Water-soluble core material for tobacco and method for preparing the same

Abstract

The application discloses a water-soluble core material for a cigarette burst ball and a preparation method thereof. The burst ball is a three-layer concentric spherical capsule structure, which is formed by a three-layer coaxial drop head. The outer wall material of the burst ball is a hydrophilic material, which supports the inner core of the burst ball during the burst ball drop process, and guarantees the roundness and strength of the burst ball. The inner wall material of the burst ball is a hydrophobic polymer blend, which includes ethylene-vinyl acetate copolymer hydrophobic material, long-chain fatty, wax material and interface bonding agent. The core material is selected from a mixed solution of essence and / or natural extract and polar solvent or a polar solvent. The application introduces wax material and long-chain fatty into the inner wall material to reduce the melting temperature and the viscosity of the blend. The interface bonding agent is introduced to improve the melt index of the blend and increase the bonding force between the outer wall material and the inner wall material. The obtained burst ball product has moderate strength, good brittleness, high water packaging rate and water retention performance, high product qualified rate and meets the food safety requirements.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of cigarettes, and particularly relates to a water-soluble core material for cigarette burst beads and a preparation method thereof. BACKGROUND

[0002] Burst bead cigarettes are increasingly favored in the cigarette market because they can provide various pre-set flavors in addition to the aroma provided by conventional tobacco combustion. The reduction of tar will significantly affect the taste of smoke, and the placement of burst beads can make up for this deficiency. The burst bead cigarettes on the current market mainly use oil-soluble flavors, although the aromatic odor of the oil agent can be removed by multiple means, the oil agent generally has high viscosity, which can block the transmission of tobacco aroma after soaking in the filter, and the types of oil-soluble flavors are limited, which cannot meet the needs of different people. Although water-soluble flavor burst beads can perfectly avoid these two shortcomings, the water-soluble flavor burst beads on the current market are not yet in vogue, which is related to the difficulty in preparing the wall material of water-soluble burst beads.

[0003] Domestic research on water-soluble burst beads for cigarettes has also yielded fruitful results in recent years, but the mechanisms or process conditions of these studies are often idealized. Chinese patent CN109222226A discloses a cigarette capsule wrapped with hydrogel beads and a preparation method thereof. The scheme of this patent is to use hydrogel beads and a hydrophobic coating layer wrapped on the outside to form water-soluble flavor burst beads. First, a hydrogel is formed by complexing sodium alginate with Ca ions, and then a hydrophobic material is atomized and uniformly sprayed onto the surface of the hydrogel using a spraying process. Although this method can prepare water-soluble flavor burst beads, it has many shortcomings. First, the sodium alginate hydrogel is prone to block the filter after kneading, affecting the flow of smoke and reducing the taste of the cigarette. Second, the stable coexistence of sodium alginate hydrogel and water-soluble flavors is a major problem. Finally, the spraying process of the outer hydrophobic material is complex and requires high standards.

[0004] Chinese patent CN110973699A discloses a water burst bead and a preparation method thereof. This patent selects water-soluble flavors, calcium chloride, and xanthan gum as the core material, drops the core material into a wall material glue solution prepared from sodium alginate and paraffin as raw materials, and then performs ion adsorption and hydrophobic modification of the sodium alginate in the wall material by fatty amines to obtain water-soluble flavor burst beads. However, this patent is too idealized. First, the use of xanthan gum can improve the surface tension of the core material, but it also means that the selection of core material flavors is reduced. Second, the core material is dropped into the wall material glue solution, although the wall material is broken, a layer of unbroken glue solution is covered on the surface, which increases the cost and brings difficulties to subsequent cleaning. Therefore, although this method has some feasibility, it has the disadvantages of low automation degree and high cost.

[0005] Chinese patent CN107361392 B discloses a three-layer water-containing capsule and a preparation method thereof, which uses a phase-changeable grease layer as an inner layer to wrap a water-containing core material, and then wraps the grease layer with natural animal and plant glue to achieve the water wrapping function. However, the material used in the grease layer generally has a lipid material aroma, and the wall thickness of the grease layer reaches 1.5 mm, close to half of the diameter of the entire capsule, which will directly lead to a very low core material content ratio, and cannot meet the use of water-soluble core material blasting beads for cigarettes.

[0006] In summary, although some theoretical method explorations have been made in the field of water-soluble core material blasting beads in China at present, the process is complicated and not practical, and cannot be practically applied. In the prior art, due to the strength of the wall material and the roundness of the dripping, it is often impossible to be formed in one step, and a secondary processing method is generally used, which brings inconvenience to production and application. SUMMARY

[0007] In view of the deficiencies and status of the prior art, the first object of the present application is to provide a water-soluble core material for cigarette blasting beads; the second object of the present application is to provide a method for preparing a water-soluble core material for cigarette blasting beads. The preparation method provided by the present application has simple process, safe and reliable and environmentally friendly raw materials, and low cost, and can be widely applied in the field of cigarette technology.

[0008] In order to achieve the above-mentioned purposes, the present application provides the following technical solutions:

[0009] The water-soluble core material for cigarette blasting beads is a three-layer concentric spherical capsule structure, which is composed of 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. 2+ The inner wall material is a blend containing a hydrophobic material, a wax material, a long-chain lipid, and an interfacial bonding agent, the hydrophobic material is ethylene-vinyl acetate copolymer, the interfacial bonding agent is selected from at least one of nano-silicon dioxide, nano-calcium carbonate, and erucic acid amide, and the core material is selected from a mixed liquid composed of a flavor and / or a natural extract and a polar solvent or a polar solvent.

[0010] In the mass composition of the blasting bead material, the parts by weight of the outer wall material is the parts by weight of the sodium alginate glue.

[0011] The water-soluble core material smoke explosion bead material of the present application provides strength with calcium alginate gel as the outer layer wall material to ensure the roundness of the explosion bead, and the inner layer wall material provides hydrophobicity. This three-layer structure not only solves the problem of the strength of the explosion bead while ensuring the water content, but also improves the qualified rate of product preparation. Of course, the weight ratio of the explosion bead material will have a certain influence on the performance of the material. Within the scope of the present application, the performance of the finally obtained explosion bead material is optimal. However, when the mass ratio of the outer layer wall material is too low, the strength of the explosion bead will be too low, the explosion bead will be easy to change and cannot provide the "pinching explosion" feeling. When the mass ratio of the outer layer wall material is too high, the strength of the explosion bead will be too large and the explosion bead cannot be pinched.

[0012] As for the composition of the inner wall material, the present application uses a hydrophobic material as the base. Considering that the core material is an aqueous solution, it will boil at 100℃ under standard atmospheric pressure, which is not conducive to the inclusion process. Therefore, a wax material is added to reduce the melting point of the blend, improve the melt index of the blend, and reduce the viscosity of the blend. In this way, the "tail phenomenon" of the drop sample can be avoided when the viscosity of the wall material glue solution is too large. The roundness of the obtained product cannot be guaranteed. In addition, a small amount of interface bonding agent is added 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, thereby further enhancing the performance of the explosion bead.

[0013] In a preferred embodiment, the wax material is selected from at least one of solid paraffin, polyethylene wax, beeswax, and tree wax.

[0014] In a preferred embodiment, the mass ratio of the hydrophobic material to the wax material in the inner layer wall material is 15-25:69.5-85.

[0015] The inventors have found that when the mass ratio of the hydrophobic material to the wax material is controlled within the above range, the qualified rate of the final explosion bead is the highest, and the anti-crushing strength is the strongest.

[0016] In a preferred embodiment, the long-chain fat is selected from at least one of stearic acid and octadecanol, and the mass ratio of the wax material to the long-chain fat is 69.5-85:0-10, preferably 69.5-85:3-5.

[0017] The inventors have found that when the inner layer wall material further adds long-chain fat, the strength of the explosion bead material can be further improved. This is because the end groups of the long-chain fat are mainly hydroxyl and carboxyl groups, which can form hydrogen bonds with the outer layer sodium alginate glue solution, thereby improving the strength to a certain extent.

[0018] In a preferred embodiment, the mass ratio of the wax material to the interface bonding agent is 69-85:0-1, preferably 69.5-85:0.3-0.7.

[0019] Preferably, the interfacial binding agent is a mixture of nanosilica, nanocalcium carbonate and erucamide, and the mass ratio of nanosilica, nanocalcium carbonate and erucamide is 1-3:1-3:2-4.

[0020] In the present application, the interfacial binding agent nanocalcium carbonate and nanosilica are rich in hydroxyl groups and can form hydrogen bond interaction with the molecular chain of the outer layer sodium alginate glue solution, increase the interaction force between the inner layer and the outer layer, and make the combination of the inner layer and the outer layer more closely. When erucamide is added as the interfacial binding agent, the erucamide can provide cations and ion adsorb with the carboxyl anions in the outer layer sodium alginate glue solution, thereby increasing the interfacial interaction between the outer layer and the inner layer to a certain extent, and the obtained burst bead particles are also improved to a certain extent. When the interfacial binding agent is used in the above-mentioned proportion and formula, the performance of the burst beads is optimal under the synergistic effect of nanosilica, nanocalcium carbonate and erucamide. However, the amount of the interfacial binding agent needs to be effectively controlled. When the interfacial binding agent is added too much, it cannot be uniformly dispersed in the blended hydrophobic wall material glue solution, which damages the film-forming property and uniformity of the hydrophobic wall material, and reduces the pass rate and the crushing strength of the sample.

[0021] Preferably, the polar solvent is at least one selected from water, ethanol, propylene glycol and glycerol.

[0022] The types of the essence and natural extract are not limited in the present application, and the commonly used water-soluble or alcohol-soluble essence or natural extract in the prior art can be used. For example, natural green tea extract, rose essence, jasmine essence, mint essence, sandalwood essence, pineapple essence and lemon essence.

[0023] The preparation method of the water-soluble core material smoke burst bead material provided by the present application comprises the following steps: heating a sodium alginate aqueous solution to obtain a sodium alginate glue solution, mixing, melting and obtaining a mixed glue solution according to a designed proportion of waxy materials, long-chain fats, hydrophobic materials and interfacial binding agents, i.e. an inner layer wall material glue solution, mixing and heating an essence and / or natural extract with a polar solvent to obtain a core material; then dropping the sodium alginate glue solution, the inner layer wall material glue solution and the core material into a cooling liquid containing Ca 2+ through three-layer nozzles from the outer layer, the middle layer and the inner layer respectively to obtain solidified water burst beads by first solidification, and then adding the solidified water burst beads into an external cooling liquid for second solidification and drying to obtain the burst bead material.

[0024] The preparation method of the present application is to obtain water-soluble core material cigarette blasting beads by three-layer coating dripping. The outer layer glue solution, the inner layer wall material glue solution and the core material are dripped into the cooling liquid through the three-layer drop head and then rapidly cooled and solidified. The outer layer glue solution is cross-linked and solidified by reacting with Ca ions in the cooling liquid. The inner layer wall material glue solution is also rapidly solidified due to the decrease of the environmental temperature to below the melting point, thereby coating the core material. The preliminary solidified blasting beads are dripped into a secondary cooling tank through a cooling liquid circulation system, continuously solidified and washed, and then dried to obtain the water-soluble core material cigarette blasting bead product.

[0025] In the actual operation process, sodium alginate is added to deionized water and fully stirred. After the sodium alginate is fully hydrated, the stirring is continued until the water solution is uniform in texture without hard lumps, thereby obtaining a sodium alginate water solution.

[0026] In a preferred embodiment, the mass ratio of sodium alginate to water in the sodium alginate water solution is 1.5-2.5:97.5-98.5.

[0027] In a preferred embodiment, the temperature of the sodium alginate glue solution is 60-85°C.

[0028] In the actual operation process, the sodium alginate water solution is heated to 60-85°C, and after the air bubbles generated by stirring are removed, the solution is kept at the temperature, thereby obtaining the sodium alginate glue solution. The heating time is 1-2h.

[0029] In a preferred embodiment, the viscosity of the sodium alginate glue solution is 20-400m·Pas.

[0030] Further preferably, the viscosity of the sodium alginate glue solution is 250-400m·Pas.

[0031] In the present application, heating can remove air bubbles in the sodium alginate glue solution. The presence of air bubbles can cause defects in the dripping product, resulting in unqualified products. In addition, the viscosity of the sodium alginate glue solution should be controlled within the range of the present application to optimize the performance of the final blasting beads. If the viscosity is too high, it can cause a "tail" phenomenon during the dripping process, which cannot guarantee the roundness. If the viscosity is too low, it can result in a low solid content of the glue solution and insufficient strength of the outer layer wall material.

[0032] In a preferred embodiment, the wax material, long-chain fat, hydrophobic material and interfacial bonding agent are mixed according to the designed proportion, heated to 120-140°C and kept at the temperature for 2-3h to obtain a mixed glue solution. Then the temperature is reduced to 80-100°C, preferably 90-100°C, to obtain the inner layer wall material glue solution.

[0033] In a preferred embodiment, the viscosity of the inner layer wall material glue solution is 50-300m·Pas.

[0034] Further preferably, the viscosity of the inner layer wall material glue solution is 200 m·Pas to 300 m·Pas.

[0035] Preferably, the temperature of the core material is 60℃ to 80℃, preferably 70℃ to 80℃.

[0036] In actual operation, first, preheat the three-layer drop head drop pill machine, set the temperature of each part, after heating, add the preheated sodium alginate glue solution, inner layer wall material glue solution and water-soluble essence into the corresponding glue solution tank, set the appropriate flow rate, the core material, the molten inner layer wall material glue solution and the outer layer wall material glue solution are collected by the glue solution pipeline and dripped into the Ca 2+ containing cooling liquid by the three-layer drop head, when contacted with the cooling liquid, the mixed liquid droplets are cooled to form water-soluble core material smoke burst beads under the action of surface tension. The preliminary solidified burst beads are discharged from the cooling circulation system of the drop pill machine and enter the external cooling liquid tank for secondary solidification. After sufficient solidification, the product is collected and air-dried.

[0037] Preferably, the temperature of the three-layer drop head is 75℃ to 90℃, preferably 80℃ to 85℃.

[0038] In the present application, the temperature of the three-layer drop head needs to be effectively controlled. If the temperature of the drop head is too high, the core material will boil, and the burst beads obtained by dripping will have defects such as bubbles in the core. If the temperature is too low, the inner layer glue solution cannot reach the molten state, and cannot be dripped.

[0039] Preferably, the sodium alginate glue solution, the inner layer wall material glue solution and the core material are dripped into the Ca 2+ containing cooling liquid at a dropping speed of 10 to 20 r / min: 2 to 10 r / min: 0.5 to 5 r / min, preferably 15 to 20 r / min: 3 to 7 r / min: 2 to 4 r / min.

[0040] The inventors found that controlling the dropping speed of the sodium alginate glue solution, the inner layer wall material glue solution and the core material within the above range can ensure that the particles are full and uniform, and control the thickness of the inner and outer layers of the wall material, so that the strength of the burst bead particles is most suitable.

[0041] Preferably, the Ca 2+ containing cooling liquid is a mixed solution of propylene glycol, calcium chloride and water, and in the Ca 2+ containing cooling liquid, the mass ratio of propylene glycol: calcium chloride: water is 20 to 50: 0.5 to 2: 48 to 79.5, preferably 40 to 45: 1 to 1.5: 53.5 to 59.

[0042] Preferably, the temperature of the Ca 2+ containing cooling liquid is 5℃ to 25℃, preferably 15℃ to 17℃.

[0043] Preferably, the first solidification time is 30s~60s.

[0044] Preferably, the external cooling liquid is a calcium chloride-containing ethanol aqueous solution, and the mass ratio of calcium chloride: ethanol: water in the external cooling liquid is 1~3: 15~30: 67~84, preferably 1:20:79.

[0045] Preferably, the temperature of the external cooling liquid is 5℃~25℃, preferably 15℃~20℃.

[0046] Preferably, the second solidification time is 10 min~20 min.

[0047] In the present application, secondary solidification is adopted to ensure complete crosslinking of the outer layer glue solution and provide sufficient strength. In addition, by adopting the above-mentioned external cooling liquid ratio, unqualified products can be floated in the external cooling liquid, thereby screening out unqualified products and reducing the workload of subsequent screening processes.

[0048] In actual operation, after the second solidification, the collected water explosion beads are washed and then dried at 20℃~25℃ to obtain the finished explosion bead material.

[0049] Advantages

[0050] 1. The wall material raw materials in the present application are non-toxic and harmless, and the cost is low, which is convenient for packaging and transportation. The inner layer wall material glue solution preparation method is simple, and the target product can be obtained by one-pot heating, melting and blending without catalysts and initiators, which reduces the cost, simplifies the preparation difficulty, and protects the environment.

[0051] 2. In actual application, the above-mentioned optimal material ratio is adopted, the solution prepared under the above-mentioned optimal conditions is used as the wall material, water and aqueous solution are used as the core material, and a large number of water-soluble core material explosion beads are efficiently prepared under the action of a three-layer coaxial dripping head by using a drop pill machine; the product is automatically collected by circulation of a cooling system, and the degree of automation is high. The obtained finished product particles are full and uniform, the wall material thickness is moderate, the qualified rate is high, the strength and water content meet the standard of tobacco explosion beads.

[0052] The wall material has the advantages of simple production process, low production cost, no environmental pollution, and easy realization of large-scale industrial production in actual application. BRIEF DESCRIPTION OF DRAWINGS

[0053] Figure 1 The photos of the prepared explosion bead samples of Example 1 are shown in the following figures. Figure 1 (a) is a sample digital photo, from which it can be seen that the explosion bead particles are full and uniform, and the surface is smooth and flat, Figure 1(b) is a cross-section view of the sample; from Figure 1 (b) can be seen that the wall thickness is moderate, and the wall material thickness is uniform. Figure 1 (c) is a schematic diagram of the drop and sample structure, and the burst ball structure can be clearly seen from the drop process.

[0054] Figure 2 is the anti-crushing strength of the sample, and from the figure it can be seen that the anti-crushing strength of the example is better than that of the comparative example.

[0055] Figure 3 is the qualified rate of the sample, and from the figure it can be seen that the qualified rate of the example sample is greater than 90%, which is significantly better than the qualified rate of the comparative example sample.

[0056] Figure 4 is the average particle size of the sample, and from the figure it can be seen that the average particle size of the example sample fluctuates less, while the average particle size of the comparative example sample fluctuates more. DETAILED DESCRIPTION

[0057] The application will be specifically described by the following examples. It is necessary to point out here that the following examples are only used to further illustrate the application and cannot be understood as limiting the protection scope of the application. Those skilled in the art can make some non-essential improvements and adjustments according to the content of the above application.

[0058] Performance evaluation comparison of the burst balls prepared in each example

[0059] (1) The burst ball qualified rate adopts a random sampling method, and 100 burst balls are randomly checked to check whether the appearance is broken and the roundness.

[0060] (2) The burst ball diameter is measured by a vernier caliper, and at least 20 are randomly measured.

[0061] (3) The burst ball anti-crushing strength is determined by a micro pressure sensing device, and at least 20 are randomly tested.

[0062] Example 1

[0063] Take 25 g of sodium alginate, slowly add 975 g of deionized water and stir for 1 hour, after the sodium alginate is completely dissolved in water, remove the stirring device, heat in a 85℃ water bath to remove the air bubbles generated by stirring, obtain a sodium alginate glue liquid with a viscosity of 350 m·Pas, keep warm, and wait for use.

[0064] Take 74.5 g of paraffin wax, heat to 130℃ and stir for 20 minutes. After the paraffin wax is completely melted, add 20 g of ethylene-vinyl acetate copolymer and 5 g of stearic acid to the molten paraffin wax oil. Continue heating for 20 minutes, then mechanically stir and add 0.5 g of nano-silicon dioxide until the mixture is uniform. Reduce the oil bath temperature to 95℃ to obtain an inner wall material glue with a viscosity of 250 m·Pas, ready for use.

[0065] Take 150 g of natural green tea extract aqueous solution and heat to 75℃. Pour the core material, inner layer blend glue and outer layer wall material glue into the preheated drop pill machine storage tank respectively and keep warm. Prepare a propylene glycol-calcium chloride aqueous solution with a mass ratio of 45:1:54, cool to 20℃ and set aside. Adjust the flow rate of the glue and core material pumps, and then start collecting when the flow rate is suitable. The flow rate setting parameters are: outer layer glue: inner layer wall material glue: core material = 15:4:3, unit: r / min.

[0066] The water explosion beads are dropped into the propylene glycol-calcium chloride aqueous solution through the three-layer nozzle at a temperature of 85℃ under the action of gravity. Due to the surface tension, the outer layer glue closes to form a sealed water explosion bead. The outer layer sodium alginate reacts with the calcium ions in the cooling liquid to form a hydrogel, and the solidified water explosion beads are formed. After 45 seconds, the water explosion beads are collected and placed in an external cooling liquid tank. The temperature of the external cooling liquid is 20℃, which is an ethanol aqueous solution containing calcium chloride with a mass ratio of ethanol:calcium chloride:water of 15:1:84. The explosion beads are taken out after 15 minutes of continuous solidification, washed with flowing deionized water and dried.

[0067] The average crushing strength of the obtained sample can reach 1.76 kgf, the average particle size is 3.64 mm, the uniformity is good, the roundness is good, and the qualified rate can reach 95%.

[0068] Comparative Example 1

[0069] The other conditions are the same as in Example 1, except that 0.5 g of nano-silicon dioxide is not added.

[0070] The average crushing strength of the obtained sample is only 1.26 kgf, the average particle size is 3.51 mm, the wall thickness is not uniform and the roundness is poor, and the qualified rate is only 79%.

[0071] Example 2

[0072] Take 25 g of sodium alginate and slowly add it to 975 g of deionized water and stir for 1 hour. After the sodium alginate is completely dissolved in water, remove the stirring device and heat in a 85℃ water bath to remove the air bubbles generated by stirring to obtain a sodium alginate glue with a viscosity of 350 m·Pas, ready for use.

[0073] Take 74.5 g of polyethylene wax, heat to 130℃ and stir for 20 minutes. After the polyethylene wax is completely melted, add 20 g of ethylene-vinyl acetate copolymer and 5 g of stearic acid to the molten polyethylene wax oil. Continue heating for 20 minutes, then mechanically stir and add 0.5 g of nano calcium carbonate until the mixture is uniform. Reduce the oil bath temperature to 95℃ to obtain an inner wall material glue with a viscosity of 273 m·Pas, ready for use.

[0074] Take 150 g of natural green tea extract aqueous solution and heat to 75℃. Pour the core material, inner layer blended glue and outer layer wall material glue into the preheated drop pill machine storage tank respectively and keep warm. Prepare a propylene glycol-calcium chloride aqueous solution with a mass ratio of 45:1:54, cool to 20℃ and set aside. Adjust the flow rate of the glue and core material pump, and start collecting after the flow rate is suitable. The flow rate setting parameters are: outer layer glue: inner layer wall material glue: core material = 15:4:3, unit: r / min.

[0075] The water explosion beads are dropped into the propylene glycol-calcium chloride aqueous solution through the three-layer nozzle at a temperature of 85℃ under the action of gravity. Due to the action of surface tension, the outer layer glue closes to form a sealed water explosion bead. The outer layer sodium alginate reacts with calcium ions in the cooling liquid to form a hydrogel, forming a solidified water explosion bead. After 45 s, the water explosion beads are collected and placed in an external cooling liquid tank. The external cooling liquid is an ethanol-calcium chloride aqueous solution with a temperature of 20℃, a mass ratio of ethanol:calcium chloride:water of 15:1:84. The beads are taken out after 15 minutes of continuous solidification, washed with flowing deionized water and dried.

[0076] The average crushing strength of the obtained sample can reach 1.56 kgf, the average particle size is 3.60 mm, the uniformity is regular, the roundness is full, and the qualified rate can reach 91%.

[0077] Comparative Example 2

[0078] The other conditions are the same as in Example 2, except that 0.5 g of nano calcium carbonate is not added.

[0079] The average crushing strength of the obtained sample is only 1.16 kgf, the average particle size is 3.67 mm, the wall thickness is not uniform and the roundness is poor, and the qualified rate is only 71%.

[0080] Example 3

[0081] Take 25 g of sodium alginate and slowly add it to 975 g of deionized water and stir for 1 hour. After the sodium alginate is completely dissolved in water, remove the stirring device and heat in a 85℃ water bath to remove the air bubbles generated by stirring. A sodium alginate glue with a viscosity of 350 m·Pas is obtained, which is kept warm and ready for use.

[0082] Take 74.5 g of beeswax, heat to 130℃ and stir for 20 minutes until the beeswax is completely melted. Then add 20 g of ethylene-vinyl acetate copolymer and 5 g of octadecyl alcohol to the molten beeswax oil. Continue heating for 20 minutes until melted, then mechanically stir and add 0.5 g of erucamide until uniformly mixed. Lower the oil bath temperature to 95℃ to obtain an inner wall material adhesive with a viscosity of 257 m·Pas, ready for use.

[0083] Take 150 g of 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 keep them at a constant temperature. Prepare a propylene glycol-calcium chloride aqueous solution at a mass ratio of 45:1:54, cool it to 20℃, and set it aside for later use. Adjust the pump flow rate of the adhesive solution and core material. Once the flow rate is suitable, begin collecting. Flow rate setting parameters: outer layer adhesive solution: inner layer wall material adhesive solution: core material = 15:4:3, unit: r / min.

[0084] Under the influence of gravity, water-bursting beads are dropped into a propylene glycol-calcium chloride aqueous solution through a three-layer dropper at 85°C. Due to surface tension, the outer layer of the solution closes, forming a sealed water-bursting bead. The outer sodium alginate layer coordinates with calcium ions in the calcium chloride in the coolant, cross-linking to form a hydrogel, thus solidifying the water-bursting bead. After 45 seconds, the water-bursting beads are collected and placed back into an external coolant tank at 20°C. This coolant is an ethanol-water aqueous solution containing calcium chloride, with a ratio of ethanol:calcium chloride:water of 15:1:84. After further solidification for 15 minutes, the beads are removed, washed with running deionized water, and dried.

[0085] The obtained samples have an average crush strength of 1.72 kgf, an average particle size of 3.65 mm, are uniform and regular, round and full, and have a pass rate of 98%.

[0086] Comparative Example 3

[0087] The other conditions were the same as in Example 3, except that 0.5 g of erucamide was not added.

[0088] The samples obtained had an average crushing strength of only 1.23 kgf, an average particle size of 3.58 mm, uneven wall thickness, and poor roundness, with a pass rate of only 77%.

[0089] Example 4

[0090] Take 25 g of sodium alginate, slowly add it to 975 g of deionized water and stir for 1 hour. After the sodium alginate is completely dissolved in the water, remove the stirring device and heat it in an 85°C water bath to remove the air bubbles generated by stirring. A sodium alginate solution with a viscosity of 350 m·Pas is obtained. Keep it warm and set aside for later use.

[0091] Take 74.5 g of tree wax, heat to 130℃ and stir for 20 minutes. After the tree wax is completely melted, add 20 g of ethylene-vinyl acetate copolymer and 5 g of octadecanol to the molten beeswax oil. Continue heating for 20 minutes, then mechanically stir and add 0.5 g of erucic acid amide until the mixture is uniform. Reduce the oil bath temperature to 95℃ to obtain an inner wall material glue solution with a viscosity of 261 m·Pas, ready for use.

[0092] Take 150 g of natural green tea extract aqueous solution and heat to 75℃. Pour the core material, inner layer blend glue solution and outer layer wall material glue solution into the preheated drop pill machine storage tank respectively and keep warm. Prepare a propylene glycol-calcium chloride aqueous solution with a mass ratio of 45:1:54, cool to 20℃ and set aside. Adjust the flow rate of the glue solution and core material pump, and start collecting after the flow rate is suitable. The flow rate setting parameters are: outer layer glue solution: inner layer wall material glue solution: core material = 15:4:3, unit: r / min.

[0093] The water explosion beads are dropped into the propylene glycol-calcium chloride aqueous solution through the three-layer nozzle at a temperature of 85℃ under the action of gravity. Due to the surface tension, the outer layer glue solution closes to form a sealed water explosion bead. The outer layer sodium alginate reacts with the calcium ions in the cooling liquid to form a hydrogel, and the solidified water explosion beads are formed after 45s. Collect the water explosion beads and put them into the external cooling liquid tank again. The temperature of the external cooling liquid is 20℃, which is an ethanol aqueous solution containing calcium chloride with a mass ratio of ethanol:calcium chloride:water of 15:1:84. Take out the beads after 15 minutes of continuous solidification, wash with flowing deionized water and dry.

[0094] The average crushing strength of the obtained sample can reach 1.51 kgf, the average particle size is 3.61 mm, the uniformity is regular, the roundness is full, and the qualified rate can reach 91%.

[0095] Comparative Example 4

[0096] The other conditions are the same as in Example 4, except that 0.5 g of erucic acid amide is not added.

[0097] The average crushing strength of the obtained sample is only 1.03 kgf, the average particle size is 3.58 mm, the wall thickness is not uniform and the roundness is poor, and the qualified rate is only 70%.

[0098] Example 5

[0099] Take 25 g of sodium alginate and slowly add it to 975 g of deionized water and stir for 1 hour. After the sodium alginate is completely dissolved in water, remove the stirring device and heat in a 85℃ water bath to remove the air bubbles generated by stirring to obtain a sodium alginate glue solution with a viscosity of 350 m·Pas, keep warm and ready for use.

[0100] Take 74.5 g of paraffin wax, heat to 130℃ and stir for 20 minutes. After the paraffin wax is completely melted, add 20 g of ethylene-vinyl acetate copolymer and 5 g of octadecanol to the molten paraffin wax oil. Continue heating for 20 minutes, then mechanically stir and add 0.5 g of nano calcium carbonate until the mixture is uniform. Reduce the oil bath temperature to 95℃ to obtain an inner wall material glue with a viscosity of 257 m·Pas, ready for use.

[0101] Take 150 g of natural green tea extract aqueous solution and heat to 75℃. Pour the core material, inner layer blended glue and outer layer wall material glue into the preheated drop pill machine storage tank respectively and keep warm. Prepare a propylene glycol-calcium chloride aqueous solution with a mass ratio of 45:1:54, cool to 20℃ and set aside. Adjust the flow rate of the glue and core material pump, and start collecting after the flow rate is suitable. The flow rate setting parameters are: outer layer glue: inner layer wall material glue: core material = 15:4:3, unit: r / min.

[0102] The water explosion beads are dropped into the propylene glycol-calcium chloride aqueous solution through the three-layer nozzle at a temperature of 85℃ under the action of gravity. Due to the surface tension, the outer layer glue closes to form a sealed water explosion bead. The outer layer sodium alginate reacts with the calcium ions in the cooling liquid to form a hydrogel, and the solidified water explosion beads are formed. After 45 s, the water explosion beads are collected and placed in an external cooling liquid tank. The temperature of the external cooling liquid is 20℃, which is an ethanol aqueous solution containing calcium chloride with a mass ratio of ethanol:calcium chloride:water of 15:1:84. The explosion beads are taken out after 15 minutes of continuous solidification, washed with flowing deionized water and dried.

[0103] The average crushing strength of the obtained sample can reach 1.77 kgf, the average particle size is 3.62 mm, the shape is uniform and regular, the roundness is full, and the qualified rate can reach 98%.

[0104] Comparative Example 5

[0105] The other conditions are the same as in Example 5, except that the amount of nano calcium carbonate added is 1.5 g.

[0106] The average crushing strength of the obtained sample is only 1.43 kgf, the average particle size is 3.55 mm, and the qualified rate is 87%.

[0107] Example 6

[0108] Take 25 g of sodium alginate and slowly add it to 975 g of deionized water and stir for 1 hour. After the sodium alginate is completely dissolved in water, remove the stirring device and heat in a 85℃ water bath to remove the air bubbles generated by stirring. A sodium alginate glue with a viscosity of 350 m·Pas is obtained, which is kept warm and ready for use.

[0109] Take 74.5 g of beeswax, heat to 130℃ and stir for 20 minutes, then add 20 g of ethylene-vinyl acetate copolymer and 5 g of octadecanol to the molten paraffin oil. Continue heating for 20 minutes, then melt, mechanically stir and add 0.2 g of nano calcium carbonate, 0.2 g of nano silicon dioxide and 0.3 g of erucic acid amide until well mixed. Reduce the oil bath temperature to 95℃ to obtain an inner wall material glue with a viscosity of 259 m·Pas, ready for use.

[0110] Take 150 g of natural green tea extract aqueous solution and heat to 75℃. Pour the core material, inner layer blended glue and outer layer wall material glue into the preheated drop pill machine storage tank respectively and keep warm. Prepare a propylene glycol-calcium chloride aqueous solution with a mass ratio of 45:1:54, cool to 20℃ and set aside. Adjust the flow rate of the glue and core material pumps, and when the flow rate is suitable, start collecting. The flow rate setting parameters are: outer layer glue: inner layer wall material glue: core material = 15:4:3, unit: r / min.

[0111] The water explosion beads are dropped into the propylene glycol-calcium chloride aqueous solution through the three-layer nozzle at a temperature of 85℃ under the action of gravity. Due to the surface tension, the outer layer glue closes to form a sealed water explosion bead. The outer layer sodium alginate reacts with the calcium ions in the cooling liquid to form a hydrogel, and the solidified water explosion beads are formed. After 45 s, the water explosion beads are collected and placed in an external cooling liquid tank. The temperature of the external cooling liquid is 20℃, which is an ethanol aqueous solution containing calcium chloride with a mass ratio of 15:1:84. The explosion beads are taken out after 15 minutes of continuous solidification, washed with flowing deionized water and dried.

[0112] The average crushing strength of the obtained sample can reach 1.79 kgf, the average particle size is 3.62 mm, the shape is uniform and regular, the roundness is full, and the qualified rate can reach 98%.

[0113] Example 7

[0114] The other conditions are the same as in Example 6, except that the interfacial bonding agent is only 0.4 g of nano calcium carbonate and 0.3 g of erucic acid amide.

[0115] The average crushing strength of the obtained sample is only 1.74 kgf, the average particle size is 3.61 mm, and the qualified rate is 94%.

[0116] Example 8

[0117] Take 25 g of sodium alginate and slowly add it to 975 g of deionized water and stir for 1 hour. After the sodium alginate is completely dissolved in water, remove the stirring device and heat in a 85℃ water bath to remove the air bubbles generated by stirring to obtain a sodium alginate glue with a viscosity of 350 m·Pas, keep warm and ready for use.

[0118] Take 74.5 g of tree wax, heat to 130℃ and stir for 20 minutes, then add 20 g of ethylene-vinyl acetate copolymer and 5 g of stearic acid to the molten tree wax oil. Continue heating for 20 minutes, then melt, mechanically stir and add 0.5 g of erucic acid amide until well mixed. Reduce the oil bath temperature to 95℃ to obtain an inner wall material glue solution with a viscosity of 257 m·Pas, ready for use.

[0119] Take 150 g of natural green tea extract aqueous solution and heat to 75℃. Pour the core material, inner layer blended glue solution and outer layer wall material glue solution into the preheated drop pill machine storage tank respectively and keep warm. Prepare a propylene glycol-calcium chloride aqueous solution with a mass ratio of 45:1:54, cool to 20℃ and set aside. Adjust the flow rate of the glue solution and core material pump, and when the flow rate is suitable, start collecting. The flow rate setting parameters are: outer layer glue solution: inner layer wall material glue solution: core material = 15:4:3, unit: r / min.

[0120] The water explosion beads are dropped into the propylene glycol-calcium chloride aqueous solution through the three-layer nozzle at a temperature of 85℃ under the action of gravity. Due to the action of surface tension, the outer layer glue solution closes to form a sealed water explosion bead. The outer layer sodium alginate reacts with calcium ions in the cooling liquid to form a hydrogel, forming a solidified water explosion bead. After 45 s, the water explosion beads are collected and placed in an external cooling liquid tank. The external cooling liquid is an ethanol aqueous solution containing calcium chloride with a mass ratio of ethanol:calcium chloride:water of 15:1:84, and the temperature is 20℃. The explosion beads are taken out after 15 minutes of continuous solidification, washed with flowing deionized water and dried.

[0121] The average crushing strength of the obtained sample can reach 1.57 kgf, the average particle size is 3.62 mm, the shape is uniform and regular, the surface is smooth and full, and the qualified rate can reach 93%.

[0122] Example 9

[0123] The other conditions are the same as in Example 8, except that 5 g of stearic acid is not added.

[0124] The average crushing strength of the obtained sample is 1.48 kgf, the average particle size is 3.63 mm, and the qualified rate is 86%.

[0125] From the examples, it can be seen that the average particle size of the sample is between 3.60 mm and 3.65 mm, indicating that the drop pill machine works smoothly during the drop process and the process parameters are well adjusted. The particle size of the sample of the comparative example fluctuates obviously.

[0126] And in the condition of EVA proportion (20%), from the results of example 1, 2, 3, 4 and the corresponding comparative examples, it can be seen that the addition of interface binding agents such as nano-silicon dioxide, nano-calcium carbonate and erucic amide can obviously enhance the anti-crushing strength of the burst beads, and the product qualified rate is also improved. This is because the surface of these interface binding agents such as nano-calcium carbonate and nano-silicon dioxide is rich in hydroxyl groups, which can form hydrogen bond interaction with the molecular chain of the outer layer of sodium alginate glue solution, increase the interaction force between the inner and outer layers, and make the inner and outer layers more closely combined. When erucic amide is added as an interface binding agent, the erucic amide can provide cations and ion adsorb with the carboxyl anions in the outer layer of sodium alginate glue solution, thereby increasing the interface interaction between the outer and inner layers to a certain extent, and the obtained burst bead particles are also improved to a certain extent. From example 5 and comparative example 5, it can be found that the addition of interface binding agents can improve the performance compared with the sample without adding. However, when too much interface binding agent is added, the film-forming property and uniformity of the hydrophobic wall material glue solution are destroyed due to the uneven dispersion, which reduces the qualified rate and anti-crushing strength of the sample. From example 6 and example 7, it can be found that the use of multiple interface binding agents can improve the performance of the burst beads, because the interface binding agents form a synergistic effect. When the number of types is reduced, the slight decrease in strength also confirms the existence of synergistic effect. From example 8 and example 9, it can be found that the presence of long-chain lipids improves the performance of the burst beads to a certain extent, because the end groups of long-chain lipids are mainly hydroxyl and carboxyl groups, which can form hydrogen bonds with the outer layer of sodium alginate, and improve the strength to a certain extent. Therefore, considering the comprehensive factors such as industrialization cost, simply selecting 20% EVA and wax materials and long-chain lipids for blending, and then adding 0.5% interface binding agent based on the total mass of the blended glue solution, can obviously increase the product strength, improve the sample qualified rate, and reduce the cost waste caused by unqualified rate.

Claims

1. A water-soluble core material for a smoking blast ball material, characterized by: The explosive bead material is a three-layer concentric spherical capsule structure, which is 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, the outer wall material is sodium alginate glue solution and Ca 2+ The cross-linking reaction obtained gel, the inner wall material is a blend containing hydrophobic material, wax material, long-chain fat and interfacial binding agent, the hydrophobic material is ethylene-vinyl acetate copolymer, the interfacial binding agent is selected from at least one of nano-silicon dioxide, nano-calcium carbonate, erucic acid amide, and the core material is selected from a mixture of essential oil and / or natural extract and polar solvent or polar solvent; The wax material is selected from at least one of solid paraffin, polyethylene wax, beeswax, and tree wax; The mass ratio of the hydrophobic material to the wax in the inner layer wall material is 15-25:69.5-85; The long-chain lipid is selected from at least one of stearic acid and octadecanol, and the mass ratio of the wax material to the long-chain lipid is 69.5-85:0-10; The mass ratio of the wax material to the interface bonding agent is 69-85:0-1.

2. The water-soluble core material for the tobacco explosion beads according to claim 1, characterized in that: The interface bonding agent is a mixture of nano-silicon dioxide, nano-calcium carbonate, and erucic acid amide, and the mass ratio of the nano-silicon dioxide, the nano-calcium carbonate, and the erucic acid amide is 1-3:1-3:2-4.

3. The water-soluble core material for the tobacco explosion beads according to claim 1, characterized in that: The polar solvent is selected from at least one of water, ethanol, propylene glycol, and glycerol.

4. The method of claim 1-3, wherein the method is characterized by: It comprises the following steps: obtaining sodium alginate glue solution by heating sodium alginate water solution, mixing, melting wax material, long-chain lipid, hydrophobic material and interface binding agent to obtain mixed glue solution, which is the inner wall material glue solution, mixing and heating essence and / or natural extract and polar solvent to obtain core material; then dropping sodium alginate glue solution, inner wall material glue solution and core material into Ca 2+ containing cooling liquid through the outer layer, middle layer and inner layer of three-layer nozzle respectively to obtain solidified water explosion beads by first solidification, then adding the solidified water explosion beads into external cooling liquid to obtain the explosion bead material by second solidification and drying.

5. The preparation method of the water-soluble core material for the tobacco explosion beads according to claim 4, characterized in that: The mass ratio of the sodium alginate to the water in the sodium alginate aqueous solution is 1.5-2.5:97.5-98.5; The temperature of the sodium alginate glue solution is 60-85°C; The viscosity of the sodium alginate glue solution is 20-400 m·Pas.

6. The preparation method of the water-soluble core material for the tobacco explosion beads according to claim 4, characterized in that: The wax material, the long-chain lipid, the hydrophobic material, and the interface bonding agent are mixed according to the design ratio, heated to 120-140°C, and kept for 2-3 hours to obtain a mixed glue solution, and then the temperature is reduced to 80-100°C to obtain the inner layer wall glue solution; The viscosity of the inner layer wall 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 for the tobacco explosion beads according to claim 4, characterized in that: The temperature of the three-layer drop head is 75-90°C. The sodium alginate glue liquid, the inner layer wall material glue liquid, and the core material are dripped into the Ca 2+ containing cooling liquid at a dropping speed of 10-20 r / min: 2-10 r / min: 0.5-5 r / min.

8. The preparation method of the water-soluble core material for the tobacco explosion beads according to claim 4, characterized in that: Ca-containing 2+ The cooling liquid is a mixed solution of propylene glycol, calcium chloride and water. In the Ca-containing 2+ cooling liquid, the mass ratio of propylene glycol to calcium chloride is 1:

1. Calcium chloride: water = 20-50: 0.5-2: 48-79.5, the Ca-containing 2+ The temperature of the coolant is 5-25°C. The first solidification time is 30-60 seconds, The external cooling liquid is an ethanol aqueous solution containing calcium chloride, and the mass ratio of the calcium chloride, the ethanol, and the water in the external cooling liquid is 1-3:15-30:67-84, The temperature of the external cooling liquid is 5-25°C, The second solidification time is 10-20 minutes.

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