Water-soluble core material for use in smoking and method for preparing the same

Abstract

The application discloses a water-soluble core material cigarette explosion bead and a preparation method thereof. The explosion bead is composed of an outer layer wall material, an inner layer wall material and a core material. The outer layer wall material is gelatin, and the inner layer wall material is a blend containing a hydrophobic material, a wax material, a long-chain lipid and an interfacial adhesive. The interfacial adhesive is at least one selected from nano-mica sheet, nano-calcium carbonate and oleic acid amide. The core material is selected from a mixed solution or a solvent composed of a flavor and / or a natural extract and a solvent. The explosion bead of the application uses gelatin as the outer layer wall material to provide strength and ensure the roundness of the explosion bead. The inner layer wall material provides hydrophobicity. Meanwhile, the interfacial adhesive is used to improve the melt index of the blend and increase the bonding force between the outer layer wall material and the inner layer wall material. The three-layer structure ensures the water content, solves the problems of the strength and the roundness of the explosion bead, and improves the qualified rate of product preparation. The preparation method of the application adopts three-layer drop heads for one-time solidification forming, and is simple and controllable.

Description

Technical Field

[0001] This invention belongs to the field of cigarette technology, specifically relating to a water-soluble core material for cigarette flavoring beads and its preparation method. Background Technology

[0002] menthol capsule cigarettes are gaining popularity in the cigarette market because they offer various pre-selected flavors in addition to the aroma provided by regular tobacco combustion. Reducing tar content significantly impacts the taste of the smoke, and menthol capsules can compensate for this deficiency. Currently, menthol capsule cigarettes on the market primarily use oil-soluble flavorings. Although the aromatic flavor of oil-based flavorings can be removed through various methods, these oils generally have high viscosity, which, when soaked in the cigarette butt, can actually block the transmission of aroma. Furthermore, the variety of oil-soluble flavorings is limited, failing to meet the needs of diverse consumers. While water-soluble flavoring menthol capsules perfectly avoid these two shortcomings, they are not yet widely available in the market, largely due to the difficulty in preparing the wall material for water-soluble menthol capsules.

[0003] Domestic research on water-soluble flavor capsules for cigarettes has yielded fruitful results in recent years. However, the mechanisms and process conditions upon which these studies are based are often overly idealistic. Chinese patent CN109222226 A discloses a cigarette capsule encapsulating hydrogel beads and its preparation method. This patent's solution involves using hydrogel beads and a hydrophobic coating layer to form water-soluble flavor capsules. First, sodium alginate aqueous solution reacts with Ca ions to form a hydrogel. Then, a spraying process is used to atomize the hydrophobic material and uniformly spray it onto the surface of the hydrogel. While this method can produce water-soluble flavor capsules, it has several shortcomings. First, the sodium alginate hydrogel, after being popped, easily clogs the cigarette butt, affecting smoke flow and reducing the cigarette's taste. Second, the stable coexistence of the sodium alginate hydrogel and water-soluble flavor is a major challenge. Finally, the spraying process for the outer hydrophobic material is complex and requires high standards.

[0004] Chinese patent CN110973699 A discloses a water-bursting bead and its preparation method. This patent uses water-soluble fragrance, calcium chloride, and xanthan gum as core materials. The core material is dropped into a wall material adhesive prepared from sodium alginate and paraffin wax. Then, the sodium alginate in the wall material is modified by ion adsorption and hydrophobicity through fatty amines to obtain water-soluble fragrance bursting beads. However, this patent is overly idealistic. First, while xanthan gum can improve the surface tension of the core material, it also means a decrease in the selectivity of fragrance types available for the core material. Second, although dropping the core material into the wall material adhesive breaks the emulsion, a layer of unbroken emulsion remains on the surface, increasing cost and making subsequent cleaning difficult. Therefore, while this method has its feasibility, it suffers from low automation and high cost.

[0005] Chinese patent CN107361392 B discloses a three-layer water-containing capsule and its preparation method. This patent uses a phase-change oil layer as the inner layer to encapsulate a water-containing core material, and then uses natural animal and plant gums to encapsulate the oil layer to achieve water encapsulation. However, the materials used in the oil layer of this patent generally have a lipid-based aromatic flavor, and the oil layer wall thickness reaches 1.5 mm, which is close to half the diameter of the entire capsule. This will directly result in a very low core material content, which cannot meet the requirements for using water-soluble core material capsules in tobacco products.

[0006] Chinese patent CN110419775 A discloses a leak-proof water-bursting bead and its preparation method. This patent describes a three-layer capsule structure: an outer rubber layer made of polyacrylic acid resin and an inner rubber layer made of photosensitive resin. The inner rubber layer material is photocured, and the bead solidifies during the dripping process. After post-treatment, a second coating of adhesive is applied to encapsulate the polyacrylic acid resin layer, resulting in water-bursting beads with good sealing properties. However, this patent requires a secondary processing step, making the process cumbersome. Furthermore, the adhesive solution needs to be protected from light during both the preparation and dripping of the inner layer, significantly limiting the production conditions.

[0007] Chinese patent CN113367379 A discloses a tobacco product containing water-bursting beads in its filter tip. This patent employs a double-layer coating method, sequentially coating the inner core with an inner and outer coating layer. The resulting product exhibits good water retention and pressure values ​​that meet industry standards. However, this coating method requires segmented processing; for example, the inner layer coating requires alternating cycles, increasing the risk of contamination to the inner core and the entire product. Furthermore, after inner layer coating, it needs to be placed in hot water for curing, which can lead to uneven distribution of wax and oil in some coating layers due to surface tension.

[0008] In summary, although some theoretical methods have been explored in China regarding water-soluble core material burst beads, the processes are often cumbersome, impractical, and unsuitable for real-world application. Existing technologies, due to considerations of wall material strength and droplet roundness, often cannot be formed in a single droplet stage, generally requiring a secondary processing method, which brings inconvenience to production and application. Summary of the Invention

[0009] To address the shortcomings and current state of existing technologies, the first objective of this invention is to provide a water-soluble core material for cigarette flavoring beads; the second objective is to provide a method for preparing water-soluble core material for cigarette flavoring beads. The preparation method provided by this invention is simple, uses safe, reliable, and environmentally friendly raw materials, and has low cost, making it widely applicable in the field of cigarette technology.

[0010] To achieve the above objectives, the present invention provides the following technical solution:

[0011] This invention discloses a water-soluble core material for cigarette flavoring beads. The flavoring bead comprises 1-2 parts by weight of an outer wall material, 8-29 parts by weight of an inner wall material, and 70-90 parts by weight of a core material. The outer wall material is gelatin, and the core material is selected from a mixture of flavoring and / or natural extracts with a polar solvent or a polar solvent. The inner wall material is a blend containing hydrophobic materials, waxes, long-chain lipids, and an interfacial binder. The hydrophobic material is an ethylene-vinyl acetate copolymer, and the interfacial binder is selected from at least one of nano-mica sheets, nano-calcium carbonate, and oleamide.

[0012] The water-soluble core material for cigarettes of this invention, the burst capsule, has a three-layer concentric spherical capsule structure. Gelatin serves as the outer wall material to provide strength and ensure the sphericity of the burst capsule, while the inner wall material provides hydrophobicity. This three-layer structure, while ensuring the moisture content, solves both the burst capsule strength problem and improves the product yield. Of course, the weight ratio of the burst capsule material will have a certain impact on the material's performance. Within the scope of this invention, the final burst capsule material exhibits optimal performance. However, if the outer wall material's weight ratio is too low, the burst capsule will have insufficient strength, be easily deformed, and fail to provide a satisfying "squeeze-to-pop" feel. Conversely, if the outer wall material's weight ratio is too high, the burst capsule will have excessive strength and will be unable to burst.

[0013] In this invention, the inner wall material uses a hydrophobic material as the matrix. Considering that the core material is an aqueous solution that boils at 100°C under standard atmospheric pressure, which is unfavorable for the encapsulation process, waxes are added. This lowers the melting point of the blend while increasing its melt index and reducing its viscosity. When the wall material adhesive viscosity is too high, the dropped sample will exhibit a "tailing" phenomenon, and the resulting product cannot guarantee roundness. The addition of waxes increases the melt index and reduces the viscosity of the blend, thus avoiding the "tailing" phenomenon that occurs when the wall material adhesive viscosity is too high, preventing the resulting product from losing roundness. In addition, a small amount of interfacial binder is added to increase the melt index of the blend and enhance the bonding force between the outer and inner wall materials, thereby improving the compatibility and fit between the inner and outer wall materials and increasing the strength of the bursting bead material. The added long-chain lipids, whose end groups are mainly hydroxyl and carboxyl groups, can form hydrogen bonds with the outer gelatin, further enhancing the performance of the bursting beads and improving the strength of the bursting bead material.

[0014] In a preferred embodiment, the wax material is selected from at least one of solid paraffin wax, polyethylene wax, insect wax, and microcrystalline wax.

[0015] In a preferred embodiment, the long-chain lipid is selected from at least one of stearic acid, octadecanol, and oleic acid.

[0016] In a preferred embodiment, the inner wall material is composed of the following mass ratio: hydrophobic material: wax material: long-chain lipid: interfacial adhesive = 15-25: 69.5-85: 0-10: 0-0.5.

[0017] The inventors discovered that by controlling the mass ratio of hydrophobic materials to waxy materials within the above-mentioned range, the final burst beads achieved the highest pass rate and the strongest shatter resistance.

[0018] In a further preferred embodiment, the inner wall material, by mass ratio, comprises hydrophobic material: wax material: long-chain lipid: interfacial adhesive = 15-25: 69.5-85: 3-7: 0.3-0.7.

[0019] In a preferred embodiment, the interface adhesive is a mixture of nano-mica sheets, nano-calcium carbonate, and oleamide. The interface binder is prepared in the following mass ratio: nano-mica sheets: nano-calcium carbonate: oleamide = 0-2: 0-2: 0-2; preferably 1-2: 1-2: 1-2.

[0020] The interfacial binders selected in this invention, such as nano-calcium carbonate and nano-mica sheets rich in hydroxyl groups, can form hydrogen bonds with the carboxyl and amino groups of the outer gelatin molecules, increasing the interaction force between the inner and outer layers and making the bonding between them tighter. Oleamide provides cations that adsorb onto the carboxyl anions in the outer gelatin solution, thereby increasing the interfacial interaction between the outer and inner layers and improving the strength of the burst beads. When the above-mentioned interfacial binder formulation is used in the above proportions, the burst bead performance is optimal due to the synergistic effect of nano-mica sheets, nano-calcium carbonate, and oleamide. However, the amount of interfacial binder added needs to be effectively controlled. If too much interfacial binder is added, it cannot be evenly dispersed in the blended hydrophobic wall material solution, thus damaging the film-forming properties and uniformity of the hydrophobic wall material, reducing the sample's pass rate and shatter resistance. Of course, there are many nanomaterials rich in hydroxyl groups. However, through a large number of experiments, this invention found that only the addition of nano-calcium carbonate and nano-mica sheets can improve performance. For example, the inventors also tried nano-silica during the experiment, but its addition did not bring about performance improvement, but instead caused performance to decline.

[0021] In a preferred embodiment, the polar solvent is selected from at least one of water, ethanol, propylene glycol, and glycerol.

[0022] This invention does not limit the types of fragrances and natural extracts; any water-soluble or alcohol-soluble fragrances or natural extracts commonly used in current technology can be used. Examples include natural green tea extract, rose fragrance, jasmine fragrance, peppermint fragrance, sandalwood fragrance, pineapple fragrance, and lemon fragrance.

[0023] This invention discloses a method for preparing water-soluble core material cigarette capsules, comprising the following steps: adding gelatin to water and heating to obtain an outer wall material adhesive solution; mixing and melting wax materials, long-chain lipids, hydrophobic materials, and interface binders according to a designed ratio to obtain an inner wall material adhesive solution; mixing fragrance and / or natural extracts with a polar solvent and heating to obtain a core material; then dripping the outer wall material adhesive solution, the inner wall material adhesive solution, and the core material into a cooling liquid through the outer, middle, and inner layers of a three-layer dripper, respectively, and curing and drying to obtain water-soluble core material cigarette capsules.

[0024] The preparation method of this invention involves obtaining water-soluble core material cigarette popping beads through a three-layer coating and dripping process. The outer layer adhesive, inner layer wall material adhesive, and core material are dripped into a cooling liquid through three layers of droppers, and then rapidly cooled and solidified. Upon contact with the cooling liquid, the outer layer adhesive rapidly cools below its freezing point and solidifies, while the inner layer wall material adhesive also solidifies rapidly due to the ambient temperature dropping below its freezing point, thus coating the core material. The popping beads are then discharged from the dropper via a cooling liquid circulation system. The beads are collected, washed to remove residual cooling liquid, and dried to obtain the water-soluble core material cigarette popping bead product.

[0025] In a preferred embodiment, gelatin is added to water and stirred at 60℃~85℃ for 1~2 hours, followed by ultrasonication for 30min~60min to obtain the outer wall material adhesive solution.

[0026] In this invention, gelatin is added to deionized water and stirred thoroughly under heating. After the gelatin has fully absorbed the water, stirring continues until the aqueous solution is homogeneous and free of lumps. Then, the air bubbles generated by stirring are removed by ultrasonication to obtain the outer wall material adhesive solution, which is then kept warm and ready for use.

[0027] In a preferred embodiment, the mass ratio of gelatin to water is 4-6:94-96.

[0028] In a preferred embodiment, the viscosity of the outer wall material adhesive is 20 mPas to 400 mPas.

[0029] In a further preferred embodiment, the viscosity of the outer wall material adhesive is 250 mPas to 400 mPas.

[0030] In this invention, heating can eliminate air bubbles in the gelatin, as the presence of air bubbles can cause defects and make the dripped product unqualified. In addition, heating can control the viscosity of the gelatin within the range of this invention to achieve the best performance of the final bursting beads. If the viscosity is too high, it will cause a "tailing" phenomenon in the dripping process and make it impossible to guarantee the roundness. If the viscosity is too low, it will result in too low solid content of the glue and insufficient strength of the outer wall material.

[0031] In a preferred embodiment, wax materials, long-chain lipids, hydrophobic materials, and interface binders are mixed according to the design ratio, heated to 120℃~140℃ and kept at that temperature for 2~3 hours to melt and obtain a mixture. Then, the mixture is cooled to 80℃~100℃, preferably 90℃~100℃, to obtain the inner wall material adhesive.

[0032] In a preferred embodiment, the viscosity of the inner wall material adhesive is 50 mPas to 300 mPas.

[0033] In a further preferred embodiment, the viscosity of the inner wall material adhesive is 200 mPas to 300 mPas.

[0034] In a preferred embodiment, the temperature of the core material is 60℃~80℃, preferably 70℃~80℃.

[0035] In actual operation, the three-layer dripper pelletizing machine is preheated, and the temperatures of each component are set. After heating, the preheated outer wall material adhesive, inner wall material adhesive, and core material are added to their respective adhesive tanks. A suitable flow rate is set, and the core material, molten inner wall material adhesive, and outer wall material adhesive converge at the three-layer dripper through the adhesive pipe and drip into the coolant. Upon contact with the coolant, the mixed droplets cool under surface tension, forming water-soluble core material burst beads. The cured burst beads are discharged from the pelletizing machine via a cooling circulation system. Washing liquid removes residual coolant from the surface, and the beads are collected and air-dried to obtain the final product.

[0036] In a preferred embodiment, the temperature of the three-layer dripper is 75℃~90℃, preferably 80℃~85℃.

[0037] In this invention, the temperature of the three-layer dripper needs to be effectively controlled. If the dripper temperature is too high, the core material will boil, resulting in defects such as bubbles in the core of the dripped popping beads. If the temperature is too low, the inner layer of adhesive will not be able to reach a melting state, making it impossible to drip.

[0038] In a preferred embodiment, the outer wall material adhesive, the inner wall material adhesive, and the core material are dripped into the coolant at a rate of 10-20 r / min: 2-10 r / min: 0.5-5 r / min, preferably 13-17 r / min: 3-7 r / min: 1-3 r / min.

[0039] The inventors discovered that by controlling the dripping rates of the outer wall material adhesive, the inner wall material adhesive, and the core material within the aforementioned range, it is possible to ensure that the particles are full and uniform, as well as to control the thickness of the inner and outer wall materials, thereby making the strength of the burst beads the most suitable.

[0040] In a preferred embodiment, the coolant is liquid paraffin oil.

[0041] The inventors discovered that only hydrophobic coolant can cool and cure the outer gelatin layer, while using liquid paraffin oil can ensure that the outer wall material is fully cured without introducing any odor.

[0042] In a preferred embodiment, the temperature of the coolant is 5℃ to 25℃, preferably 20℃ to 25℃.

[0043] In actual operation, after curing, the beads are washed with an ethanol-water solution and then dried with cold air at 20℃~25℃ to obtain the popping beads. The preferred mass ratio of ethanol to water is 95:5.

[0044] Beneficial effects:

[0045] 1. The wall material raw materials described in this invention are all non-toxic and harmless, and are inexpensive and easy to package and transport. The preparation method of the inner wall material adhesive is simple; the target product can be obtained by heating, melting, and blending in one pot without the need for catalysts, initiators, etc., which reduces costs, simplifies preparation, and protects the environment.

[0046] 2. In practical applications, this invention uses the above-mentioned optimal material ratio and the solution prepared under the above-mentioned optimal conditions as the wall material, and water and aqueous solutions as the core material. A dropper is used to efficiently produce a large number of water-soluble core material capsules under the action of three coaxial droppers. The product is automatically collected through a cooling system, resulting in a high degree of automation. The resulting finished product has full and uniform particles, moderate wall material thickness, a high pass rate, and strength and moisture content that meet the standards for cigarette capsules. This wall material has the advantages of simple production process, low production cost, no environmental pollution, and ease of large-scale industrial production in practical applications. Attached Figure Description

[0047] Figure 1 This is a photograph of the popping bead sample prepared in Example 1. It can be seen that the popping bead particles are full and uniform, with a smooth and flat surface.

[0048] Figure 2 The figure shows the shatter resistance of the samples. As can be seen from the figure, the shatter resistance of the examples is better than that of the comparative examples.

[0049] Figure 3 The figure shows the pass rate of the samples. As can be seen from the figure, the pass rate of the sample in the example is greater than 90%, which is significantly better than the pass rate of the sample in the comparative example.

[0050] Figure 4 The average particle size of the sample is shown in the figure. As can be seen from the figure, the average particle size of the sample in the example has smaller fluctuations, while the average particle size of the sample in the comparative example has larger fluctuations. Detailed Implementation

[0051] The present invention will now be described in detail through embodiments. It should be noted that the following embodiments are only for further illustration of the present invention and should not be construed as limiting the scope of protection of the present invention. Those skilled in the art can make some non-essential improvements and adjustments based on the above description of the present invention.

[0052] Comparison of performance evaluation of the popping beads prepared in each embodiment

[0053] (1) The pass rate of the popping beads is determined by random sampling. 100 popping beads are randomly selected to check whether they are broken and whether they are round.

[0054] (2) The diameter of the popping beads is measured with vernier calipers, and at least 20 beads are randomly measured.

[0055] (3) The crush resistance strength of the burst beads was determined by a miniature pressure sensor device, and at least 20 beads were randomly tested.

[0056] Example 1

[0057] Take 50g of gelatin, slowly add it to 950g of deionized water and stir for 1 hour. Heat it in an 85℃ water bath until the gelatin is completely dissolved in the water. Then, sonicate it at 85℃ for half an hour to remove the air bubbles generated by stirring to obtain gelatin with a viscosity of 350m·Pas. Continue to keep it warm for later use.

[0058] Take 74.5g of paraffin wax, heat to 130℃ and stir for 20 minutes until the paraffin wax is completely melted. Then add 20g of ethylene-vinyl acetate copolymer and 5g of stearic acid to the molten paraffin oil. Continue heating for 20 minutes until melted, then mechanically stir and add 0.5g of nano-mica flakes until uniformly mixed. Lower the oil bath temperature to 95℃ to obtain an inner wall material adhesive with a viscosity of 237 mPas, ready for use.

[0059] Take 150g of a natural green tea extract aqueous solution and heat it to 75℃. Pour the core material, inner layer blending solution, and outer layer wall material solution into the preheated pellet mill storage tank and let them stand at the desired temperature. Adjust the pump flow rate of the solution and core material. Once the flow rate is suitable, begin collecting. Flow rate setting parameters: outer layer solution: inner layer wall material solution: core material = 15:4:3, unit: r / min.

[0060] Under the influence of gravity, the outer layer wall material adhesive, the inner layer wall material adhesive, and the core material are dripped into a coolant through a three-layer dripper at 85℃ (outer layer, middle layer, and inner layer), and then into liquid paraffin oil at 20℃. Due to surface tension, the outer layer adhesive closes, forming sealed droplets. The outer gelatin layer rapidly cools and solidifies upon contact with the liquid paraffin oil, forming solidified droplets. The droplets are collected and repeatedly washed and dried with an ethanol-water solution.

[0061] The obtained samples have an average crush strength of 1.83 kgf, an average particle size of 3.42 mm, are uniform and regular, round and full, and have a pass rate of 97%.

[0062] Comparative Example 1

[0063] The other conditions were the same as in Example 1, except that 0.5g of nano-mica sheets were not added.

[0064] The samples obtained had an average crush strength of only 1.52 kgf, an average particle size of 3.49 mm, uneven wall thickness, and poor roundness, with a pass rate of only 83%.

[0065] Example 2

[0066] Take 50g of gelatin, slowly add it to 950g of deionized water and stir for 1 hour. Heat it in an 85℃ water bath until the gelatin is completely dissolved in the water. Then, sonicate it at 85℃ for half an hour to remove the air bubbles generated by stirring to obtain gelatin with a viscosity of 350m·Pas. Continue to keep it warm for later use.

[0067] Take 74.5g of polyethylene wax, heat to 130℃ and stir for 20 minutes until the polyethylene wax is completely melted. Then add 20g of ethylene-vinyl acetate copolymer and 5g of octadecyl alcohol to the molten polyethylene wax. Continue heating for 20 minutes until melted, then mechanically stir and add 0.5g of nano-calcium carbonate until uniformly mixed. Lower the oil bath temperature to 95℃ to obtain an inner wall material adhesive with a viscosity of 269 mPas, ready for use.

[0068] Take 150g of a natural green tea extract aqueous solution and heat it to 75℃. Pour the core material, inner layer blending solution, and outer layer wall material solution into the preheated pellet mill storage tank and let them stand at the desired temperature. Adjust the pump flow rate of the solution and core material. Once the flow rate is suitable, begin collecting. Flow rate setting parameters: outer layer solution: inner layer wall material solution: core material = 15:4:3, unit: r / min.

[0069] Under the influence of gravity, the outer layer wall material adhesive, the inner layer wall material adhesive, and the core material are dripped into a coolant through a three-layer dripper at 85℃ (outer layer, middle layer, and inner layer), and then into liquid paraffin oil at 20℃. Due to surface tension, the outer layer adhesive closes, forming sealed droplets. The outer gelatin layer rapidly cools and solidifies upon contact with the liquid paraffin oil, forming solidified droplets. The droplets are collected and repeatedly washed and dried with an ethanol-water solution.

[0070] The obtained samples have an average crush strength of 1.72 kgf, an average particle size of 3.51 mm, are uniform and regular, round and full, and have a pass rate of 93%.

[0071] Comparative Example 2

[0072] The other conditions were the same as in Example 2, except that 0.5g of nano calcium carbonate was not added.

[0073] The samples obtained had an average crushing strength of only 1.32 kgf, an average particle size of 3.31 mm, uneven wall thickness, and poor roundness, with a pass rate of only 79%.

[0074] Example 3

[0075] Take 50g of gelatin, slowly add it to 950g of deionized water and stir for 1 hour. Heat it in an 85℃ water bath until the gelatin is completely dissolved in the water. Then, sonicate it at 85℃ for half an hour to remove the air bubbles generated by stirring to obtain gelatin with a viscosity of 350m·Pas. Continue to keep it warm for later use.

[0076] Take 74.5g of insect wax, heat to 130℃ and stir for 20 minutes until the insect wax is completely melted. Then add 20g of ethylene-vinyl acetate copolymer and 5g of oleic acid to the molten insect wax. Continue heating for 20 minutes until melted, then mechanically stir and add 0.5g of oleic acid amide until uniformly mixed. Lower the oil bath temperature to 95℃ to obtain an inner wall material adhesive with a viscosity of 282 mPas, ready for use.

[0077] Take 150g of a natural green tea extract aqueous solution and heat it to 75℃. Pour the core material, inner layer blending solution, and outer layer wall material solution into the preheated pellet mill storage tank and let them stand at the desired temperature. Adjust the pump flow rate of the solution and core material. Once the flow rate is suitable, begin collecting. Flow rate setting parameters: outer layer solution: inner layer wall material solution: core material = 15:4:3, unit: r / min.

[0078] Under the influence of gravity, the outer layer wall material adhesive, the inner layer wall material adhesive, and the core material are dripped into a coolant through a three-layer dripper at 85℃ (outer layer, middle layer, and inner layer), and then into liquid paraffin oil at 20℃. Due to surface tension, the outer layer adhesive closes, forming sealed droplets. The outer gelatin layer rapidly cools and solidifies upon contact with the liquid paraffin oil, forming solidified droplets. The droplets are collected and repeatedly washed and dried with an ethanol-water solution.

[0079] The obtained samples have an average crush strength of 1.87 kgf, an average particle size of 3.47 mm, are uniform and regular, round and full, and have a pass rate of 92%.

[0080] Comparative Example 3

[0081] The other conditions were the same as in Example 3, except that 0.5g of oleamide was not added.

[0082] The samples obtained had an average crush strength of only 1.37 kgf, an average particle size of 3.57 mm, uneven wall thickness, and poor roundness, with a pass rate of only 86%.

[0083] Example 4

[0084] Take 50g of gelatin, slowly add it to 950g of deionized water and stir for 1 hour. Heat it in an 85℃ water bath until the gelatin is completely dissolved in the water. Then, sonicate it at 85℃ for half an hour to remove the air bubbles generated by stirring to obtain gelatin with a viscosity of 350m·Pas. Continue to keep it warm for later use.

[0085] Take 74.5g of microcrystalline wax, heat to 130℃ and stir for 20 minutes until the microcrystalline wax is completely melted. Then add 20g of ethylene-vinyl acetate copolymer and 5g of oleic acid to the molten microcrystalline wax. Continue heating for 20 minutes until melted, then mechanically stir and add 0.5g of nano-mica sheets until uniformly mixed. Lower the oil bath temperature to 95℃ to obtain an inner wall material adhesive with a viscosity of 271m·Pas, ready for use.

[0086] Take 150g of a natural green tea extract aqueous solution and heat it to 75℃. Pour the core material, inner layer blending solution, and outer layer wall material solution into the preheated pellet mill storage tank and let them stand at the desired temperature. Adjust the pump flow rate of the solution and core material. Once the flow rate is suitable, begin collecting. Flow rate setting parameters: outer layer solution: inner layer wall material solution: core material = 15:4:3, unit: r / min.

[0087] Under the influence of gravity, the outer layer wall material adhesive, the inner layer wall material adhesive, and the core material are dripped into a coolant through a three-layer dripper at 85℃ (outer layer, middle layer, and inner layer), and then into liquid paraffin oil at 20℃. Due to surface tension, the outer layer adhesive closes, forming sealed droplets. The outer gelatin layer rapidly cools and solidifies upon contact with the liquid paraffin oil, forming solidified droplets. The droplets are collected and repeatedly washed and dried with an ethanol-water solution.

[0088] The obtained samples have an average crush strength of 1.73 kgf, an average particle size of 3.41 mm, are uniform and regular, round and full, and have a pass rate of 96%.

[0089] Comparative Example 4

[0090] The other conditions are the same as in Example 4, except that the amount of nano-mica sheets added is 1.5g.

[0091] The samples obtained had an average crush strength of only 1.51 kgf, an average particle size of 3.37 mm, uneven wall thickness, and poor roundness, with a pass rate of only 82%.

[0092] Example 5

[0093] Take 50g of gelatin, slowly add it to 950g of deionized water and stir for 1 hour. Heat it in an 85℃ water bath until the gelatin is completely dissolved in the water. Then, sonicate it at 85℃ for half an hour to remove the air bubbles generated by stirring to obtain gelatin with a viscosity of 350m·Pas. Continue to keep it warm for later use.

[0094] Take 74.5g of paraffin wax, heat it to 130℃ and stir for 20 minutes until the paraffin wax is completely melted. Then add 20g of ethylene-vinyl acetate copolymer and 5g of octadecyl alcohol to the molten paraffin wax. Continue heating for 20 minutes until melted, then mechanically stir and add 0.2g of nano-mica flakes, 0.2g of nano-calcium carbonate, and 0.2g of oleamide until uniformly mixed. Lower the oil bath temperature to 95℃ to obtain an inner wall material adhesive with a viscosity of 237 mPas, which is ready for use.

[0095] Take 150g of a natural green tea extract aqueous solution and heat it to 75℃. Pour the core material, inner layer blending solution, and outer layer wall material solution into the preheated pellet mill storage tank and let them stand at the desired temperature. Adjust the pump flow rate of the solution and core material. Once the flow rate is suitable, begin collecting. Flow rate setting parameters: outer layer solution: inner layer wall material solution: core material = 15:4:3, unit: r / min.

[0096] Under the influence of gravity, the outer layer wall material adhesive, the inner layer wall material adhesive, and the core material are dripped into a coolant through a three-layer dripper at 85℃ (outer layer, middle layer, and inner layer), and then into liquid paraffin oil at 20℃. Due to surface tension, the outer layer adhesive closes, forming sealed droplets. The outer gelatin layer rapidly cools and solidifies upon contact with the liquid paraffin oil, forming solidified droplets. The droplets are collected and repeatedly washed and dried with an ethanol-water solution.

[0097] The obtained samples have an average crush strength of 1.81 kgf, an average particle size of 3.41 mm, are uniform and regular, round and full, and have a pass rate of 98%.

[0098] Example 6

[0099] The other conditions are the same as in Example 5, except that only 0.3g of nano-mica sheets and 0.3g of oleic acid amide are added to the interface binder.

[0100] The average crushing strength of the obtained samples was only 1.76 kgf, the average particle size was 3.44 mm, and the pass rate was 97%.

[0101] Example 7

[0102] The other conditions were the same as in Example 5, except that 10g of octadecyl alcohol was added to the long-chain lipids.

[0103] The obtained samples had an average crushing strength of 1.74 kgf, an average particle size of 3.43 mm, and a pass rate of 90%.

[0104] Example 8

[0105] The other conditions are the same as in Example 5, except that no long-chain lipids were added.

[0106] The obtained samples had an average crushing strength of 1.71 kgf, an average particle size of 3.42 mm, and a pass rate of 90%.

[0107] As can be seen from the examples, the average particle size of the sample samples was between 3.40 mm and 3.50 mm, indicating that the pelletizing process of the pellet mill was stable and the process parameters were well adjusted. In contrast, the particle size of the comparative sample fluctuated significantly.

[0108] Under the condition of EVA content (20%), the results of Examples 1, 2, 3 and the corresponding comparative examples show that adding interfacial binders such as nano-mica sheets, nano-calcium carbonate, and oleamide can significantly enhance the shatter resistance of the burst beads, and the product qualification rate is also improved. This is because these interfacial binders, such as nano-calcium carbonate and nano-mica sheets, are rich in hydroxyl groups on their surface, which can form hydrogen bond interactions with the carboxyl and amino groups of the outer gelatin molecules, increasing the interaction force between the inner and outer layers, making the inner and outer layers more tightly bonded. When oleamide is added as an interfacial binder, since oleamide can provide cations, it can undergo ion adsorption with the carboxyl anions in the outer gelatin solution, thereby increasing the interfacial interaction between the outer and inner layers to a certain extent, and the resulting burst bead particles are also improved to a certain extent. From Example 4 and Comparative Example 4, it can be seen that adding an interfacial binder can improve the performance compared to the sample without it. However, when too much interfacial binder is added, it cannot be evenly dispersed in the blended hydrophobic wall material adhesive, thus damaging the film-forming properties and uniformity of the hydrophobic wall material, reducing the sample pass rate and shatter resistance. Examples 5 and 6 show that using multiple interfacial binders in combination can improve the performance of the burst beads, because a synergistic effect is formed between the interfacial binders. The slight decrease in strength when the number of different types is reduced also confirms the existence of this synergistic effect. Examples 5, 7, and 8 show that the presence of long-chain lipids further improves the performance of the burst beads, because the end groups of long-chain lipids are mainly hydroxyl and carboxyl groups, which can form hydrogen bonds with the outer gelatin layer, increasing strength to some extent. However, when there is too much long-chain lipid, the target sites in the gelatin that can form hydrogen bonds are occupied by the long-chain lipids, making it difficult to form hydrogen bonds with the interfacial binder, thus leading to a decrease in the strength of the burst beads. Therefore, considering factors such as industrialization costs, simply using 20% ​​EVA and waxes and long-chain lipids in a blend, and then adding 0.5% of the total mass of the blended adhesive as an interface binder, can significantly increase product strength, improve sample pass rate, and reduce cost waste caused by non-compliance rate.

Claims

1. A water-soluble core material for a smoking blast ball, characterized by comprising: The explosive beads are composed of 1-2 parts by weight of outer wall material, 8-29 parts by weight of inner wall material, and 70-90 parts by weight of core material, wherein the outer wall material is gelatin, the core material is selected from a mixed solution of essence and / or natural extract and polar solvent or polar solvent, and the inner wall material is a blend containing hydrophobic material, wax material, long-chain fat and interfacial binding agent, wherein the hydrophobic material is ethylene-vinyl acetate copolymer, and the interfacial binding agent is at least one of nano-mica sheet, nano-calcium carbonate and oleic acid amide. The wax material is at least one of solid paraffin, polyethylene wax, insect wax and microcrystalline wax. The long-chain fat is at least one of stearic acid, octadecanol and oleic acid. In the inner wall material, the mass ratio of hydrophobic material:wax material:long-chain fat:interfacial binding agent is 15-25:69.5-85:0-10:0-0.

5.

2. The water-soluble core material cigarette explosive beads according to claim 1, characterized in that: The interfacial binding agent is a mixture of nano-mica sheet, nano-calcium carbonate and oleic acid amide, and the mass ratio of nano-mica sheet:nano-calcium carbonate:oleic acid amide in the interfacial binding agent is 0-2:0-2:0-2.

3. The water-soluble core material for a smoking explosion ball according to claim 1, characterized by: The polar solvent is at least one of water, ethanol, propylene glycol and glycerol.

4. The method of claim 1-3, wherein the method is characterized by: The preparation method comprises the following steps: adding gelatin into water, heating to obtain outer wall material glue solution, mixing and melting wax material, long-chain fat, hydrophobic material and interfacial binding agent to obtain inner wall material glue solution according to the designed proportion, mixing essence and / or natural extract with polar solvent, and heating to obtain core material; and then the outer wall material glue solution, the inner wall material glue solution and the core material are dripped into a cooling liquid through the outer layer, the middle layer and the inner layer of a three-layer dripping head respectively, and solidified and dried to obtain water-soluble core material cigarette explosive beads.

5. The preparation method of the water-soluble core material cigarette explosive beads according to claim 4, characterized in that: The gelatin is added into water, stirred at 60-85°C for 1-2 h, and then ultrasonically treated for 30-60 min to obtain the outer wall material glue solution. The mass ratio of gelatin to water is 4-6:94-96. The viscosity of the outer wall material glue solution is 20-400 m·Pas.

6. The preparation method of the water-soluble core material cigarette explosive beads according to claim 4, characterized in that: The wax material, the long-chain fat, the hydrophobic material and the interfacial binding agent are mixed and heated to 120-140°C for 2-3 h to obtain a mixture, and then the temperature is reduced to 80-100°C. The viscosity of the inner wall material glue solution is 50-300 m·Pas. The temperature of the core material is 60-80°C.

7. The preparation method of the water-soluble core material cigarette explosive beads according to claim 4, characterized in that: The temperature of the three-layer dripping head is 75-90°C.

8. The preparation method of the water-soluble core material cigarette explosive beads according to claim 4, characterized in that: The outer layer wall material glue liquid, the inner layer wall material glue liquid and the core material are dropped into the cooling liquid at a dropping speed of 10-20 r / min:2-10 r / min:0.5-5 r / min.

9. The preparation method of the water-soluble core material smoke explosion beads according to claim 4, characterized in that: The cooling liquid is liquid paraffin oil; The temperature of the cooling liquid is 5-25 DEG C.

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