Water-in-cigarette blasting bead as well as preparation and application thereof
By using monomer in situ polymerization to form hydrophobic wall materials in the preparation of water-in-filled beads for smoke, combined with the treatment methods of functional additives, divalent electrolytes and water retention agents, the problem of unsatisfactory strength, water-in-filled rate and water retention rate of water-in-filled beads for smoke is successfully solved, and efficient preparation adapted to the needs of cigarette use is achieved.
Patent Information
- Application Number
- CN202311782515.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-22
- Publication Date
- 2025-06-24
AI Technical Summary
The existing water-in-filled beads for water-in-filled beads have low water-in-filled rate, difficult to control their strength, and poor water retention rate, making it difficult to adapt to the needs of cigarette use.
The preparation method of water-in-filled explosive beads formed by forming hydrophobic wall materials based on in-situ polymerization and curing of monomers is adopted. By combining the permeation treatment process and parameters of the monomer 1, the functional additives in the aqueous core material, and the divalent electrolyte and the water-retaining agent solution in the curing liquid, the regulation of strength, water-in-filled rate and water-retaining effect is achieved.
The water-in-filled beads for cigarettes with controllable strength, excellent water-in-filled rate and water retention rate were successfully prepared, which can adapt to the needs of cigarette use, and solve the problem that the strength of the water-in-filled beads is difficult to control and the water-in-filled rate and water retention rate in the prior art is not ideal.
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Figure CN120188916A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of cigarette materials, and particularly to the technical field of water-filled bursting beads for cigarettes. Background Art
[0002] Bursting bead cigarettes refer to cigarettes containing one or more flavor capsules in the filter tip, which will make a slight sound when broken, so they are called bursting bead cigarettes. For filter tip flavor enhancement technologies such as flavor wire (sheet) filter tips and filter tips containing flavor additives, the natural volatilization of flavor components during storage results in a deteriorated flavor enhancement effect. Wrapping flavor components in bursting beads can greatly delay the natural loss of flavor components, achieve artificially controllable release of characteristic flavors, and improve the sensory quality of cigarettes.
[0003] A bursting bead consists of two parts: a wall material and a core material. The wall material serves as a seal and has usage effects such as being hard, brittle, and making a sound; the core material is a liquid or suspension that is insoluble in the wall material. By squeezing and breaking the wall, flavor components can be delivered to the user. The main methods for preparing bursting beads that have been industrially applied are the dropping method and the interfacial polymerization method. However, for bursting beads with a thin wall material that meet the requirements of breaking pressure and food safety requirements and can achieve the encapsulation of water-soluble and alcohol-soluble flavors, there are currently no successful products or R & D solutions at home and abroad. Generally, hydrophobic materials such as plastics and waxes are used as the wall material at home and abroad in an attempt to prepare such bursting beads, but there are many defects in terms of safety and the quality required for cigarette materials. In recent years, many foreign cigarette brands have developed cigarette series products with bursting beads inserted, and the manufacturing technology of these products is relatively mature. However, domestic research started relatively late. Currently, it is mostly in the product development stage, with immature technology, difficult mass production, and unstable product quality, which lengthens the development cycle of such cigarette products.
[0004] Microfluidic technology can prepare emulsified droplets with uniform size and precise control and unique performance in terms of shape. In a single emulsion system, microcapsules can be obtained through phase separation, interfacial reaction, and assembly. Microcapsules can also be conveniently prepared from a multiple emulsion system through different shell curing processes, such as triggered polymerization, solvent evaporation, phase change, and desiccation. Since various substances can be used as the core and / or shell compositions, such microcapsules can be customized according to specific uses.
[0005] Existing cigarette popping beads usually use water-based polymers as wall materials, use the pellet method to make a prototype capsule, solidify the wall material by ion polymerization, and make brittle capsules after drying (Chinese patent publication numbers CN105536656 A, CN101564667A, CN102824887A, etc.). This type of hydrophilic wall material is usually used to prepare brittle capsules containing oil-soluble flavors and drug core materials. For water-soluble flavors / drugs, the existing method usually carries them in ester solvents that are miscible with water / alcohol (CN106215818A), so the carrying capacity is usually low, which seriously affects the product quality.
[0006] In view of this, the present invention is proposed. Summary of the invention
[0007] In view of the problems of low water packaging rate, difficult to control strength, and unsatisfactory water retention rate of water-packed bursting beads for cigarettes, the first purpose of the present invention is to provide a method for preparing water-packed bursting beads for cigarettes, aiming to prepare water-packed bursting beads for cigarettes with controllable strength, adaptable to the needs of cigarette use, and taking into account excellent water packaging rate and water retention rate.
[0008] The second purpose of the present invention is to provide water-explosive beads for cigarettes prepared by the preparation method and their application in cigarettes.
[0009] The third object of the present invention is to provide a cigarette product comprising the water-bursting beads for cigarette wrapping.
[0010] Different from capsules in other fields such as medicine, tobacco-use popping beads have special property control requirements in order to meet tobacco-use requirements. The prior art reports some ideas for forming popping beads by photocuring, but most of them are difficult to meet the property, preparation and smoking requirements of tobacco-use popping beads.
[0011] In view of the problems that the strength of water-encapsulated popping beads for cigarettes is difficult to control, the water-encapsulation rate, and the water retention effect are not ideal, most of the existing technologies directly use hydrophobic polymer solutions as wall materials. However, there are still problems such as poor controllability of the strength of the popping beads for cigarettes and difficulty in obtaining popping beads that meet the requirements of tobacco use. In view of this problem, the present invention proposes a preparation idea of water-encapsulated popping beads based on in-situ polymerization and curing of monomers to form hydrophobic wall materials. However, previous studies have shown that inappropriate in-situ polymerization methods are likely to lead to failure in the preparation of water-encapsulated popping beads, and the performance of the prepared water-encapsulated popping beads cannot adapt to the requirements of cigarette use. In view of this problem, the present invention has conducted in-depth research and provides the following improvement scheme:
[0012] A method for preparing water-packed popping beads for cigarettes, comprising the following steps:
[0013] Step (1):
[0014] Obtaining a hydrophobic wall material solution comprising a monomer of Formula 1 and a photoinitiator, and an aqueous core material solution comprising a functional additive;
[0015]
[0016] R1 is H or an alkyl group having 1 to 6 carbon atoms;
[0017] The functional auxiliary agent is PVA, and its concentration in the aqueous core material solution is 10 wt.% or more;
[0018] Step (2):
[0019] Using the drop pill method, the hydrophobic wall material solution is coated on the aqueous core material solution to form a prototype vesicle, and the prototype vesicle is placed in a curing solution for photoirradiation curing to obtain capsule A; wherein, the curing solution is an aqueous solution of a divalent electrolyte, and the concentration of the divalent electrolyte is 1.5 wt.% or more;
[0020] Step (3):
[0021] Capsule A is placed in a water retention agent-containing solution for osmotic treatment to obtain capsule B, wherein the concentration of the water retention agent in the water retention agent-containing solution is 30 wt.% or more;
[0022] Capsule B is subjected to wax sealing treatment to obtain the water-containing bursting beads for cigarettes.
[0023] Aiming at the problems that in-situ polymerization makes it difficult to successfully encapsulate and prepare water-containing bursting beads, and the strength, water encapsulation rate, water retention rate, etc. cannot meet the requirements of tobacco use, etc., based on the idea of constructing a water-containing structure by in-situ polymerization, the present invention further combines the monomer of formula 1, the functional auxiliary agent in the aqueous core material, the divalent electrolyte in the curing solution, and the osmotic treatment process and parameters of the water retention agent-containing solution. In this way, it can unexpectedly achieve synergy, and can successfully prepare water-containing bursting beads based on the in-situ polymerization method. Moreover, it can effectively control the strength, water encapsulation rate and water retention effect of the water-containing bursting beads.
[0024] In the present invention, the combination and synergy of the monomer of formula 1, the aqueous core material solution and the curing solution are one of the keys to realizing the preparation of the water-containing bursting beads for cigarettes.
[0025] In the present invention, R1 can be a straight-chain or branched-chain alkyl group having 1 to 6 carbon atoms. Further, in the monomer of formula 1, R1 is methyl or ethyl.
[0026] In the present invention, the photoinitiator can be any component in the industry that can promote photoinitiation, for example, it can be at least one of dimethoxybenzene, photoinitiator 617, and photoinitiator 614.
[0027] In the present invention, in the hydrophobic wall material solution, the content of the photoinitiator is 0.5-5 wt%, preferably 1-3 wt%. Considering the simplicity of the process, the remaining components can be the monomer of formula 1.
[0028] In the present invention, in the hydrophobic wall material, other auxiliary components such as liquid paraffin are also allowed to exist.
[0029] In the present invention, a water-soluble solution containing PVA is used as the core material, which is beneficial to combine with the monomer wall material of formula 1 and the curing liquid, synergistically improve the in-situ polymerization encapsulation effect, and further prepare a water-containing bursting bead suitable for the use requirements of tobacco.
[0030] In the present invention, a water-soluble additive is further added to the water-containing core material solution.
[0031] In the present invention, the water-soluble additive is a water-soluble additive allowed in tobacco products, preferably at least one of water-soluble flavors, harm reduction agents, atomizing agents, flavor correctors, auxiliary shaping agents, etc. The auxiliary shaping agent is, for example, a divalent electrolyte, and further can be calcium chloride.
[0032] In the present invention, in the water-containing core material solution, the content of the functional auxiliary agent is 10-30 wt.%, further preferably 10-15 wt.%;
[0033] Preferably, the content of the water-soluble additive in the water-containing core material solution is below 80 wt.%, preferably 1-50 wt.%;
[0034] In the present invention, the balance of the water-containing core material solution is water.
[0035] In the present invention, the hydrophobic wall material solution and the water-containing core material solution can be encapsulated by conventional means to obtain a prototype vesicle with the wall material coating the core material. For example, by means of a conventional coaxial double needle, the water-containing core material solution can be output synchronously through its inner hole, and the hydrophobic wall material solution can be output through its outer hole to achieve encapsulation.
[0036] In the present invention, during the dropping process, the volume flow ratio of the water-containing core material solution to the hydrophobic wall material solution is, for example, 1:1-6:1.
[0037] In the present invention, under the combination of the monomer wall material of formula 1 and the water-containing core material of the PVA functional auxiliary agent, it is further combined with a system containing a divalent electrolyte for curing, which is beneficial to the in-situ polymerization, reduces the breakage rate of the bursting bead, and regulates its strength.
[0038] In the present invention, the divalent electrolyte in the curing liquid is a water-soluble salt of at least one ion among Ca, Mg, and Zn, preferably at least one of chloride salts, nitrate salts, and acetate salts; preferably, the divalent electrolyte is calcium chloride.
[0039] In the present invention, in the curing liquid, the concentration of the divalent electrolyte is 2-5 wt.%; more preferably 2-4 wt.%.
[0040] In the present invention, during photoirradiation curing, the prototype vesicles are completely immersed in the curing liquid. For example, the liquid volume ratio of the curing liquid to the prototype vesicles is above 5 ml / g, preferably 10-50 ml / g.
[0041] In the present invention, the wavelength band of the light in the photoirradiation curing stage is 254-450 nm, and the light intensity is 0.2-20 w / cm 2 ;
[0042] In the present invention, the photoirradiation curing stage is carried out under stirring, and the stirring speed can be determined according to the preparation scale. For example, it can be less than or equal to 300 r / min, and further can be 100-200 r / min;
[0043] In the present invention, there is no special requirement for the time of photoirradiation curing, which can be determined according to the preparation scale. For example, it is 0.1-2 Min.
[0044] In the present invention, the capsule A is subjected to osmosis treatment in a water-retaining agent solution, and the concentration of the water-retaining agent during the treatment process is controlled, which is beneficial to improving the water-retaining ability of the bursting beads and helps to further improve the application advantages in the field of tobacco products.
[0045] In the present invention, the water-retaining agent solution is an aqueous solution containing a water-retaining agent. The water-retaining agent can be any component with water-retaining ability in the industry. For example, it can be at least one of glycerol and ethylene glycol;
[0046] In the present invention, in the water-retaining agent solution, the content of the water-retaining agent is 40-60 wt.%.
[0047] In the present invention, the wax-sealing process can be conventional in the industry.
[0048] The present invention also provides a water-containing bursting bead for cigarettes prepared by the above-mentioned preparation method.
[0049] The water-containing bursting bead for cigarettes prepared by the preparation method of the present invention has the special physical and chemical structural characteristics given by the preparation method, and the water-containing bursting bead prepared by the preparation method can unexpectedly match the usage requirements of tobacco products and can obtain excellent application effects in the field of tobacco.
[0050] The present invention also provides an application of the water-containing bursting beads prepared by the described preparation method, which is used to prepare tobacco products.
[0051] The present invention also provides a tobacco product, which contains the water-containing bursting beads prepared by the preparation method of the present invention.
[0052] In the tobacco product of the present invention, the water-containing bursting beads are arranged in the filter tip of the tobacco product.
[0053] In the present invention, based on the known tobacco preparation principles, methods and equipment, the water-containing bursting beads prepared by the present invention can be used to prepare the required tobacco products.
[0054] Beneficial effects:
[0055] 1) Based on the idea of in-situ polymerization to construct a water-containing structure, the present invention further combines the monomer of formula 1, the functional additives in the water-containing core material, the divalent electrolyte in the curing solution and the penetration treatment of the water-retaining agent solution, so as to unexpectedly achieve synergy, and can successfully prepare the water-containing bursting beads based on the in-situ polymerization method. Moreover, it can effectively control the strength, water content rate and water-retaining effect of the water-containing bursting beads.
[0056] The present invention can isolate the core material from the air environment, greatly reduce the quality loss of the water-based core material caused by long-term storage, realize the long-term and efficient encapsulation of water-soluble and alcohol-soluble core materials, and solve the bottleneck problem that hydrophilic core materials cannot be encapsulated for a long time in the industry; Description of the drawings
[0057] Figure 1 Brittle capsules (a, b) and wax-sealed brittle capsules (c) prepared in Example 1. Detailed implementation manners
[0058] The following further illustrates the present invention with specific examples, but does not limit the present invention in any way.
[0059] In the present invention, the described bursting beads can be prepared based on conventional dropping pill equipment.
[0060] In the following cases, unless otherwise specified, the water used is distilled water.
[0061] Example 1:
[0062] Step 1:
[0063] Core material solution: 10 wt.% functional additive (PVA), 2.2 wt.% calcium chloride, and the balance is distilled water;
[0064] Wall material solution: 1 wt.% dimethylbenzoin ether, with the balance being monomers (Formula 1-A, specifically Formula 1 where R is methyl).
[0065] UV curing solution: 3.3 wt.% aqueous solution of calcium chloride;
[0066] Penetrating solution: 50 wt.% aqueous solution of glycerol;
[0067] Step 2:
[0068] Input the above-mentioned core material and wall material into the inner tube and outer tube of the dropping pill nozzle respectively (inner tube inner diameter 2 mm, outer diameter 2.5 mm; outer tube inner diameter 3.5 mm, outer diameter 4 mm). Use the dropping method (the flow volume ratio of core material / wall material is 3:1) to prepare the prototype capsules. Drop the prototype capsules into the UV curing solution, and at the same time irradiate the entire curing tank with ultraviolet light of 365 nm with an intensity of 800 mW / cm 2 and apply uniform stirring at 120 rpm. Stop applying ultraviolet irradiation and stirring after the core material and wall material are completely consumed (the entire curing time in this case is 1 - 1.5 min). The brittle capsules obtained sink to the bottom of the curing tank, are collected, and capsule A is obtained;
[0069] Step 3:
[0070] Soak capsule A in the penetrating solution for 48 h, take it out and dry it at low temperature and high humidity (4 °C, humidity 60%), and store it at 4 °C to obtain brittle capsules (capsule B);
[0071] Step 4:
[0072] Perform conventional beeswax sealing treatment on capsule B to obtain the finished brittle capsules. The physical picture of the obtained product is shown in Figure 1 .
[0073] Experimental Example 1
[0074] Place the brittle capsules and the finished brittle capsules described in Example 1, as well as a commercially available brittle capsule product (Adous mixed flavor), on a mechanical testing machine, execute the compression program, and detect the crushing strength.
[0075] Table 1 Different capsule rupture strength tests
[0076]
[0077] The results in Table 1 show that the two brittle capsules produced in Example 1 have good performance in terms of structural stiffness and crushing strength compared with the commercially available products, and are significantly better than the existing commercially available products. The finished brittle capsules with secondary encapsulation using beeswax, compared with the brittle capsules without wax sealing, although sacrificing some stiffness due to the introduction of the wax layer, further improve the overall crushing strength of the capsules and optimize the toughness and stability of the capsule products.
[0078] Experimental Example 2:
[0079] The brittle capsule products described in Example 1 were stored at 37°C under environments with relative humidity (RH) of 10% and 60% respectively, and the quality changes at different time points were detected to measure their water retention ability.
[0080] Table 2 Water Retention Ability Test of Different Capsules
[0081]
[0082] The results in Table 2 show that among the two brittle capsules produced in Example 1 under dry conditions, the brittle capsule products obtained through the wax-sealing step showed better water retention ability compared to the unsealed capsules. The extremely small quality difference in the short term can be regarded as the drying process of the residual moisture on the shell surface. Under high humidity storage conditions, the quality changes of both capsule products can be ignored.
[0083] Example 2:
[0084] Compared with Example 1, the difference is only that the wall material solution in Step 1 was changed, and the experimental groups are as follows:
[0085] Group A: The monomer in the wall material solution was changed to Formula 1-B, specifically the monomer of Formula 1 with R1 being H;
[0086] Group B: The wall material solution was changed to a PEGDA solution (10wt% PEG600DA)
[0087] Group C: The components of the wall material solution were changed to Formula 1-A and liquid paraffin, with a volume fraction of 9 / 1
[0088] Group D: The components of the wall material solution were changed to Formula 1-A, liquid paraffin and beeswax, with a volume fraction of 9 / 1
[0089] The brittle capsules obtained in each group in Step 3 were used to detect the rupture strength of the above-mentioned products in each group by the method of Experimental Example 1. The results of each group in Example 2 were as follows:
[0090] Group A: Rupture strength 3.44 - 7.62 N, compression displacement 505.4 - 1023.6 μm
[0091] Group B: Rupture strength 5.45 - 12.47 N, compression displacement 1037.6 - 2021.3 μm
[0092] Group C: Rupture strength 1.02 - 5.71 N, compression displacement 104.2 - 352.1 μm
[0093] Group D: Rupture strength 2.33 - 8.41 N, compression displacement 94.1 - 238.9 μm
[0094] All of the above results are inferior to the product of the present invention in terms of crushing strength, and at the same time, there are obvious differences in terms of compression displacement, which cannot meet the application requirements of cigarette bursting beads. In summary, it shows that the formula of the present invention has significant advantages and beneficial effects.
[0095] Example 3:
[0096] Compared with Example 1, the difference is only that the core material solution in Step 1 is changed, and the experimental groups are as follows:
[0097] Group A: Change the content of the functional additive in the core material solution to 5 wt.%.
[0098] Group B: Change the content of the functional additive in the core material solution to 20 wt.%.
[0099] Group C: Change the content of the functional additive in the core material solution to 1 wt.%.
[0100] Group D: Change the content of the functional additive in the core material solution to 30 wt.%.
[0101] Group E: Replace the PVA with CTAB of the same concentration.
[0102] Group F: Replace the PVA with SDS of the same concentration.
[0103] Detect the product yield of the brittle capsules in Step 3 of each group above, that is, the integrity of the product shell structure.
[0104] The results of each group in Example 3 are as follows:
[0105] Example 1: Defective rate 0%; Group A: Defective rate 32.3%; Group B: Defective rate 0%; Group C: Defective rate 87.5%; Group D: Defective rate 0%; Group E: Defective rate 95.6%; Group F: Defective rate 100%;
[0106] The above results show that using the functional additive described in the present invention, when the content is above 10%, it can ensure the product integrity and 0 defective rate, and other additives with similar functions cannot obtain such beneficial effects; in addition, for the high additive content groups (B, D), although they can ensure 0 defective rate, excessive functional additives will significantly reduce the moisture content of the core components, which is not conducive to subsequent loading. In summary, it shows that the formula of the present invention has significant advantages and beneficial effects.
[0107] Example 4:
[0108] Compared with Example 1, the difference is only that the UV curing solution is changed, and the experimental groups are as follows:
[0109] Group A: Curing solution pure water;
[0110] Group B: The solidifying liquid is an aqueous solution of 3.3 wt.% magnesium chloride;
[0111] Group C: The solidifying liquid is an aqueous solution of 1 wt.% calcium chloride;
[0112] Group D: The solidifying liquid is an aqueous solution of 5 wt.% calcium chloride;
[0113] Group E: The solidifying liquid is an aqueous solution of 3.3 wt.% sodium chloride;
[0114] Group F: The solidifying liquid is an aqueous solution of 3.3 wt.% zinc chloride;
[0115] Group G: The solidifying liquid is an aqueous solution of 3.3 wt.% iron(III) chloride;
[0116] Group H: The solidifying liquid is an aqueous solution of 3.3 wt.% copper(II) chloride;
[0117] Detect the yield of the brittle capsule products obtained in Step 3 of each of the above groups, that is, the integrity of the product shell structure. The results of each group in Example 4 are as follows:
[0118] Group A: The defective rate is 78.4%; Group B: The defective rate is 0.1%; Group C: The defective rate is 35.3%; Group D: The defective rate is 0%; Group E: The defective rate is 75.5%; Groups F, G, and H: The defective rate is 0%;
[0119] The above results show that: (1) The introduction of cations with a valence of 2 or more helps to stabilize the interface, improve the product yield, and the improvement in efficiency is positively correlated with the ion concentration; (2) Although the high-valence ions have good interface stability ability, the heavy metal ions in Groups F to H are likely to remain in the product, causing safety problems.
[0120] Further, detect the bursting strength of the brittle capsule products obtained in Step 3 of Group B by the method of Experimental Example 1. The results are as follows: The crushing strength is 0.57 - 4.64 N, and the compression displacement is 35.5 - 91.0 μm. It shows that although magnesium ions have an interface stabilizing effect, they will directly affect the mechanical properties of the product. In summary, it shows that the formula of the present invention has significant advantages and beneficial effects.
[0121] Example 5:
[0122] Compared with Example 1, the only difference is that the permeating liquid is changed. The experimental groups are as follows:
[0123] Group A: The permeating liquid is pure water without glycerol;
[0124] Group B: The concentration of glycerol in the permeating liquid is 30%;
[0125] Group C: The concentration of glycerol in the permeating liquid is 80%;
[0126] Group D: The penetrant is an aqueous ethanol solution with an ethanol concentration of 80%.
[0127] Group E: The penetrant is an aqueous isopropanol solution with an isopropanol concentration of 80%.
[0128] Using the method described in Experimental Example 2, the water retention performance of the brittle capsule products obtained in Step 3 of each group was detected at 37°C and RH = 10%. The results of each group in Example 5 were as follows:
[0129] Group A: Weight loss of 1.63 ± 0.47 mg in 24 hours; Group B: Weight loss of 0.85 ± 0.23 mg in 24 hours; Group C: Weight loss of 0.23 ± 0.06 mg in 24 hours; Group D: Weight loss of 4.59 ± 1.77 mg in 24 hours; Group E: Weight loss of 3.24 ± 1.01 mg in 24 hours.
[0130] The above results show that when using glycerol as the penetrant, the water retention effect of the product improves with the increase in the glycerol content; cleaning and penetration with other common alcohols will significantly reduce the water retention ability of the product. In summary, it shows that the formula of the present invention has significant advantages and beneficial effects.
[0131] Example 6:
[0132] Compared with Example 1, the difference is only that the parameters of each solution are changed, and other operations and parameters are the same as in Example 1. Specifically:
[0133] Core material solution: 10 wt.% functional additive (PVA), the balance is distilled water;
[0134] Wall material solution: 1 wt.% benzoin dimethyl ether, 8.5 wt.% liquid paraffin, the balance is monomer (Formula 1-A, specifically Formula 1 where R is methyl)
[0135] UV curing solution: 2.7 wt.% aqueous calcium chloride solution;
[0136] Penetrant: 50 wt.% aqueous glycerol solution; other operations and parameters are the same as in Example 1. A similar bursting bead can be obtained as in Example 1.
[0137] For any person skilled in the art, without departing from the scope of the technical solution of the present invention, many possible changes and modifications can be made to the technical solution of the present invention by using the technical content disclosed above, or modified into equivalent embodiments with equivalent changes. Therefore, any simple modification, equivalent change, and modification made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention shall still fall within the scope of protection of the technical solution of the present invention.
Claims
1. A preparation method of a water-filled bursting bead for cigarettes, characterized in that the steps Comprising: Step (1): Obtain a hydrophobic wall material solution containing Formula 1 monomer and photoinitiator, and an aqueous core material solution containing functional additives; In the said Formula 1, R1 is H or an alkyl group with 1 - 6 carbon atoms; The functional additive is PVA, and its concentration in the aqueous core material solution is 10 wt.% or more; Step (2): Using the drop pill method, coat the aqueous core material solution with the hydrophobic wall material solution to form prototype vesicles, and place the prototype vesicles in a curing solution for photo - irradiation curing to obtain Capsule A; wherein, the curing solution is an aqueous solution of divalent electrolyte, and the concentration of the divalent electrolyte is 1.5 wt.% or more; Step (3): Place Capsule A in a solution containing water - retaining agent for osmotic treatment to obtain Capsule B, wherein the concentration of the water - retaining agent in the solution containing water - retaining agent is 30 wt.% or more; Perform wax - sealing treatment on Capsule B to obtain the water - filled bursting beads for cigarettes.
2. The preparation method of the water-filled bursting beads for cigarettes according to claim 1, wherein In the said Formula 1 monomer, R1 is methyl or ethyl.
3. The preparation method of the water-filled bursting beads for cigarettes according to claim 1, wherein, The photoinitiator is at least one of benzoin dimethyl ether, photoinitiator 614, and photoinitiator 617.
4. The preparation method of the water-filled bursting beads for cigarettes according to any one of claims 1 to 3, characterized in that, In the hydrophobic wall material solution, the content of the photoinitiator is 0.5 - 5 wt%, preferably 1 - 3 wt%.
5. The preparation method of the water-filled popping beads for cigarettes according to claim 1, wherein In the said aqueous core material solution, a water - soluble additive is further added.
6. The preparation method of the water-filled bursting beads for cigarettes according to claim 5, characterized in that, The water - soluble additive is a water - soluble additive allowed to be added in tobacco products, preferably at least one of water - soluble flavor, harm - reduction agent, atomizing agent, flavor - correcting agent, and auxiliary forming agent.
7. The preparation method of the water-bursting beads for cigarettes according to claim 1, 5 or 6, characterized in that In the said aqueous core material solution, the content of the functional additive is 10 - 30 wt.%; Preferably, the content of the water - soluble additive in the aqueous core material solution is 80 wt.% or less, preferably 1 - 50 wt.%.
8. The preparation method of the water-filled popping beads for cigarettes according to claim 1, characterized in that, During the dropping process, the volume ratio of the flow rate of the aqueous core material solution to the hydrophobic wall material solution is 1:1 - 6:
1.
9. The preparation method of the water-filled popping beads for cigarettes according to claim 1, wherein, The divalent electrolyte in the curing solution is a water - soluble salt of at least one ion of Ca, Mg, Zn, preferably at least one of chloride, nitrate, and acetate; preferably, the divalent electrolyte is calcium chloride.
10. The preparation method of the water-containing bursting beads for cigarettes according to claim 1 or 9, characterized in that, In the curing solution, the concentration of the divalent electrolyte is 2 - 5 wt.%; further preferably 2 - 4 wt.%.
11. The preparation method of the water-bursting beads for cigarettes according to claim 1, characterized in that, During photo - irradiation curing, the prototype vesicles are completely immersed in the curing solution; Preferably, the liquid volume ratio of the curing solution to the prototype vesicles is 5 ml / g or more, preferably 10 - 50 ml / g.
12. The preparation method of the water-filled bursting beads for cigarettes according to claim 1, characterized in that, The wavelength range of the light in the photoirradiation curing stage is 254 - 450 nm, and the light intensity is 0.2 - 20 w / cm 2 ; Preferably, the photo - irradiation curing stage is carried out under stirring, and the stirring speed is less than or equal to 300 r / min; Preferably, the time of photo - irradiation curing is 0.1 - 2 Min.
13. The preparation method of the water-filled popping beads for cigarettes according to claim 1, wherein, The solution containing water - retaining agent is an aqueous solution containing a water - retaining agent; Preferably, the water - retaining agent is at least one of glycerol and ethylene glycol; Preferably, in the solution containing water - retaining agent, the content of the water - retaining agent is 40 - 60 wt.%.
14. A water - filled bursting bead for cigarettes prepared by the preparation method according to any one of claims 1 - 13.
15. Use of the water-containing bursting beads for cigarettes prepared by the preparation method according to any one of claims 1 to 13, characterized in that, Use it for preparing tobacco products.
16. A tobacco product, characterized in that, Comprising a water - filled bursting bead for cigarettes prepared by the preparation method according to any one of claims 1 - 13.
17. The tobacco product according to claim 16, wherein, The said water - filled bursting bead for cigarettes is arranged in the filter tip of tobacco products.
Citation Information
Patent Citations
Method for preparing alginate soft capsule
CN101564667A
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CN102824887A
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CN105536656A
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CN106215818A