of Irgacure184 dropwise and let it dissolve completely on the stirring table to form a film solution.
[0088] Step 12: Place the PNIPAM / SiO2 microspheres in a glass petri dish, and pour one of the prepared resin formulations into the petri dish containing the microspheres, ensuring that the microspheres are completely immersed in the resin and completely coated by the resin.
[0089] Step 13: Remove the microspheres one by one from the glass petri dish and place them on a polytetrafluoroethylene (PTFE) plate, wiping away any excess resin deposited on the plate. Place the resin containing the microspheres in a shaker, turn on the shaker, and rotate the microspheres in the PTFE plate at maximum speed for 30 seconds to 1 minute. Then turn on the LED light in the above experimental apparatus at a wavelength of 365 nm and irradiate continuously for 1 minute and 30 seconds.
[0090] Step Fourteen: Repeat Steps Three and Four twice to ensure that the microspheres can be coated with three layers.
[0091] Step 15: The final product is dried at room temperature to obtain PNIPAM / SiO2 microcapsules with a photocurable film.
[0092] III. Composite of PNIPAM / SiO2 microcapsules with photocurable films and filter rods
[0093] See the schematic diagram of the filter rod structure containing the supporting components. Figure 2 .
[0094] Step 1: First, make the core, i.e. the inner tube. The forming paper is 8000CU high transparency forming paper with a circumference of 15.3mm ± 0.1.
[0095] Step 2: First, the grooved paper made of non-woven fabric is pressed using a square gear roller with a width of 1mm, a depth of 1mm, and a spacing of 1mm. That is to say, the cross-sectional shape of the groove in the groove layer (3) is "trapezoidal".
[0096] Step 3: The microcapsules from Examples 1, 2, and 3 are uniformly added to the cellulose acetate tow (filter rod) at a dosage of 0.5 mg / mm². This cellulose acetate tow is a diacetate tow. After the tow has cured for 2 hours, it can uniformly fill a 1 mm groove, serving as the outer ring filter rod. The grooves formed during the lamination process increase the air permeability of the filter rod after it hardens.
[0097] Step 4: The square groove has a larger contact area with the outermost tipping paper, and is more closely bonded to the normal forming paper. Hot melt adhesive with a viscosity of 6000±500mPa.s is used to form a cigarette filter rod unit with the normal rod core, i.e., the outer tube, with a circumference of 22.1mm±0.1.
[0098] Step 5: The filter rod 11 containing the support component from Step 3 is combined with the filter rod 12 without microcapsule tow, with a combined length of 23mm + 7mm. See Figure 3 .
[0099] The cross-sectional shape of the trench layer (3) can also be "V-shaped", see Figure 4 In addition, the cross-sectional shape of the trench layer (3) can also be "U-shaped".
[0100] In this embodiment, the cigarette sample formed by combining the microcapsules and grooved filter rods prepared in this embodiment with other units is named Example 1 - Grooved Filter Rod. For comparison, the cigarette sample formed by combining the microcapsules and ordinary filter rods (that is, the outer tube has cellulose acetate bundles inside and does not have a groove structure) prepared in this embodiment with other units is named Example 1 - Ordinary Filter Rod.
[0101] Comparative Example
[0102] The comparative example is a filter rod without internal support components, which differs from Example 1 only in that the filter rod does not contain support components.
[0103] Among them, the cigarette sample composed of a filter rod with a grooved structure and other units was named the comparative example - grooved filter rod, and the cigarette sample composed of a regular filter rod (that is, the outer tube has cellulose acetate bundles and does not have a grooved structure) and other units was named the comparative example - regular filter rod.
[0104] Example 2
[0105] The filter rod in this embodiment contains a support component, but the difference from embodiment 1 is that the microcapsules used for the support component are PNIPAM / SiO2 microcapsules and do not contain a photocurable film. More specifically, the photocurable film coating in step (3) is not performed on the basis of embodiment 1.
[0106] In this embodiment, the cigarette sample formed by combining the microcapsules and grooved filter rods prepared in this embodiment with other units is named Example 2 - Grooved Filter Rod. For comparison, the cigarette sample formed by combining the microcapsules and ordinary filter rods (that is, the outer tube has cellulose acetate bundles inside and does not have a groove structure) prepared in this embodiment with other units is named Example 2 - Ordinary Filter Rod.
[0107] The composite filter rods from the comparative example, Example 1, and Example 2 were rolled into cigarettes to obtain samples: Example 1 - grooved filter rod, Example 1 - ordinary filter rod, Example 2 - grooved filter rod, Example 2 - ordinary filter rod, comparative example - grooved filter rod, and comparative example - ordinary filter rod. All samples were equilibrated in a constant temperature and humidity chamber for 48 hours, and five cigarettes were selected as test samples according to an average mass ±0.02g. Ordinary cigarettes were used as blank samples. The thermal collapse test of the filter rods was performed using the method in the standard "YC / T354-2010 Determination of Physical Properties of Cigarettes and Filter Rods - Thermal Collapse".
[0108] Table 1. Ordinary filter rods with microcapsules directly added according to Examples 1 and 2.
[0109]
[0110] Table 2 shows the grooved filter rods with microcapsules added in the form of grooved fasteners, as described in Examples 1 and 2.
[0111]
[0112] The outer groove (external groove) refers to the groove on the side of the outer pipe within the main groove, while the inner groove (internal groove) refers to the groove on the side of the inner pipe within the main groove (i.e., the filling groove). Figure 2 and Figure 4 (The groove for filling support components).
[0113] As can be seen from the implementation data table, comparing the comparative examples and Examples 1-2, it is evident that the thermal collapse values of the microcapsule filter rods containing PNIPAM are all reduced, and the range is smaller compared to the blank sample. Furthermore, when measuring the outer and inner grooves, the thermal collapse at the inner groove location is larger, which also indirectly indicates that filter rods with more microcapsule-filled portions can reduce the thermal collapse value during aspiration.
[0114] A comparative analysis of Examples 1 and 2 reveals that preparing a photocurable water-retaining resin film on the surface of PNIPAM / SiO2 microcapsules improves the water retention performance of the PNIPAM / SiO2 microcapsules, thereby enhancing the stability of the wall material. This ensures that the PNIPAM core inside the capsule wall does not dry out or leak out during cigarette transportation or shelf life, and also prevents the instantaneous release of the PNIPAM core during smoking. Especially when the PNIPAM also stores flavorings, the photocurable water-retaining resin film ensures slow release from the capsule wall, allowing the PNIPAM inside to slowly release the flavorings. In Example 2, because no photocurable film was applied, the capsule wall was prone to rupture, resulting in partial loss of the PNIPAM core. However, the PNIPAM core that did not leak out after smoking and heating contributes to the hardness of the filter rod. More importantly, after sensory evaluation, the sample from Example 1 exhibited a richer aroma and higher aroma quality.
Claims
1. A filter rod containing a supporting component, characterized in that, It includes an outer tube (1) and a support component (4) located inside the outer tube (1), the support component (4) including a filler and microcapsules dispersed in the filler; The capsule wall is made of silica, and the capsule core is made of poly(N-isopropylacrylamide).
2. The filter rod containing a supporting component according to claim 1, characterized in that, The outer layer of the capsule wall of the microcapsule also has a photocurable film.
3. The filter rod containing a supporting component according to claim 1, characterized in that, The filter rod containing the internal support component also includes an inner tube (2) and a groove layer (3) located between the outer tube (1) and the inner tube (2), wherein the groove layer (3) has a support component (4) in the cavity on the side near the inner tube (2); The inner tube (2) has a filter rod core (5) inside its cavity; The inner tube (2) is selected from 8000CU-10000CU high-transparency forming paper, the outer tube (1) is selected from forming paper, and the groove layer (3) is selected from non-woven fabric or forming paper; The cross-sectional shape of the trench layer (3) is "U-shaped", "V-shaped" or "trapezoidal".
4. The filter rod containing a support component according to claim 1, characterized in that, The filler is a diacetate cellulose bundle or a polylactic acid cellulose bundle, wherein the amount of microcapsules added to the filler is 0.5mg-0.6mg microcapsule / 1mm cellulose bundle.
5. A method for preparing a filter rod containing a support component as described in any one of claims 1-4, characterized in that, The method for preparing the microcapsules includes the following steps: (a) Preparation of hollow silica microspheres, (b) Poly-N-isopropylacrylamide was dispersed in hollow silica microspheres using ultrasound to obtain silica microspheres containing poly-N-isopropylacrylamide, namely PNIPAM / SiO2 microcapsules.
6. The preparation method according to claim 5, characterized in that, The preparation method of microcapsules includes the following steps: (a) Preparation of hollow silica microspheres: (a1) Measure out a hexadecyltrimethylammonium bromide (CTAB) aqueous solution and pour it into a three-necked flask, then fix the apparatus; (a2) Add urea and mechanically stir at room temperature to dissolve the urea and form an aqueous solution A; (a3) Add cyclohexane, n-hexadecane (HD) and tetraethyl orthosilicate (TEOS) sequentially to the aqueous solution A in step (a2); (a4) Pre-emulsify by stirring at room temperature, transfer to a colorimetric tube, and further emulsify by ultrasound; (a5) After being placed at room temperature and aged, the mixture was placed in a heated oil bath for reaction. After centrifugation with anhydrous ethanol at a volume ratio of 1:1 to 1:1.2, a white solid was obtained. (a6) The white solid obtained in step (a5) is dried to obtain hollow SiO2 microspheres; (b) Dispersing poly-N-isopropylacrylamide within hollow silica microspheres using ultrasound: (b1) At a temperature of 20℃-25℃, weigh hollow silica microspheres and place them in a centrifuge tube, then add an aqueous solution of poly-N-isopropylacrylamide; (b2) After ultrasonic dispersion, poly-N-isopropylacrylamide enters the interior of the hollow silica microspheres through the surface pores to form microcapsules, and is then allowed to stand before being evacuated. (b3) Then the product from step (b2) is centrifuged, the sample is ultrasonically washed three times with ethanol and then dried to obtain silica microspheres containing poly(N-isopropylacrylamide), namely PNIPAM / SiO2 microcapsules.
7. The preparation method according to claim 6, characterized in that, In step (a1), the concentration of hexadecyltrimethylammonium bromide is 10-11 mmol / L; in step (a2), the stirring speed is 250-300 rpm, and the stirring time is 30 min-1 h; in step (a4), the stirring speed is 250-300 rpm, and the stirring time is 30 min-1 h, with further emulsification using 80 kHz ultrasonic fine emulsification for 30 min-1 h; in step (a5), the aging time is 12 h-36 h, and the oil bath temperature is 60-70℃. The reaction time is 24-36 h; in step (a6), the drying temperature is 50℃-60℃ and the drying time is 12-24 h; in step (b1), the mass fraction of the poly-N-isopropylacrylamide aqueous solution is 10-12 wt%; in step (b2), the ultrasonic frequency is 20 kHz, the ultrasonic time is 30 min-1 h, the standing time is 24-36 h, and the vacuum time is 10 min-30 min; in step (b3), the drying conditions are: drying in a vacuum drying oven at 20℃ for 24 h-48 h.
8. The preparation method according to claim 5, characterized in that, The outer layer of the microcapsule wall also has a photocurable film, and the method for preparing the filter rod containing the internal support component further includes step (c) forming a photocurable film on the surface of the PNIPAM / SiO2 microcapsule: (c1) Take an active diluent, wherein the active diluent comprises one or more of the following: trifunctional trimethylolpropane triacrylate (TMP3EOTA), dual-functional dipropylene glycol diacrylate (TPGDA), and single-functional isoborneol methacrylate (IBOA). (c2) Place the main resin, epoxy soybean oil acrylate (AESO), in a disposable flat-bottomed centrifuge tube in the laboratory and add the reactive diluent from step (c1). (c3) After stirring, Irgacure184 is added dropwise and dissolved on the stirring table to form a film solution; (c4) Place the PNIPAM / SiO2 microspheres in a glass petri dish, and pour the membrane solution prepared in step (c3) into the petri dish containing the microspheres, ensuring that the microspheres are completely immersed in the resin so that the microspheres are completely coated by the resin. (c5) Take the microspheres out one by one from the glass petri dish and place them on a polytetrafluoroethylene plate. Wipe off any excess membrane solution deposited on the plate. Place the membrane solution containing the microspheres in a shaker and turn on the shaker to roll the microspheres in the polytetrafluoroethylene plate for 30 seconds to 1 minute. Then turn on the LED light in the experimental equipment to irradiate the microspheres. (c6) Repeat steps (c3) and (c4) twice to ensure that the microspheres can be coated with three layers of photocurable film; (c7) The final product is dried to obtain PNIPAM / SiO2 microcapsules with a photocurable film.
9. The preparation method according to claim 8, characterized in that, In step (c1), the trifunctional trimethylolpropane triacrylate (TMP3EOTA) accounts for 0.2%-0.4% of the main resin by mass, the dimethylolpropane diacrylate (TPGDA) with two functional groups accounts for 0.1% of the main resin by mass, and the isoborneol methacrylate (IBOA) with one functional group accounts for 0.2%-0.5% of the main resin by mass. In step (c5), the LED lamp irradiation wavelength is 365nm-395nm, and the continuous irradiation time is 1.5min-2min. In step (c7), the drying conditions are: room temperature drying for 24h-36h.
10. A cigarette comprising a filter rod containing a support member as described in any one of claims 1-4.
Citation Information
Patent Citations
Hydroxy propyl methyl cellulose (HPMC) modified cigarette filter tip prepared by polypropylene fiber and preparation method thereof
CN103110189A
KR20210104400A